TW200426206A - Cerium-based abrasive - Google Patents

Abstract

It is an object of the present invention to provide a cerium-based abrasive, which enables higher polishing speed and generates fewer scratches. The cerium-based abrasive according to the present invention contains rare earth oxide as a main component, which includes fluorine, and as rare-earth elements, at least cerium lanthanum, praseodymium, and neodymium. In the cerium-based abrasive, the proportion of content of neodymium oxide to that of the total rare-earth oxides (Nd2O3/TREO) accounts for 0.001-5.0 wt%. Polishing an object to be polished such as a glass by means of the abrasive will require shorter period of time compared to the conventional cerium-based abrasives. Additionally, the present abrasive can securely inhibit generation of scratches on a polished face.

Description

200426206 V. Description of the invention (l) [Technical field to which the invention belongs] The so-called # 系 研 The present invention relates to a grinding material mainly composed of gaseous UA and cerium hydrazone. [Prior technology]: The grinding materials are rich in raw materials such as Π, crushed, roasted, and graded as needed: i ,,, and the brocade-based grinding materials used are mainly oxidized (Ce02, etc.) = • j (La2G3) oxides of rare earth elements other than 4 钸.

As for the polishing material with a higher polishing speed, the right side is given as J. JP 2002-0 9 745 7) = = series polishing material (refer to the example, but 'as the polishing material, it is required to obtain the smoothest possible polishing surface .. : F ft T-excellent & low after polishing. That is, it is used as a material for grinding between j 迓 degrees. And it is not easy to scratch the polished surface as it can obtain a smoother surface with a more southern polishing speed. Abrasive materials are required to be polished. However, in the past, the occurrence of samarium-based wounds containing fluorine was not necessarily caused by ft. In areas where the grinding speed and the demand for scraping abrasive materials have increased: fine ::! Sieve-based grinding and other applications require grinding speed; high-grade surface grinding "1" abrasive materials that are not easy to occur. [Abstract] 200426206 V. Description of the invention (2) The present invention is produced in order to solve the above problems, The subject of the present invention is to provide a high-speed grinding material with less occurrence of scratches. The present inventors have conducted research and discussion on the grinding speed of concrete-based abrasive materials or the occurrence of them. The grinding speed of the oxidized abrasive material will be further increased, and this will form the present invention. The wound is more difficult. The present invention is a samarium-based abrasive material. In addition to fluorine, the rare earth element contains at least europium (Ce), Lanthanum (La), praseodymium (pr) and "(_)" are mainly composed of member oxides, and the weight of the oxide's equivalent to the total rare earth oxide equivalent weight = soil (hereinafter referred to as TRE0) (Nd203) / TRE〇) in 〇 · 〇〇1 =% by weight. And the so-called TRE0 refers to the total weight of the rare earth oxides in the object when converted into rare earth oxides. The total weight is obtained by decantation and calculation of the composition of the object. In the case of #object composition system 2, the TRE0 system is subject to pretreatment such as dissolution and dilution (based on the two σ requirements), and then all the rare earth elements are precipitated as oxalate. Bran: filter, dry, and roast. After the formation of rare earth oxides, it can be measured and calculated. The method of Ribéry is, for example, the weight ratio (hereinafter referred to as the content rate) of titanium oxide to TRE0 in the conventional samarium-based abrasive material described in Patent Document 1. Compared with this, the samarium-based abrasive of the present invention The oxidation of the material contains ❶ ^, which is low. As a result of research and discussion, it was found that TRE◦ medium-range oxidized decorative abrasive materials have a higher polishing speed and are easier to grow. Therefore, when using the abrasive material of the present invention to target the surface, it is the same as that of conventional abrasive materials. Compared with the situation on page 11, 2169-6178-PF (N2) .ptd 200426206 V. Description of the invention (3) Grinding is completed in ΓίΓ 丨 and the grinding hair obtained by grinding can be more surely suppressed. In addition, as explained previously In the present invention: In the second material, the weight ratio of titanium oxide to TRE0 is easily Λ amount% 5 weight Γ. This is because less than 0.001% by weight, the scratch is low, and abrasion is easy to occur. For Γίη θ to be 2% by weight or less, it is more preferable to be 0.5% by weight or less. 〇 · 1% by weight or less is more preferable. ③ The i + ϋt abrasive material is roughly a fluorocarbon ore concentrate or Rare earth-based rare earth & acid salts or rare earth oxides are pulverized, wet processing such as fine inorganic acid treatment or chemical treatment is required for burning, classification (as required), and production of μ α 丄 々之 扃 料 畀 # 尨 " 来 衣 的 的。 And The invented samarium-based abrasive materials are most commonly used for rare earth concentrates such as random carbon agglomerates, monoside concentrates, and China = concentrates. ^ Hall processing or dissolving separately, volume, m, and spleen: Rare earth synthesis plant with reduced impurities other than woodycin, II =,; t / night), mixed with precipitants such as ammonium bicarbonate, ammonia, etc. i π 5 丨 二 Ｍ # prepares a series of burned materials (such as rare earth oxidation = 5 substances (such as rare earth carbonate)) or the rare earth-based capacitors obtained by ion purification to filter the precipitate to achieve separation. And 10 times "above, refined $ ^ / (^ 制 液), _2〇3 / TREO is usually used as raw materials for 糸 grinding materials (2169-6178-PF (N2) .ptd like this invention. Page 12 200426206 5 Description of the invention (4)

