CN101660123A - Nickel-based target and production process - Google Patents
Nickel-based target and production process Download PDFInfo
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- CN101660123A CN101660123A CN200810032181A CN200810032181A CN101660123A CN 101660123 A CN101660123 A CN 101660123A CN 200810032181 A CN200810032181 A CN 200810032181A CN 200810032181 A CN200810032181 A CN 200810032181A CN 101660123 A CN101660123 A CN 101660123A
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Abstract
The invention discloses a nickel-based target and a production process. The production process comprises working procedures of cold rolling, high-temperature vacuum heat treatment, ammonia atmosphereprotective heat treatment, primary rolling, welding, precision rolling, annealing and the like. The production process has no high-temperature processes of smelting, hot rolling and the like, and alsohas no high-pollution processes of acid washing, alkali washing and the like. Therefore, compared with the conventional process, the production process reduces the energy consumption by 30 percent and the metal loss by 50 percent, improves the one-time yield by over 10 percent, has high comprehensive utilization rate of resources, and is environmentally-friendly; and the process is simple and convenient to operate, can effectively guarantee the purity of a electrolytic nickel thin plate, improve the comprehensive mechanical property and physical property of the electrolytic nickel thin plateand replace the prior production process for smelting and hot-rolling the nickel target, and is suitable for industrialized production.
Description
Technical field
The invention discloses a kind of magnetron sputtering with nickel-based target and production technique, be meant cold rolling nickel-based target of a kind of high purity electrolytic nickel and production technique especially, belong to the metal material processing technical field.
Background technology
The metallic nickel thin plate is widely used in the BLD electronic product, as its starting material, requires it to have good electrical conductivity and enough thin thickness, and the quality of conductivity is directly related with nickel-based target purity, promptly directly related with foreign matter content in the nickel-based target; The thickness of nickel-based target is then relevant with the nickelalloy heterogeneous microstructure, nickel-based target generally adopts electrolytic nickel as starting material production, electrolytic nickel is as a kind of matallurgical products, purity itself can reach more than 99.9%, if directly carry out cold rolling processing, because of process is physical refining process completely, its composition can not change, metal losses such as adhesion, scaling loss can be do not produced yet, thereby the purity and the excellent conducting performance of nickel-based target can be guaranteed; But because electrolytic nickel is in the electrometallurgy process, nickel crystallite is all piled up for the vertical panel face and is formed, no matter its grain orientation still is the intercrystalline bonding strength, all be not suitable for cold rolling processing, therefore, traditional nickel-based target production can not directly be carried out electrolytic nickel cold rolling and obtain meeting electronic product producing desired thickness, but adopts following production process route:
Electrolytic nickel → melting → plane ingot → hot rolling → alkali cleaning → pickling → cold rolling → annealing → cold rolling → alkali cleaning → pickling → finished product thermal treatment.
GB regulation (GB5235-85): the purity of N6 nickel-based target is Ni+Co 〉=99.5%, and micro impurity element accounts for 0.5%, is respectively: C :≤0.1; Cu :≤0.06; Fe :≤0.1; Si :≤0.1; Mn :≤0.05; Mg :≤0.1; S :≤0.005; P :≤0.002; Pb :≤0.002; Bi :≤0.002; As :≤0.002; Sb :≤0.002; Zn :≤0.007; Cd :≤0.002; Sn :≤0.002; In above-mentioned production technique, earlier electrolytic nickel is carried out melting, hot rolling, adjust its heterogeneous microstructure, carry out follow-up manufacturing procedure then; In melting and hot procedure, often inevitably be accompanied by the increase of impurity element such as C, S, P, O, Cu, Fe etc., originally purified metal purity is reduced, therefore, traditional nickel-based target production technique is difficult to guarantee to produce the nickel-based target that meets GB (GB5235-85) requirement; Particularly separate out at crystal boundary under the impurity element normal temperature such as C, S, P, O, Cu, Fe and be enriched in the crystal boundary place, the conductivity of severe exacerbation nickel-based target and solidity to corrosion.In addition, in melting and hot procedure, because the adhesion of metal melt and oxidization burning loss also will cause the metal loss about 6%, energy consumption height, labour intensity are big, discharge a large amount of CO
2Isothermal chamber gas, its resource utilization and production efficiency are low; And the nickel-based target performance of production can not satisfy the requirement of BVD electronic product.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and provide a kind of technology is simple, energy consumption is low, the metal loss amount is little, purity is high magnetron sputtering with nickel target and production technique.
