CN1136565C - A method for manufacturing a magneto-optical disk recording medium target - Google Patents
A method for manufacturing a magneto-optical disk recording medium target Download PDFInfo
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- CN1136565C CN1136565C CNB981119964A CN98111996A CN1136565C CN 1136565 C CN1136565 C CN 1136565C CN B981119964 A CNB981119964 A CN B981119964A CN 98111996 A CN98111996 A CN 98111996A CN 1136565 C CN1136565 C CN 1136565C
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- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title abstract description 8
- 239000000956 alloy Substances 0.000 claims abstract description 36
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 35
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 5
- 239000010959 steel Substances 0.000 claims abstract description 5
- 238000010894 electron beam technology Methods 0.000 claims abstract description 4
- 238000003466 welding Methods 0.000 claims abstract description 4
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 3
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 10
- 150000002910 rare earth metals Chemical group 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 230000007704 transition Effects 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 238000009694 cold isostatic pressing Methods 0.000 claims description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims 2
- 238000003723 Smelting Methods 0.000 abstract description 16
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000013077 target material Substances 0.000 abstract description 4
- 238000001513 hot isostatic pressing Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000000462 isostatic pressing Methods 0.000 abstract description 2
- 239000010453 quartz Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005477 sputtering target Methods 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 238000003754 machining Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 241001062472 Stokellia anisodon Species 0.000 description 2
- DVZWMWMGZSBXML-UHFFFAOYSA-N [Co].[Fe].[Tb].[Gd] Chemical compound [Co].[Fe].[Tb].[Gd] DVZWMWMGZSBXML-UHFFFAOYSA-N 0.000 description 2
- FOPBMNGISYSNED-UHFFFAOYSA-N [Fe].[Co].[Tb] Chemical compound [Fe].[Co].[Tb] FOPBMNGISYSNED-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 description 1
- ZDHFLALWDIPABU-UHFFFAOYSA-N cobalt dysprosium iron terbium Chemical compound [Co][Fe][Dy][Tb] ZDHFLALWDIPABU-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- HQWUQSSKOBTIHZ-UHFFFAOYSA-N gadolinium terbium Chemical compound [Gd][Tb] HQWUQSSKOBTIHZ-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- -1 rare earth transition metal Chemical class 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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Abstract
本发明提供了一种磁光盘记录介质靶材制备方法，属于合金冶炼技术领域，其特点在于使用磁力搅拌悬浮熔炼技术熔炼合金，靶材等静压成型模具由定位钢圈，定位板和橡胶压板组成，并由螺栓紧固密封，热等静压烧结包套用真空电子束焊接密封，可有效地解决已有技术中合金熔炼时的材料污染，成份均匀性不易控制等问题，主要用于制造磁光盘记录介质。
The present invention provides a method for preparing a target material for a magneto-optical disc recording medium, and belongs to the technical field of alloy smelting. The method is characterized in that the alloy is smelted by a magnetic stirring suspension smelting technology, the target material isostatic pressing forming die is composed of a positioning steel ring, a positioning plate and a rubber pressing plate, and is fastened and sealed by bolts, and the hot isostatic pressing sintering package is sealed by vacuum electron beam welding, which can effectively solve the problems of material pollution during alloy smelting and difficulty in controlling component uniformity in the prior art, and is mainly used for manufacturing magneto-optical disc recording media.
Description
本发明涉及合金冶炼技术领域，特别涉及稀土族与过渡族元素的混合冶炼The invention relates to the technical field of alloy smelting, in particular to the mixed smelting of rare earth and transition elements
技术领域。technology field.