NdJVTREO solvent extraction at a certain range), it is best to strengthen the reduction of rare earths on the side of the rare earth or heavier than “, to obtain low-concentration rare earths such as Nd 2 03 / TRE0 below 5% by weight). j In the samarium-based abrasive material of the present invention, the ratio of the total weight of samarium, lanthanum, fins, and condensed rare earth oxides to TRE0 is preferably 97% by weight or more. It is possible to more reliably obtain a high polishing rate and a scratch prevention effect. In addition, i does obtain these effects, and the ratio value is more preferably 98% by weight or more, and 99% by weight or more. The appropriate content of each rare earth oxide in TRE0. If the root oxide is specified separately, the weight ratio (Ce02 / TRE0) of hafnium oxide to TRE0 is preferably 50% to 90% by weight. Oxidation bromide is the most abrasive substance in the total oxides' weight ratio, value, and needs to be carried out in the raw material refining step; on the other hand, if it exceeds the upper limit and the cost increases, the productivity will deteriorate ^ dtr time or contention Take a look at π to see 0 / tongue. The weight ratio of the emulsified decoration to TRE0 is more preferably 55 weights and 85 weights ... 60% by weight to 80%. Lanthanum oxide accounts for the heavy weight of TRE0, and the weight is also king heart% ~ 45% by weight. Lanthanum oxide series rare earth β2 3 RE〇) Take a good 2 weight of the substance, which exists in the rare earth that is mainly decorated with ornaments: arrows? / ㈣ Oxide (U0F or CeLa2 03F3t = H shell oxide, or it will slowly release gasification when grinding with chaotic glass. During grinding, especially in glass, it has the effect of increasing the grinding speed. M: They have a chemical effect. If the above lower limit is exceeded, the weight ratio of the conversion to tre0 will be reduced if j & 化 the effect of the above-mentioned effects will be reduced, research on page 13 2169-6178-PF (N2) .ptd 200426206 V. Invention Note (5) The ground surface obtained by grinding will instead become a rough surface. On the other hand, the limit value cannot be used to achieve sufficient grinding. ° M tongue Dan a 7 丨 hit, ^ said mystique. Therefore 'Emulsified lanthanum accounted for Ding RE0 = Proportion is 5% by weight, 10% by weight to 37.5% by weight. 0: 1% by weight. The weight ratio of Pr0 (Pr60ll / TREO) is preferably 0.1%. Xia% to 10% by weight and 8% by weight are more preferred. The fluorine content in the actinide-based abrasive material is preferably 0.5% by weight to 丨 0%. If the lower limit is not reached, it cannot be achieved. To obtain a sufficient grinding speed, if it exceeds the upper limit, grinding scratches easily occur. And from the two aspects of grinding speed and grinding scratches, " A higher effect is obtained, and the gas content is more preferably 1% to 8% by weight, and more preferably 2% to 7% by weight. In addition, the fluorine (F) contained in the actinide-based abrasive material and the content of The molar ratio (F / (La + Pr)) between lanthanum (La) and praseodymium (PR) is preferably 0.2 to 3. If I is less than the value, when the samarium-based abrasive is stored or ground In particular, the π valley is liable to generate hydroxides on the grinding day. The grinding material in the state of hydroxide generation has the problem of low grinding speed (grinding force). And if iron i oxide is easily formed during grinding, the There is another problem that the polishing rate is reduced in a short time. For example, if the molar ratio exceeds the upper limit, the chemical action of fluorine during polishing is too strong, and the polishing surface obtained after polishing may become rough. When the X-ray peak intensity is measured by a fork-ray diffraction method using Cu-K α line or Cu-K α! Line as a X-ray source, it appears in a range of 2 (9 (diffraction angle) = 2Odeg to 3 0deg, And the strongest X-ray peak intensity of the X-ray peak intensities of rare earth fluorine oxides and the strongest X-ray peak intensity of the X-ray peak intensities of thorium oxide The line intensity ratio of the peak intensity (rare earth fluoride oxide / cerium oxide) -based

II 2169-6l78-PF (N2) .ptd Page 14 200426206 V. Description of the invention (6) 0 · 0 5 ~ 0 · 6 The decorative system is ground well and permanently | Earth Fluorine Oxide (LnOF), 'to :: ：: f 外 'Here the so-called rare earth component of the cubic crystal rare earth ^^ with f said 1 refers to the degree of brocade. ux0y is usually the diffraction X-ray peak intensity of i 5 < y / x = compound αηΛ)

