CN104646930A - Manufacturing method of Ni-W-Cr alloy target - Google Patents
Manufacturing method of Ni-W-Cr alloy target Download PDFInfo
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- CN104646930A CN104646930A CN201310596415.5A CN201310596415A CN104646930A CN 104646930 A CN104646930 A CN 104646930A CN 201310596415 A CN201310596415 A CN 201310596415A CN 104646930 A CN104646930 A CN 104646930A
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a manufacturing method of a Ni-W-Cr alloy target. The method orderly comprises a blending step, a smelting and ingot casting step, a forging step, a primary heat treatment step, a rolling step, a secondary heat treatment step and a machining finished-product production step. The Ni-W-Cr alloy target manufactured by use of the method has the advantages of accurate finished product component control, uniform component distribution, no segregation, no inclusion, fine and even crystal grains, high finished product purity and the like; specifically, the component control accuracy is less than or equal to 0.2at%, the mean grain size is not greater than 16 microns, and the purity is above 99.95%.
Description
Technical field
The invention belongs to metallurgical preparation field, particularly a kind of manufacture method of Ni-W-Cr alloy target material, it is specially adapted to magnetron sputtering.
Background technology
Hard disk is the data Primary memory part of computer, in recent years due to all kinds of consumer electronics product, as computer, mobile phone, camera, portable large capacity voice and video player, game machine, palm PC, vehicle-mounted digital product etc., and hospital, school, bank, industrial automation and traffic safety etc. constantly increase the demand read and write data, although have semiconductor storage and optical storage etc. to compete with it, but because it has high cost performance, the product that can substitute it completely is not also had to come out, in today of scientific and technological high speed development, the importance of magnetic recording hard disk is self-evident, this just requires that the area of single recorded bit in magnetic material is more and more less.
In addition, along with human knowledge's nature and exploitation are naturally progressive, magnetic recording hard disk, except the use met under general condition, also will meet the normal work in adverse circumstances, especially in the environment of some warm moist, so the video disc of magnetic recording hard disk will possess certain etch resistant properties.At present, conventional nickel-base alloy has NiV, NiW, NiCr, Ni-W-Cr etc., and the shortcoming of NiV or NiW alloy is that such alloy corrosion resistance is poor, after particularly rete exceedes certain thickness.Comparatively speaking, Ni-W-Cr alloy is a kind of important corrosion resistant alloy coating materials.Except film material will meet certain corrosion resistance, whether membranous layer ingredient is even, and have segregation-free, rete is with or without being mingled with, whether film surface is smooth very crucial, and these sputtering target materials all with used are relevant, and the Ni-W-Cr alloy manufactured at present is easy to occur large-area micro components segregation, therefore develops Composition Control accurate, distributed components, segregation-free, without being mingled with, uniform small grains, the Ni-W-Cr alloy target material that finished product purity is high is very necessary.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of manufacture method of Ni-W-Cr alloy target material, the finished product Composition Control of the Ni-W-Cr alloy target material that the method obtains is accurate, distributed components, segregation-free, without being mingled with, uniform small grains, finished product purity is high, is specially adapted to magnetron sputtering.
To achieve these goals, present invention employs following technical scheme:
A manufacture method for Ni-W-Cr alloy target material, comprises batching step successively, melting, ingot casting stage, forging step, a heat treatment step, and milling step, secondary heat treatment step and machined manufacture a finished product step, wherein:
In described melting, ingot casting stage, described melting adopts vacuum induction melting, and wherein refining time is 10 ~ 15 minutes; Cast when alloy liquid temperature reaches more than liquidus curve 50 ~ 100 DEG C;
In described forging step, carry out forging to obtain forging stock after ingot casting is incubated 2 ~ 4 hours under 1050 ~ 1250 DEG C of conditions;
In a described heat treatment step, forging stock is incubated under 1200 DEG C ~ 1320 DEG C conditions and within 12 ~ 36 hours, heat-treats;
In described milling step, carry out hot rolling after the slab after a heat treatment is incubated 1 ~ 1.5 hour under 1050 ~ 1250 DEG C of conditions, be then cooled to room temperature and carry out cold rolling at ambient temperature, described cold rolling total deformation is more than 50%.
