CN102400073A - Method for manufacturing nickel target blank and target - Google Patents

Method for manufacturing nickel target blank and target Download PDF

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Publication number
CN102400073A
CN102400073A CN2011103705091A CN201110370509A CN102400073A CN 102400073 A CN102400073 A CN 102400073A CN 2011103705091 A CN2011103705091 A CN 2011103705091A CN 201110370509 A CN201110370509 A CN 201110370509A CN 102400073 A CN102400073 A CN 102400073A
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China
Prior art keywords
nickel
target base
nickel target
ingot
manufacture
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Pending
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CN2011103705091A
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Chinese (zh)
Inventor
姚力军
相原俊夫
大岩一彦
潘杰
王学泽
袁海军
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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Priority to CN2011103705091A priority Critical patent/CN102400073A/en
Publication of CN102400073A publication Critical patent/CN102400073A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for manufacturing a nickel target blank and a nickel target. The method for manufacturing the nickel target blank comprises the following steps of: providing nickel ingots; forging the nickel ingots; rolling the forged nickel ingots to form the nickel target blank; and annealing the nickel target blank, wherein the annealing temperature is 300 to 500 DEG C, and the heat preservation time is 1 to 2 hours. The internal texture of the nickel target blank manufactured by the technical scheme is relatively uniform, grains of the nickel target blank are fine, the nickel target blank is used for manufacturing the nickel target for semiconductors, and a film formed by sputtering the nickel target has good quality.

Description

The method of manufacture of nickel target base and target
Technical field
The present invention relates to the target manufacture field, the method for manufacture of particularly a kind of nickel target base and target.
Background technology
Physical vapor deposition (PVD; Physical Vapor Deposition) is widely used in the high-end industries such as optics, electronics, information; For example: unicircuit, liquid-crystal display (LCD, Liquid Crystal Display), industrial glass, CG, information storage, boats and ships, chemical industry etc.The metal targets of using among the PVD then is one of most important starting material in the manufacturing processedes such as unicircuit, liquid-crystal display.
Continuous development along with the PVD technology improves metal targets demand and specification of quality day by day, and the crystal grain of metal targets is thin more, and composition is organized even more, and its surfaceness is more little, and is just even more through the film that PVD forms on silicon chip.In addition, the purity of the film of formation and the purity of metal targets are also closely related, so the quality of PVD rear film quality depends primarily on factors such as the purity, microtexture of metal targets.
Nickel (Ni) target is a kind of more typical metal targets, because the corrosion resistance of nickel target is good, capability of electromagnetic shielding is good; And can be used as important characteristics such as energy and material use; So be widely used among the PVD, for example: nickel can be used in other metallic surfaces as decorating and the protective coating use the most important starting material sponge nickel that in nickel metal hydride battery, uses; Also can produce through the mode of the nickel target being carried out vacuum sputtering; The compliant conductive cloth surface of in electromagnetic shielding material, using also uses the nickel target as sputtering source, in addition, has also all used the nickel target in large quantities in fields such as plastics metal-coated membrane, building glass metal-coated membranes.
The nickel target is welded by nickel target base and backboard, and nickel target base is then processed acquisition to the nickel ingot accordingly, and therefore, whether the nickel target that the internal structure of nickel target base, the size of crystal grain become final acquisition can satisfy the key factor of semi-conductor sputter demand.
For now, the nickel ingot is when being used to make nickel target base, and its purity requirement is more than 4N (Ni content is not less than 99.99%).And in the prior art; High-purity nickel ingot is carried out viscous deformation to be made semi-conductor and relates to less with the complete processing of high purity nickel target base to reach; Therefore, how to produce and be suitable for semi-conductor and become one of present problem demanding prompt solution with the nickel target base of high purity nickel sputtering target material.
Use the correlation technique of target can be referring to the one Chinese patent application of publication number as CN101224496A about semi-conductor, it discloses a kind of method of manufacture that under low cost, produces high-quality sputtered target material.