~ H.a75, or Ce: C h big Kenji! : Η Λ 2〇3 / m〇 is small and called 5〇1.75, or CeQ7sNd "is 4 as e_ ^

糸 Servants private n ° .75 a ° .25〇75). At that time, it was identified as Ce-Nd-O county injection oblique object. When the above-mentioned intensity ratio is found to be less than the lower limit value, Rongshang p? # 目 | 研 ί has caused orange peel holes with adverse effects. 1 If the intensity ratio exceeds the upper limit, the grinding speed will decrease. .2~. .4 ": The system with a better L ratio. Yu Xia Ding's diffraction measurement system uses the x-rays with the above characteristics to check the incidence; :: bu + f abrasive material), along the periphery of the circle centered on the sample Scanning or semiconductor detector), measuring diffracted x-rays ^: solution: χ-ray diffraction intensity curve obtained by jin, for material identification II: then: using Cu-K α as X-ray source ' The angle (2 θ) of the line I or Cu-K αι line feeling I is 20deg ~ 30deg rare earth fluoride oxide, its maximum = the ray peak intensity usually appears in the range of 26.5deg ± 0.5deg. 'Same range 2 The maximum x-ray peak intensity of thorium oxide (Ce02) appears in the range of 28.1 deg · 0 deg. ^ ^ The diffraction X-ray peak intensity measured by the X-ray diffraction measurement method is dry, and the right is at 20 ( Diffraction angle) = 24.2deg ± 〇5deg appears most in the range of page 15 2169-6178-PF (N2) .ptd V. Description of the invention (7) Large peak, the intensity of X-ray peak of rare earth fluoride, and oxidation The intensity ratio (LnF3 / Ce〇2) of the strongest X-ray peak intensity of the X-ray peak intensity of 钸 (Ce%) is preferably less than 0.04. When the intensity is above 0.004, It is easy to grind and scratch. The rare earth fluorides (LnFs) referred to here include, for example, lanthanum fluoride (LaF3). The diffraction angle (2 θ) is in the range of 20deg to 30deg. The largest peak does not appear in the range of 24 · 2 ± 0. 5deg, but appears at a position close to the largest peak of thorium oxide. However, due to the ringing of the largest peak of thorium oxide, it is difficult to accurately determine the rare earth fluoride. Strength. Therefore, in the present invention, for the rare earth fluoride, the maximum range of 24,2 deg ± 0.5 deg. Is used. The target used for X-ray diffraction measurement is considered to be represented by copper (Cu), molybdenum (Cu) Mo), iron (Fe), cobalt (co), tungsten (w), silver (Ag), etc., but the largest peak intensity, from the point of more accurate measurement, the beam is suitable. The system with better pore volume 〇 soil 0 0 2cmvg ～ 〇 · lcmVg, 〇 0 0 5 cm3 / g ～ 0. 〇8cra3 / g is more rational. At the lower limit, the grinding speed is large, but the grinding scraping Injuries are easy to occur 'and = the upper limit value is exceeded, the grinding speed is too low, the # method can get enough grinding speed As described above, the rubbing-based abrasive material of the present invention has less pot height and less grinding scratches. Therefore, the eight grinding speed is more Θ pounds. This material is used to grind the surface of the object to be polished, which is different from the use of conventional rubbing materials. Compared with the abrasive material, it can finish grinding in a shorter period of time. "Month / Scratched hair on the abrasive surface. Totally and more reliably suppress the research. 5. Description of the invention (8) [Embodiment] In order to explain the The best embodiment of the samarium-based abrasive material of the present invention has a difference of 1 degree and a shape-bearing oxidation condition) is a purity of cerium oxide (CeO2), lanthanum oxide (La2O3), and each rare earth # 4 小 4 Burnt down. In the prepared rare earth oxides, the number of contact pieces in the rare earth oxides was less than 0.1%. In addition, the oxygen content of the target rare earth oxides, the content of impurities, and the purity (the ratio of ^ 1 ^ to 0_ ^ weight 5 in TRE0) are all 99.99% by weight or more, Γ = Among the oxides, all rare earth oxides other than oxides are oxidized in heavy denier plants. The weight ratio of emulsification (Nd2 03 / TRE0) is less than 0.001, and the combined rate of L + radon is 0 · 0 The weight is less than 01% by weight. Properly weigh the mixed raw materials in order to ping: mg of mixed raw materials. In this way, I: osmium, lanthanum oxide, ytterbium oxide, oxidation — 3 different types of different ancient rates Abrasive performance of brocade grinding materials A shoulder +: Medium: 1: Purity of rare earth oxides to modulate the original talents.-The general recognition of the content of the oxides, and the At rare earth oxidation of the manufactured abrasive material Γ Erzhong The weight ratio of the materials is the same, so the description is omitted— (refer to Table 1, Table 1). And the comparative raw materials are not mixed with oxidative convergence. / 0 (4 total &) does not reach 100%, which means The raw materials are mixed with Peng oxide.