The present invention, the component following (weight percent) of the special-purpose nickel-based target of a kind of battery:
Ni+Co：≥99.98；C：≤0.002；Si：≤0.0001；Cu：≤0.0001；Fe：≤0.001；S：≤0.0002；Zn：≤0.0002Pb：≤0.0002
Trace impurity :≤0.0162.
The present invention, magnetron sputtering comprises the steps: with the nickel-based target production technique
1) cold rolling: the deflection by 8～30% is cold rolling to sheet nickel;
2) high-temperature heat treatment: the blank vacuum (perhaps protective atmosphere) after step 1 processing is heated to 1000～1400 ℃, is incubated 1～3 hour, stove is chilled to below 100 ℃ and comes out of the stove;
3) repeating step 1,2, reach 40～100um to the blank grain-size;
4) atmosphere protection thermal treatment: step 3 gained blank is heated to 600～700 ℃ under protective atmosphere, is incubated 2～5 hours, stove is chilled to below 100 ℃;
5) cold rolling: as to be undertaken cold rolling by 8～30% deflection step 4 gained blank;
6) repeating step 4,5, reach≤10um up to the blank grain-size;
7) breaking down:, and roll and be as thin as certain thickness with the shaping of step 6 gained blank;
8) finish rolling: it is the required panel material of client that step 7 gained blank is rolled into thickness;
9) annealing: step 8 gained sheet material is annealed in vacuum or atmosphere furnace.
10) moulding: be processed into the regulation shape by groove rolling or other working methods.
11) surface treatment: the surface is handled to satisfy service requirements
Among the present invention protective atmosphere thermal treatment can adopt ammonia decomposing protection atmosphere, pure hydrogen atmosphere, argon gas, nitrogen, very aerial any one.
The present invention is owing to adopt above-mentioned processing method, at first, by cold rolling and high-temperature heat treatment repeatedly, make blank produce limited amount viscous deformation, on the one hand, thick grain structure in the broken sheet nickel, on the other hand, in blank, produce certain prestress, in the high-temperature vacuum thermal treatment of carrying out subsequently, make crystal grain along the prestressed direction of growth, reach the purpose that makes grain orientation progressively consistent, simultaneously, during high-temperature heat treatment, a large amount of gas atoms (mainly being Sauerstoffatom) that are in the crystal boundary place are overflowed from crystal boundary, thereby, realize adjusting blank microtexture and air content, crystal grain thinning, the purpose of change grain growing direction.Subsequently, carry out cold rolling and protective atmosphere thermal treatment repeatedly, on the one hand, the thickness of blank is constantly reduced, on the other hand, high-temperature heat treatment under protective atmosphere can make crystal grain generation recovery and recrystallization broken in the cold-rolled process, makes grain structure more tiny, even, further improves every physicals of electrolytic nickel thin plate; Then, carry out conventional breaking down, finish rolling, finished products, realize the cold rolling processing of the Ni-based target of high purity.By above analysis as can be known, the course of processing of sheet nickel is physical refining process completely, its composition can not change, and also can not produce metal losses such as adhesion, scaling loss, particularly adopt deformation and heat treatment phase joining technique, make recrystallize after the primary electroforming historrhexis, effectively improved its heterogeneous microstructure and comprehensive physicals, simultaneously, utilize vacuum and the dissolution characteristics of gas with various molecule in nickel, solved the gassiness problem of electrolytic nickel.Because to the processing of sheet nickel all are physical processes, avoid hot procedures such as melting, hot rolling fully, can guarantee that final nickel-based target product keeps the purity of sheet nickel, Ni+Co 〉=99.9%, thus reduced impurity to tissue and Effect on Performance.Simultaneously, in the course of processing, we use deformation+heat-treating methods, effectively improve the performance of nickel plate.The electric conductivity of nickel plate is≤7.8 μ Ω .cm.The present invention has born advantage for the purity that guarantees nickel target product; The purity of the nickel-based target product of producing is Ni+Co 〉=99.9%, C≤0.02% wherein, and S, P, O, Cu, Fe are all than traditional N
6Nickel-based target has significantly minimizing; The present invention organizes dressing technique, degassing technology etc. by electrolytic zinc-coated steel sheet, realizes the regulation and control of the inherent microstructure of nickel-based target product are reached the purpose that directly is processed into nickel-based target by electrolytic nickel.The nickel target product electric conductivity that the present invention produces is≤7.8 μ Ω.Production technique of the present invention does not have melting, and high temperature processes such as hot rolling do not have high pollution operations such as pickling, alkali cleaning yet.Therefore, reduce by 30% than traditional technology energy consumption, metal loss reduces by 50%, and the once lumber-preserving rate improves more than 10%, and comprehensive utilization of resources rate height is environmentally friendly.