Summary of the invention
The problem that the present invention solves provides a kind of method of manufacture of nickel target base, and internal structure is even, crystal grain is tiny to obtain, and meets to be used to make the nickel target base of semi-conductor with the nickel target.
For addressing the above problem, the present invention provides a kind of method of manufacture of nickel target base, comprising:
The nickel ingot is provided;
Said nickel ingot is forged;
Nickel ingot to after forging rolls, and forms nickel target base;
Said nickel target base is annealed, and said annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h.
Optional, the method for manufacture of said nickel target base also comprises: before said nickel ingot is forged, said nickel ingot is heated to more than the recrystallization temperature, said recrystallization temperature is 320 ℃~380 ℃.
Optional, the method for manufacture of said nickel target base also comprises: the nickel target base to after the annealing cools off.
Optional, the said type of cooling is a water-cooled, be 30~60s cooling time.
Optional, said calendering comprises colds pressing or hot pressing.
Optional, said nickel ingot after forging is rolled comprises: the nickel ingot after forging is carried out the multi-pass calendering.
Optional, every time calendering amount is 10%~20% of a nickel ingot height.
Optional, every time calendering back rotation predetermined angle is rolled again.
Optional, the method for manufacture of said nickel target base also comprises: before the nickel ingot after forging is rolled, the nickel ingot after forging is annealed.
For addressing the above problem, the present invention also provides a kind of method of manufacture of nickel target, comprising:
Adopt above-mentioned nickel target base method of manufacture to obtain nickel target base;
Said nickel target base is carried out mechanical workout;
Nickel target base and backboard after the mechanical workout are welded.
Compared with prior art, technical scheme of the present invention has the following advantages:
Through nickel target base is annealed, and said annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h.Improved the physicals of nickel target base to a great extent, made that the interior tissue of the final nickel target base that obtains is more even, yield rate is high, and then makes that the quality of the film that sputter nickel target forms is better when adopting said nickel target base to make semi-conductor with the nickel target.
Nickel target base to after the annealing cools off, and makes that the crystal grain after the annealing stops growing, and then makes that the crystal grain of the final nickel target base that obtains is tiny, and is evenly distributed.
Through the nickel ingot after forging is carried out the multi-pass calendering; Nickel target base makes that the nickel target base internal stress distribution that obtains is even, so can not crack; Produce the nickel target base that meets demand, reduced the waste that does not meet the material that semi-conductor nickel target causes with the requirement of nickel target base because of nickel target base.
Description of drawings
Fig. 1 is the schema of method of manufacture of the nickel target base of the embodiment of the invention;
Fig. 2 is the schema of method of manufacture of the nickel target of the embodiment of the invention.
Embodiment
As described in the background technology; Make semi-conductor and relate to less to reach through high-purity nickel ingot being carried out viscous deformation in the prior art with the complete processing of high purity nickel target base; Therefore, the contriver proposes, through the nickel ingot is forged, calendering, annealed mode make nickel target base.Further; The contriver is definite through long-term and unremitting studying assiduously; The parameter of nickel target base being carried out annealing process has played a crucial factor for the performance of the nickel target base of final formation, therefore, and can be according to the parameters that meets the nickel target base that sputter uses that finally will obtain; And then the parameter of control annealing process, obtain to meet the nickel target base of demand.
See also Fig. 1, Fig. 1 is the schema of method of manufacture of the nickel target base of the embodiment of the invention, and as shown in Figure 1, the method for manufacture of said nickel target base comprises:
Step S11: the nickel ingot is provided.
Step S12: said nickel ingot is forged.
Step S13: the nickel ingot to after forging rolls, and forms nickel target base.
Step S14: said nickel target base is annealed, and said annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h.
Performing step S11, the nickel ingot that provides in the present embodiment are the high-purity nickel ingot of purity more than or equal to 4N (Ni content is not less than 99.99%).
