CN102989767A - Hot rolling process for high-performance tantalum target - Google Patents
Hot rolling process for high-performance tantalum target Download PDFInfo
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- CN102989767A CN102989767A CN2012102914624A CN201210291462A CN102989767A CN 102989767 A CN102989767 A CN 102989767A CN 2012102914624 A CN2012102914624 A CN 2012102914624A CN 201210291462 A CN201210291462 A CN 201210291462A CN 102989767 A CN102989767 A CN 102989767A
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- rolling
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- hot rolling
- tantalum target
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a hot rolling process for a high-performance tantalum target. The method comprises the following steps of: preheating a forged blank to 900-1,200 DEG C; rolling; and performing acid cleaning till tantalum metal luster occurs, and mottles are eliminated. A high-performance tantalum target which comprises uniform and consistent texture components (over 50 percent) with superior textures along the thickness direction (100) of the target and meets the use requirements of a high-end sputtering base can be obtained by using a high-performance tantalum target rolling blank produced by heating and rolling. Compared with a normal tantalum target, the high-performance tantalum target has the advantages that: texture components of over 50 percent of textures along the thickness direction (100) of the target are realized, higher requirement on the uniformity of the textures is met, and a consistent sputtering rate in a using process is ensured.
Description
Technical field
The present invention relates to the non-ferrous metallurgy technology field, particularly relate to a kind of hot rolling technology of high-performance tantalum target.
Background technology
Tantalum target is mainly used in the semiconductor coated film industry.
Physical vapor deposition (PVD) is one of technique of most critical in the semiconductor chip production process, its objective is the form of the compound of metal or metal with film deposited on silicon chip or other the substrate, and subsequently by the cooperating of the techniques such as photoetching and corrosion, finally form distribution structure complicated in the semiconductor chip.Physical vapour deposition (PVD) is finished by sputtering machine table, and sputtering target material is exactly a very important crucial consumptive material for above-mentioned technique.Common sputtering target material has high-purity Ta, also has the non-ferrous metals such as Ti, Al, Co and Cu.
Along with wafer size from the 200mm(8 inch) increase to the 300mm(12 inch), corresponding sputtering target material size must increase the basic demand that could satisfy the PVD plated film thereupon, simultaneously, live width is reduced to 90-45nm from (130-180nm), based on the electric conductivity of conductor and the matching performance of barrier layer, then sputtering target material will be to be converted into ultra-pure Cu/Ta to be from ultra-pure Al/Ti also, and the Ta target is increasing in the importance of semiconductor sputter industry, and demand is also increasing simultaneously.
In the prior art, tantalum target mainly is to adopt cold rolling or the cold-forging technique acquisition, the texture component of gained target thickness direction is inhomogeneous, up and down two aspects (100) texture that is mainly manifested in target is dominant, the centre is dominant with (111) texture, this class target can use at the low board of instructions for use, but " sputter rate that occurs when contour terminal platform uses is inhomogeneous to be unacceptable 12.
Summary of the invention
Purpose of the present invention just is to overcome the defective of above-mentioned prior art, provides a kind of texture component of target thickness direction even, the hot rolling technology of the uniform high-performance tantalum target of sputter rate when final assurance is used.
The present invention is based on following principle and designs:
The uniformity of silicon chip upper film thickness after the sputter, very important concerning final products, this depends on interior tissue and the texture orientation of tantalum target, uniform crystal particles refinement, the target that crystal grain crystalline orientation convergence is identical, in sputter, can make identical by the crystal grain sputter rate convergence of sputter, sputtered atom angular distribution track convergence is identical, will obtain like this coating of film thickness uniformity, the materials'use rate of tantalum target also is largely increased simultaneously.
For this reason, the present invention adopts following technical scheme:
A kind of hot rolling technology of high-performance tantalum target is characterized in that: at first forging blank is preheated to 900-1200 ℃, then rolling, pickling to tantalum metallic luster gets final product without assorted spot.
The rolling general working rate is controlled at 65%-85%, and rolling temperature is controlled at 800-1200 ℃.
