CN106282945A - A kind of preparation method of ultra-pure aluminum target - Google Patents

A kind of preparation method of ultra-pure aluminum target Download PDF

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Publication number
CN106282945A
CN106282945A CN201610846416.4A CN201610846416A CN106282945A CN 106282945 A CN106282945 A CN 106282945A CN 201610846416 A CN201610846416 A CN 201610846416A CN 106282945 A CN106282945 A CN 106282945A
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China
Prior art keywords
ultra
pure aluminum
ingot casting
preparation
hot rolling
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Granted
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CN201610846416.4A
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CN106282945B (en
Inventor
冉继龙
李谢华
黄瑞银
徐始祥
罗筱雄
陈国生
詹开严
刘华春
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Chinalco Ruimin Co Ltd
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Chinalco Ruimin Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metal Rolling (AREA)

Abstract

The present invention relates to the preparation method of a kind of ultra-pure aluminum target, comprise the following steps: purity is more than the ultra-pure aluminum ingot casting of 99.999wt% and carries out surface milling by (1), removes the oxide layer on surface;(2) ingot casting is heated to 230~400 DEG C;(3) ingot casting after heating carries out the hot rolling of 10 ~ 20 passages, and single pass drafts controls at 20 ~ 60mm, controls the finishing temperature of final pass below 350 DEG C;(4) aluminium sheet completing hot rolling being carried out temperature is 200~300 DEG C, and temperature retention time is the annealing of 1~2h;(5) to carrying out Milling Process after sheet material leveling, it is thus achieved that average crystal grain 80~150um ultra-pure aluminum target.It is high that the present invention can prepare purity, and crystal grain is tiny and uniform target, and texture orientation is consistent, meets the use requirement of PVD;Technique is simple simultaneously, it is easy to operation, it is simple to large-scale industrial production, effectively reduces energy consumption, reduces cost.

Description

A kind of preparation method of ultra-pure aluminum target
Technical field
The present invention relates to a kind of metal material processing technology, the preparation method of specific design a kind of ultra-pure aluminum target.
Background technology
TFT-LCD (Thin film transistor-Liquid crystal display) tft liquid crystal shows Show device, be commonly called as liquid crystal panel, be widely used in the various products such as mobile phone, display, television set.TFT-LCD produces and closes most The technique of key is physical vapor deposition (PVD), and PVD splash-proofing sputtering metal boots material is that semiconductor chip produces and TFT-LCD prepares and adds One of most important raw material during work.
The technique of target as sputter deposition thin film is the common method producing function film, and sputtering method is to use high-energy ion bombardment Target material surface, makes the atom of target material surface or molecular jet at substrate surface, forms the process of one layer of dense film.Splash-proofing sputtering metal What in target, consumption was maximum is ultra-pure aluminum and the pure alloy of superelevation.Rafifinal target (ultra-pure aluminum of 5N~6N), purity > 99.999%, product specification exists: 12~20mmx180~1731mmx1700~2650mm, and added value of product is high, but production difficulty Greatly, in addition to purity requirement, crystallite dimension, the crystal grain uniformity and texture orientation etc. being had strict demand, crystallite dimension is general Require within 200um.
Rafifinal target preparation method currently mainly has: (1) equal channel angular hubbing (Equal Channel Angular Drawing is called for short ECAD), (2) multiway forging method (Multiple Forging is called for short MF), (3) rolling, Front 2 kinds of processing methods can only process undersized target, for large-size target, such as 1950x1580x14mm and 2650*210* The target of 18.3mm specification, can only use rolling to produce.
Summary of the invention
In view of this, it is an object of the invention to provide the preparation method of a kind of ultra-pure aluminum target, crystal grain can be prepared thin Little and uniform target, meets PVD and uses requirement.
The present invention uses below scheme to realize: the preparation method of a kind of ultra-pure aluminum target, comprises the following steps: (1) will The purity ultra-pure aluminum ingot casting more than 99.999wt% carries out surface milling, removes the oxide layer on surface;(2) ingot casting is heated to 230~400 DEG C;(3) ingot casting after heating carries out the hot rolling of 10 ~ 20 passages, and single pass drafts controls at 20 ~ 60mm, control The finishing temperature of final pass processed is below 350 DEG C;(4) aluminium sheet completing hot rolling being carried out temperature is 200~300 DEG C, insulation Time is the annealing of 1~2h;(5) to carrying out Milling Process after sheet material leveling, it is thus achieved that average crystal grain 80~150um super Rafifinal target.
Further, in step (1), milling amount is not less than 3mm.
Further, step (2) use pushing type heating furnace ingot casting is heated;Step (3) uses reversible Hot-rolling mill carries out hot rolling to ingot casting.
Further, in step (3) in the hot rolling, sheet material single track is controlled by control deflection and cooling emulsion Secondary hot-rolled temperature is changed to 3 ~ 8 DEG C.
Compared with prior art, the method have the advantages that the present invention may be used to prepare large-size target, preparation The target purity gone out is high, and crystal grain is tiny and uniform, and texture orientation is consistent, meets the use requirement of PVD;Technique is simple simultaneously, easily In operation, it is simple to large-scale industrial production, effectively reduce energy consumption, reduce cost.
For making the purpose of the present invention, technical scheme and advantage clearer, below will be by specific embodiment and phase Close accompanying drawing, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the polarisation tissue of the ultra-pure aluminum target that the present invention prepares.
Detailed description of the invention
The preparation method of a kind of ultra-pure aluminum target, comprises the following steps: purity is more than the superelevation of 99.999wt% by (1) Fine aluminium ingot casting carries out surface milling, removes the oxide layer on surface;(2) ingot casting is heated to 230~400 DEG C;(3) by after heating Ingot casting carries out the hot rolling of 10 ~ 20 passages, and single pass drafts controls at 20 ~ 60mm, controls the finishing temperature of final pass 350 Below DEG C;(4) aluminium sheet completing hot rolling being carried out temperature is 200~300 DEG C, and temperature retention time is the annealing of 1~2h;(5) To carrying out Milling Process after sheet material leveling, it is thus achieved that average crystal grain 80~150um ultra-pure aluminum target.
In the present embodiment, in step (1), the ultra-pure aluminum ingot casting of 99.999wt% is by the high purity aluminium casting ingot of 99.9wt% Obtained by three-layer-liquid electrolysis and segregation method production.
In the present embodiment, in step (1), milling amount is not less than 3mm.
In the present embodiment, step (2) use pushing type heating furnace ingot casting is heated;Using in step (3) can Inverse formula hot-rolling mill carries out hot rolling to ingot casting, and concrete hot rolling pass is that the thickness according to aluminium sheet determines.
In the present embodiment, in step (3) in the hot rolling, sheet material is controlled by control deflection and cooling emulsion Single pass hot-rolled temperature is changed to 3 ~ 8 DEG C.
The object, technical solutions and advantages of the present invention are further described by above-listed preferred embodiment, are answered It is understood by, the foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.