Embodiment
The specific embodiment of the present invention is sketched in following:
The main raw material that the embodiment of the invention adopts is a sheet nickel, and its main component is Ni+Co 〉=99.98%.
Embodiment 1
1, gets electrolytic nickel slab material, cut into the wide lath shape of 115mm;
2, cold rolling by deflection a time of 8%;
3, the blank with step 2 places vacuum heat treatment furnace, is heated to 1000 ℃, insulation 1h, and stove is chilled to below 100 ℃ and comes out of the stove;
4, the blank of step 3 is cold rolling by deflection a time of 8%;
5, the blank with step 4 places vacuum heat treatment furnace, is heated to 1000 ℃, insulation 1h, and stove is chilled to below 100 ℃ and comes out of the stove;
6, the blank of step 5 is cold rolling by deflection a time of 8%;
7, the blank with step 6 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 600 ℃ of insulation 2h, and stove is chilled to below 100 ℃ and comes out of the stove;
8, the blank of step 7 is cold rolling by deflection a time of 8%;
9, the blank with step 8 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 600 ℃ of insulation 2h, and stove is chilled to below 100 ℃ and comes out of the stove;
10, the blank of step 9 is cold rolling by deflection a time of 8%;
11, the blank with step 10 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 600 ℃ of insulation 2h, and stove is chilled to below 100 ℃ and comes out of the stove;
12., breaking down: use two roller levelling machines,, and roll and be as thin as certain thickness the blank thin plate shaping of step 11;
14, finish rolling: use finishing mill, the blank plate of step 12 is rolled into client's desired thickness
15, annealing: place vacuum or well formula atmosphere furnace to anneal step 14 gained blank plate.
16. moulding:, be processed into client's desired size and shape with wire cutting machine tool with 15 gained nickel plates
17, surface finish is handled
Through checking: the finished product that step 15 obtains, Ni+Co:99.99; C:0.001; Si:0.0001; Cu:0.0001; Fe:0.001; S:0.0002; Zn:0.0002Pb:0.0002
Trace impurity :≤0.0162,
Resistance: 7.5 μ Ω .cm.
Embodiment 2:
1, gets electrolytic nickel slab material, cut into the wide lath shape of 100mm;
2, cold rolling by deflection a time of 8%;
3, the blank with step 2 places vacuum heat treatment furnace, is heated to 1200 ℃, insulation 2h, and stove is chilled to below 100 ℃ and comes out of the stove;
4, the blank of step 3 is cold rolling by deflection a time of 8%;
5, the blank with step 4 places vacuum heat treatment furnace, is heated to 1200 ℃, insulation 2h, and stove is chilled to below 100 ℃ and comes out of the stove;
6, the blank of step 5 is cold rolling by deflection a time of 8%;
7, the blank with step 6 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 650 ℃ of insulation 3.5h, and stove is chilled to below 100 ℃ and comes out of the stove;
8, the blank of step 7 is cold rolling by deflection a time of 8%;
9, the blank with step 8 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 650 ℃ of insulation 3.5h, and stove is chilled to below 100 ℃ and comes out of the stove;
10, the blank of step 9 is cold rolling by deflection a time of 8%;
11, the blank with step 10 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 650 ℃ of insulation 3.5h, and stove is chilled to below 100 ℃ and comes out of the stove;
12., breaking down: use two roller levelling machines,, and roll and be as thin as certain thickness the blank thin plate shaping of step 11;
14, finish rolling: use finishing mill, the blank plate of step 12 is rolled into client's desired thickness
15, annealing: place vacuum or well formula atmosphere furnace to anneal step 14 gained blank plate.