目前制造磁光盘记录介质合金靶材的方法主要有铸造法和粉末冶金法。前者将一定成份配比的合金原料熔炼，再将合金熔液浇注于模具中，形成铸锭，最后经机械加工制成靶材；后者则是首先将一定成份配比的合金原料熔炼，浇注成锭后再粉碎，将粉碎形成的粉末经等静压成形，再高温烧结，最终制成靶材。还有一种方法是将过渡族金属粉末(或泡沫状薄片)与事先炼好的稀土族过渡合金锭放入铸模内，在过渡金属熔点与合金铸锭熔点之间的某一温度对材料及锭模加热，最后再对成形体进行冷加工制成靶材。熔炼磁光盘用稀土过渡族金属合金材料的方法有电炉熔炼和石英管真空保护熔炼等。所谓电炉熔炼是指将装有合金原料的坩埚放入熔炼电炉中，再对坩埚和炉膛抽真空或抽真空后充入惰性气体，随后加热熔化合金，再将合金熔液倒入浇注模具中；所谓真空石英管真空保护熔炼是指将合金原料放入石英管中，再对石英管抽真空后密封，加热至一定温度将合金熔化，在熔炼过程中不断转动石英管，待冷却后打碎石英管。上述方法存在的主要问题是前者很易造成坩埚材料的污染，且成份及其均匀性不易控制，后者也难以均匀化成份且成本高，效率低。At present, the methods for manufacturing alloy targets for magneto-optical disk recording media mainly include casting method and powder metallurgy method. The former melts the alloy raw materials with a certain composition ratio, and then pours the alloy melt into the mold to form an ingot, and finally makes the target through machining; the latter first melts the alloy raw materials with a certain composition ratio, pours After forming an ingot, it is crushed, and the powder formed by crushing is formed by isostatic pressing, and then sintered at a high temperature to finally be made into a target. Another method is to put the transition metal powder (or foam flake) and the pre-smelted rare earth transition alloy ingot into the mold, at a certain temperature between the melting point of the transition metal and the melting point of the alloy ingot. The mold is heated, and finally the formed body is cold-processed to make a target. The methods of smelting rare earth transition metal alloy materials for magneto-optical discs include electric furnace smelting and quartz tube vacuum protection smelting. The so-called electric furnace smelting refers to putting the crucible containing the alloy raw material into the melting electric furnace, then vacuuming the crucible and the furnace or filling it with an inert gas, then heating and melting the alloy, and then pouring the alloy melt into the casting mold; The so-called vacuum protection smelting of vacuum quartz tube refers to put the alloy raw material into the quartz tube, then vacuumize the quartz tube and seal it, heat it to a certain temperature to melt the alloy, continuously rotate the quartz tube during the smelting process, and break the quartz after cooling Tube. The main problem of the above method is that the former is easy to cause pollution of the crucible material, and the composition and its uniformity are not easy to control, and the latter is also difficult to homogenize the composition and has high cost and low efficiency.
本发明的目的是提供一种磁光盘记录介质靶材制备方法，它能有效地解决电炉熔炼和石英管真空保护熔炼所导致的合金中成份不均匀问题。The object of the present invention is to provide a method for preparing a magneto-optical recording medium target, which can effectively solve the problem of uneven composition in the alloy caused by electric furnace smelting and quartz tube vacuum protection smelting.
本发明的目的可以由以下技术方案实现：The purpose of the present invention can be achieved by the following technical solutions:
(1)靶材所使用的原料包括稀土族金属和过渡族金属。稀土族金属指重稀土族铽(Tb)、镝(Dy)、钆(Gd)等元素中的至少一种元素或轻稀土族金属如钕(Nd)、钐(Sm)等元素中的至少一种元素；过渡族金属指如铁(Fe)、钴(Co)、铬(Cr)等元素中的至少一种元素。(1) The raw materials used in the target include rare earth metals and transition metals. Rare earth metals refer to at least one element of heavy rare earth terbium (Tb), dysprosium (Dy), gadolinium (Gd) and other elements or at least one of light rare earth metals such as neodymium (Nd) and samarium (Sm) Elements; transition group metals refer to at least one element in elements such as iron (Fe), cobalt (Co), and chromium (Cr).
(2)制造过程中将上述稀土族和过渡族单金属原料或预先炼制的中间合金按设计重量称好放入磁力搅拌悬浮熔炼炉的水冷坩埚中进行感应加热悬浮熔炼，熔炼过程中借助磁场作用对熔体进行搅拌，从而使合金成份更加均匀。(2) During the manufacturing process, the above-mentioned rare earth and transition group single metal raw materials or pre-refined master alloys are weighed according to the design weight and put into the water-cooled crucible of the magnetic stirring suspension melting furnace for induction heating and suspension melting. During the melting process, the magnetic field is used The effect is to stir the melt, so that the alloy composition is more uniform.