The rolling adopts tandem rolling, and each rolling direction is for turning 45 jiaos clockwise, and the first eight pass reduction is controlled at 50%-95%, afterwards rolling to look for tolerance as main.
Every rolling 2-6 passage is melted down heating, heating-up temperature 900-1200 ℃ during the rolling.
Evenly smear the thick glass dust of 1-3mm in blank surface before the rolling.
Above-mentioned pickling is to be 5 in volume ratio: the HCl of 3:2, HF and H
2SO
4Mix acid liquor in carry out, pickling time is controlled at 5-10 minutes.
The present invention is by the rolling blank of heating rolling production high-performance tantalum target, cardinal principle is: distortion uneven distribution and shape parameter of transforming field on the rolled piece profile height have much relations, shape parameter of transforming field L(L=(R △ h)/h) (R: roller radius; △ h: drafts; H: average thickness) less, impact will become outstanding on deformation process in the outer end, and it is inner that compression can not be deep into the tantalum base, is only limited near the zone of superficial layer, and this moment, the distortion of superficial layer wanted large than central core, and metal flow speed and stress distribution are all inhomogeneous.By heating, flowability that can the Effective Raise material realizes larger rolling of shape parameter of transforming field.It is inner that rolling compression is deep into the tantalum base fully, and it is equal or slightly bigger with the superficial layer distortion to form the central core distortion, impels the slab rolling distortion to be " waist drum " shape but not " hyperbola " shape.Rolling by this method, it is the more broken thick columnar grain that carries over from last process, because this process can cause more dislocation and pile up along thick crystal boundary, further slab crystal grain is carried out even refinement, and impel crystal grain in a plurality of slide surfaces (line) slippage, for forming the γ strong-texture, subsequent heat treatment carries out the processing in early stage.The rolling blank of the high-performance of utilizing the present invention to prepare can obtain the texture component (proportion is more than 50%) that target thickness direction (100) texture is dominant, and uniformity, satisfy the high-performance tantalum target of high-end sputter base station instructions for use, compare with common tantalum target, the high-performance tantalum target has realized that not only target thickness direction (100) texture reaches the texture component more than 50%, and the texture uniformity also proposed higher requirement, thereby guaranteed that in use sputter rate is consistent.
The specific embodiment
The hot rolling technology of high-performance tantalum target of the present invention is specially:
1, forging blank is preheated to 900-1200 ℃.
2, rolling, control thickness is that the customer requirement finished product thickness adds the 2-4mm machining allowance.
1) in order to reduce the oxidation of material in the operation of rolling, smear glass dust in blank surface before rolling, glass dust is smeared and is wanted uniformity, and THICKNESS CONTROL is at 1-3mm.
2) the rolling power that always adds is controlled at 65%-95%.
Every rolling 2-6 passages need to be melted down heating when 3) rolling, and heating-up temperature is with the blank preheat temperature, namely 900-1200 ℃.
By remote sensing thermo detector Real-Time Monitoring temperature of charge, rolling temperature must not be lower than 800 ℃, is controlled at 800-1200 ℃ when 4) rolling.
5) adopt tandem rolling, each rolling direction is for turning 45 jiaos clockwise.The first eight pass reduction is controlled at 50%--75%, afterwards rolling to look for tolerance as main, with the plate thickness allowance control in 0.5mm.
3, pickling is to carry out in the mix acid liquor of hydrochloric acid, hydrofluoric acid and sulfuric acid, wherein HCl: HF:H
2SO
4=5: the 3:2(volume ratio), pickling time is controlled at 5-10 minutes, removes surface impurity, visually observes visible tantalum metallic luster and gets final product without assorted spot.
Claims (6)
1. the hot rolling technology of a high-performance tantalum target, it is characterized in that: at first forging blank is preheated to 900-1200 ℃, then rolling, pickling to tantalum metallic luster gets final product without assorted spot.
2. according to the hot rolling technology of high-performance tantalum target claimed in claim 1, it is characterized in that: the rolling general working rate is controlled at 65%-85%, and rolling temperature is controlled at 800-1200 ℃.