In described secondary heat treatment step, the slab obtained after cold rolling is incubated 30 ~ 120 minutes, air cooling of coming out of the stove under 900 DEG C ~ 1100 DEG C conditions.
In the above-mentioned methods, adopt vacuum induction melting, avoid the introducing of field trash; After forging, carry out high temperature solution treated, eliminate component segregation; Carry out cold rolling after hot rolling, ensure cold rollingly have the deflection being greater than 50% with Broken Crystal; Recrystallization process is carried out to control crystallite dimension after cold rolling.The purity > 99.95% of the Ni-W-Cr alloy target material obtained by said method, mean grain size controls within 15 μm, without component segregation.
In order to more detailed, said method is described, said method can exemplarily be described as: in described melting, ingot casting stage, described refining time can be 10min, 12min, 13min or 14min, the alloy liquid temperature after melting reach more than liquidus curve 55 DEG C, 65 DEG C, 70 DEG C, 80 DEG C or 95 DEG C time cast;
In described forging step, described ingot casting can be incubated 2h, 2.5h, 3h or 4h under 1055 DEG C, 1150 DEG C, 1190 DEG C, 1230 DEG C or 1245 DEG C of conditions;
In a described heat treatment step, described forging stock is incubated 12h, 18h, 23h, 28h, 32h, 35h or 36h hour under 1200 DEG C, 1220 DEG C, 1260 DEG C, 1285 DEG C, 1290 DEG C or 1315 DEG C of conditions;
In described milling step, hot rolling is carried out after slab after a heat treatment is incubated 1h, 1.2h or 1.5h under 1050 DEG C, 1070 DEG C, 1090 DEG C, 1102 DEG C, 1150 DEG C, 1180 DEG C, 1210 DEG C or 1250 DEG C of conditions, then be cooled to room temperature and carry out cold rolling at ambient temperature, described cold rolling total deformation can be 50-55%, 60-70%, 53%, 58% or 67%, is preferably 50-60%;
In described secondary heat treatment step, described cold rolling after the slab that obtains under 900 DEG C, 950 DEG C, 1000 DEG C, 1050 DEG C, 1070 DEG C or 1100 DEG C of conditions, be incubated 35min, 50min, 70min, 90min or 110min.
In the above-mentioned methods, described batching step refers to and takes Ni(nickel by the constituent content of designed Ni-W-Cr alloy target material), W(tungsten), Cr(chromium) raw metal, as a kind of preferred embodiment, the Ni-W-Cr alloy target material of the method manufacture is made up of following element by atomic percent: Cr4-20%, W5-15%, Ni65 ~ 91%, described Ni-W-Cr alloy target material is preferably made up of following element by atomic percent: Cr8-15%, W7-12%, Ni75-85%.
In the above-mentioned methods, as a kind of preferred embodiment, in described milling step, the slab after a heat treatment is put into the Muffle furnace of steel rolling heating to be incubated 1 ~ 1.5 hour under 1100 ~ 1200 DEG C of conditions.
In the above-mentioned methods, raw metal is high-purity, and purity is more than 99.95%.
Compared to prior art, the present invention has following beneficial effect: it is accurate that the present invention has finished product Composition Control, distributed components, segregation-free, without being mingled with, and uniform small grains, finished product purity advantages of higher.Above-mentioned advantage is specific as follows: Composition Control accurately≤0.2at%, mean grain size is not more than 16 μm, high purity more than 99.95%, is less than 100ppm by the content selecting vacuum high in raw material, fusion process and heating process to realize nonmetallic inclusion oxygen in target, the content of carbon is less than 50ppm.