Claims (4)

1. the preparation method of a ultra-pure aluminum target, it is characterised in that: comprise the following steps: purity is more than by (1) The ultra-pure aluminum ingot casting of 99.999wt% carries out surface milling, removes the oxide layer on surface;(2) ingot casting is heated to 230~400 ℃;(3) ingot casting after heating carries out the hot rolling of 10 ~ 20 passages, and single pass drafts controls at 20 ~ 60mm, controls last road Secondary finishing temperature is below 350 DEG C;(4) aluminium sheet completing hot rolling being carried out temperature is 200~300 DEG C, temperature retention time be 1~ The annealing of 2h;(5) to carrying out Milling Process after sheet material leveling, it is thus achieved that average crystal grain 80~150um ultra-pure aluminum target Material.
The preparation method of ultra-pure aluminum target the most according to claim 1, it is characterised in that: in step (1), milling amount is not Less than 3mm.
The preparation method of ultra-pure aluminum target the most according to claim 1, it is characterised in that: step (2) uses and advances Ingot casting is heated by formula heating furnace;Step (3) use reversible hot rolling mill ingot casting is carried out hot rolling.
The preparation method of ultra-pure aluminum target the most according to claim 1, it is characterised in that: hot rolled in step (3) Cheng Zhong, controls sheet material single pass hot-rolled temperature be changed to 3 ~ 8 DEG C by controlling deflection and cooling emulsion.
CN201610846416.4A 2016-09-26 2016-09-26 A kind of preparation method of ultra-pure aluminum target Active CN106282945B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106947926A (en) * 2017-04-21 2017-07-14 中铝瑞闽股份有限公司 A kind of preparation method of large scale rafifinal target
CN106987788A (en) * 2017-03-07 2017-07-28 新疆众和股份有限公司 It is a kind of that the hot-working method that 1090 minute surface woollens are provided is rolled for specular aluminium
CN107030108A (en) * 2017-04-21 2017-08-11 中铝瑞闽股份有限公司 A kind of rafifinal target heavy reduction rolling method
CN109174996A (en) * 2018-08-24 2019-01-11 爱发科电子材料(苏州)有限公司 The plate calendering technology of TFT liquid crystal display panel wiring layer rafifinal target
CN110205590A (en) * 2019-05-08 2019-09-06 东莞市欧莱溅射靶材有限公司 A kind of ultra-pure aluminum sputtering target material and its milling method
CN110484874A (en) * 2019-08-16 2019-11-22 韶关市欧莱高新材料有限公司 A kind of preparation method of high-purity aluminum pipe sputtering target material
CN110709532A (en) * 2017-06-22 2020-01-17 株式会社Uacj Sputtering target material, sputtering target, aluminum plate for sputtering target, and method for producing same
CN111318570A (en) * 2020-03-05 2020-06-23 爱发科电子材料(苏州)有限公司 Process for manufacturing micronized target material crystal grains
CN116732479A (en) * 2023-07-28 2023-09-12 宁波江丰电子材料股份有限公司 Manufacturing method of integrated high-purity aluminum target for LCD