3. according to the hot rolling technology of claim 1 or 2 described high-performance tantalum targets, it is characterized in that: the rolling adopts tandem rolling, each rolling direction is for turning 45 jiaos clockwise, and the first eight pass reduction is controlled at 50%-95%, afterwards rolling to look for tolerance as main.
4. according to the hot rolling technology of claim 1 or 2 described high-performance tantalum targets, it is characterized in that: every rolling 2-6 passage during the rolling, melt down heating, heating-up temperature 900-1200 ℃.
5. according to the hot rolling technology of claim 1 or 2 described high-performance tantalum targets, it is characterized in that: evenly smear the thick glass dust of 1-3mm in blank surface before the rolling.
6. according to the hot rolling technology of high-performance tantalum target claimed in claim 1, it is characterized in that: above-mentioned pickling is to be 5 in volume ratio: the HCl of 3:2, HF and H
2SO
4Mix acid liquor in carry out, pickling time is controlled at 5-10 minutes.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210291462.4A CN102989767B (en) | 2012-08-16 | 2012-08-16 | The hot rolling technology of high-performance tantalum target |
| PCT/CN2013/081617 WO2014026631A1 (en) | 2012-08-16 | 2013-08-16 | Hot rolling process for high-performance tantalum target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210291462.4A CN102989767B (en) | 2012-08-16 | 2012-08-16 | The hot rolling technology of high-performance tantalum target |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102989767A true CN102989767A (en) | 2013-03-27 |
| CN102989767B CN102989767B (en) | 2015-12-16 |
Family
ID=47919171
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210291462.4A Expired - Fee Related CN102989767B (en) | 2012-08-16 | 2012-08-16 | The hot rolling technology of high-performance tantalum target |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN102989767B (en) |
| WO (1) | WO2014026631A1 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014026631A1 (en) * | 2012-08-16 | 2014-02-20 | 宁夏东方钽业股份有限公司 | Hot rolling process for high-performance tantalum target |
| WO2014026639A1 (en) * | 2012-08-16 | 2014-02-20 | 宁夏东方钽业股份有限公司 | Method for preparing high-performance tantalum target |
| CN104128740A (en) * | 2013-05-02 | 2014-11-05 | 宁波江丰电子材料股份有限公司 | Preparation method of copper target |
| CN104762619A (en) * | 2015-04-02 | 2015-07-08 | 长沙南方钽铌有限责任公司 | Preparation method of matt tantalum coiled strips |
| CN106521434A (en) * | 2016-11-07 | 2017-03-22 | 长沙南方钽铌有限责任公司 | Preparation method of high-purity tantalum target material with preferred orientation |
| CN110000211A (en) * | 2018-01-05 | 2019-07-12 | 宁波江丰电子材料股份有限公司 | Target milling method |
| CN110735068A (en) * | 2019-11-21 | 2020-01-31 | 中南大学 | Preparation method and application of cobalt-tantalum-zirconium alloy target |
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| CN1718865A (en) * | 2005-07-05 | 2006-01-11 | 何明威 | Method of removing oxidized skin on hot rolling nickel stainless steel material |
| CN101704187A (en) * | 2009-11-13 | 2010-05-12 | 西北稀有金属材料研究院 | Texture forming method of tantalum target |
| KR20110082338A (en) * | 2010-01-11 | 2011-07-19 | 한국생산기술연구원 | A method of texture control using differential speed rolling for ta sputtering target and sputtering target |
| US20110265921A1 (en) * | 2006-04-13 | 2011-11-03 | Ulvac, Inc. | Ta SPUTTERING TARGET AND METHOD FOR PRODUCING THE SAME |
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| CN102489508A (en) * | 2011-12-06 | 2012-06-13 | 无锡乐普金属科技有限公司 | Cross rolling method of molybdenum-copper alloy foil |
| CN102517531A (en) * | 2011-12-31 | 2012-06-27 | 宁波江丰电子材料有限公司 | Method for preparing high-purity tantalum target |
