TWI249570B - Cerium-based abrasive containing fluorine and method of producing the same - Google Patents
Cerium-based abrasive containing fluorine and method of producing the same Download PDFInfo
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- TWI249570B TWI249570B TW93119008A TW93119008A TWI249570B TW I249570 B TWI249570 B TW I249570B TW 93119008 A TW93119008 A TW 93119008A TW 93119008 A TW93119008 A TW 93119008A TW I249570 B TWI249570 B TW I249570B
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- rare earth
- abrasive material
- abrasive
- fluorine
- raw material
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- 238000000034 method Methods 0.000 title claims abstract description 117
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 62
- 239000011737 fluorine Substances 0.000 title claims abstract description 62
- 229910052684 Cerium Inorganic materials 0.000 title abstract description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title abstract description 8
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 title abstract 2
- 239000002245 particle Substances 0.000 claims abstract description 75
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 21
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 20
- 239000003082 abrasive agent Substances 0.000 claims description 100
- 239000002994 raw material Substances 0.000 claims description 77
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 75
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 59
- -1 rare earth compound Chemical class 0.000 claims description 57
- 238000001354 calcination Methods 0.000 claims description 55
- 238000004519 manufacturing process Methods 0.000 claims description 49
- 238000011282 treatment Methods 0.000 claims description 43
- 238000003682 fluorination reaction Methods 0.000 claims description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 25
- 150000002910 rare earth metals Chemical class 0.000 claims description 22
- 239000011575 calcium Substances 0.000 claims description 20
- 238000010304 firing Methods 0.000 claims description 19
- 229910052746 lanthanum Inorganic materials 0.000 claims description 15
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 15
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 13
- 150000002602 lanthanoids Chemical class 0.000 claims description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims description 9
- 239000011574 phosphorus Substances 0.000 claims description 9
- 229910052788 barium Inorganic materials 0.000 claims description 8
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims 1
- 229940125904 compound 1 Drugs 0.000 claims 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims 1
- 238000012876 topography Methods 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 10
- 229910052776 Thorium Inorganic materials 0.000 abstract description 4
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract description 3
- 230000007423 decrease Effects 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 description 57
- 239000000463 material Substances 0.000 description 51
- 238000005498 polishing Methods 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 25
- 239000000047 product Substances 0.000 description 24
- 238000010298 pulverizing process Methods 0.000 description 24
- 238000011156 evaluation Methods 0.000 description 17
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 16
- 239000011521 glass Substances 0.000 description 16
- 150000001875 compounds Chemical class 0.000 description 15
- 239000002002 slurry Substances 0.000 description 13
- 239000012141 concentrate Substances 0.000 description 12
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 9
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 9
- 229910052707 ruthenium Inorganic materials 0.000 description 9
- 231100000241 scar Toxicity 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 206010036790 Productive cough Diseases 0.000 description 6
- 229910052797 bismuth Inorganic materials 0.000 description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 208000024794 sputum Diseases 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229910052787 antimony Inorganic materials 0.000 description 5
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 5
- 238000002309 gasification Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000002285 radioactive effect Effects 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- 210000003802 sputum Anatomy 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000000691 measurement method Methods 0.000 description 4
- 238000012552 review Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000004438 BET method Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 208000032544 Cicatrix Diseases 0.000 description 3
- 238000010411 cooking Methods 0.000 description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000037387 scars Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 235000021028 berry Nutrition 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000012857 radioactive material Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 102100035290 Fibroblast growth factor 13 Human genes 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 101000878176 Homo sapiens Fibroblast growth factor 13 Proteins 0.000 description 1
- 241000282849 Ruminantia Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 241000270666 Testudines Species 0.000 description 1
- 235000006545 Ziziphus mauritiana Nutrition 0.000 description 1
- 240000000038 Ziziphus mauritiana Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-O azanium;hydrofluoride Chemical compound [NH4+].F LDDQLRUQCUTJBB-UHFFFAOYSA-O 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000009837 dry grinding Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002603 lanthanum Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- YBSLUBPQYDULIZ-UHFFFAOYSA-N oxalic acid;urea Chemical compound NC(N)=O.OC(=O)C(O)=O YBSLUBPQYDULIZ-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 150000003304 ruthenium compounds Chemical class 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
Description
五、發明說明(1) 【發明所屬之技術領域】 法 本發明係關於一種含有氟之鈽系研磨材料及其製造方 【先前技術】 制、生作☆為飾系研磨材料係以氟碳鈽鑛精鑛作為原料而進行 ^ k (>考日本特開2 0 〇 3 一 2 1 3 2 5 0號公報)。其製造方法係 才曰相1 對於氟碳鈽鑛進行濕式粉碎,對於得到之漿體來 ^打乾燥、焙燒及放冷,對於得到之燒成品,進行粉碎及 勿級,。在此種製造方法,在製造不容易產生研磨傷痕等之 研磨精度高之研磨材料之狀態下,將焙燒製程之焙燒溫 度,設定在比較低之溫度,在製造更高之研磨速度之研 材料之,態y,將焙燒溫度設定在比較高之溫度。 但是,氟碳鈽鑛精鑛係含有適量之氟等,具有作為 系研磨材料之原料之良好特性,但是,在另一方面,具有 所明以钍(Th)或鈾(u)和氟碳鈽鑛精鑛之全稀土類氧化物 換算量(TREO)間之比率((Th + u)/TRE〇)而成為大約〇丨^% 含有量之特性。由於這樣,目此,提供減低处或鈾之含有 ”2ί”研磨材料之方法。此外,,亥製造方法係指 在! 日寺’在對於氟碳飾鑛精鑛等之稀土類鑛 Γ Γ寻到減低1 土或轴等之放射性元素、鹼金 含有率之輕稀土類碳酸鹽後,在該輕 稀土 Γΐ:換添加氣’對於這個進行部分氟化,對於所 得到者進灯培燒U尤以上之背景技術而言V. EMBODIMENT OF THE INVENTION (1) Technical Field of the Invention The present invention relates to a fluorinated lanthanum-based abrasive material and a manufacturer thereof. [Prior Art] Manufactured as a decorative material fluorocarbon 钸The ore concentrate is used as a raw material to carry out ^ k (> Japanese Patent Laid-Open No. 2 0 〇 3 - 2 1 3 2 5 0). The manufacturing method is the wet pulverization of the fluorocarbon antimony ore, and the obtained slurry is dried, calcined and allowed to cool, and the obtained calcined product is pulverized and not graded. In such a manufacturing method, the baking temperature of the baking process is set to a relatively low temperature in a state in which the polishing material having high polishing precision such as polishing scratches is not easily generated, and the material of the higher grinding speed is produced. , state y, the calcination temperature is set at a relatively high temperature. However, the bastnasite concentrate contains an appropriate amount of fluorine and the like, and has good characteristics as a raw material of the abrasive material, but on the other hand, it has a known ruthenium (Th) or uranium (u) and fluorocarbon ruthenium. The ratio of the total rare earth oxide equivalent amount (TREO) of the concentrate to (Th + u)/TRE〇 is a characteristic of about 〇丨^%. Because of this, it is intended to provide a method of reducing the amount of uranium containing "2" abrasive material. In addition, the Hai manufacturing method refers to! In the case of a rare earth ore such as a fluorocarbon ore concentrate, it is found that the light rare earth carbonate is reduced by the radioactive element or the alkali gold content of the earth or the shaft. Gas's partial fluorination for this, for the background technology of the winners
2169-64l4-PF(N2);Ahddub.ptd2169-64l4-PF(N2); Ahddub.ptd
第11頁 1249570 五、發明說明(2) 平9 —183966號公報)。 座:此H用後者之製法時,得到減低趾或1由之含有 率^鋪糸研磨材料。但是,在後者之製法,即使是 立 燒溫度在比較咼之溫度而製造$ σ 無法製造例如藉由前者之速度之研磨材料’也 研磨速度之研磨材料 去所付到之鈽系研磨材料之高 聿右ΓΓ月之課題係提供一種減低鈒或轴等之含有 率並且具有相等於習知品之同卞I否百 研磨㈣以及提供其製造方4、。 之南研磨速度之鈽系 【發明内容】 本發明係解決此種課題,係含 料’其特徵在於:全稀土類氧化物換算質)量=研磨= 為TRE0)相對於研磨材料質量之質量比' 圯載 ⑻之合計含有量相對於該全=二:上,, 里之貝里比((Th + U)/TRE0)成為〇· 05wt%以、、开 均粒徑⑷成為15㈣〜2.5㈣。 乂下布來恩法平Page 11 1249570 V. Description of invention (2) Journal No. 9-183966). Block: When H is used in the latter method, it is obtained by reducing the toe or the content of 1 by the abrasive material. However, in the latter method, even if the vertical firing temperature is made at a relatively high temperature, $σ cannot be manufactured, for example, by the abrasive material of the former speed, and the abrasive material of the grinding speed is high. The subject of the 聿 ΓΓ 提供 提供 提供 提供 提供 之 之 之 之 之 之 之 之 之 之 之 之 课题 课题 课题 课题 课题 课题 课题 课题 课题 课题 课题 课题 课题 课题 。 。 。 。 。 。 。 。 。 The present invention is directed to solving such a problem, and is characterized in that the material is characterized by a total rare earth oxide conversion mass = grinding = TRE0) mass ratio with respect to the mass of the abrasive material. The total content of the load (8) is equal to the total = two: upper, and the ratio of the ratio of (B) is (〇 + U / TRE0) to 〇 · 05wt%, and the average particle size (4) is 15 (four) ~ 2.5 (four) . His Majesty Brian Faping