In order to eliminate casting flaws such as the inner original cast structure of nickel ingot is loose, optimize the inner heterogeneous microstructure of nickel ingot, particularly; The column crystal of nickel ingot is broken for close grain, repairs the inner pore of nickel ingot, and then make its internal structure by the loose consolidation that becomes; Performing step S12 forges said nickel ingot, and before said nickel ingot is forged; Need said nickel ingot be heated to more than the recrystallization temperature; Recrystallize is meant generally that annealing temperature is enough high, the time is during sufficiently long, in the microstructure of deformable metal or alloy, produces strainless new crystal grain-recrystallize core.New crystal grain is constantly grown up, and until original Deformation structure's completely dissolve, noticeable change also takes place the performance of metal or alloy, and this process is called recrystallize.Wherein, the temperature that begins to generate new crystal grain is called the initial recrystallization temperature, and microstructure all is called end of a period recrystallization temperature or perfect recrystallization temperature by the occupied temperature of new crystal grain.In general, said recrystallization temperature then is meant the arithmetical av of initial recrystallization temperature and end of a period recrystallization temperature.The recrystallization temperature of said nickel ingot is 320 ℃~380 ℃, preferably heats in the present embodiment more than the said nickel ingot to 350 ℃.
In the present embodiment, can repeatedly forge, and the size of the nickel ingot after repeatedly forging is because of according to follow-up when the nickel ingot is rolled to said nickel ingot, the passage of calendering, every time calendering amount and the nickel target base after the final calendering that obtains size and decide.
And,, need anneal to the nickel ingot after forging in order to eliminate inner unrelieved stress and the inner tissue defects of nickel ingot after the forging; The annealed temperature can be a little more than the recrystallization temperature of nickel; In the present embodiment, annealing temperature is 450 ℃~500 ℃, and soaking time is 2~3 hours (h).
Performing step S13 rolls the nickel ingot after forging, and particularly, rolls forging back and annealed nickel ingot exactly.Nickel ingot after adopting rolling press to annealing in the present embodiment rolls, and both can adopt the mode of colding pressing that said nickel ingot is rolled, and also can adopt hot pressed mode that said nickel ingot is rolled; Said calendering is multi-pass calendering, and the passage of calendering can be decided by practical situation, every time calendering amount can difference also can be identical; In the present embodiment, every time calendering amount is all identical, is 10%~20% of nickel ingot height to be rolled; And the more even unanimity of various piece for the nickel target base after the feasible calendering; Preferably, said nickel ingot is whenever carried out a time calendering, all can be to descending the calendering of a time after the rotation of the nickel ingot after the calendering predetermined angle again; In the present embodiment, said predetermined angle is between 30 °~150 °.Roll through the nickel ingot being carried out multi-pass, and then can be so that the stress distribution of nickel target base inside is even, therefore; The nickel target base that forms can not crack; Meet the demand of semi-conductor, owing to the nickel target base that forms can not crack, therefore with the nickel target; Also reduce the waste of nickel material in the production process, reduced production cost.
Through above-mentioned calendering mode, the nickel ingot is rolled, formed nickel target base.
Performing step S14: said nickel target base is annealed, and particularly, the annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h.Nickel ingot (nickel target base) to after the calendering carries out the annealing of above-mentioned condition, can be so that the interior tissue of the final nickel target base that forms be more even, and crystal grain is tiny; The distribution of crystal grain is even more, and in annealing process, in order to make the final nickel target base that obtains meet demand; Also need accurately control the annealed temperature, the deviation of annealing temperature is no more than ± and 3 ℃, for instance; If the selective annealing temperature is 360 ℃, in the then whole annealing process, annealing temperature is controlled at 357 ℃~363 ℃.
Size for the crystal grain of the nickel target base of controlling final acquisition; Except controlling annealed temperature and annealed the time; Also need the nickel target base after the annealing be cooled off; Nickel target base after promptly insulation being finished cools off, so that crystal grain stops growing, and then makes that the crystal grain of the final nickel target base that obtains is tiny.Both can adopt the mode of water-cooled also can adopt the mode of air cooling that said nickel target base is cooled off in the present embodiment, and preferably, adopt the mode of water-cooled that said nickel target base is cooled off, be 30~60 seconds (s) cooling time.