| CN102517550A (en) * | 2011-12-20 | 2012-06-27 | 宁波江丰电子材料有限公司 | High purity tantalum target and preparation process thereof |
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| US7081148B2 (en) * | 2001-09-18 | 2006-07-25 | Praxair S.T. Technology, Inc. | Textured-grain-powder metallurgy tantalum sputter target |
| CN102989767B (en) * | 2012-08-16 | 2015-12-16 | 宁夏东方钽业股份有限公司 | The hot rolling technology of high-performance tantalum target |
-
2012
- 2012-08-16 CN CN201210291462.4A patent/CN102989767B/en not_active Expired - Fee Related
-
2013
- 2013-08-16 WO PCT/CN2013/081617 patent/WO2014026631A1/en active Application Filing
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1718865A (en) * | 2005-07-05 | 2006-01-11 | 何明威 | Method of removing oxidized skin on hot rolling nickel stainless steel material |
| US20110265921A1 (en) * | 2006-04-13 | 2011-11-03 | Ulvac, Inc. | Ta SPUTTERING TARGET AND METHOD FOR PRODUCING THE SAME |
| CN101704187A (en) * | 2009-11-13 | 2010-05-12 | 西北稀有金属材料研究院 | Texture forming method of tantalum target |
| KR20110082338A (en) * | 2010-01-11 | 2011-07-19 | 한국생산기술연구원 | A method of texture control using differential speed rolling for ta sputtering target and sputtering target |
| CN102296272A (en) * | 2011-08-17 | 2011-12-28 | 宁波江丰电子材料有限公司 | Manufacturing method of tantalum target material |
| JP2012052235A (en) * | 2011-09-12 | 2012-03-15 | Toyo Tanso Kk | Manufacturing method of tantalum tube and pit carbon core, tantalum tube and pit carbon core, manufacturing method of tantalum carbide wiring, and tantalum carbide wiring |
| CN102489508A (en) * | 2011-12-06 | 2012-06-13 | 无锡乐普金属科技有限公司 | Cross rolling method of molybdenum-copper alloy foil |
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| CN102517531A (en) * | 2011-12-31 | 2012-06-27 | 宁波江丰电子材料有限公司 | Method for preparing high-purity tantalum target |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014026631A1 (en) * | 2012-08-16 | 2014-02-20 | 宁夏东方钽业股份有限公司 | Hot rolling process for high-performance tantalum target |
| WO2014026639A1 (en) * | 2012-08-16 | 2014-02-20 | 宁夏东方钽业股份有限公司 | Method for preparing high-performance tantalum target |
| US9957603B2 (en) | 2012-08-16 | 2018-05-01 | Ningxia Orient Tantalum Industry Co., Ltd. | Method for preparing high-performance tantalum target |
| CN104128740A (en) * | 2013-05-02 | 2014-11-05 | 宁波江丰电子材料股份有限公司 | Preparation method of copper target |
| CN104762619A (en) * | 2015-04-02 | 2015-07-08 | 长沙南方钽铌有限责任公司 | Preparation method of matt tantalum coiled strips |
| CN104762619B (en) * | 2015-04-02 | 2018-10-12 | 长沙南方钽铌有限责任公司 | A kind of preparation method of matt tantalum coiled strip |
| CN106521434A (en) * | 2016-11-07 | 2017-03-22 | 长沙南方钽铌有限责任公司 | Preparation method of high-purity tantalum target material with preferred orientation |
| CN106521434B (en) * | 2016-11-07 | 2019-01-22 | 长沙南方钽铌有限责任公司 | A kind of preparation method of the high-purity tantalum target with preferred orientation |
| CN110000211A (en) * | 2018-01-05 | 2019-07-12 | 宁波江丰电子材料股份有限公司 | Target milling method |
| CN110735068A (en) * | 2019-11-21 | 2020-01-31 | 中南大学 | Preparation method and application of cobalt-tantalum-zirconium alloy target |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102989767B (en) | 2015-12-16 |
| WO2014026631A1 (en) | 2014-02-20 |
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Inventor after: Zhong Jingming Inventor after: Wang Kai Inventor after: Wang Li Inventor after: Li Zhaobo Inventor before: Zhang Chunheng Inventor before: Li Guipeng Inventor before: Tong Lei Inventor before: Wang Kai Inventor before: Li Zhaobo |
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