進行檢。才,結果得知:本發明之鈽系 制於原料之種类員’具有相同或更加高於於鈽^ :: 作為f料所製造之習知之鋪系研磨材料之研磨3鑛;; 糸研磨材料係適合於例如液晶 。錢 板之一次研磨戍者讲府 更磲用或先罩用玻璃基 用述。防止研磨速度之降低之理由係不―定研^之 認為深切地關係到研磨材料之粒徑設定之基準成為^恩 瞧 2169-6414-PF(N2);Ahddub.ptd 第12頁 m 1249570 ' ----- 五、發明說明(3) 法平均粒徑(DB )。在鈽系研磨材料之製造,例如設定配合 於「精加工用」等之研磨材料之用途所製造之研磨材料之 粒從。接著,在該粒徑設定’使用由藉著雷射繞射·散亂 板度分布測定法所測定之小粒徑側之累積體積成為5 〇wt% 之粒子之粒徑(Dm )。但是,在減低鉦或鈾之含有率並且製 造高研磨速度之#系研磨材料之狀態下,即使是使用該粒 梭(%〇)於基準而進行粒徑之設定,也大多是製造之研磨材 料成為低研磨速度之狀態。由於這樣,因此,即使是使用 習知之粒徑(Dm)於基準而進行粒徑之設定,也無法控制研 磨材料粒子之粒度分布而確保必要之研磨速度,因此,認 ^即使是進行目前為止之粒度設定,也無法製造具有發 前述要求位準之研磨速度性能之粒度分布 [ 在粒度設定而使用布萊恩法平均粒 之-;ί ΐ:系研磨材料係具有前述要求位準或這個以上 度設定之鈽系研磨材料係控制研磨材料之i 料。也就是說,認為粒度設定之Ϊ準:f ί度之研磨材 徑(db)並且該平均:皁成為布萊恩法平均粒 磨材料係具有發揮前 :内之t發明之鈽系研 狀態。 旱之研磨速度性能之粒子之 速度態3;:::使】之狀態等之特別要求高研磨 ⑷之理想範圍係正、:二f过材料之布萊恩法平均粒徑 JU Π1 别面敘述,成為15 #m〜2. m 2169-6414-PF(N2);Ahddub.ptd 第〗3頁 1249570 五、發明說明(4) 由於在該平均粒徑(D )去、戈 速度之緣故。另—t下限值,無法確保充分之研磨 產生大的傷痕或彎曲,值時’在被研磨面, 無法除去。因此,在考;ί此即使是進行精加工研磨’也 恩法平均粒徑(Db)成為广7:之兩面時’更加理想是布萊 合計含有量相對於細t j"m〜2.3#m。此外,钍和鈾之 于;鈽系研磨材料之TRE〇之曾旦屮 ((Th + U)/TRE0)成為〇 〇5wt〇/以^之1之貝里比 更加理想是0· 0005wt%以下°所下、取好是〇. 005wt%以下、 含有量係最好是儘量^。下。所謂轴或鉉之放射性物質之 上。系研磨材料質量之質量比係90㈣以 加理相β i :G/、°兄,TRE〇之比例係最好是90wt%以上、更 j土素甚至最好是93wt%以上。由於在各個 古,則超1择Λ綠I成為一定之狀態下,TRE〇之質量比越 ΐ磨材料“:之:^物中之最有助於研磨之氧化鈽之 浐故。士冰,、»山斤占有之比例,可以確保高研磨速度之 '2 ^ m,争,於成為一種傷痕發生原因之不純物之含 有率變,,更加確實地防止傷痕發生之緣故。 但是,進行檢討,結果,tre〇所占 之比例(Ce〇2/T_係最好是5〇wt%〜7。。::=二 容W生傷痕,在超過前述上二: 低,則研磨速度越加降低,在:;前::鋪之比例變得越 保充分之研磨速度。纟低於別迷下限值時,無法確 氟(F)之含有率係最好是4 〇wt%〜1〇wt%。由於在氟之 五、發明說明(5) 含有率變得過低時’無法確保充分之研磨速度之緣故, =方面,由於在變得過高時,發生研磨傷痕之緣故。接 著’在考慮這些之兩面時,更加理想是氟之含有率係 5. Owt% 〜9· Owt% 〇 此外,氟碳鈽鑛精鑛等之使用作為鈽系研磨材料之 料之鑛石係也在所謂鈾或鉦之放射性物質以外,還含 : 多之鈣(Ca)、鋇(Ba)、鐵(Fe)和磷(P)等之元素。因此,呤 製造含有許多之由這些元素所構成之不純物之#系研磨’ 料。含有此種不純物之研磨材料係大多容易發生研磨材 痕,成為低研磨速度。此外,在這些不純物(特別是 ”磨面時,降低被研磨構件之電氣或磁性之特 H,因此’作為鋪系研磨材料係最好是舞、鋇 和%之&計含有量相對於TRE〇之質量比 载 ((Ca + Ba + Fe + P)/TRE0)成為2. 〇wt% 以 1. Owt% . τ ^ ^ t ^ 5wt% ^ τ 〇 -- 該原料,也最好是該質晉h G P使疋作為 以下。 疋以下、甚至最好是0.5wt% 接著,作為鈽系研磨材料係最好是此 為l.OmVg〜3.5mVg。由於RFT、“μ | T法比表面積成 磨速度越加降低,在/、ft E+T法比表面積變得越大,則研 研磨速度之緣故。;=述上限值時’無法確保充分之 小,則越加容易產峰復广丄由於BET法比表面積變得越 要求高精度研磨產4::域===* 1249570 五、發明說明(6) ί i°. 2!νΛί Φ a ^ -ΒΕΤ ^ ^ ^ ^ 一直到目前為止,古备、士 α 少 說明,但是,接著,就ti發明之飾糸研麵斗,來進行 行說明。j吏用由氟碳鈽鑛铲:系::材料之製造方法而進 精鑛等之鑛石原料並精鑛、中國複雜鑛 土類碳酸鹽等之稀土類:im之含有率所得到之稀 料之萝造方法係通當且亡〇專來作為原料之鈽系研磨材 ,磨材料之製造方〉去’配合於需要而在培燒製程前,=Check it out. </ RTI> </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> The material is suitable for example for liquid crystals. The one-time grinding of the money board is more expensive or the first cover is made of glass. The reason for preventing the decrease in the polishing rate is not that the basis of the particle size setting of the abrasive material is considered to be 2N-6169-6414-PF(N2); Ahddub.ptd page 12 m 1249570 ' ---- V. Description of the invention (3) The average particle size (DB). In the production of the lanthanum-based abrasive material, for example, the grain of the abrasive material produced by the use of the abrasive material such as "finishing" is set. Then, in the particle size setting, the particle diameter (Dm) of the particles having a cumulative volume on the small particle diameter side measured by the laser diffraction/scattering platelet distribution measurement method was 5 〇wt%. However, in the state in which the content of bismuth or uranium is reduced and a high polishing rate is produced, even if the particle size is set using the granules (% 〇), most of the materials are manufactured. It becomes a state of low grinding speed. Because of this, even if the particle size is set using the conventional particle diameter (Dm) on the basis of the standard, the particle size distribution of the polishing material particles cannot be controlled, and the necessary polishing rate can be ensured. Therefore, even if it is performed so far With the particle size setting, it is also impossible to produce a particle size distribution with the grinding speed performance of the above-mentioned required level [the use of the Bryan method for granules in the particle size setting;; ΐ ΐ: the abrasive material has the aforementioned required level or this degree setting The abrasive material is the material that controls the abrasive material. That is to say, it is considered that the particle size setting is the standard: the abrasive material diameter (db) of the f ί degree and the average: the soap becomes the Brian method average granulation material system has the : 研 research state of the invention before the invention. The speed state of the particles of the dry grinding speed performance is 3;::: the state of the state of the special requirements, etc. The high range of the high grinding (4) is positive: the average particle size of the Brian method of the two f-materials is JU Π1 It becomes 15 #m~2. m 2169-6414-PF(N2); Ahddub.ptd No. 3 page 1249570 V. Description of the invention (4) Because of the average particle diameter (D), the speed of Ge. In addition, the lower limit of t cannot ensure sufficient grinding to cause large scratches or bending. When the value is 'on the surface to be polished, it cannot be removed. Therefore, in the test; ί, even if it is finishing the grinding 'the average particle size (Db) of the method becomes broad 7: the two sides are more ideally the total content of the blister relative to the fine t j "m~2.3#m . In addition, tantalum and uranium are used in the TRE〇 of the tantalum-based abrasive material ((Th + U)/TRE0) to become 〇5wt〇/Beri ratio of ^1 is more preferably 0. 0005wt% or less °, the best is 〇 005wt% or less, the content is best to try ^. under. The so-called radioactive material of the shaft or sputum. The mass ratio of the mass of the abrasive material is 90 (4). The ratio of the additive phase β i : G / , ° brother, TRE 系 is preferably 90% by weight or more, more preferably more than 93% by weight. Because in each ancient case, the quality of TRE〇 is higher than that of the more honed material “: it is the most beneficial to the oxidized enamel of the grinding. , the proportion of the mountain jin, which can ensure the high grinding speed of '2 ^ m, is the content of the impure substance that becomes a cause of the scar, and it is more sure to prevent the occurrence of the scar. However, the review is carried out. The proportion of tre〇 (Ce〇2/T_ is preferably 5〇wt%~7..::=二容W, the wound is more than the above two: low, the grinding speed is lower, In the front of:: The ratio of the paving becomes more and more sufficient to maintain the grinding speed. When the 纟 is lower than the lower limit, the content of the fluorine (F) cannot be determined to be 4 〇wt%~1〇wt%. In the case of fluorine 5, the description of the invention (5), when the content rate is too low, 'there is a sufficient polishing rate cannot be ensured. In the case of =, the polishing scratches occur when the content is too high. Then, On both sides of these, it is more desirable that the content of fluorine is 5. Owt% 〜9· Owt% 〇 In addition, fluorocarbon antimony concentrate In addition to the radioactive materials of uranium or thorium, the ore system used as the material of the lanthanide abrasive material also contains: calcium (Ca), barium (Ba), iron (Fe) and phosphorus (P). Therefore, 呤 manufactures a #-based abrasive material containing many impurities composed of these elements. Most of the abrasive materials containing such impurities are likely to cause abrasive traces and become low polishing speeds. Moreover, in these impurities ( In particular, "When grinding the surface, the electrical or magnetic properties of the member to be polished are lowered. Therefore, it is preferable that the material used as the paving abrasive is the mass ratio of the dance, the 钡 and the % of the material to the TRE ( ( (Ca + Ba + Fe + P) / TRE0) becomes 2. 〇wt% to 1. Owt% . τ ^ ^ t ^ 5wt% ^ τ 〇-- The raw material, also preferably the quality of the gold GP 疋The following is even more preferably 0.5% by weight. Next, it is preferable that the lanthanum-based abrasive material is 1.0 mVg to 3.5 mVg. Since the RFT and the "μ | T method have a specific surface area, the grinding speed is lowered. When the /, ft E+T method has a larger specific surface area, the grinding speed is increased. To ensure that it is sufficiently small, it is easier to produce peaks and complexes. Because the BET specific surface area becomes more and more high-precision grinding is required. 4:: domain ===* 1249570 V. Invention description (6) ί i°. 2!νΛί Φ a ^ -ΒΕΤ ^ ^ ^ ^ Up to now, the ancient and the syllabus are less described, but then, the ti invention is invented for the purpose of the description. j吏 using fluorocarbon shovel : Department:: The manufacturing method of materials and the ore raw materials such as concentrates and concentrates, rare earths such as China's complex mineral carbonates: the content of im is obtained from the thin material. 〇Specially used as the raw material of the 研磨-based abrasive material, the manufacturer of the grinding material> go 'fit with the need before the simmering process, =
燥製"化製程或除去不純物之處 ^專之濕式處理’或者是在培燒製程後,進行 製程、乾燥製程、分級製程等。 鮮午J 像這樣,纟具有少咅燒原赤斗之製程之飾系研磨材料之製 以方法,在使用作為供應於前述焙燒製程之原料係含有經 ,焙燒所得到之含氟稀土類化合物並且該原料之全稀土類 氧=物換算質量所占有之前述含氟稀土類化合物之氧化物 換算質量之比例成為30wt%以上而且钍(Th)和鈾(u)之合計 含有量相對於該全稀土類氧化物換算量之質量比 ((Th + U)/TRE0)成為0.05wt%以下者時,製造相等或更加高 於以氟碳鈽鑛精鑛作為原料所製造之鈽系研磨材料等之^ 知之鈽系研磨材料之研磨速度的鈽系研磨材料。 在使用此種原料時,良好之理由係不一定明確,但 是,認為深切地關係到在原料中而包含經過培燒所得到之 第16頁 1249570 五、發明說明(7) 一 二化合物。原料中之含氣稀土類化合物 造階段,來進行培燒。也就===研f材料製 合物係在狀態下,進行2次以上 中之3齓稀土類化 研磨材料為止。接著,進行产 而一直到成為鈽系 樣在含有氟之;ί犬態而經過複數次之培 =^ 糸研磨材料係在比起僅進行】 凡 < 斤衣w之鈽 之粒子妝能3 I Wα -人^燒者日才,鈽系研磨材料 時,由於ΓΡ使是二由:二:f比較兩種鈽系研磨材料 得到之被研磨面之傷ί發吏:在實際進行研磨所 過複數次之焙燒製程所製造^ ^ 值(研磨速度)係經 故。 70衣枉所衣w之鈽系研磨材料比較良好之緣 作為用以製造實用之讲府 述,使用含氟稀土 = 正如前面敘 i 無法充分地防止傷痕發生 作為含==:::=研磨速度)之緣故。因此, 理想是7〇wt%以上。〇在 ^係最好是5〇wt%以上、更加 土類化合物係可w原料之含氟稀 單氧化碳酸鹽混合稀土類之碳酸鹽、 :荨之稀土類化合物和說化 2化 含氟化合物後而對於得到之混合物(稀心 第17頁Drying "chemical process or removal of impurities. ^Special wet treatment' or after the cooking process, process, drying process, classification process, etc. In the case of the fine-grained material, the method of producing the decorative material of the ruthenium-based ruthenium-based process is used, and the fluorine-containing rare earth compound obtained by the calcination is contained in the raw material supplied to the calcination process. The proportion of the oxide-converted mass of the fluorine-containing rare earth compound which is contained in the total rare earth oxygen/substance conversion mass of the raw material is 30% by weight or more, and the total content of cerium (Th) and uranium (u) is relative to the total rare earth. When the mass ratio of the oxide-based conversion amount ((Th + U)/TRE0) is 0.05% by weight or less, the production is equal to or higher than that of the lanthanide-based abrasive material produced by using the fluorocarbon sulphide concentrate as a raw material. Known as the lanthanide abrasive material for the grinding speed of the abrasive material. In the case of using such a raw material, the reason for the goodness is not necessarily clear, but it is considered to be deeply related to the inclusion of the raw material in the raw material, which is obtained by the calcination. Page 16 1249570 V. Inventive Note (7) One or two compounds. The gas-containing rare earth compound in the raw material is produced at the stage of cultivation. In other words, the material composition of the product was subjected to two or more rare earth-based abrasive materials in two or more stages. Then, the production is carried out until it becomes a sputum-like sample containing fluorine; ί 犬 。 。 。 。 。 。 = = = = = = = = 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 糸 粒子 粒子 粒子 粒子 粒子 粒子 粒子I Wα -人^烧者日才, 钸 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨The ^^ value (grinding speed) produced by the plurality of firing processes is delayed. 70 枉 枉 枉 w 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 作为 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟 含氟) for the sake of it. Therefore, the ideal is 7 〇 wt% or more. 〇 ^ 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好 最好After that, for the mixture obtained (Sparse page 17