The obtained raw material (a mixture of rare earth oxides) was mixed with pure water having a weight twice as much as that of the raw material, and wet-pulverized in a grinder (at tr i tor) to obtain a slurry. In the grinder, a stainless steel ball with a diameter of 5 mm was used as the S pulverizing medium. The crushing time was 8 hours. Next, 10% hydrofluoric acid was added to the obtained slurry to prepare a weight ratio (F / (TRE0 + F)) of the fluorine component in the slurry, and the slurry was stirred for 30 minutes (chemical treatment). In each of the examples other than Examples 1 and 2, and each of the comparative examples other than Comparative Examples 5 and 6, each slurry was prepared so that the weight-to-day ratio (F / (TRE0 + F)) of the fluorine component was 6%. In addition, the weight ratio of the fluorine component was adjusted to be 1.5% in Example 12, 10% in Example 13, and 15% in Comparative Example 6, respectively. This fluorination treatment was not performed in Comparative Example 5. Thereafter, the solid content was precipitated, the upper clear solution was taken out, pure water was added and repulp was washed, and the washed slurry was filtered by a pressure filtration method. And the obtained filter cake was dried at 140 t for 48 hours. The obtained dried cake was pulverized with a light crusher, and the obtained pulverized product was 950. 〇Baking for 18 hours. This baked product was pulverized with a sample mill, and the obtained pulverized product was classified with an impeller classifier (set a classification point at 3 # m) to obtain a milled-type ground material. Table 1 shows the weight ratio of each rare earth oxide in TRE0 of the obtained samarium-based abrasive material. Measurement of I Concentration The fluorine-containing content of the actinide-based abrasives obtained in each of Examples and Comparative Examples was measured. For the measurement of the fluorine concentration, in addition to the abrasive material obtained in Comparative Example 5, the fluorine analysis was performed by using the method of ionization, warm water extraction, and fluoride ion electrode. And

200426206 V. Description of the invention (10) The measurement of the densities of the obtained abrasives was performed using a thermal hydrolysing method ^ · Hou machine, alizarin complexing agent photometric method. The measurement results are as shown in the tables. The evaluation first solidifies the formed body. The results are shown in the following tables using the lapping speed of the sacrificial abrasive materials obtained in each of the Examples and Comparative Examples. . ϋ The ratio of the rotation of the grinding pad to the testing machine on one side of the flat panel machine. 'Mix the powdery decorative abrasive powder with pure water and adjust the knife / chendo 15 weight 2: 2% abrasive slurry. This abrasive slurry was used to grind the surface of the glass for flat panels using a polishing tester (HSP-2ί type, manufactured by Taito Seiki Co., Ltd.). After the grinding is completed, the glass is washed with pure water and dried in a dust-free state. In this polishing test, a polishing material slurry was supplied to the surface to be polished, and the surface was polished with a polishing pad. The polishing pad was made of polyurethane. Grinding The pressure on the ground surface is 5.9 kPa (60 g / cm2). And set the grinding trial speed to 100 rpm. The supply amount of the abrasive slurry was 5 liters / minute. G Milling speed Tang Xi iyjg Measure the weight of the glass before and after grinding, and determine the reduction in glass weight due to grinding 'to obtain the grinding value based on this value. In this polishing test, the polishing value was used to evaluate the polishing rate. In addition, here, the polishing value at the time of polishing using the polishing material obtained in Comparative Example 3 was used as a reference (100). Page 19 2169-6178-PF (N2) .ptd 200426206 V. Description of the invention (π) After the evaluation of grinding Hungarian wound and the grinding is finished, the polished surface after washing with pure water and in a dust-free state is scratched. Evaluation. The evaluation of scratches uses 300,000 lux ^ dihalogen lamps as the light source, observes the surface of the broken glass by the reflection method, and counts the number of points from the larger month to the number of injuries, which is reduced by the full point price. In this scratch evaluation, the polishing accuracy required for fine polishing of a glass substrate for a hard disk or an LCD is used as a judgment criterion. Specifically, in Tables 丨 to 4, "◎" represents more than 98 points (very suitable for ribs and LC) fine polishing of glass slabs, and "〇" represents 98 points and less than 95 points (applicable) ^ Using glass substrate for fine grinding), "△" represents 95 points less than 902 (may be used for HD. LCD glass substrate for fine grinding), fine research ^ Table 90 points are not full (cannot be used For Xianxian, use the evaluation of the cleanliness of the glass substrate and the detergency of the abrasive material. ^ Wash and dry first &# and detergency evaluation, in the first slurry,- 31 Slide for microscope observation "Crush in a grinder, dry for 5 minutes at 0 ° C / #, and then immerse it in a container filled with pure water to take out the slide glass. Use it for washing. After ultrasonic cleaning, slide the glass from the container. Then wash it with light! ^ 1 f line f water to obtain the residual particles of the abrasive material of the observation object. Observe the residual on the broken surface of the slide In the table, “〇” is used to represent the cleanliness. Specifically, Tables 1 to 4 are used to describe the residue of the abrasive particles, which is very suitable for 2169-6178-PF (N2) .ptd. 20 200 426 206