16. moulding:, be processed into client's desired size and shape with wire cutting machine tool with 15 gained nickel plates
17, surface finish is handled
Through checking: the finished product that step 15 obtains, Ni+Co: 〉=99.98; C:0.0015; Si:0.00012; Cu:0.0001; Fe:0.001; S:0.00018; The Zn:0.0002Pb:0.0002 trace impurity :≤0.0162, resistance 7.85 μ Ω .cm.
Embodiment 3:
1, gets electrolytic nickel slab material, cut into the wide lath shape of 100mm;
2, cold rolling by deflection a time of 10%;
3, the blank with step 2 places vacuum heat treatment furnace, is heated to 1400 ℃, insulation 3h, and stove is chilled to below 100 ℃ and comes out of the stove;
4, the blank of step 3 is cold rolling by deflection a time of 10%;
5, the blank with step 4 places vacuum heat treatment furnace, is heated to 1400 ℃, insulation 3h, and stove is chilled to below 100 ℃ and comes out of the stove;
6, the blank of step 5 is cold rolling by deflection a time of 10%;
7, the blank with step 6 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 700 ℃ of insulation 5h, and stove is chilled to below 100 ℃ and comes out of the stove;
8, the blank of step 7 is cold rolling by deflection a time of 10%;
9, the blank with step 8 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 700 ℃ of insulation 5h, and stove is chilled to below 100 ℃ and comes out of the stove;
10, the blank of step 9 is cold rolling by deflection a time of 10%;
11, the blank with step 10 places cracked ammonium atmosphere protection heat treatment furnace to be heated to 700 ℃ of insulation 5h, and stove is chilled to below 100 ℃ and comes out of the stove;
12., breaking down: use two roller levelling machines,, and roll and be as thin as certain thickness the blank thin plate shaping of step 11;
14, finish rolling: use finishing mill, the blank plate of step 12 is rolled into client's desired thickness
15, annealing: place vacuum or well formula atmosphere furnace to anneal step 14 gained blank plate.
16. moulding:, become client's desired size and shape with the hole shape Roller Machining with 15 gained nickel plates
17, surface finish is handled, and shaping
Through checking: the finished product that step 15 obtains, Ni+Co: 〉=99.985; C :≤0.0019; Si:0.0001; Cu:0.0001; Fe:0.001; S:0.00017; The Zn:0.00019Pb:0.0002 trace impurity :≤0.0162, resistance 7.80 μ Ω .cm.
Claims (3)
1, a kind of nickel-based target, percentage composition is as follows by weight:
Ni+Co：≥99.98；C：≤0.002；Si：≤0.0001；Cu：≤0.0001；Fe：≤0.001；
S：≤0.0002；Zn：≤0.0002Pb：≤0.0002
Trace impurity :≤0.0162.
2, a kind of nickel-based target production technique comprises the steps:
1) cold rolling: the deflection by 8～30% is cold rolling to sheet nickel;
2) high-temperature heat treatment: the blank vacuum (perhaps protective atmosphere) after step 1 processing is heated to 1000～1400 ℃, is incubated 1～3 hour, stove is chilled to below 100 ℃ and comes out of the stove;
3) repeating step 1,2, reach 40～100um to the blank grain-size;
4) atmosphere protection thermal treatment: step 3 gained blank is heated to 600～700 ℃ under protective atmosphere, is incubated 2～5 hours, stove is chilled to below 100 ℃;
5) cold rolling: as to be undertaken cold rolling by 8～30% deflection step 4 gained blank;
6) repeating step 4,5, reach≤10um up to the blank grain-size;
7) breaking down:, and roll and be as thin as certain thickness with the shaping of step 6 gained blank;
8) finish rolling: it is the required panel material of client that step 7 gained blank is rolled into thickness;
9) annealing: step 8 gained sheet material is annealed in vacuum or atmosphere furnace.