2169-6414-PF(N2);Ahddub.ptd 1249570 五、發明說明(8) 化合物之混合物)來進行焙燒所得到者等。 作為含氟稀土類化合物之焙燒溫度係最好是3〇〇 〇c〜 11〇〇°C、更加理想是40(TC〜l〇〇(rC。在使用藉由在未滿 值之溫度之焙燒所得到之含氟稀土類化合物來作為原 ,時’容易製造低研磨速度之鈽系研磨材料。另一方面, ,^在超過上限值之焙燒溫度之焙燒所得到之含氟稀土類 二,係容易成為大粒徑且堅硬者,在使用此種者來作為 4,簡單地製造容易發生研磨傷痕之鈽系研磨材料。 ^二士 Γ為藉由培燒所得到之含氟稀土類化合物係可以列 1 m /種方法所得到者。作為某一例子係可以列舉在含 =鈽糸研磨材料之製造、在㈣製程後❿進行分級 來付到微粒之研磨姑粗夕灿自t 、 粗粉側者。 下、在該分級製程來回收於2169-6414-PF(N2); Ahddub.ptd 1249570 V. Inventive Note (8) A mixture of compounds) is obtained by calcination. The calcination temperature of the fluorine-containing rare earth compound is preferably 3 〇〇〇 c 11 11 ° C, more preferably 40 (TC 〜 l 〇〇 (rC. used in baking at a temperature below the full temperature) When the obtained fluorine-containing rare earth compound is used as the original, it is easy to produce a lanthanum-based abrasive having a low polishing rate. On the other hand, the fluorine-containing rare earth compound obtained by calcination at a baking temperature exceeding the upper limit is It is easy to be a large-sized and hard-wearing material, and it is easy to manufacture the bismuth-based abrasive which is likely to cause scratches by using the above-mentioned four. ^Two strontium is a fluorine-containing rare earth compound obtained by culturing It can be obtained by the method of 1 m / kind. As an example, it can be exemplified by the manufacture of the material containing the 钸糸 、, the grading of the 在 制 after the (4) process, and the addition of the granules to the granules. Later, in the grading process to recover
在確Ϊ3::之含氟稀土類化合物以外之部分係 碳酸鹽、草酸:稀ΐ類之:炭:鹽、單氧化碳酸鹽、鹽基性 這些稀土類化:物:專之稀土類化合物或者是對於 著了即使是在行1 吾燒(或假燒)所得到者等。接 所得到之強熱假燒列舉之稀土類化合物 加理想是1〇对%以下成去為以下、最好是15衬%以下、更 列舉之稀土類化人私或者疋精由在高溫呈長時間地焙燒 化物係特別最好是八,侍到之強熱減量幾乎成為0wt%之氧 後容易得到粒徑大二氟稀土類化合物以外之部分。由於最 此外,在前錦系研磨材料之緣故。 丰發明之鈽系研磨材料之製造方法,作 2169-6414-PF(N2);Ahddub.ptd 第18頁 1249570 五、發明說明(9) ' --- $ 1減低鉦或鈾等之含有率之原料(中間原料)供應於焙燒 衣私之方法係考慮各種方法。例如如果使用減低钍或鈾等 =放射性疋素之含有率者來作為起始原料的話,則能夠將 2低钍或鈾等之含有率之原料(中間原料),來供應於焙燒 衣程。作為該原料係最好是钍(Th)和鈾(u)之合計含有量 相對於原料之全稀土類氧化物換算量之質量比 ((Th + U)/TqRE〇)成為〇.05wt%以下、更加理想是〇〇〇5wt%以 :、、、甚至最好是〇· 〇〇〇5wt%以下。在使用此種原料時,製 仏減,,(Th)和轴(u )之合計含有量相對於全稀土類氧化 物換,^之質量比((Th + u)/TRE〇)並且具有相等或更加高 於以說,飾鑛精鑛作為原料所製造之鈽系研磨材料等之習 头之鈽系研磨材料之研磨速度的鈽系研磨材料。此外,作 為由匕3钍或鈾等之放射性元素之鑛石等來製造減低這些 έ,率之原,之方法係有記載於專利文獻2之化學處理方 ί等之ί種習知方法。在列舉1個具體例時,可以列舉所 二,如藉由利用硫酸分解法或鹼分解法而分解氟碳鈽鑛精 、’-等之精鑛進行分別沉澱或分別溶解等之處理,減低及 ^去鈾、钍、鈣、鋇、鐵、磷等之不純物,來得到稀土類 ::液、1 f:周ί所得到之稀土類溶液之稀土類成分之組成 合調整組成之稀土類溶液和沉澱劑(例如碳酸氫 ,&反叙兔酸氫納、碳酸鈉、氨水、草酸、草酸銨、 草次納尿素專)而生成稀土類化合物(例如碳酸鹽、鹽基 =反鲅鹽:單氧化碳酸鹽、氫氧化物、草酸鹽等)之沉 '’又對於這個進行過濾及水洗,得到本發明之鈽系研磨材In addition to the 3:: fluorine-containing rare earth compound, the carbonate, oxalic acid: dilute: carbon: salt, monooxycarbonate, salt-based rare earths: substances: special rare earth compounds or It is for those who are even in the line 1 (or fake burn). The rare earth compound listed in the strong heat and the smoldering is preferably 1 〇 to 5% or less, preferably 15 lin % or less, and the rare earth liquefied or sputum is long at high temperature. The time-calcined compound system is particularly preferably eight, and it is easy to obtain a portion other than the particle size large difluoro rare earth compound after the strong heat loss is almost 0% by weight. Because of the most, in the former Jinshi abrasive materials. Manufacture method of abrasive material for the invention, 2169-6414-PF(N2); Ahddub.ptd page 18 1249570 V. Invention description (9) ' --- $ 1 Reduce the content of bismuth or uranium The method in which the raw material (intermediate raw material) is supplied to the roasting garment is considered in various methods. For example, if the content of radioactive halogen or the like is reduced as a starting material, the raw material (intermediate raw material) having a low content of ruthenium or uranium or the like can be supplied to the baking process. The raw material is preferably a mass ratio ((Th + U) / TqRE 〇) of the total amount of lanthanum (Th) and uranium (u) to the total amount of the rare earth oxide of the raw material of 〇.05 wt% or less. More preferably, 〇〇〇5wt% is:,, or even preferably 〇·〇〇〇5wt% or less. When such a raw material is used, the total content of (Th) and the axis (u) is changed with respect to the total rare earth oxide, and the mass ratio ((Th + u) / TRE 〇) is equal. Or a cerium-based abrasive material which is higher than the polishing rate of the cerium-based abrasive material, such as a cerium-based abrasive material manufactured by using a mineral concentrate as a raw material. In addition, a method of reducing the enthalpy of the ruthenium or the like by using a radioactive element such as ruthenium or ruthenium or the like is a conventional method described in the chemical treatment of Patent Document 2. In the case of exemplifying one specific example, for example, by using a sulfuric acid decomposition method or an alkali decomposition method to decompose the concentrate of the fluorocarbon antimony ore, '-, etc., to separate or dissolve separately, etc., ^To remove impurities such as uranium, thorium, calcium, barium, iron, phosphorus, etc., to obtain rare earths:: liquid, 1 f: the rare earth component of the rare earth solution obtained by Zhou, and the composition of the rare earth solution Precipitant (such as hydrogencarbonate, & reverse naphthyl hydrogenate, sodium carbonate, ammonia, oxalic acid, ammonium oxalate, oxalic acid urea) to form rare earth compounds (such as carbonate, base = ruminant salt: single The oxidized carbonate, hydroxide, oxalate, etc.) is filtered and washed with water to obtain the lanthanide abrasive of the present invention.
2169-6414-PF(N2);Ahddub.ptd 第19頁 1249570 五、發明說明(10) ___ 料用原料之方法。此外,也 — 假燒)之氧化物或者县士 4 用由這些所燒成(藉由 為原料。像這樣如^^/化物間之中間體者,來作 7禾错由該方法的含壬 低鈣、鋇、鐵、磷等之不純物之含有冑:則也能夠同時減 此外,正如前面敘述,在根據藉 度分布測定法所剛定之粒徑 2 _射繞射.散亂粒 劣’因此’在就所謂傷痕評價5°或研磨= 斷研磨特性 特性之優劣和顯示研磨材料之粒^ (研磨速度)之研磨 關關係而進行檢討時, 二 4之各種物性間之相2169-6414-PF(N2); Ahddub.ptd Page 19 1249570 V. INSTRUCTIONS (10) ___ Method of raw materials for materials. In addition, the oxide of the sham-burning or the county shovel 4 is burned by these (by the raw material, such as the intermediate of the ^^/interstitial, the 壬 containing the method) The content of impurities such as low calcium, barium, iron, phosphorus, etc. 胄: can also be reduced at the same time, as described above, in the particle size determined by the degree of distribution measurement method 2 _ ray diffraction. 'In the case of the evaluation of the so-called flaw evaluation 5° or the grinding = the characteristics of the broken grinding characteristics and the polishing relationship of the grain of the abrasive material (grinding speed), the phase between the various physical properties of the second and fourth
粒徑(DB )成為既定範圍之二=斤二兒明的’布萊恩法平均 磨值(研磨速度)之方 ’士 tyL 料係在傷痕評價或研 樣,因此,鈽系研磨材料製造::2:f:性。由於這 萊恩法平均粒徑Q)丨# 、"又δ又定之基準成為布 發明之飾系研磨材义=平均粒徑成為前述範圍内之本 性能之粒子^ 4係具有發揮前述要求位準之研磨速t 接著’就進行複數次之焙 檢討。結果得知:作為在 =係而進行 之培燒製程之培燒溫度係最=二= 内並且更加高於原料所包含 〇 c之乾圍The particle size (DB) becomes the two of the established range = the average value of the 'Brian's method of grinding (grinding speed)', and the tyL material is evaluated in the flaw or sample. Therefore, the manufacture of the lanthanum abrasive material: 2: f: sex. Since the average particle size of the Ryan method Q) 丨#, " and δ is determined to be the basis of the invention of the abrasive material of the invention, the average particle diameter becomes the particle of the above-mentioned range. The grinding speed t is then followed by a plurality of baking reviews. As a result, it was found that the temperature of the calcination process in the firing process was the most = two = and was higher than the dry circumference of the raw material.
之焙燒之焙燒溫度101以上之^度。頌化合物生成時 由:在培燒溫度變低時,;;最後得 粒徑不變大同時研磨速度變 =之 不充=地==故粒分地變大’同時’研磨速度 之、♦故另—方面,由於在焙燒溫度變高 2169-6414-PF(N2);Ahddub. ptd 第20頁The calcination temperature of the calcination is above 101 degrees. When the ruthenium compound is formed, when the simmering temperature becomes low, the particle size is not changed at the same time, and the polishing speed is changed to φ = = = = = = = = = = = = = = = = = = = = = = = = = On the other hand, since the calcination temperature becomes higher 2169-6414-PF(N2); Ahddub. ptd第20页
II 1249570 五、發明說明(11) k ’會有最後得到之研磨 /一上 磨傷痕之傾向產生,在超;二徑,大同時容易發生研 徑變得過大,同時,產生° α恤度乾圍之上限值時,粒 在考慮這些方面時,2二:,研磨傷痕之緣故。因此, 11 5 〇 t。 里心疋焙燒溫度成為9 5 0 t〜 此外,本製造方法之 包含之含氣之稀土類化= ί溫度和在原料所 溫度差係越加變小,越加不容。之:燒溫度間之 易成為低研磨:;之粒徑變小,並且,容 想是2 0t以上、甚至最: = 該溫度差係更加理 :外,在使用具有氣化處理 造方法之狀態下,即使是蕤由m +制:于、研纪材枓之製 低鉦或鈾等之含有率,S 下之衣&方法,也可以減 _鑛精鑛作為原料所製造===㈡於以 飾糸研磨,料之研磨速度的飾系研磨材料。十 S知之 造方nm1 系研磨材料之製 M ^ 之在鈽糸研磨材料之原料中冬右 ίν=2 ί理5程並且具有進行於氟化處理製程後之炉燒 =後=燒製程之次數係2次以上’供應於最初之培燒 衣2之焙k對象物(中間原料)係钍(Th)和鈾(U)之合計A 有里相對於全稀土類氧化物換算量之質量比 — ((Th+U)/TRE0)成為〇·〇5wt% 以下。 第21頁II 1249570 V. INSTRUCTIONS (11) k 'There will be a tendency to produce the final grinding/abrasion scar, in the super; the second diameter, the large diameter is also prone to become too large, and at the same time, produce a ° When the upper limit is exceeded, the grain considers these aspects, 2 2: the cause of grinding scratches. Therefore, 11 5 〇 t. The calcination temperature of the inner core is 950 t~ In addition, the rare earth of the gas contained in the production method = temperature and the temperature difference in the raw material become smaller and smaller. It is easy to become low-polishing between firing temperatures: the particle size becomes smaller, and it is expected that it is more than 20 tons, or even the most: = the temperature difference is more reasonable: in addition, in the state of using a gasification treatment method Next, even if the + is made of m + system: the content of 钲 、 研 研 研 研 研 研 研 钲 , , , , , , , , & & & & & & & & & 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿 矿The finishing material is ground with a grinding speed and a grinding speed of the material. 10 S knows that the manufacturing method of the nm1-based abrasive material M ^ is in the raw material of the 钸糸 abrasive material, and the temperature is ίν=2 5 5 steps and has the number of times after the fluorination treatment process = after the firing process 2 times or more 'The total amount of 焙 (Th) and uranium (U) of the baked object (intermediate raw material) supplied to the first sinter 2 is the mass ratio of the total amount of lanthanum to the total rare earth oxide - ((Th+U)/TRE0) becomes 〇·〇5wt% or less. Page 21
2169-6414-PF(N2);Ahddub.ptd 1249570 五、發明說明(12) ___ 在檢討中,得知:僅在進行2次以上之 無法得到要求之鈽系研磨材料;以芬 夂如凡衣#王’也 是將含有氣之錦系研磨材料之原二(及包含各二 :堯之製程;因此,以致於想到本二二 係具有進行於焙燒製程前之氟化處理製程,二衣匕方法 處理係進行於第1次之焙燒製程前。:之亂化 _:以後口剛㈣話, 方之培燒製程間,進行追加之氟化處理。接著,二ς二二2169-6414-PF(N2); Ahddub.ptd 1249570 V. Description of invention (12) ___ In the review, it was learned that only the abrasive materials that could not be obtained more than 2 times were required; #王' is also the original two of the abrasive materials containing the gas, and the process of containing each two: ;; therefore, it is thought that the second bismuth has a fluorination treatment process before the roasting process, and the second enamel method is treated. It is carried out before the first roasting process.: The chaos is _: After the mouth is just (four), the additional fluorination treatment is carried out between the recipes of the simmering process. Next, two twenty-two
= ; = =具;:ί;: = =使: 料所製造之鈽系研磨材料等之習知之鈽系::::: ”磨速度的鈽系研磨材料。認為由於在焙燒對象:: 二:以藉由培燒而適度地生成大粒徑之焙燒品,容: 製仏更咼之研磨速度之研磨材料之緣故。 易, 〜:乍為原料係進行確認’但是,使用稀土類之碳酸趟’ = 、鹽基性碳酸鹽、草酸鹽、氫氧化物等:稀 =化合物或者是對於這些稀土類化稀 到者等。接*,即使是在這些當中仃也〜。= ; = = with;: ί;: = = make: 习 研磨 研磨 研磨 研磨 : :: :::: 磨 速度 速度 研磨 研磨 研磨 。 。 。 。 。 。 。 。 。 。 。 。 。 : A calcined product having a large particle size is appropriately produced by simmering, and it is used for the purpose of making a polishing material having a higher polishing rate. Easy, ~: 乍 is confirmed as a raw material system 'But, using rare earth carbonate趟' = , salt-based carbonates, oxalates, hydroxides, etc.: dilute compounds or rare earths for these rare earths, etc., even if it is in these.