2169-6178-PF (N2) .ptd 200426206 V. Description of the invention (13) [Table 1] Honing performance of actinic grinding materials ※ [八 ^ 2) Grinding scratch of each rare earth oxide in treo TREO conversion weight Effective rate conversion weight f Evaluation of weight halo speed (wt%) (wt%) Ce〇2 La2〇3 Pr6〇ll Nd2〇3 4 kinds of combined comparative examples 1 5.3 94.5 65.0 31.0 4.0 < 0.001 100 128 Δ Δ I Example 1 5.2 94.5 65.0 30.99 4.0 0.01 100 152 ◎ 0 Rich Example 2 5.2 94.7 65.0 30.9 4.0 0.1 100 145 ◎ 0 冨 Example 3 5.2 94.5 65.0 30.5 4.0 0.5 100 138 (〇) 0 冨 Example 4 5.2 94.5 65.0 30.0 4.0 1.0 100 132 @ 0 Example 5 5.2 94.3 65.0 28.0 4.0 3.0 100 121 0 0 Comparative Example 2 5.1 94.4 65.0 25.0 4.0 6.0 100 103 Δ Δ Comparative Example 3 4.9 94.1 65.0 21.0 4.0 10.0 100 100 Δ Δ Example 3 52 94.5 65.0 30.5 4.0 0.5 100 138 ◎ 0 Example 6 5.2 94.4 65.0 29.5 4.0 0.5 99.0 134 0 Example 7 5.2 94.5 65.0 28.5 4.0 0.5 98.0 129 0 Example 8 5.2 94.3 65.0 26.5 4.0 0.5 96.0 118 0 0 Example 9 5.8 93.9 40.0 47.0 12.0 1.0 100 120 0 0 I Example 4 5.2 94.5 65.0 30.0 4.0 1.0 100 132 @ 0 I Example 10 4.3 95.1 80.0 15.0 4.0 1.0 100 147 (S) 0 霣 Example U 2.5 97.0 95.0 3.0 1.0 1.0 100 135 0 Δ Rich Example 5 5.2 943 65.0 28.0 4.0 3.0 100 121 0 0 Comparative Example 4 52 94.0 65.0 32.0 0 3.0 100 104 Δ Δ ※ Work) The proportion of the weight of fluorine element to the weight of the abrasive material. * The ratio of TREO conversion weight cypress to the weight of honing material is shown in Table 1. Examples 1 to 5 Different from the abrasives of Comparative Examples 1 to 3

2169-6178-PF (N2) .ptd Page 22 200426206 V. Description of the invention (14) The weight ratio of oxidized convergence (%) in TRE0 is different. Among them, each > 1 to 5 abrasives has a high grinding speed and is difficult to be subjected to grinding scraping. In contrast, the abrasives of Comparative Example 丨 without oxidative convergence were ground. Although the abrasives of Comparative Examples 2 and 3 of σσ are 7 ^, the grinding speed is low, and abrasive scratches are liable to occur. From these results, it is known that in the actinide-based abrasive material, oxidation = weight ratio of TRE0 (Nd203 / TRE0) is preferably 0.001% by weight. As for the polishing rate, when comparing the examples, it can be seen that the weight ratio of oxidative convergence in tre0 is preferably 2% by weight or less, more preferably 5% by weight, and more preferably 0.1% by weight or less. In addition, the abrasives of Examples 6 to 8 include four kinds of oxides, "Ce02", lanthanum oxide (La2O3), osmium oxide, and "(n), and the total weight of Tn0 accounts for 100% of TRE0. It is less than or equal to wt%, and the value of the example in each example is not the same. From Examples 1 to δ including these examples, it can be seen that the ratio of the total right weight $ is 96% by weight. The grinding speed can also prevent the occurrence of grinding scratches. If the total content rate is f 97% by weight or more, a higher grinding speed can be ensured and the occurrence of grinding scratches can be more surely prevented. In Example 10, not only the ratio of oxidation to TREO (Nd2 03 / TRE0) is a suitable value, but also Ce02 / TRE0, La2〇3 / TRE0, and P1Ά / TRE0 are suitable values. The grinding speed is high, almost No abrasive scratch occurred 'and no residual abrasive was observed. In contrast, Example 9 and Example 11' Nd2 03 / TRE0 are appropriate values, but Ce02 / TRE0,

At least one of La2 03 / TRE0, Pr6〇u / TRE〇 is not an appropriate value, the grinding speed is p. 23 See 2169-6178-PF (N2) .ptd 200426206