10) moulding: be processed into the regulation shape by groove rolling or other working methods.
11) surface treatment: the surface is handled to satisfy service requirements.
3, the production technique of a kind of nickel-based target according to claim 2 is characterized in that: protective atmosphere thermal treatment can adopt ammonia decomposing protection atmosphere, pure hydrogen atmosphere, argon gas, nitrogen, very aerial any one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810032181 CN101660123B (en) | 2008-08-28 | 2008-08-28 | Nickel-based target and production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810032181 CN101660123B (en) | 2008-08-28 | 2008-08-28 | Nickel-based target and production process |
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| CN101660123A true CN101660123A (en) | 2010-03-03 |
| CN101660123B CN101660123B (en) | 2013-08-14 |
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| CN 200810032181 Expired - Fee Related CN101660123B (en) | 2008-08-28 | 2008-08-28 | Nickel-based target and production process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102672447A (en) * | 2011-03-17 | 2012-09-19 | 沈翠珊 | Manufacturing method of high-purity nickel strap |
| CN105296941A (en) * | 2015-11-23 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Preparing of nickel base tube-shaped cathode target material and application in vacuum electric arc plating coating and plating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1715454A (en) * | 2001-08-01 | 2006-01-04 | 株式会社日矿材料 | Method for producing high-purty nickel, high-purity nickel formed sputtering target and thin film formed by using said sputtering target |
| CN1723292A (en) * | 2002-12-09 | 2006-01-18 | 霍尼韦尔国际公司 | High purity nickel/vanadium sputtering components, and methods of making sputtering components |
| US20060292028A1 (en) * | 2003-10-07 | 2006-12-28 | Nikko Materials Co., Ltd. | High-purity ni-v alloy target therefrom high-purity ni-v alloy thin film and process for producing high-purity ni-v alloy |
-
2008
- 2008-08-28 CN CN 200810032181 patent/CN101660123B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1715454A (en) * | 2001-08-01 | 2006-01-04 | 株式会社日矿材料 | Method for producing high-purty nickel, high-purity nickel formed sputtering target and thin film formed by using said sputtering target |
| CN1723292A (en) * | 2002-12-09 | 2006-01-18 | 霍尼韦尔国际公司 | High purity nickel/vanadium sputtering components, and methods of making sputtering components |
| US20060292028A1 (en) * | 2003-10-07 | 2006-12-28 | Nikko Materials Co., Ltd. | High-purity ni-v alloy target therefrom high-purity ni-v alloy thin film and process for producing high-purity ni-v alloy |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102672447A (en) * | 2011-03-17 | 2012-09-19 | 沈翠珊 | Manufacturing method of high-purity nickel strap |
| CN102672447B (en) * | 2011-03-17 | 2014-04-30 | 沈翠珊 | Manufacturing method of high-purity nickel strap |
| CN105296941A (en) * | 2015-11-23 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Preparing of nickel base tube-shaped cathode target material and application in vacuum electric arc plating coating and plating |
| CN105296941B (en) * | 2015-11-23 | 2017-12-19 | 沈阳黎明航空发动机(集团)有限责任公司 | The preparation and the application in vacuum arc plating coating of a kind of Ni-based sleeve cathode target |
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| CN101660123B (en) | 2013-08-14 |
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Effective date of registration: 20190408 Address after: 410100 No.1 Sanyi Road, Changsha Economic and Technological Development Zone, Hunan Province Patentee after: HUNAN XIANDENG INTELLIGENT TECHNOLOGY CO., LTD. Address before: 410100 Longping High-tech Park, Hi-tech Industrial Development Zone, Furong District, Changsha City, Hunan Province Patentee before: Changsha Tianying Metal Materials Co., Ltd. |
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