2 L:精以由下假燒/]舉之稀土類化合物所得到之強熱減量成取為 或者。是萨由在▲好是15wt%以下、更加理想是i〇wt%以下者 得到之=㈡之稀土類化合物所 到粒徑大之錦系研磨= 緣。:"化物。由於最後容易得 氟化處理係可以藉由混合飾系研磨材料之原料(包含2 L: The strong heat loss obtained by the rare earth compound from the under-fired/] is taken as or. In the case of ▲, it is preferably 15% by weight or less, more preferably i〇wt% or less, and the rare earth compound obtained by (2) has a large particle size of the grinding system. :"Chemical. Since it is easy to obtain the fluorination treatment, it can be made by mixing the raw materials of the decorative materials (including
1249570 五、發明說明(13) 中間原料)和含氟化合物而實施。作 氟化氫酸、氟化銨、氟化氫銨等之含"、、 口物係使用^ 化物、稀土類氧化氟化物等含 "或稀土類氟 X ^ X Λ 3亂稀土類化合物。伯阜,1249570 5. Inventive Note (13) Intermediate raw material) and fluorine-containing compound. It is a rare earth compound containing " or rare earth fluorine X ^ X Λ 3 containing "hydrofluoric acid, ammonium fluoride, ammonium hydrogen fluoride, etc.", and the use of a compound, a rare earth oxidized fluoride, and the like. Bo,
含亂稀土類化合物係不需要藉由焙燒所得仁丈S 藉由稀土類碳酸鹽等之稀土類化合 彳如可以= 化合物間之混合所得到。這個係由於藉由含=t等之含f :而進行氟化處理之原料來經過2次以…燒製 右率2:李:ί使用本製造方法而製造減低鈒或銷等之含 有率之鈽糸研磨材料之方法係考慮各種方法。例如如果使 用減低钍或鈾等之放射性元素之含有率者來作 4方 法之起始原料的言舌,則能夠製造減低鉉或鈾等ς含=之 :(序ThKLt作為原料係也正如前面所說明㈤,最好是 、’ :、(u)之合計含有量相對於該原料之全稀土類氧 化物換算量之質量比((Th+u)/TRE0)成為0 、、 0 .0β0 0 05^ 二此ί f ί含钍或轴等之放射性元素之鑛石等來製造減低 k二3有率之原料之方法而言,正如前面所說明的,在 此,省略其說明。 ^ π & ί =,進仃檢討,結果,以最初之焙燒製程為首之各 :製程之焙燒溫度係最好是70(rc以上,最後之焙燒 衣程之焙燒溫度係最好是9〇(rc〜12〇〇t,第2次以後之各 :^ io衣私之焙燒溫度係最好是更加高於各個焙燒製程之 正刖方之焙燒製程之焙燒溫度丨〇 〇c以上之溫度。 2169-6414-The rare earth-containing compound does not need to be obtained by calcination, and the rare earth compound such as rare earth carbonate or the like can be obtained by mixing the compounds. This is because the raw material which is subjected to the fluorination treatment by containing f: such as = t is burned twice to produce a right rate 2: Li: ί is manufactured using the present manufacturing method to reduce the content of defects or pins. The method of grinding the material is to consider various methods. For example, if the content of the radioactive element such as ruthenium or uranium is used as the starting material for the four methods, it is possible to produce a reduction of yttrium or uranium, etc. (the order of ThKLt as a raw material system is also as described above). In the case of (5), it is preferable that the mass ratio of the total content of ':, (u) to the total rare earth oxide equivalent amount of the raw material ((Th+u)/TRE0) becomes 0, 0. 0β0 0 05 ^ f ί f ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί =, review, the results, starting with the first roasting process: the firing temperature of the process is preferably 70 (rc or more, the final calcination temperature of the roasting process is preferably 9 〇 (rc ~ 12 〇 〇t, after the second and subsequent: ^ io clothing private baking temperature is preferably higher than the firing temperature of the roasting process of each of the roasting processes 丨〇〇 c above the temperature. 2169-6414-
PF(N2);Ahddub.r 1249570 五、發明說明(14) 、〜由於在各個培燒製程之焙燒溫度未滿70 0 °C,幾乎無 ^侍到所謂藉由焙燒而成長粒子之效果,無法製造具有要 =之研磨速度之研磨材料之緣故。接著,即使是各個焙燒 製程之焙燒溫度成為70 0 t以上,也在最後之焙燒製程之 焙燒溫度變低時,會有最後得到之研磨材料之粒徑不變大 同時研磨速度變低之傾向產±,在未滿9〇〇。。時,粒徑不 f刀地變大,同時,研磨速度不充分地變大。另一方面, 於在最後之焙燒製程之焙燒溫度變高時,會有最後得到 2研磨材料之粒徑變大同時容易發生研磨傷痕之傾向產 讲麻ί超過1 20 0 °C時,粒徑變得過大,同時,產生許多之 戶成A qtn。。因Λ ’在考慮這些方面時,更加理想是焙燒溫 度成為 950C 〜1150。("。1士从 .^ ^ 、,立、陡制 11 DU C。此外,在著眼於第2次以後之某個 口 = ^:正””程之培燒溫度係最好是更加 石加 I 刖方之焙燒製程之焙燒温度,但是, :堯’皿二之溫度差越小,’加不•易進行焙燒之燒 :變ΐ者並ί溫;製造之飾系研磨材料係粒 各個梧燒製程之正前方之二:匕:/丄最好是更加 -^ . . , . θ φ 之尨k衣私之焙燒溫度10 °c以上之 ::更加理想疋更加高於2(rc以上之 更加鬲於50 °C以上之溫度。 仓芏琅好疋 此外’不同於這裡所却日日 / 法,先前所說明之製造方法(成之A鈽勺糸八研磨材料之製造方 原料經過㈣所彳含氟(稀燒製程之 氣稀土類化合物之製造方法)係 1249570 五、發明說明(15) 不一定需要氟化處理製程之製造方法,但是,在使用該製 造方法時,可以製造被研磨面之傷痕發生狀態或研磨值 (研磨速度)良好之#系研磨材料。由於先前說明之製造方 法係使用含有含氟豨土類化合物之原料之方法之緣故。如 果在原料中包含已經含有氟成分之含氟稀土類化合物的 活,則不需要在研磨材料製造階段,重新進行氟化處理。 此外,在一直到目前為止所說明之本發明之各個製造 方法,在製造既定粒徑之研磨材料(例如布萊恩法平均粒 徑(DB)成為1·5 //Π1〜2·5 //m之研磨材料)之狀態下,正如在 後面敘述之實施形態所說明的,在適當之階段,進行粉 (解碎)或分級等。 ,接著,作為使用一直到目前為止所說明之本發明之各 個製造方法而製造減低鈣(Ca)、鋇(Ba)、鐵(Fe)、磷(ρ) 之含有率之鈽系研磨材料之方法係使用減低鈣、鋇、鐵、 =之έ有率者來作為其原料之方法。在使用此種原料之狀 悲下’作為鈽系研磨材料之原料係最好是該原料之鈣、 鋇:鐵和磷之合計含有量相對於全稀土類氧化物換算量之 貝里比(^Ca + Ba + Fe + P)/TRE0)成為2.0wt%以下。在使用此 種原料%二製造減低鈣、鋇、鐵和磷之合計含有量相對於 全稀土類氧化物換算量之質量比以^^ + ^ +以+ ^^/了^⑻至 2· Owt/。以下的鈽系研磨材料。此外,正如先前所說明的, 在製造減低鉦或鈾等之放射性元素之含有率之原料時,同 時也,造減低鈣、鋇、鐵和磷之含有率之原料,因此,在 此省略關於減低甸、鋇、鐵和碟之含有率之原料之製造PF(N2); Ahddub.r 1249570 V. Inventive Note (14) ~ Since the calcination temperature of each firing process is less than 70 ° C, there is almost no effect of growing particles by roasting. The reason is that an abrasive material having a grinding speed of = is produced. Then, even if the calcination temperature of each of the calcination processes is 70 kt or more, and the calcination temperature of the final calcination process becomes low, there is a tendency that the particle diameter of the finally obtained abrasive material does not become large and the polishing rate becomes low. ±, less than 9〇〇. . At the same time, the particle size is not increased, and the polishing rate is not sufficiently increased. On the other hand, when the calcination temperature of the final calcination process becomes high, there is a tendency that the particle size of the second abrasive material becomes large and the scratch is likely to occur, and the particle size is more than 1 20 0 °C. It has become too big, and at the same time, many households have become A qtn. . In view of these aspects, it is more desirable that the baking temperature be 950C to 1150. ("1士从.^^,,立,深制11 DU C. In addition, in the mouth after the second time = ^: 正"" Cheng Zhi Pei burning temperature system is best more stone plus I 刖The calcination temperature of the roasting process of the square, however, the smaller the temperature difference of the crucible is, the addition is not easy to roast the roast: the crucible is changed and the temperature is tempered; the decorative abrasive material is made into various calcining processes. In front of the second: 匕: / 丄 is better - ^ . . , . θ φ 尨 k clothing private roasting temperature of 10 °c or more:: more ideal 疋 more than 2 (rc above the 鬲Temperature above 50 °C. Cangjie is better than the 'different from here, the daily method / method, the manufacturing method described previously (made into the A, the scoop of eight grinding materials, the raw materials of the manufacturing side (4) Fluorine (manufacturing method of rare earth compound in a rare-burning process) is 1249570. 5. Description of the invention (15) A manufacturing method of a fluorination treatment process is not necessarily required, but when the manufacturing method is used, a flaw on a polished surface can be produced. #系研磨材料 that has a good state or a grinding value (grinding speed). Due to the previous description The manufacturing method is a method of using a raw material containing a fluorine-containing alumina compound. If the raw material contains a fluorine-containing rare earth compound which already contains a fluorine component, it is not necessary to perform the fluorination treatment at the manufacturing stage of the abrasive material. Further, in the respective manufacturing methods of the present invention which have been described so far, an abrasive material having a predetermined particle diameter is produced (for example, the Bryan method average particle diameter (DB) becomes 1. 5 //Π1 to 2·5 // In the state of the abrasive material of m, as described in the embodiment described later, powder (crushing), classification, etc. are carried out at an appropriate stage. Next, as the use of the present invention as described so far The method for producing a lanthanum-based abrasive material having a reduced content of calcium (Ca), barium (Ba), iron (Fe), and phosphorus (ρ) by each production method is to reduce the rate of calcium, barium, iron, and As a raw material method, in the case of using such a raw material, it is preferable that the raw material of the lanthanum-based abrasive material is calcium or lanthanum of the raw material: the total content of iron and phosphorus is converted relative to the total rare earth oxide. The ratio of berry ratio (^Ca + Ba + Fe + P) / TRE0) is 2.0 wt% or less. The total content of calcium, barium, iron and phosphorus is reduced relative to the total rare earth oxide by using the raw material %2. The mass ratio of the converted amount is ^^ + ^ + with + ^^ / ^ (8) to 2 · Owt /. The following lanthanide abrasive materials. In addition, as explained earlier, in the manufacture of radioactive elements such as reduced uranium or uranium In the case of the raw material of the content rate, the raw material of the content of calcium, barium, iron and phosphorus is also reduced, and therefore, the manufacture of the raw material for reducing the content of the deuterium, tantalum, iron and the dish is omitted here.