Degree, abrasive scratch, and detergency. i " Huanxian μμM Η η is superior to Examples 4 and Examples. Grinding = the reason that the value of the person is nr ^ He3 has fins, Pr60u / TRE0 is not the reason for the mouth value, and the grinding performance is worse than that of Example 5. 6 u According to the fluorine in the actinide-based grinding material and its molar amount (m0l / L), tube seven actinides; ^ 0 #The above-mentioned mother 1 kg of abrasive material and actinide contain JII. Fluorine content and lanthanum osmium ytterbium; 2 (La + Po). The calculated values are as shown in Table 2. Two / = two V "j and the sacrificial abrasive material of the comparative example ^ ^

Ce02 / TRE0 is 65% by weight, La2 03 / TRE0 is 30.9% by weight,

Pr60n / TRE0 is 4.0% by weight, and Nd203 / TRE0 is 0.1% by weight. [Table 2] The molar amount of honing material per 1kg of honing material. Molar ratio. Surface energy (mol / k). Fluorine-containing meal is to be avoided. F La Pr Nd La / Pr Nd / Pr F / La Ten Pr Honing Scratch Washing Efficiency Conversion Weight Speed Evaluation Net (wt%) (wt%) Comparative Example 5 < 0.001 99,8 < 0.005 1, 89 0,234 0,006 8.09 0.03 < 0.001 35 〇X Example 12 1.2 98.4 0,63 1,87 0,231 0,006 8.08 0.03 0.30 123 ◎ 0 Bao Shi 2 5.1 94.7 2.68 1,80 0,223 0.006 8,05 0.03 1.33 145 ◎ 0 Example 13 8,4 91,0 4.42 1.73 0.214 0,005 8.07 0.03 2.28 163 〇0 Comparative Example δ 12.5 87.9 6,58 1,67 0,207 0,005 8.05 0.03 3.51 166 X △ ※ "Fluorine element pets account for the proportion of the weight of honing materials ※ The ratio of the weight of Ding REO g to the weight of the honing material is shown in Table 2. For the abrasive materials of Examples 2, 1, 2, 13 and Comparative Examples 5 and 6, the fluorine content in each abrasive material is different. Among them, the abrasive materials of Examples 2, 1, 2, and 13 had high grinding speed, and it was difficult for grinding scratches to occur.

2169-6178-PF (N2) .ptd Page 24 200426206 V. Description of the invention (16) _ —--- 2 lifespan In contrast, the abrasive of Comparative Example 5 which contains almost no fluorine, was polished: significantly reduced. In the abrasive of Comparative Example 6, which has a high fluorine content, the grinding speed is stomach, but abrasive scratches easily occur. From these results, we can see that starting from the two aspects of degree and grinding scratch, the higher the effect is, the more white and the better the ratio is 2% to 7% by weight. The molar ratio (F / (La + Pr)) of the content ratio of fluorine to the total content ratio of lanthanum and copper is preferably 0.2 to 3. In the second embodiment, the first embodiment of the present invention will be described using a raw material different from that in the first embodiment to produce a milled grinding material of the present invention. ^ First, ‘prepared rare earth carbonate (produced in China) based on rhenium. Among the rare earth carbonates, TRE0 is 52.3% by weight, Ce02 / TRE0 is 52.1%, La203 / TRE0 is 26.7%, Pr60u / TRE0 is 7.2%,

Nd203 / TREO is 13.0%. In Examples 14 to 17 and Comparative Example 7 of this embodiment (see Tables 3 and 4 below), Comparative Example 7 directly used the rare earth carbonate as a raw material. Further, in Examples 14 to 17 and Comparative Examples 8 to 10, the rare earth carbonate was dissolved with hydrochloric acid, and the obtained carbonate solution was separated and purified by a solvent extraction method to obtain a lanthanum-reduced rare earth solution (refined solution). ), The obtained rare-earth solution is mixed with an aqueous ammonium bicarbonate solution (precipitant) to generate a precipitate of the rare-earth carbonate, and then filtered and washed with a centrifuge to obtain a rare-earth carbonate (Nd2 03 / TRE0) as a raw material. Department 0.1% ~ 6.3% by weight). Here, the solvent% in this embodiment will be described.该 solve extract