So far, through the method for manufacture of above-mentioned nickel target base, obtained to be used to make the nickel target base that the nickel target is used; After this also need the nickel target base that obtain be detected; Whether for example: whether detect its diameter, thickness and edge has wrinkle, surface to have phenomenon such as crackle to produce, and whether the size of the crystal grain of the nickel target base of producing meets the requirements, whether the internal organizational structure of nickel target base is even etc., if meet basically; Think that then this nickel target base is qualified, can be used for of the production of follow-up semi-conductor with the nickel target.
The embodiment of the invention also provides a kind of method of manufacture of nickel target, sees also Fig. 2, and Fig. 2 is the schema of method of manufacture of the nickel target of the embodiment of the invention, and as shown in Figure 2, the method for manufacture of said nickel target comprises:
Step S21: the nickel ingot is provided.
Step S22: said nickel ingot is forged.
Step S23: the nickel ingot to after forging rolls, and forms nickel target base.
Step S24: said nickel target base is annealed, and said annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h.
Step S25: the nickel target base to after the annealing cools off.
Step S26: cooled nickel target base is carried out mechanical workout.
Step S27: nickel target base and backboard after the mechanical workout are welded.
Below the manufacturing processed of nickel target is simply described, in the present embodiment step S21~step S25 for making nickel target base, particularly, similar with the method for manufacture of above-mentioned nickel target base; Be about to high-purity nickel ingot and be heated to more than the recrystallization temperature, then it is repeatedly forged, the nickel ingot after forging is annealed; Eliminate the internal stress of nickel ingot, the nickel ingot after the annealing is carried out the multi-pass calendering, form nickel target base; Nickel target base to after the calendering is annealed, and the annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h; Nickel target base to after the insulation carries out quick water-cooled, and be 30~60s cooling time, to obtain to meet the nickel target base of demand.
Performing step S26; Cooled nickel target base is carried out mechanical workout; In the present embodiment, the mechanical workout that said nickel target base is carried out is turning processing, is used to remove the zone of oxidation on said nickel target base surface; Make follow-uply when said nickel target base and backboard are welded, can combine better between the face of weld.
Performing step S27: nickel target base and backboard after the mechanical workout are welded.Backboard described in the present embodiment is the aluminium backboard, and particularly, said nickel target base and said aluminium backboard can be welded through the mode of diffusion welding, for example: can be welded through hot pressed mode, also can be welded through the mode of hot isostatic pressing.
In sum, technical scheme of the present invention has following beneficial effect at least:
Through nickel target base is annealed, and said annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h.Improved the physicals of nickel target base to a great extent, made that the interior tissue of the final nickel target base that obtains is more even, yield rate is high, and then makes that the quality of the film that sputter nickel target forms is better when adopting said nickel target base to make semi-conductor with the nickel target.
Nickel target base to after the annealing cools off, and makes that the crystal grain after the annealing stops growing, and then makes that the crystal grain of the final nickel target base that obtains is tiny, and is evenly distributed.
Through the nickel ingot after forging is carried out the multi-pass calendering; Nickel target base makes that the nickel target base internal stress distribution that obtains is even, so can not crack; Produce the nickel target base that meets demand, reduced the waste that does not meet the material that semi-conductor nickel target causes with the requirement of nickel target base because of nickel target base.
Though the present invention with preferred embodiment openly as above; But it is not to be used for limiting the present invention; Any those skilled in the art are not breaking away from the spirit and scope of the present invention; Can utilize the method and the technology contents of above-mentioned announcement that technical scheme of the present invention is made possible change and modification, therefore, every content that does not break away from technical scheme of the present invention; To any simple modification, equivalent variations and modification that above embodiment did, all belong to the protection domain of technical scheme of the present invention according to technical spirit of the present invention.

Claims (10)

1. the method for manufacture of a nickel target base is characterized in that, comprising:
The nickel ingot is provided;
Said nickel ingot is forged;
Nickel ingot to after forging rolls, and forms nickel target base;
Said nickel target base is annealed, and said annealed temperature is 300 ℃~500 ℃, and soaking time is 1~2h.