第25頁 2169-6414-PF(N2);Ahddub.ptd 1249570 五、發明說明(16) 方法之說明。 此外,即使 製造方法,也使 有量相對於全稀 是5.0 〜12wt%、 得f/treo成為此 1 Owt%、甚至5. 0 正如以上, 低钍或鈾等之含 研磨速度之所謂 是在以上 得在最後 土類氧化 特別最好 種範圍而 〜9. Owt% 如果藉由 有率並且 研磨特性 說明之任何一種鈽系研磨材料之 之焙燒製程所供應之原料之氟含 物(TRE0)之質量比(F/TRE0)最好 疋6 · 0〜1 1 w t %。由於可以藉由使 容易製造氟含有率成為4.0〜 之鈽系研磨材料之緣故。 本發明的話,則能夠提供一種減 具有同等於習知品之同等以上之 良好之鈽系研磨材料。 【實施方式】 【發明之最佳實施形態】 以下,就本發明之含氟鈽系研磨枒柯 ^ 啊枓之適當之實絲形 態而進行說明。 <ι田心貝她形 第1貫施形態 ^實施形態’準備具有^所示之物性 研磨材料用之原料。 τ 表1Page 25 2169-6414-PF(N2); Ahddub.ptd 1249570 V. Description of the invention (16) Description of the method. In addition, even if the manufacturing method is such that the amount is 5.0 to 12 wt% with respect to the total dilution, the f/treo becomes this 1 Owt%, or even 5.0. As above, the so-called polishing rate of low bismuth or uranium or the like is The above is the most preferred range of the oxidation of the soil at the end of the -9. Owt% of the fluorine content (TRE0) of the raw material supplied by the roasting process of any of the lanthanum abrasive materials indicated by the yield and the abrasive characteristics. The mass ratio (F/TRE0) is preferably 疋6 · 0~1 1 wt %. This makes it possible to easily produce a bismuth-based abrasive material having a fluorine content of 4.0 Å. According to the present invention, it is possible to provide a lanthanide-based abrasive which is excellent in equivalent or equivalent to the conventional one. [Embodiment] BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a suitable solid wire form of the fluorine-containing fluorene-based polishing material of the present invention will be described. < 田田心贝儿形 The first embodiment is applied. ^ Embodiments The material for the abrasive material shown in Fig. is prepared. τ Table 1
ΓρΠ Th 丄 I I lrv_~^ _sm 含有率 (wt%) F 強熱 減量 (wt%) TREO (wt%) <0.1 9.7 8 —ΓρΠ Th 丄 I I lrv_~^ _sm Content rate (wt%) F Strong heat loss (wt%) TREO (wt%) <0.1 9.7 8 —
— 2i69-6414-PF(N2);Ahddub.ptd 第26頁 ---- 1249570 五、發明說明(17) 在2種原料中,原料A係藉由在65(TC,對於稀土類石炭 酸鹽進行1 2小時之假燒而得到。此外,為了得到原料a而 準備之稀土類碳酸鹽係全稀土類氧化物換算質量(TRE〇)成 為4 5wt%、Ce02/TRE0 成為61wt%、(Th + U)/TRE0 成為未滿 0· 0005wt%、(Ca + Ba + Fe + P)/TRE0 未滿〇· 4wt%、就(卩)未滿 0 · 1 w t % 〇 實施例1 :本實施例係使用原料A。概略地說,對於原 料A進行濕式粉碎、氣化處理(第1次)、洗淨·過濾、乾 燥、解碎、焙燒(第1次)、乾式粉碎、氟化處理(第2次)、 洗淨·過濾、乾燥、解碎、焙燒(第2次)、乾式粉碎及分 級而製造飾系研磨材料之方法。以下,詳細地進行說明。 首先,在原料A,混合該原料2倍質量之純水,藉由乾式粉 碎機而對於得到之混合物,來進行濕式粉碎。使用在該粉 碎之粉碎媒體係直徑5mm之氧化錘球,粉碎時間係8小時。 接著,在藉由粉碎所得到之原料漿體,攪拌這個,同時, 添加10wt%之氟化氫酸,然後,繼續進行i小時之攪拌(第工 次之氟化處理)。l〇wt%氟化氫酸之添加量係藉由1〇衬%氟 化氫酸之添加所添加之氟質量和原料衆體之全稀土類氧化 物換算質量(TRE0)間之質量比(F/TRE〇)成為4. 5以%之量。 然後,進行所謂沉澱1體中之固態成分而拉出上澄清液來 加C 2水之再漿料化洗淨,•由過濾沖壓法而過濾洗淨後 j體。接著’在15(rc ’對於得到之過濾勒,進行 ’ #由輥式破碎機而解碎得到m查。得 解碎品之平均粒徑(I)係1.12 _。接著,對於得到— 2i69-6414-PF(N2); Ahddub.ptd Page 26---- 1249570 V. INSTRUCTIONS (17) Among the two raw materials, the raw material A is at 65 (TC, for rare earth carbonates) The obtained rare earth carbonate-based total rare earth oxide-converted mass (TRE〇) prepared to obtain the raw material a is 45 wt%, and Ce02/TRE0 is 61 wt%, (Th + U)/TRE0 becomes less than 0. 0005wt%, (Ca + Ba + Fe + P) / TRE0 is less than 〇 · 4wt%, and (卩) is less than 0 · 1 wt % 〇 Example 1: This embodiment is Raw material A is used. Briefly, raw material A is subjected to wet pulverization, gasification treatment (first time), washing, filtration, drying, pulverization, calcination (first time), dry pulverization, and fluorination treatment ( 2 times), washing, filtration, drying, pulverization, calcination (second time), dry pulverization, and classification to produce a decorative abrasive material. Hereinafter, the method will be described in detail. First, the raw material A is mixed. 2 times the mass of pure water, and the obtained mixture is subjected to wet pulverization by a dry pulverizer. The oxidized hammer ball having a system diameter of 5 mm was pulverized for 8 hours. Next, the raw material slurry obtained by pulverization was stirred, and 10 wt% of hydrogen fluoride was added thereto, and then stirring was continued for 1 hour. The second fluorination treatment). l〇wt% hydrogen fluoride acid is added by the addition of 1 lining% hydrogen fluoride acid and the quality of the total rare earth oxide conversion mass (TRE0) The ratio (F/TRE〇) is 4.5% by weight. Then, the solid component in the body of the precipitate is precipitated, and the supernatant liquid is pulled out to re-slurry the C 2 water. After filtering, the j body is filtered, and then 'at 15 (rc 'for the obtained filter, it is carried out' # is broken by a roller crusher to obtain m check. The average particle size (I) of the obtained scrap product is 1.12. _. Next, for getting
1249570 五、發明說明(18) ' ^解碎品,進行焙燒(第丄次之培燒製程)。培燒條件係所 :焙燒溫度95(TC、焙燒時間12小時,在焙燒後,藉由樣 本軋機而對於得到之焙燒品,來進行乾式粉碎。 接著,在該粉碎品,混合該粉碎品2倍質量之純水, 對$得到之粉碎品,調整漿體,在該漿體中,攪拌這個, 同時,添加10wt%之氟化氫酸,然後,進行所謂時攪拌 之氟化處理(第2次之氟化處理)。1〇wt%氟化氫酸之添加量 係含有成為氟化處理對象之焙燒品之氟質量(F1)和藉由 i〇w口t%氟化氫酸之添加所添加之氟質量(F2)之合計以9及焙 燒品之全稀土類氧化物換算質量(TRE0)間之質量比 σ ((F1+F2)/TRE0)成為 6· Owt% 之量。此外,(F1+F2)/TRE〇 係 也表現成為F/TRE0,來作為F1+F2 = F。然後,進行再漿料、 化洗淨,藉由過濾沖壓法而過濾洗淨後之漿體,在丨5〇 °C,對於得到之過濾濾渣,進行24小時之乾燥,藉由輥式 破碎機而解碎得到之乾燥濾渣,對於得到之解碎品,進行 焙燒(第2次之焙燒製程)。焙燒條件係所謂焙燒溫度1〇5〇 C、焙燒時間1 2小時。在焙燒後,藉由樣本軋機而對於得 到之焙燒品,來進行乾式粉碎,藉由渦輪分級機(設定分 級點在9# m)而對於得到之粉碎品,進行分級而得到鈽系 研磨材料。此外,得到之研磨材料之(Th + u)/TRE〇成為未 滿 0.0 0 0 5Wt%,(Ca + Ba + Fe + P)/TREO 成為未滿〇.4wt% / ^ 比較例1 :該比較例係比起實施例1時,除了一直到進 灯於第1次之焙燒製程後之乾式粉碎製程為止而使得氟化 處理之10wt%氟化氫酸之添加量及焙燒溫度變得不同以1249570 V. Description of invention (18) ' ^ Disintegration, roasting (the second cooking process). The firing conditions were: calcination temperature 95 (TC, calcination time 12 hours, after calcination, the obtained calcined product was dry-pulverized by a sample rolling mill. Next, the pulverized product was mixed twice as much as the pulverized product. Pure water of mass, adjust the slurry for the obtained pulverized product, stir this in the slurry, and simultaneously add 10% by weight of hydrogen fluoride, and then perform fluorination treatment of so-called stirring (the second fluorine) The amount of 1% by weight of hydrogen fluoride added is the fluorine mass (F1) of the calcined product to be subjected to the fluorination treatment and the fluorine mass (F2) added by the addition of the i%w port t% hydrofluoric acid. The mass ratio σ ((F1+F2)/TRE0) between the total mass of rare earth oxides (TRE0) of 9 and the calcined product is 0.001 wt%. Further, (F1+F2)/TRE〇 It is also expressed as F/TRE0 as F1+F2 = F. Then, it is re-slurryed and washed, and the washed slurry is filtered by a filtration press method at 丨5 ° ° C for The filter residue is filtered, dried for 24 hours, and the dried filter residue is obtained by a roller crusher. The obtained pulverized product is calcined (the second baking process). The calcination conditions are a so-called calcination temperature of 1 〇 5 〇 C and a calcination time of 12 hours. After calcination, the obtained calcined product is obtained by a sample rolling mill. The dry pulverization was carried out, and the obtained pulverized product was classified by a turbo classifier (setting a classification point at 9 # m) to obtain a lanthanum-based abrasive. Further, the obtained abrasive material (Th + u) / TRE 〇 It becomes less than 0.00 0 5Wt%, (Ca + Ba + Fe + P) / TREO becomes less than 〇. 4wt% / ^ Comparative Example 1: This comparative example is compared with Example 1, except that it is always in the light The dry pulverization process after the first baking process makes the addition amount of the 10% by weight of the fluorination treatment and the baking temperature different.