2169-6178-PF (N2) .Ptd

200426206 V. Description of the invention (17) As the organic solvent, extractant (pC-88A • • Big Eight = manufactured) and diluent (eupsol extractive petrochemical dagger: extraction agent / diluent) 1 / The ratio of 2 is equal to the ratio of the ratio of the ratio of Lib (carbonate solution (^ EG24Gg / L) to the flow ratio (organic bath solution) of 8/1. Into an organic solvent. At this time, the lanthanum of Example 16 is left in an aqueous solution. And the other examples and ratios are: = almost all extracted into the organic solvent. The adjustment of the extraction is =. After that, the organic solvent containing rare earth elements is dissolved; = the solution is countercurrently contacted in multiple stages (3. stage), and the concentration and comparison are compared; the rare earth elements in the organic solvent (thorium to heavy rare earth and concubine are taken to; In an organic solvent, extract most of the lanthanum, brocade, and cans and a part of the tank into an aqueous solution of hydrochloric acid to obtain a refined solution. 1 knife + change the flow rate of the aqueous solution of hydrochloric acid to perform (organic, (3) The flow rate of gluant is constant.) Use the same steps as in the first embodiment. The obtained salt metaphosphate was made into a decorative abrasive material. From the above description, it can be seen that the raw material of the second solid & The ratio is low. In the second embodiment, pure water is mixed with the raw material twice the weight of the raw material to obtain the mixture; the mixture is pulverized by grinding to obtain a slurry. The full-grinding time of the grinder is 10 small days. : In the fluorinated virgin li with 10% hydrofluoric acid added to the slurry obtained by the wet pulverization, the slurry was made so that the fluorine component (F / (TR foot)) in # was 7%. No. 2169-6178-PF (N2) .ptd Page 26 200426206 V. Description of the Invention (18) 17 and 18 and Comparative Examples 9 and 10 are the same as the first embodiment at 95 ° C. The calcination temperature was 6500 ° C in Comparative Example 9, 7750 ° C in Example 1 and 7100 ° C in Example 1 and 1800 ° C in Example 1 and 120 ° C in Comparative Example 10. The manufacturing conditions of the other abrasive materials are the same as those of the first embodiment. Therefore, the description of the manufacturing steps of the abrasive materials is omitted here. [Table 3] Honing performance of the 钸 series abrasive materials ^ TREO T Grinding and scratching of each rare earth oxide in the RE0-converted amount of the child contains the converted ratio of children's maggots (wt%). Continuity evaluation rate Zhang Jing Ce〇2 La2〇3 Pr5〇ll Nd2〇3 (wt%) (wl% ) Total Comparative Example 7 6.5 92.0 52.1 26.7 7.2 13.0 99.0 95 Δ Δ Comparative Example 8 63 92.5 58.5 30.2 4.5 63 99.5 " 7〇2 △ △ Example W 6.4 92.6 60.4 31.5 3.6 4.2 99.Γ 120 〇〇 Rich Example 15 6.1 93.0 63.7 33.6 2.3 0.2 99.8 131 ◎ 〇 霣 Example 16 5.7 93.3 79.5 19.6 0.7 0.1 99.9 142 Γ \ ※ 丄) The proportion of the weight of fluorine element to the weight of honing material— ^ ^ 1 ^ 2) TREO exchange fThe ratio of the amount of the child to the weight of the abrasive

Although Nd ^ / TREO exceeds 5%, the abrasives of Examples 14 to 16 in which secondary production and j were reduced by solvent extraction (Nd ^ / TREO is less than 5%), and Xing Nu Chen Gu Beishi Moon Dagger. In contrast, Comparative Example 7, Nd2 03 / TRE0 exceeding 5%, sm

. ^ ^ 7T material, compared with the grinding material of the examples, the grinding speed and scraping properties are poor. ”Sweat and buckle and wash. For the actinide-based abrasive material manufactured, J, > 0-ray λ-ray peak 200426206 was measured.

V. Description of the invention (19) Intensity, average particle size (D 50 pore volume measurement line diffraction surveying, X-ray diffraction device (made by MaCScience Co., Ltd.), X-ray diffraction analysis, measuring the peak intensity of diffraction 1 ray. In this measurement, a copper (Cu) target is used to diffract the diffraction in a pattern of diffraction 1 ray (the line ⑸-κ obtained by irradiating the ⑸-κ α line). The angle of incidence (2 peaks within 20deg ~ 30deg is analyzed. Other measurement conditions are tube voltage 40kv, tube current 150mA, measurement range 2 0 = 5 ~ 80 °, sample width 〇 · 〇2ά ^ δ The scanning speed is 4 deg / min. Further, the X-ray peak intensity of fluoridated oxide with respect to thorium oxide (je〇2), which is read from the X-ray diffraction measurement results of the samarium-based abrasives of each of the examples and comparative examples, is fluoridated The X-ray peak intensities of lanthanum (La〇F) and the X-ray peak intensities of lanthanum fluoride (LAFS) are shown in Table 4.) (Made by Shimadzu Corporation: SALD-20 0 0A), the particle size distribution of the actinide-based abrasive material is measured, and the average particle size ((DS ( ): The cumulative volume from the side of the small particle size is 50% of the particle size control.) Jg, the measurement of the volume of the hole i. The pore volume measurement device (C0ULTER SA3100) is used to measure the pore volume of the 研磨 series abrasive material. Page 2169 -6178-PF (N2) .ptd 200426206 V. Description of the invention (20) [袠 4] X-ray peak mmm of 钸 series abrasive material Grinding performance ~ intensity ratio wind m) 〇The average particle size of each rare earth LaOF LaF3 in the conversion of the amount Grinding scratches Contamination ratio containing TREO oxides / Ce〇2 / Ce〇2 Diameter (Dso) Volumetric Connectivity Evaluation Net Rate Conversion (wt%) (m only) (m3 / g) Properties (wt%) Weight Ce〇2 La2〇3 PreOn Nd2 03 (wt%) ratio g Example 9 6.7 93.0 63.7 33.6 2.3 02 0.02 0.05 0.47 0.132 25 Δ X Example 17 6.4 93.0 63.7 33.6 2.3 02 0.15 < 0.01 0.69 0.092 115 0. Example 15 6.1 93.0 63.7 33.6 2.3 0.2 0.27 < 0.01 0.97 0.047 131 © 〇 " Example 18 5.7 93.0 63.7 33.6 2.3 0.2 0.43 < 0.01 1.27 0.0055 155 0 6 Comparative Example 10 5.2 93.0 63.7 33.6 2.3 02 0.72 < 0.01 2.05 0.0009 163 X 0 · ---- ※ 丄) Fluorine The ratio of the child's weight to the weight of the abrasive material 2) The ratio of TREO conversion weight cypress to the weight of the abrasive material In the abrasive materials of the examples and comparative examples shown in Table 4, the intensity ratio of the X-ray peak intensity (LaOF / Ce〇2) The polishing material of the examples in the range of 0.05 to 0.6 has a good polishing speed, and abrasion scratches are unlikely to occur. In contrast, in the abrasive material of Comparative Example 9 having a small strength ratio (LaOF / Ce02), the polishing rate was significantly reduced, and polishing scratches occurred. In Comparative Example 丨 0, which has a large strength ratio, although the grinding speed was high, it was obvious that scratches occurred. From this result, it is understood that the grinding material having an intensity ratio (LaOF / Ce〇2) of X-ray peak intensity in the range of 0.05 to 0.6 is preferable. The abrasive material of the example having a pore volume of 0.002 cm3 / g to 0.005 cmVg has a high polishing speed, and abrasion scratches are unlikely to occur, which is good. versus