2. the method for manufacture of nickel target base as claimed in claim 1 is characterized in that, also comprises: before said nickel ingot is forged, said nickel ingot is heated to more than the recrystallization temperature, said recrystallization temperature is 320 ℃~380 ℃.
3. the method for manufacture of nickel target base as claimed in claim 1 is characterized in that, also comprises: the nickel target base to after the annealing cools off.
4. the method for manufacture of nickel target base as claimed in claim 3 is characterized in that, the said type of cooling is a water-cooled, and be 30~60s cooling time.
5. the method for manufacture of nickel target base as claimed in claim 1 is characterized in that, said calendering comprises colds pressing or hot pressing.
6. the method for manufacture of nickel target base as claimed in claim 1 is characterized in that, said nickel ingot after forging is rolled comprises: the nickel ingot after forging is carried out the multi-pass calendering.
7. the method for manufacture of nickel target base as claimed in claim 6 is characterized in that, every time calendering amount is 10%~20% of a nickel ingot height.
8. the method for manufacture of nickel target base as claimed in claim 6 is characterized in that, every time calendering back rotation predetermined angle is rolled again.
9. the method for manufacture of nickel target base as claimed in claim 1 is characterized in that, also comprises: before the nickel ingot after forging is rolled, the nickel ingot after forging is annealed.
10. the method for manufacture of a nickel target is characterized in that, comprising:
Adopt each described nickel target base method of manufacture of claim 1~9 to obtain nickel target base;
Said nickel target base is carried out mechanical workout;
Nickel target base and backboard after the mechanical workout are welded.
CN2011103705091A 2011-11-18 2011-11-18 Method for manufacturing nickel target blank and target Pending CN102400073A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104674170A (en) * 2013-11-26 2015-06-03 宁波江丰电子材料股份有限公司 Manufacturing method of nickel target billet and nickel target material
CN111088481A (en) * 2018-10-23 2020-05-01 宁波江丰电子材料股份有限公司 Nickel target blank and method for manufacturing target material
CN114000073A (en) * 2021-10-28 2022-02-01 宁波江丰电子材料股份有限公司 Process method for improving internal structure of high-purity nickel target material
CN115261806A (en) * 2022-08-01 2022-11-01 宁波江丰电子材料股份有限公司 Nickel-aluminum alloy sputtering target material and hot isostatic pressing preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1578849A (en) * 2001-11-26 2005-02-09 株式会社日矿材料 Sputtering target and production method therefor
CN1615374A (en) * 2002-01-18 2005-05-11 株式会社日矿材料 Target of high-purity nickel or nickel alloy and its producing method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1578849A (en) * 2001-11-26 2005-02-09 株式会社日矿材料 Sputtering target and production method therefor
CN1615374A (en) * 2002-01-18 2005-05-11 株式会社日矿材料 Target of high-purity nickel or nickel alloy and its producing method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
劳动和社会保障部等: "《变配电室值班电工(基础知识)》", 30 April 2003 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104674170A (en) * 2013-11-26 2015-06-03 宁波江丰电子材料股份有限公司 Manufacturing method of nickel target billet and nickel target material
CN111088481A (en) * 2018-10-23 2020-05-01 宁波江丰电子材料股份有限公司 Nickel target blank and method for manufacturing target material
CN114000073A (en) * 2021-10-28 2022-02-01 宁波江丰电子材料股份有限公司 Process method for improving internal structure of high-purity nickel target material
CN115261806A (en) * 2022-08-01 2022-11-01 宁波江丰电子材料股份有限公司 Nickel-aluminum alloy sputtering target material and hot isostatic pressing preparation method thereof
CN115261806B (en) * 2022-08-01 2023-09-08 宁波江丰电子材料股份有限公司 Nickel-aluminum alloy sputtering target material and hot isostatic pressing preparation method thereof

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Application publication date: 20120404