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001115257A (en) * 1999-10-15 2001-04-24 Honeywell Electronics Japan Kk Manufacturing method for sputtering target material
CN101638760A (en) * 2009-07-30 2010-02-03 上海交通大学 Preparation method of ultra-pure aluminum ultrafine grain sputtering target
CN102002653A (en) * 2010-11-27 2011-04-06 东北大学 Method for preparing superhigh-purity aluminum fine grain high-orientation target
JP2014047383A (en) * 2012-08-30 2014-03-17 Nippon Steel & Sumitomo Metal Sputtering target material of highly pure aluminum, and method for producing the same
CN103834924A (en) * 2013-12-25 2014-06-04 利达光电股份有限公司 Method for preparing ultra-high purity aluminium and ultra-high purity aluminium alloy sputtering target material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001115257A (en) * 1999-10-15 2001-04-24 Honeywell Electronics Japan Kk Manufacturing method for sputtering target material
CN101638760A (en) * 2009-07-30 2010-02-03 上海交通大学 Preparation method of ultra-pure aluminum ultrafine grain sputtering target
CN102002653A (en) * 2010-11-27 2011-04-06 东北大学 Method for preparing superhigh-purity aluminum fine grain high-orientation target
JP2014047383A (en) * 2012-08-30 2014-03-17 Nippon Steel & Sumitomo Metal Sputtering target material of highly pure aluminum, and method for producing the same
CN103834924A (en) * 2013-12-25 2014-06-04 利达光电股份有限公司 Method for preparing ultra-high purity aluminium and ultra-high purity aluminium alloy sputtering target material

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106987788A (en) * 2017-03-07 2017-07-28 新疆众和股份有限公司 It is a kind of that the hot-working method that 1090 minute surface woollens are provided is rolled for specular aluminium
CN106987788B (en) * 2017-03-07 2019-03-26 新疆众和股份有限公司 It is a kind of to provide the hot-working method of 1090 mirror surface woollens for specular aluminium rolling
CN106947926A (en) * 2017-04-21 2017-07-14 中铝瑞闽股份有限公司 A kind of preparation method of large scale rafifinal target
CN107030108A (en) * 2017-04-21 2017-08-11 中铝瑞闽股份有限公司 A kind of rafifinal target heavy reduction rolling method
CN106947926B (en) * 2017-04-21 2018-04-03 中铝瑞闽股份有限公司 A kind of preparation method of large scale rafifinal target
CN110709532A (en) * 2017-06-22 2020-01-17 株式会社Uacj Sputtering target material, sputtering target, aluminum plate for sputtering target, and method for producing same
US11618942B2 (en) 2017-06-22 2023-04-04 Uacj Corporation Sputtering-target material, sputtering target, sputtering-target aluminum plate, and method of manufacturing the same
CN109174996A (en) * 2018-08-24 2019-01-11 爱发科电子材料(苏州)有限公司 The plate calendering technology of TFT liquid crystal display panel wiring layer rafifinal target
CN110205590A (en) * 2019-05-08 2019-09-06 东莞市欧莱溅射靶材有限公司 A kind of ultra-pure aluminum sputtering target material and its milling method
CN110484874A (en) * 2019-08-16 2019-11-22 韶关市欧莱高新材料有限公司 A kind of preparation method of high-purity aluminum pipe sputtering target material
CN111318570A (en) * 2020-03-05 2020-06-23 爱发科电子材料(苏州)有限公司 Process for manufacturing micronized target material crystal grains
CN116732479A (en) * 2023-07-28 2023-09-12 宁波江丰电子材料股份有限公司 Manufacturing method of integrated high-purity aluminum target for LCD

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