2169-6178-PF (N2) .ptd Page 29 200426206 V. Description of the invention (21) In contrast, the abrasive of Comparative Example 9 with a large pore volume has a significantly reduced grinding speed. In the abrasive material of Comparative Example 10 having a small pore volume, scratches occurred. From this result, it is understood that the pore volume is preferably an abrasive material of 0.002 cm3 / g to 0.1 cm3 / g. Industrial Applicability The abrasive material of the brocade of the present invention has fewer injuries. If this surface is used, the polishing can be completed in a shorter time than with the conventional brocade. And it can happen. Therefore, it is very suitable for applications such as surface polishing of precision parts. ’Its grinding speed is higher, and it can be used to more accurately suppress the grinding surface, electronic equipment, or these when compared to the case of grinding materials such as glass and grinding materials by grinding scrapers and abrasives |

200426206 Schematic description

2169-6178-PF (N2) .ptd Page 31

Claims (1)

200426206 6. Scope of patent application 1. A samarium-based abrasive material. In addition to fluorine, rare earth elements contain at least europium (Ce), lanthanum (La), praseodymium (Pr), and (Nd). The composition is characterized in that the weight ratio (Nd2O3 / TRE0) of the chemical conversion to the total rare earth oxide conversion (TRE0) is in the range of 0.001 to 2. 2. As in the scope of the patent application The ratio of the total weight of the rare earth oxides of the above-mentioned rhenium-based abrasive materials to the total weight of the rare earth oxides is more than 97% by weight. "3", as described in ## Abrasive material in the scope of the patent application, in the bean, the worms account for 80% by weight of the total rare earth oxide equivalent weight (Ce02 / TRE0), 50% by weight, and the oxide steel accounts for The weight ratio of the total soil conversion weight (La203 / T_ osmium oxide dioxide accounts for 45% of the total rare earth oxide conversion weight, and (PhOn / TREO) is 0.1% to 10% by weight. Example 4. Such as Items No. 专利, No. 2 or No. 3 in the scope of patent application, in which 'fluorine content rate is 05% by weight to ι〇 Weight: decorative abrasive material 5 · As in No. 1, 2, and 3 ° of the scope of patent application, which contains Fluorine (F), and the right-containing fluorene-based abrasive material (F / (La + Pr)) is 0.2 ~ 3 mills, * and P (Pr) in the right. Ranges 1, 2, 3, and 4 type r-milling materials, in which X-ray diffraction is used to measure X-ray sound sores α 1 using Cu-Kα rays or Cu-Kα lines as described in X-ray diffraction as an X-ray source , Angle), in the range of deg ·, the strongest and strongest X-ray peak intensities appear, and the most intense X-ray peak intensities of porphyrites and x-ray peaks are shown in page 32. 178-PF (N2) .ptd 200426206 6. The ratio of the intensity of X-ray peak intensity (rare-type fluorine oxide / hafnium oxide) with strong patent application range is 0 · 0 5 ~ 0 · 6 〇7. The actinide-based abrasive material according to item 1, 2, 3, 4, 5, or 6, wherein the pore volume is from 0 0 2 c m3 / g to 0 · 1 c m3 / g. 2169-6178-PF (N2) .ptd p. 33 200426206 2169-6178-PF (N2) .ptd Page 8