2i69-6414-PF(N2);Ahddub.ptd 第28頁 1249570 五、發明說明(19) " 外,其餘係相同於實施例1。 接著’在本比較例,在焙燒後之乾式粉碎後,不進行 在實施例1之氟化處理(第2次),藉由渴輪分級機(設定分 =點在9 vm)而對於利用乾式粉碎所得到之粉碎品(平均粒 徑(D^1· 17 "m),進行分級而得到鈽系研磨材料。此 外,在^氟處理,添加丨0wt%氟化氫酸之添加量而使得藉由 酸,添加所添加之氟質量和原料漿體之全稀 ;哲ί 換异質量(TRE0)間之質量比(F/TRE0)成為既定 所示該既定之質量比(f/tre〇)及培燒溫度條件係正 起杳二二例!6及比較例2〜5:這些實施例及比較例係比 起貝她例1日寸,除了使得氟化處理之 外’在第1 _人之氟處理,添加J 〇wt% 曰 得藉由1 Owt%氟化氳酸之天加所鼠化虱馱之添加罝而使 之全稀土類氧化物換加門之”量和原料装體 為既定之質量比。此外第τ :〇)之間龜之上量比("τ_)成 化氯酸而使得含有成為氟化f理·;之象^^,口添之加 合計量以及成為氣化處加之氣質量⑽)之 ^ ^ f *(TRE0) # % 既定之質量比。該既定之f量 〇)成為 係正如表2所示。 負里比(F/TM〇)及焙燒溫度條件 實施例7 ··該實施例得卜扣 例係比起貫施例10寺’除了一直到進 _ 2169-6414-PF(N2);Ahddub.ptd 第29頁 1249570 五、發明說明(20) 行於第1次之焙燒製程後之乾式粉碎製程為止而使得氟化 處理之1 0 w t %氟化氫酸之添加量變得不同以, 同於實施例1。 八餘係、相 接著,在本比較例,在焙燒後之乾式粉碎後, 在實施例1之氟化處理(第2次),就藉由乾式粉碎所 粉碎品而言,還進行第2次之焙燒。接著,對於藉由該 次焙燒製程所得到之焙燒品,進行乾式粉碎,進行分級 得到鈽系研磨材料。第2次焙燒製程以後之各個 丰 同於實施例匕。此外’在第i次之氟處理,添力“二:: 氟化氫酸之添加所添加之 =dm ί王ί 土類氧化物換算質量(tre〇)間之 貝里( 0)成為既定之質量比。該既定之曾旦士 (F/TRE0)及各個焙燒製程之焙燒溫度係正如表〗、里一 比較例6 :本比較例係製造習知之鈽系研 = 子,係企圖使用原料B(氟碳鈽鑛精鑛 := 這個來製造研磨速度吨大1系研 燒 先,以相同於實施例丨之相同條件,來對於原例子。百 粉碎。接著,在藉由粉碎所得到之、進仃c式 同時,添加相當於漿體之液體f量之5w=之旦攪拌這個, 酸,然後,持續地進行1小時之攪 °里之35%鹽2i69-6414-PF(N2); Ahddub.ptd page 28 1249570 V. Inventive Note (19) " The rest is the same as Embodiment 1. Then, in this comparative example, after the dry pulverization after the calcination, the fluorination treatment in the first embodiment (the second time) was not carried out, and the dry type was used by the thirteen round classifier (set point = point at 9 vm). The obtained pulverized product (average particle diameter (D^1·17 "m) is pulverized and classified to obtain a lanthanum-based abrasive. Further, in the fluorination treatment, the addition amount of 丨0 wt% of hydrogen fluoride is added to cause Acid, adding the added fluorine mass and the whole slurry of the raw material slurry; the mass ratio (F/TRE0) between the Zheli variation quality (TRE0) becomes the established mass ratio (f/tre〇) and culture The burning temperature conditions are starting from 22 cases! 6 and Comparative Examples 2 to 5: These examples and comparative examples are 1 day in comparison with the case of Ba, and except for the fluorination treatment, the fluorine in the first _ person Treatment, adding J 〇wt% 曰 藉 藉 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 The mass ratio. In addition, the amount of the turtle above the τ:〇) is converted to chloric acid, so that it contains fluorinated The sum of the masses and the mass of the gas added to the gasification (10)) ^ ^ f *(TRE0) # % The established mass ratio. The established f quantity 〇) is as shown in Table 2. Negative ratio (F/TM〇) And the calcination temperature condition of the embodiment 7 ···································································· Description (20) The amount of 10% by weight of hydrogen fluoride added in the fluorination treatment is changed until the dry pulverization process after the first firing process is the same as in the first embodiment. In the comparative example, after the dry pulverization after the calcination, in the fluorination treatment (the second time) of the first embodiment, the pulverized product by the dry pulverization was further subjected to the second calcination. The calcined product obtained by the calcination process is subjected to dry pulverization and classified to obtain a lanthanide-based abrasive. The second calcination process is the same as in the example 匕. In addition, the fluorine treatment at the i-th time is added. "II:: Addition of hydrogen fluoride acid added =dm ί Wangί Berry between the amount (tre〇) (0) become established the mass ratio. The calcination temperature of the established Zengdanshi (F/TRE0) and each roasting process is as shown in Table 〖, Comparative Example 6: This comparative example is a conventional method of manufacturing the raw material B (fluorocarbon). Antimony ore concentrate: = This is to produce a grinding speed of 1 ton, and the same conditions as in the example, for the original example. One hundred crushing. Then, by pulverizing, it is obtained. At the same time, adding 5w= of the amount of liquid f corresponding to the slurry, stirring this, acid, and then, continuously performing 3 hours of salt in 1 hour of stirring
^里係進行用以減低若干之妈等之不純物之該鹽酸T 後’進行所謂沉殿漿體中之固態成分 J 漿體。接著,一^之 第30頁 2169-6414-PF(N2);Ahddub.ptd 1249570In the case of the hydrochloric acid T which is used to reduce the impurities of some mothers and the like, the solid component J slurry in the so-called sinking slurry is carried out. Next, one ^ page 30 2169-6414-PF (N2); Ahddub.ptd 1249570
五、發明說明(21) _ 時之乾燥,藉由輥式破碎機而解 之解碎品之平均粒彳f ( D ) #〗 侍到之乾燥濾渣。得到 解碎品,進行焙燒,藉5G由樣太=m。接著,對於得到之 之焙燒品,來進行乾式粉碎 =對於利m堯所得到 點在9 #m)而對於得到之粉错,由渴輪分級機(設定分級 磨材料。焙燒製程之、炉_、、w 進仃分級來得到鈽系研 飾系研磨材料之評價“皿度之條件係正如表2所示。 就藉由各個實施例及比較 言,測定I含有率、布萊因法侍到之鈽糸研磨材料而 射·散亂法粒度分布均粒徑(Db)、根據雷射繞 面積。接著,。平均粒徑(〜)及BET法比表 研磨材料,進行研“ί:施例及比較例所得到之飾系 之研磨面之傷痕評價?:測二 2。此外,測定方法、研磨古及广貝結果,顯不在表 價方法係正如以下。 驗方法、各種研磨特性之評 氡化將使用藉由驗試藥(碳酸鈉、碳酸鉀、氫 得到之鈽系研磨材料;實施例及㈣例所 定試料之驗溶融.溫:J:驗,:及溫水萃取者來作為測 右楚因it 尺卒取·鼠離子電極法予以採用。 之物理試^方法K 52Q1_1 997(水泥 山度P (g/m3)。接著,藉由數學式(1)而舅V. INSTRUCTIONS INSTRUCTIONS (21) _ Drying, the average particle size of the mashed product by the roller crusher f ( D ) # 〗 The dried filter residue. The decomposed product is obtained and calcined, and the sample is too = m by 5G. Next, for the obtained calcined product, dry pulverization is performed = the point obtained for the profit is 9 #m), and the obtained powder is wrong, and the quenching wheel classifier is set (the grading mill material is set. The roasting process, the furnace _ ,, w, and grading to obtain the evaluation of the abrasive materials of the enamel system. The conditions of the dish are as shown in Table 2. By using the various examples and comparisons, the I content is determined, and Blyin is served. Then, the abrasive material is sprayed and scattered, and the particle size distribution average particle diameter (Db) is based on the area around the laser. Next, the average particle diameter (~) and the BET method are used to grind the material. And the evaluation of the flaw on the polished surface of the decorative system obtained in the comparative example?: Measurement 2: In addition, the measurement method, the polishing history and the Guangbei result are not as follows. The evaluation method and evaluation of various polishing characteristics The test will use the test materials (sodium carbonate, potassium carbonate, hydrogen to obtain the lanthanide abrasive material; the examples and (4) examples of the sample test melt. Temperature: J: test, and warm water extractor as the right Chu was adopted by the ruler and the rat ion electrode method. Physical test methods ^ K 52Q1_1 997 (cement Santos P (g / m3). Next, by equation (1) and uncle
2169-6414-PF(N2);Ahddub.ptd 第31頁 1249570 五、發明說明(23) ---- 19.6kPa( 200g/m3),將研磨試驗機之旋轉速度,設定在 2 00rpm 〇 研磨值(研磨速度)之評價:在研磨開始之3〇分鐘後, 交換研磨對象之平面面板用破璃,裝設研磨值敎用之平 面面二巧璃。此外二藉由交換所裝設之平面面板用玻璃 係僅疋夤$測《。接著’在交換平面面板用玻璃後,進行 1 0分鐘之研磨,求出由於研磨所造成之玻璃質量之減少, 根據該值而求出「研磨值」。此外,比較例1之研磨材料 之研磨值係成為基準(1 0 〇 )。 研磨傷痕之評價·就研磨之平面面板用玻璃而言,藉 由純水而進行洗淨,就在無塵狀態而進行乾燥之研磨面, 來進行傷痕評價。傷痕評價係藉由使用30萬勒克司之齒素 燈來作為光源之反射法而觀察玻璃表面,對於大傷痕及微 細傷痕之數目來進行點數化,以1 0 0點成為滿點,藉由減 點評價之方式而進行傷痕評價。在該評價,以在硬碟用或 LCD用之玻璃基板之研磨所要求之研磨精度,來作為判斷 基準。具體地說,在表2及表4中,「〇」係表示92點以上 (適合於HD用、LCD用玻璃基板之研磨),「△」係表示未 滿92點、85點以上(可以使用於〇用、LCD用破璃基板之研 磨)’接著’ 「x」係表示未滿8 5點(不可使用於η d用、 LCD用玻璃基板之研磨)。2169-6414-PF(N2); Ahddub.ptd Page 31 1249570 V. Description of invention (23) ---- 19.6kPa (200g/m3), set the rotation speed of the grinding tester to 200 rpm 〇 grinding value Evaluation of (grinding speed): After 3 minutes from the start of the polishing, the flat panel for polishing the object was exchanged for the glass, and the flat surface of the polishing value was used. In addition, the glass system for the flat panel installed by the exchange is only measured. Then, after the glass for the flat panel was exchanged, it was polished for 10 minutes to determine the decrease in the quality of the glass due to the polishing, and the "grinding value" was obtained from the value. Further, the polishing value of the abrasive of Comparative Example 1 was used as a reference (10 〇 ). Evaluation of the polishing scratches. The glass for the flat panel to be polished is cleaned by pure water, and the dried polished surface is cleaned in a dust-free state to perform flaw evaluation. The scar evaluation was performed by using a 300,000 lux tooth source lamp as a light source reflection method to observe the glass surface, and the number of large scratches and fine flaws was counted to become a full point at 100 points. The evaluation of the flaw was made by reducing the price. In this evaluation, the polishing accuracy required for the polishing of the glass substrate for hard disk or LCD is used as a criterion for determination. Specifically, in Tables 2 and 4, "〇" indicates 92 points or more (suitable for polishing of HD and LCD glass substrates), and "△" means less than 92 points and 85 points or more (can be used) For polishing, the polishing of the glass substrate for LCD) "Next" "x" indicates that it is less than 8 5 points (cannot be used for polishing of ηd or glass substrate for LCD).
1249570 —一五、發明說明(24) 表2 力)製造條件 铈系研磨材料 寅施例/比較例 衆2) 起 始 原 料 氟化 處理 溧1次) TREO (Wt%) 愤燒 製程 澤1次) 焙燒 溫度 (C) 匍化 處理 (H2 次) TREO (wt%) 培燒 製程 CH2 次) 焙燒 溫度CC) TREO (Wt%)1249570 -15, invention description (24) Table 2 Force) Manufacturing conditions: 研磨-based abrasive materials 寅Examples/Comparative examples 2) Starting materials fluorination treatment 溧 1 time) TREO (Wt%) Inflation process Chengze 1 time Calcination temperature (C) Deuteration treatment (H2 times) TREO (wt%) Burning process CH2 times) Calcination temperature CC) TREO (Wt%)
Th + UTh + U
Ba Fe + PBa Fe + P
Ca TREO (wt%) TREO (Wt%) S(F) 之含 有率 (wt%) ^3) 平均 粒徑 Db 嵌4〕 平均 粒徑 Dso (μηη) (μηι) BET法 比表 面積 (m2/g) 研磨特性 來5) 研 磨 値 傷 痕 評 價 比1 WT m 5T W3ΪΕΤ 寅4 S2 寰5 菁6 寰7 比6 3.0 Ts" 8.0 1050J5〇7 "950~~ 150~jlF 75「 一 850— 4.0Ca TREO (wt%) TREO (Wt%) S(F) content (wt%) ^3) Average particle diameter Db embedded 4] Average particle size Dso (μηη) (μηι) BET specific surface area (m2/g ) Grinding characteristics to 5) Grinding flaws evaluation ratio 1 WT m 5T W3ΪΕΤ 寅4 S2 寰5 Jing 6 寰7 to 6 3.0 Ts" 8.0 1050J5〇7 "950~~ 150~jlF 75" 850-4.0
8.0 IT 3H W "8F 1050 1050 1050 1050 1050 850 950 94.2 96.8 95.3 94.0 91.9 91.5 93.4 93.8 <0.0005 <0.0005 <0.0005 <0.0005 < 0.0005 <0.0005 <0.0005 <0.00058.0 IT 3H W "8F 1050 1050 1050 1050 1050 850 950 94.2 96.8 95.3 94.0 91.9 91.5 93.4 93.8 <0.0005 <0.0005 <0.0005 <0.0005 < 0.0005 <0.0005 <0.0005 <0.0005