(3)制造过程中将合金锭粉碎，球磨制粉，合金粉末的颗粒直径在0.5-400μm之间。(3) During the manufacturing process, the alloy ingot is pulverized and ball milled to make powder, and the particle diameter of the alloy powder is between 0.5-400 μm.
(4)制造过程中将合金粉末放入模具中进行冷压成型。使用冷等静压技术成型时，成型模具由内壁为锥台形的定位钢圈、定位板和橡胶压板组成，使用螺栓紧固密封，以防渗油。(4) During the manufacturing process, the alloy powder is put into a mold for cold pressing. When using cold isostatic pressing technology to form, the forming mold is composed of a truncated cone-shaped positioning steel ring, a positioning plate and a rubber pressure plate, which are tightly sealed with bolts to prevent oil leakage.
(5)制造过程中对冷压成型体进行高温烧结，烧结环境应是真空或惰性气体。(5) During the manufacturing process, the cold-pressed body is sintered at high temperature, and the sintering environment should be vacuum or inert gas.
(6)制造过程中对冷压成型体进行高温热等静压烧结，这时烧结包套应使用真空电子束焊接技术对包套进行密封。(6) During the manufacturing process, the cold-pressed molded body is subjected to high-temperature hot isostatic pressing sintering. At this time, the sintered sheath should be sealed by vacuum electron beam welding technology.
与现有技术相比本发明的效果和优点在于：可有效地解决已有技术中合金熔炼时的材料污染，成份均匀性不易控制等问题，从而可获得均匀而高纯度的合金，且能提高效率，降低成本。Compared with the prior art, the effect and advantage of the present invention are: it can effectively solve the problems of material pollution during alloy smelting in the prior art, and difficult control of composition uniformity, thereby obtaining a uniform and high-purity alloy, and improving Efficiency and cost reduction.
本发明附图说明如下：图1为本发明模具剖视图图2为本发明模具上定位板俯视图The accompanying drawings of the present invention are as follows: Fig. 1 is a sectional view of the mold of the present invention Fig. 2 is a top view of the upper positioning plate of the mold of the present invention
本发明实施例如下：Embodiments of the present invention are as follows:
实施例1(铽—铁—钴溅射靶)：Embodiment 1 (terbium-iron-cobalt sputtering target):
(1)配制按重量百分比为铽23％—铁68％—钴9％的具有足够高纯度的单金属原料；称量铽时应考虑熔炼时的烧损量。(1) Prepare monometallic raw materials with sufficient high purity of terbium 23%-iron 68%-cobalt 9% by weight percentage; the burning loss during smelting should be considered when weighing terbium.
(2)将金属原料放入悬浮熔炼炉坩埚中，对坩埚抽真空，再充入纯度为99999.5％氩气，之后进行熔炼，熔炼后的合金锭为半圆形。(2) Put the metal raw material into the crucible of the suspension melting furnace, evacuate the crucible, and then fill it with argon gas with a purity of 99999.5%, and then smelt it. The smelted alloy ingot is semicircular.
(3)在真空环境下粉碎合金锭，然后放入球磨机中研磨，获得粒度为0.5-400μm的粉末。(3) Pulverize the alloy ingot in a vacuum environment, and then grind it in a ball mill to obtain a powder with a particle size of 0.5-400 μm.
(4)将粉末放入模具中，模具内径尺寸为115～120mm，利用定位钢圈5及橡胶压板4(6)定位板3(7)并使用螺栓2紧固密封，通过抽气孔1抽真空后在冷等静压机中冷压成型并利用机械使用成型体出模。(4) Put the powder into the mold, the inner diameter of the mold is 115 ~ 120mm, use the
(5)将冷压成型体在真空烧结炉中进行高温真空烧结。(5) Carry out high-temperature vacuum sintering of the cold-pressed molded body in a vacuum sintering furnace.
(6)对烧结后的成型体进行机械加工，获得直径约115mm厚度5mm的铽—铁—钴溅射靶材。(6) Machining the sintered molded body to obtain a terbium-iron-cobalt sputtering target with a diameter of about 115 mm and a thickness of 5 mm.
(7)将靶材进行真空塑料封装。(7) The target material is vacuum plastic packaged.