<0.4 <0.4~ < 0.4 < ΰ A <0_4— <〇X <0.4— <〇T<0.4 <0.4~ < 0.4 < ΰ A <0_4 - <〇X <0.4- <〇T
6.5 ~22 互 *9TTT3 ΎΙ ~6T 1.23 T35 T59 Z07 Z43 274 F89 T52 2.45Z3T Ίλϊ Z65 T24 3Λ2 ΪΤ57 Z24 2.5 T.9 T.7ΤΓ1.4 T94 T8 ΤΓ 100 Ϊ52 21? 257 287 305 JTll36.5 ~ 22 Mutual *9TTT3 ΎΙ ~6T 1.23 T35 T59 Z07 Z43 274 F89 T52 2.45Z3T Ίλϊ Z65 T24 3Λ2 ΪΤ57 Z24 2.5 T.9 T.7ΤΓ1.4 T94 T8 ΤΓ100 Ϊ52 21? 257 287 305 JTll3
AA
AA
AA
AA
A 950 1050 1200 8.0 8.0 8.0 1050 1150 1300 94.0 94.4 96.0 6.0 8.0 1050 950 1050 8.0 1050 1050 93.6 93.6 86.1 <0.0005 <0.0005 <0.0005 <0.0005 <0.0005 0.10 <0.4 <0.4 <0.4A 950 1050 1200 8.0 8.0 8.0 1050 1150 1300 94.0 94.4 96.0 6.0 8.0 1050 950 1050 8.0 1050 1050 93.6 93.6 86.1 <0.0005 <0.0005 <0.0005 <0.0005 <0.0005 0.10 <0.4 <0.4 <0.4
<0.4 "<〇T 5.2 6.8 4.3 6.9 6.6 6.2 2.07 2.46 2.71 1.82 1.73 1.78 2.51 2.87 2.92 2.45 2.56 2.38 1.6 」·2 2.2 2.4 257 295 314 206 201 193 Δ Δ Χ1)表中之「一」係表示並無進行氟化處理茇/或焙燋製程。 X2)就各個原料(Α,Β)之詳細資料而言,#考表1。 X3)DB :布萊恩法平均粒徑 X4)D5D :在雷射繞射散亂法粒度分布而由小粒徑側閔飴之累積趙積50wt%之粒子之粒徑 X5)〇:幾乎無研磨傷痕、適合作爲研磨材料。 △:有若千之研磨傷痕,但是,成爲少蚤,適合作爲研磨材料。 X :研磨傷痕非苐多,不適合作爲研磨材料。 正如表2所不’在比較各個貫施例之研磨材料和比車六 例6之研磨材料時’並沒有在氟含有率、平均粒徑(d ^ BET法比表面積,發現差異,但是,研磨特性係各個B實施 例之研磨材料比較明顯地良好。結果,得知:在製造$ 1 之研磨值(研磨速度)之鈽系研磨材料之狀態下,作=^回 料係比起使用氟碳鈽鑛精鑛(原料B ),還更加最士 ”、、/、原 稀土類碳酸鹽假燒品(原料A )。 用 比較例1及比較例2之研磨材料係在比較於實施例^〜<0.4 "<〇T 5.2 6.8 4.3 6.9 6.6 6.2 2.07 2.46 2.71 1.82 1.73 1.78 2.51 2.87 2.92 2.45 2.56 2.38 1.6 ”2 2.2 2.4 257 295 314 206 201 193 Δ Δ Χ 1) “1” in the table Indicates that no fluorination treatment/or baking process has been carried out. X2) For details of each raw material (Α, Β), #表表1. X3) DB: Brian's method average particle size X4) D5D: particle size distribution in the laser diffraction scattering method and the particle size of the 50% by weight of the accumulated particles of the small particle size side X5) 〇: almost no abrasive scratches, Suitable as an abrasive material. △: There are thousands of abrasive scratches, but they are less suitable and are suitable as abrasive materials. X: Grinding scars are not too many, and are not suitable as abrasive materials. As shown in Table 2, when comparing the abrasive materials of each of the various examples and the abrasive materials of the six cases of the vehicle, the fluorine content and the average particle diameter (d ^ BET specific surface area were found, but the difference was found, but the grinding was not performed. The characteristics of the abrasive materials of the respective B examples were relatively good. As a result, it was found that in the state of manufacturing the abrasive value (grinding speed) of 1, the fluorocarbon was used instead of the fluorocarbon. The antimony concentrate (raw material B) is also more the most ", /, / the original rare earth carbonate pseudo-sintered product (raw material A). The abrasive materials of Comparative Example 1 and Comparative Example 2 are compared with the examples ^~
2i69-6414-PF(N2);Ahddub.ptd 第34頁 1249570 五、發明說明(25) ^ 之研磨材料時,研磨值轡 ^ ^ 例3之研磨材料係在比值較文於小實^^3干/痕。此外,比較 易發生研磨傷痕。相對於這只:’:二,二磨材料時,容 皆具有良好之研磨特性。因 之研磨材料係 粒徑時,在平均粒徑(口= 眼於研磨材料之平均 檢討,結之值而言,進行 〜2· 5 /zm之研磨材料。 上(B)成為1· 5 =製造條件時’作為製造條件係ν好是進 =:= 之研::料:較:4磨之值研變 係在比較於實你你丨2、ζΐ、ς * 卜b較例5之研磨材料 傷#。® # 、之研磨材料時,容易發生研磨2i69-6414-PF(N2); Ahddub.ptd Page 34 1249570 V. Inventive Note (25) ^ When grinding materials, the grinding value 辔 ^ ^ The abrasive material of Example 3 is in the ratio compared with the text in Xiaoshi ^^3 Dry/mark. In addition, it is more prone to grinding scars. Compared with this: ': two, when the two grinding materials, the capacity has good grinding characteristics. Because of the particle size of the abrasive material, the average particle size (mouth = eye on the average of the abrasive material, the value of the junction, the abrasive material is carried out ~ 2 · 5 / zm. The upper (B) becomes 1 · 5 = When manufacturing conditions, 'as a manufacturing condition, ν is good === Research::Material: Compared with: 4 grinding value, the research is in comparison with you, you 2, ζΐ, ς * 卜b When the material is damaged #.® #, the abrasive material is prone to grinding
:展因此朵就研:材料之平均粒徑(Db)而進行檢 果传知.最好是布萊恩法平均粒徑(db)成為丨5 R 作為製造條件係最好是最後之培燒製程之培声严 度成為9〇Qt:〜1200 °C之範圍。 ①皿 每# ί 9比較實施例2之研磨材料和比較例6之研磨材料時, 二把/列2係比較具有良好之研磨特性。結果,得知:在進 人辑之θ培燒製程之狀態下,第2次之梧燒製程之培燒溫度 係取好疋更加高於第1次之焙燒製程之焙燒溫度。 —ρ在比較實施例3之研磨材料和實施例7之研磨材料時, 貫鉍例3係比較具有良好之研磨特性。結果,得知:最好The exhibition is carried out on the basis of the average particle size (Db) of the material. It is best to use the Brian method to achieve the average particle size (db) of 丨5 R as the manufacturing condition. The sound of the sound is 9〇Qt: ~1200 °C. 1 dish per # ί 9 When the abrasive material of Example 2 and the abrasive material of Comparative Example 6 were compared, the two/column 2 series had better polishing characteristics. As a result, it was found that, in the state in which the θ 烧 firing process was carried out, the simmering temperature of the second sinter firing process was taken to be higher than the firing temperature of the first firing process. When ρ was compared with the abrasive material of Example 3 and the abrasive material of Example 7, the Example 3 was comparatively excellent in polishing characteristics. The result, I learned: the best
1249570 五、發明說明(26) 二在于2次之焙燒製程之狀態下,在 刖,進仃鼠化處理。 圪I私 第2實施形態 在本貝形態’將混合稀土類碳 和對於該稀土類侧假 : = :(原, 得到之含氟稀土類化合物者,使用作培燒所 原料。在此,作A M t $ 〃、碑糸研磨材料用之 能,採用作五假燒品係在第1實施形 飾系研磨材料用原料所使用之原料a。另一 = 土類碳酸鹽假燒品之含氣稀土類化合物 製造之各個含氟稀土類化合物(D1〜 D5及Εΐγ之物性係正如表3所示。 妗二氣二土f化合物(D1)之製造:對於稀土類碳酸鹽假 工⑽(原枓A)進行濕式粉碎、氟化處理、洗 燥、解碎及培燒而得到含氣稀土類化合物m 由;乾 碎開始而-直到解碎為止之各個製程之條牛:除 广:氣化氣酸之添加量和培燒之培燒嶋 I解碎於由實施例1之最初之濕式粉碎開始至第1次 之解早I私為止。此外,藉由敦化處理所得到之氣⑴相 ΐ ΐί稀。土類氧化物換算f i(TRE0)間之質量比(F/TRE0) 成為Wt%。此外,焙燒製程之焙燒溫度係70(TC(參考圖 3) ° 含氟稀土類化合物(D2〜D5)之製造: 化合物之製造方法係除了氣處理之10%氣化氯-酸3之:稀力^ 及/或焙燒條件變得不同以外’其餘相同於含氟稀土類化1249570 V. INSTRUCTIONS (26) Secondly, in the state of the roasting process of 2 times, in the sputum, the rat is treated.圪I private second embodiment in the form of Benbe's mixed rare earth carbon and false side of the rare earth: = : (originally, the obtained fluorine-containing rare earth compound is used as a raw material for the cooking. Here, AM t $ 〃, 糸 糸 糸 糸 糸 〃 〃 糸 糸 糸 糸 〃 〃 〃 〃 AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM AM Each of the fluorine-containing rare earth compounds produced by the rare earth compound (the physical properties of D1 to D5 and Εΐγ are shown in Table 3. The production of the compound of the second gas and the two earth f (D1): for the rare earth carbonate fake (10) (original A) Wet pulverization, fluorination treatment, washing, pulverization and sintering to obtain a gas-containing rare earth compound m; starting from the dry smashing - until the smashing of the various processes of the cattle: except for wide: gasification The amount of gas acid added and the calcined sputum I were pulverized from the first wet pulverization of Example 1 to the first solution. In addition, the gas (1) phase obtained by the Dunhua treatment was obtained. ΐ ΐί稀. The mass ratio (F/TRE0) between the soil oxide conversion fi(TRE0) becomes Wt%. The baking temperature of the baking process is 70 (TC (refer to FIG. 3) ° The manufacture of the fluorine-containing rare earth compound (D2 to D5): The manufacturing method of the compound is 10% gasification of chlorine-acid 3 except gas treatment: thin force ^ And/or the firing conditions become different, the rest are the same as the fluorine-containing rare earths
1249570 五、發明說明(27) — 合物(D 1 )之製造方法。藉由各個含氟稀土類化合物(D 2〜 D5)之製造之氟化處理所得到之氟(F)相對於全稀土類〜 物換算質量(TRE0)間之質量比(F/TRE〇)和焙燒條件係正如 表3所示。正如表3所示,在含氟稀土類化合物(D2)之製Π 造,並無進行焙燒。此外,含氟稀土類化合物(D3〜的\ 製造之焙燒條件係除了焙燒溫度變得不同以外,其 於含氟稀土類化合物(D1 )之培燒條件。 、 含氟稀土類化合物(E1)之製造:除了一直 之稀土類碳酸鹽假燒品(原料六)進 于於旱備 / k ’慮、乾_、解碎及培燒之势藉糸^ / 處理之1 0 %氟化氫酸之添加量 Y為止而使侍氟 不同以外,其餘相同於含及L = 去口 .L 朴丄 稀土類化合物(D 1 )之萝诰制 釭。此外,精由氟化處理所得 H磁衣 氧化物換算質量(TRE0)間之質旦μ r 目對於全稀土類 焙燒製程之焙燒溫度係85〇。心(F::RE0)成為8· Owt%, 土類化合物(El)之製造,還_由::3)。接著,在含氟稀 所得到之焙燒品,來進行9裘本軋機而對於利用焙燒 定分級點在6" m)而對於碎,藉由渦輪分級機(設 著,藉由樣本軋機而對於利用粉^品,進行分級。接 子,來進行乾式粉碎,藉由 ^刀級所回收於粗粉側之粒1249570 V. INSTRUCTION OF THE INVENTION (27) The method for producing the compound (D 1 ). The mass ratio (F/TRE〇) between the fluorine (F) obtained by the fluorination treatment of each of the fluorine-containing rare earth compounds (D 2 to D5) relative to the total rare earth equivalent mass (TRE0) The firing conditions are as shown in Table 3. As shown in Table 3, the firing of the fluorine-containing rare earth compound (D2) was not carried out. In addition, the firing condition of the fluorine-containing rare earth compound (D3~) is a sintering condition of the fluorine-containing rare earth compound (D1) in addition to the baking temperature, and the fluorine-containing rare earth compound (E1). Manufacture: In addition to the rare earth carbonate calcined product (raw material 6), it is added to the drought/k', dry _, smashing and simmering 糸 ^ / treatment of 10% hydrogen fluoride Y is the same as that of the fluorine, and the rest is the same as that of the rare earth compound (D 1 ) containing L = 去 .. L 釭 釭 釭 釭 釭 釭 釭 釭 釭. The temperature of the (TRE0) is the calcination temperature of the whole rare earth roasting process of 85 〇. The heart (F::RE0) becomes 8.0 wt%, the manufacture of the soil compound (El), and _ by: 3). Next, the calcined product obtained by the fluorine-containing rare product is subjected to a 9-inch mill, and the classification point is 6" m) by the roasting, and the crushing is performed by a turbo classifier (provided by the sample mill) Powder, graded, and smashed, dry pulverized, and recovered from the coarse powder side by the knife level
ΠΟ而對於得到之粉碎品f進,輪分級機(設定分級點在4 A 級所回收於粗粉側之粒子,:分級。接著,得到藉由該分 成為含氟稀土類化合物(E1)。 1249570 表3 製造條件 組成 含氟稀土類 化合物 (D1 〜D5、E1) 氟化 處理條件 F 培燒溫度 ΓΟ TREO (wt°/〇) 氟(F)之 含有率 (wt°/o) F TREO (wt%) TREO (wt%) 一 D1 20 700 87.1 15.2 17.5 叫〕D2 15 一 83.8 10.5 14.5 D3 15 700 89.1 11.6 13.0 D4 15 1200 94.3 7.3 7.7 D5 10 700 93,8 7.6 8·1 ~ dunn 8.0 850 94.4 6.8 7.2 ---____ 糸1)在D2之製造τ並無進行培燒,Then, the obtained pulverized product f is fed into a wheel classifier (particles collected on the coarse powder side at a classification point of 4 A), and classified. Then, a fluorine-containing rare earth compound (E1) is obtained by this fraction. 1249570 Table 3 Manufacturing conditions Composition of fluorine-containing rare earth compounds (D1 ~ D5, E1) Fluorination treatment conditions F Burning temperature ΓΟ TREO (wt ° / 〇) Fluorine (F) content rate (wt ° / o) F TREO ( Wt%) TREO (wt%) A D1 20 700 87.1 15.2 17.5 is called] D2 15 - 83.8 10.5 14.5 D3 15 700 89.1 11.6 13.0 D4 15 1200 94.3 7.3 7.7 D5 10 700 93,8 7.6 8·1 ~ dunn 8.0 850 94.4 6.8 7.2 ---____ 糸1) In the manufacture of D2, τ is not burnt,