实施例2(铽—钆—铁—钴溅射靶)：Embodiment 2 (terbium-gadolinium-iron-cobalt sputtering target):
(1)配制按重量百分比为铽17％—钆8％—铁67％—钴9％的铽—钆—铁—钴的具有足够高纯度的单金属原料；称量铽和钆时应考虑熔炼时的烧损量。(1) Preparation of terbium-gadolinium-iron-cobalt single metal raw material with sufficient high purity of 17% terbium-gadolinium 8%-iron 67%-cobalt 9% by weight percentage; smelting should be considered when weighing terbium and gadolinium The amount of burning loss at the time.
(2)将金属原料放入悬浮熔炼炉坩埚中，对坩埚抽真空，再充入纯度为99999.5％的氩气之后进行熔炼，熔炼后的合金锭为半圆形。(2) Put the metal raw material into the crucible of the suspension melting furnace, evacuate the crucible, fill it with argon gas with a purity of 99999.5%, and then smelt it. The smelted alloy ingot is semicircular.
(3)在真空环境下粉碎合金锭，然后放入球磨机研磨，获得粒度为0.5-400μm的粉末。(3) Pulverizing the alloy ingot in a vacuum environment, and then putting it into a ball mill for grinding to obtain a powder with a particle size of 0.5-400 μm.
(4)将粉末放入模具中，模具内径尺寸为115～120mm，利用橡胶压板4(6)定位板3(7)并使用螺栓2紧固密封，通过抽气孔1抽真空后在冷等静压机中冷压成型并利用机械使用成型体出模。(4) Put the powder into the mold, the inner diameter of the mold is 115-120mm, use the rubber pressure plate 4 (6) and the positioning plate 3 (7) and use the
(5)使用厚度为0.1-0.20mm的不锈钢板作冷压成型体烧结包套，在真空电子束焊机中对冷压成型体包套进行焊接密封。(5) A stainless steel plate with a thickness of 0.1-0.20mm is used as the sintered sheath of the cold-pressed molded body, and the sheath of the cold-pressed molded body is welded and sealed in a vacuum electron beam welding machine.
(6)将冷压成型体在热等静压烧结炉中进行高温烧结。(6) The cold-pressed molded body is sintered at a high temperature in a hot isostatic pressing sintering furnace.
(7)对烧结后成型体进行机械加工，获得直径约115mm厚度5mm的铽—镝—铁—钴溅射靶材，靶材成份按重量百分比大致为铽17％—镝8％—铁67％—钴8％。(7) Machining the sintered molded body to obtain a terbium-dysprosium-iron-cobalt sputtering target with a diameter of about 115mm and a thickness of 5mm. The target composition is roughly 17% terbium-8% dysprosium-67% iron - Cobalt 8%.
(8)将靶材进行真空塑料封装。(8) The target material is vacuum plastic packaged.
Claims (5)
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| Application Number | Priority Date | Filing Date | Title |
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| CNB981119964A CN1136565C (en) | 1998-05-06 | 1998-05-06 | A method for manufacturing a magneto-optical disk recording medium target |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB981119964A CN1136565C (en) | 1998-05-06 | 1998-05-06 | A method for manufacturing a magneto-optical disk recording medium target |
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| CN1234580A CN1234580A (en) | 1999-11-10 |
| CN1136565C true CN1136565C (en) | 2004-01-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745974B (en) * | 2008-12-17 | 2011-12-14 | 北京有色金属研究总院 | Method for directly preparing high temperature superconductive flat pre-sintered target blank by isostatic pressing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100445417C (en) * | 2006-12-27 | 2008-12-24 | 湖南中精伦金属材料有限公司 | Production method of cobalt base alloy target for vertical magnetic recording medium soft magnetization bottom |
| JP4678062B2 (en) | 2008-09-22 | 2011-04-27 | Ｔｄｋ株式会社 | Optical media and manufacturing method thereof |
| CN106591790B (en) * | 2016-12-28 | 2019-12-13 | 杭州大立微电子有限公司 | Target material preparation method and getter film forming method |
| CN110256080A (en) * | 2019-06-28 | 2019-09-20 | 先导薄膜材料（广东）有限公司 | Indium selenide target prepares mold and preparation method |
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1998
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745974B (en) * | 2008-12-17 | 2011-12-14 | 北京有色金属研究总院 | Method for directly preparing high temperature superconductive flat pre-sintered target blank by isostatic pressing method |
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| CN1234580A (en) | 1999-11-10 |
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