五、發明說明(28) 一 ^ 彳久比巷 使用混合稀土類碳酸鹽 :D4、Ε1)者。稀 土類^ 係正如表4所示。 例,對於藉由混合所得 解碎、焙燒、乾式粉碎及 種製程所構成之各個實施 第1貫施形態之比較例1之 處理及連接於該氟化處理 。因此,省略就各個製程 κ施例8、9、1 1及比較例8 例’作為飾系研磨材料之原料係 (原料A)和含氟稀土類化合物(D1 酸鹽及含氟稀土類化合物之比例 接著,在這些實施例及比較 之原料,進行濕式粉碎、乾燥、 分級而得到鈽系研磨材料。由此 例之研磨材料之製造方法 製造方法時,除7 # ” 之洗淨·過二卜,行氟化 之詳細說明外’其餘皆相同 實施例1 〇、工2 · 作為鈽系研磨材料 =例7 ·在這些實施例及比較例, Α)和含氟稀土 _ # 料係使用混合稀土類碳酸藥(原料 大只化合物(Dl H 、土 D5 E1)者。稀土類碳酸鹽及V. INSTRUCTIONS (28) A ^ 彳久比巷 Use mixed rare earth carbonates: D4, Ε 1). The rare earth class ^ is shown in Table 4. For example, the treatment of Comparative Example 1 in which the first embodiment was carried out by the mixing, the calcination, the calcination, the dry pulverization, and the seeding process were carried out, and the fluorination treatment was carried out. Therefore, the raw material system (raw material A) and the fluorine-containing rare earth compound (D1 acid salt and fluorine-containing rare earth compound) which are used as the decorative material for the decorative system are omitted for each of the processes κ, the examples 8, 9, 11 and the comparative example 8 In the examples, the raw materials of these examples and the comparative materials were subjected to wet pulverization, drying, and classification to obtain a lanthanum-based abrasive. In the production method of the method for producing the abrasive material, the washing method of the 7 # ”卜, the detailed description of the fluorination is the same as the other embodiment 1 〇, 2 2 as a lanthanide abrasive material = Example 7 · In these examples and comparative examples, Α) and fluorine-containing rare earth _ # material system use mixing Rare earth carbonates (large raw materials (Dl H, soil D5 E1). Rare earth carbonates and
第38頁 2169-6414-PF(N2);Ahddub.ptd 1249570 五、發明說明(29) 含氟稀土類化合物之比例係正如表4所八 接著,在這些實施例及比較例,$ 之原料,進行濕式粉碎、氟化處理、冰=精由混合所得到 解碎、培燒、&式粉碎及分級而得输;^ •過遽、乾燥、 是說’這些實施例及比較例係除J:系研磨材料。也就 之1〇衬%氟化氫酸之添加量變得不二乂不同以及氟化處理 較例!。此夕卜,氟化處理之10wt%氣门化其餘相曰同於比 成為氟化處理對象之原料(原料漿體:: ! _氟化氫酸之添加所添加之氟質量二里二和及糟由 料漿體之全稀土類氧化物換算質量(TR σ '、 ((FHF2)/TRE〇--F/TREO)成為8· 〇wt% 之量]之貝里比 錦系研磨材料之評價 就藉由各個實施例及此產 … 言,測定I含有率、布萊因、:::付到之飾系研磨材料而 射.散亂法粒度分布所心/ 句粒徑(Db )、根據雷射繞 面積。此外,使用夢A ^成之平均粒徑(D及BET法比表 研磨材料,進行研=個實施例及比較例所得到之飾系 之研磨面之傷痕砰價°。^,進行研磨值(研磨速度)及得到 4。此外,測定方、去、、將測定值及評價結果,顯示在表 價方法係共通於篦!每研磨試驗方法、各種研磨特性之評 A弟1果施形態。Page 38 2169-6414-PF(N2); Ahddub.ptd 1249570 V. DESCRIPTION OF THE INVENTION (29) The ratio of the fluorine-containing rare earth compound is as shown in Table 4, and in these examples and comparative examples, the raw materials of $, Wet pulverization, fluorination treatment, ice = finely obtained by mixing, smashing, simmering, & pulverization and classification to obtain the output; ^ • over-drying, drying, say 'these examples and comparative examples J: is an abrasive material. In other words, the amount of fluorinated hydrogen fluoride added is different, and the fluorination treatment is more common! . Further, the remaining 10% by weight of the fluorination treatment is the same as the raw material which is the object of the fluorination treatment (the raw material slurry::! _hydrofluoric acid added, the fluorine content added to the second and the worse The evaluation of the total rare earth oxide conversion mass (TR σ ', ((FHF2)/TRE〇--F/TREO) of the slurry is 8·〇wt%] According to various embodiments and the production, the I content, Bryin, and:: the amount of the abrasive material to be applied and the particle size distribution of the particle size distribution (Db), according to the laser In addition, the average particle diameter of the dream A (the D and BET method is used to grind the material, and the flaws of the polished surface of the decorative system obtained in the examples and the comparative examples are measured. The polishing value (polishing rate) and the obtained value 4. In addition, the measurement method, the measurement value, and the evaluation result are shown in the table of the price method, which is common to each of the polishing methods, and the evaluation of various polishing characteristics. form.
2169-6414-PF(N2);Ahddub.ptd 第39頁 1249570 五、發明說明(30) 表4 寅 施 例 例 % >製造條件 铈系研磨材料 采2〕 原 料 之 横 成 原料之 混合比率(%) (TREO基準) ®化 處理 F 焙燋 溫度 (C) TREO (wt%) Th + U Ca + Ba + Fe + P S(F) 之含 有率 (wt%) 來3〕 平均 粒徑 Db (μιη) 楽4〕 平均 粒徑 Dso (l^m) BET法 研磨 特性 稀土類 碳酸鹽 假焼品 源料A) 含® 稀土頬 化合物 (D1 〜D5 Έ1) 比表 面積 (m2/g) 研 磨 値 來5〕 傷 痕 評 價 TREO (wt%) TREO (Wt%) TREO (wt%) 寅8 A+D1 55 45 — 1050 94.3 <0.0005 <0.4 6.5 1.73 2.41 1.6 239 Δ W7 A+D1 75 25 3.0 1050 94.2 <0.0005 <0.4 6.4 1.31 2.53 2.1 135 △ tt8 A+D2 45 55 — 1050 93.7 <0.0005 <0.4 6.8 1.27 2.17 2.6 122 Δ A+D3 40 60 — 1050 94.2 <0.0005 <0.4 6.7 1.98 2.73 1.5 263 〇 比9 A+D4 0 100 — 1050 93.6 <0.0005 <0.4 7.1 2.69 3.03 0.91 298 X g1〇 A+D5 50 50 3.0 1050 93.9 <0.0005 <0.4 6.5 2.11 2.62 1.7 285 〇 寳11 A+E1 10 90 — 1050 95.3 <0.0005 <0.4 5.5 1.83 2.52 1.6 234 〇 寅12 A+E1 10 90 3.0 1050 93.5 <0.0005 <0.4 6.9 2.24 2.65 1.5 259 〇 X1)表中之「一」保表示並無進行氟化處理。 Χ2)各個原料中之物質(A、D1〜D5、Ε1)之詳钿資料保參考表1茇表3» X3)DB :布萊恩法平均粒徑 X4)D5i):在雷射緒射散亂法粒度分布而由小粒徑側関飴之累稜雔稜50wt%之粒子之粒徑 X5)〇:幾乎無硏磨傷痕、適合作爲硏磨材料。 Δ :有若千之研磨傷痕,但是,成爲少是,適合作爲研磨材料。 X :研磨傷痕非常多,不適合作爲研磨材料。 正如表4所示,比較例7和比較例8之研磨材料係在比 較於實施例之研磨材料時,研磨值變小。此外,比較例9 之研磨材料係在比較於實施例之研磨材料時,容易發生研 磨傷痕。相對於這些,實施例之研磨材料係皆具有良好之 研磨特性。因此,就研磨材料之平均粒徑(DB)而進行檢 討,結果,得知:最好是布萊恩法平均粒徑(DB )成為1. 5 // m〜2. 5 // m之研磨材料。接著,得知:在著眼於研磨材料 之原料時,例如由實施例9和比較例8之比較而瞭解比起準 備氟含有率變高之含氟稀土類化合物來使用比較少量者, 還更加最好是準備氟含有量變低之含氟稀土類化合物來使2169-6414-PF(N2); Ahddub.ptd Page 39 1249570 V. Inventive Note (30) Table 4 Example Example % > Manufacturing Conditions 铈 System Abrasive Material 2) Mixed Ratio of Raw Materials %) (TREO standard) ® treatment F baking temperature (C) TREO (wt%) Th + U Ca + Ba + Fe + PS (F) content rate (wt%) to 3] average particle diameter Db (μιη楽4] Average particle size Dso (l^m) BET method grinding characteristics Rare earth carbonate false sputum source material A) Contains ® Rare earth lanthanum compound (D1 ~ D5 Έ1) Specific surface area (m2/g) Grinding 値 5 〕 Scar evaluation TREO (wt%) TREO (Wt%) TREO (wt%) 寅8 A+D1 55 45 — 1050 94.3 <0.0005 <0.4 6.5 1.73 2.41 1.6 239 Δ W7 A+D1 75 25 3.0 1050 94.2 <;0.0005<0.4 6.4 1.31 2.53 2.1 135 △ tt8 A+D2 45 55 — 1050 93.7 <0.0005 <0.4 6.8 1.27 2.17 2.6 122 Δ A+D3 40 60 — 1050 94.2 <0.0005 <0.4 6.7 1.98 2.73 1.5 263 〇 9 9 A+D4 0 100 — 1050 93.6 <0.0005 <0.4 7.1 2.69 3.03 0.91 298 X g1〇A+D5 50 50 3.0 1050 93.9 <0.0005 <0.4 6.5 2.11 2.62 1.7 285 〇宝11 A+E1 10 90 — 1050 95.3 <0.0005 <0.4 5.5 1.83 2.52 1.6 234 〇寅12 A+E1 10 90 3.0 1050 93.5 <0.0005 <0.4 6.9 2.24 2.65 1.5 259 〇X1) "One" guarantees that no fluorination treatment has been carried out. Χ 2) Details of the substances in each raw material (A, D1 ~ D5, Ε 1) are listed in Table 1 茇 Table 3» X3) DB: Brian's average particle size X4) D5i): scattered in the laser Particle size distribution and particle size of 50% by weight of the edge of the small particle size side of the edge of the X5) 〇: almost no honing scar, suitable as a honing material. Δ: There are thousands of abrasive scratches, but it is less suitable and is suitable as an abrasive. X: There are many grinding scars and it is not suitable as an abrasive material. As shown in Table 4, the abrasive materials of Comparative Example 7 and Comparative Example 8 were smaller than the abrasive materials of the examples. Further, the abrasive material of Comparative Example 9 was liable to be scratched when compared with the abrasive material of the example. In contrast to these, the abrasive materials of the examples all have good abrasive properties. Therefore, the average particle size (DB) of the abrasive material is reviewed. As a result, it is found that the average particle size (DB) of the Brian method is 1. 5 // m~2. . Then, it is understood that, when focusing on the raw material of the polishing material, for example, it is understood from the comparison between Example 9 and Comparative Example 8 that the fluorine-containing rare earth compound having a higher fluorine content is used, and a smaller amount is used. It is good to prepare a fluorine-containing rare earth compound having a low fluorine content to make
第40頁 2169-6414-PF(N2);Ahddub.ptd 1249570 五、發明說明(31) 用比較多者 接著,由實施例8之研磨材 之比較而得知理想之原料。也就9 ★、,杈曰例7之研磨材料間 料中包含經過培燒所得到之含;二$得知··最好是在原 之全稀土類氧化物換算質量所占 2化合物並且該原料 物之氧化物換算質量之比例成為3二前述含氟稀土類化合 外,由實施例8之研磨材料和比 之原料。此 而得知··包含於原料中之合Λ π之研磨材料間之比較 於D2。也就是說,得知土所類化合物係最好抓大 之含氟稀土類化合物係比起鼓:過過培燒所得到 想。此外,接著由實施船 ‘;每還更加地理 材料間之比較而得知:在培心和貫施例12之研磨Page 40 2169-6414-PF(N2); Ahddub.ptd 1249570 V. INSTRUCTION DESCRIPTION (31) Use more. Next, the ideal material is obtained from the comparison of the abrasive materials of Example 8. In other words, the material of the abrasive material of the example 7 contains the content obtained by the calcination; the second $ is known to be the best compound in the original total rare earth oxide conversion and the raw material The ratio of the oxide-converted mass of the material is the same as that of the above-mentioned fluorine-containing rare earth compound, and the abrasive material of Example 8 and the raw material. Therefore, it is known that the composite material contained in the raw material π is compared with D2. That is to say, it is known that the fluorine-containing rare earth compound which is the best for the soil-based compound is better than the drum: it has been obtained. In addition, it is then learned by the ship's implementation; each comparison of more geographical materials: grinding in the heart and the example 12
係付到更加良好之研磨特性之研磨材料。衣私I 璃某nm磨材料係使用在例如光碟或磁碟用玻 璃基板、主動矩陣型LCD(液晶顯示器)、液晶午 f片、。時鐘、電子計算機、相機則⑶、太陽能電池等: 顯示器用玻璃基板、LSI光罩用玻璃基板或光= 之玻璃基板或者是光學用透鏡等 ㈣鏡4 2169-6414-PF(N2);Ahddub.ptd 1249570 圖式簡單說明 第42頁 2169-6414-PF(N2);Ahddub.ptdIt is an abrasive material that pays for better abrasive properties. The clothing I glass is used in, for example, a glass substrate for a disk or a magnetic disk, an active matrix type LCD (liquid crystal display), or a liquid crystal film. Clock, computer, camera (3), solar cell, etc.: Glass substrate for display, glass substrate for LSI mask, glass substrate for light = optical lens, etc. (4) Mirror 4 2169-6414-PF(N2); Ahddub. Ptd 1249570 Schematic description of page 42 2169-6414-PF(N2); Ahddub.ptd
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