Accompanying drawing explanation
Fig. 1 is the high power metallographic structure figure of the Ni-W-Cr alloy target material that the embodiment of the present invention 1 obtains.
Fig. 2 is the ESEM back scattering figure of the Ni-W-Cr alloy target material that the embodiment of the present invention 1 obtains.
Fig. 3 is the ESEM back scattering figure of the Ni-W-Cr alloy target material that comparative example 1 obtains.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail, but the present invention is not limited to this.
Four embodiments have prepared 4 batches of Ni-W-Cr alloy disks respectively according to the manufacture method of Ni-W-Cr alloy target material of the present invention below.
Embodiment 1
Ni-W-Cr alloy disks prepared by the present embodiment is made up of following element by atomic percent: Ni:81%, W:15%, Cr:4%.
The specification of alloy disks prepared by the present embodiment is Φ 170 × 6.35mm.
Manufacture method is as follows:
(1) prepare burden: by the designing requirement of above-mentioned alloy target material composition take the nickel of 99.95%, the High Pure Chromium of 99.95% and 99.95% high-purity tungsten bar;
(2) melting, ingot casting: the nickel weighed up, chromium and tungsten metal derby are put into vacuum induction melting furnace, (namely smelting by technique well known in the art) is smelted by normal smelting process, wherein during melting vacuum degree control at 0.1Pa, smelting temperature controls 1650 ~ 1700 DEG C (the present embodiment controls at about 1680 DEG C), refining time is 15min, and cast temperature is 1580 DEG C;
(3) forge: melting gained ingot blank is put into Muffle furnace, carry out forge hot 1250 DEG C of insulations after 4 hours, obtain the slab of 218*174*35.5mm specification;
(4) heat treatment: the slab after forging is put into Muffle furnace, 1320 DEG C of insulations 30 hours;
(5) rolling: the Muffle furnace slab after a heat treatment being put into steel rolling heating, hot rolling is carried out after 1.5 hours 1250 DEG C of insulations, pass deformation is (pass deformation of the present embodiment is about 22%) between 20% ~ 25%, obtains the slab of 455*176*16.5mm specification; Then naturally cool to room temperature also at room temperature cold rolling, time cold rolling, pass deformation is 10%, and total deformation is 53%, and the specification of cold rolling rear slab is 995*177*7.5mm;
(6) secondary heat treatment: Muffle furnace put into by the slab that rolling is good, 1100 DEG C of insulations 30 minutes, air cooling of coming out of the stove;
(7) machined: by the Ni-W-Cr alloy slab after secondary heat treatment by dimensional requirement machined, first Linear cut becomes the disk of given size, then become to meet the Ni-W-Cr alloy target material of dimensional accuracy with lathe car.
Alloy target material end properties prepared by the present embodiment is see table 1, and figure is see Fig. 1 in its metallographic structure.
As can be seen from Fig. 1, crystal grain is even, and mean grain size is less than 16 μm; As can be seen from Fig. 2, target finished product is without component segregation.
Embodiment 2
Ni-W-Cr alloy disks prepared by the present embodiment is made up of following element by atomic percent: Ni:82%, W:10%, Cr:8%.
The specification of alloy disks prepared by the present embodiment is Φ 170 × 6.35mm.
Manufacture method is as follows:
(1) prepare burden: by the designing requirement of above-mentioned alloy target material composition take the nickel of 99.95%, the High Pure Chromium of 99.95% and 99.95% high-purity tungsten bar;
(2) melting, ingot casting: the nickel weighed up, chromium and tungsten metal derby are put into vacuum induction melting furnace, (namely smelting by technique well known in the art) is smelted by normal smelting process, wherein during melting vacuum degree control at 0.1Pa, smelting temperature controls 1650 ~ 1700 DEG C (the present embodiment controls at about 1650 DEG C), wherein refining time is 15min, and cast temperature is 1550 DEG C;
(3) forge: melting gained ingot blank is put into Muffle furnace, carry out forge hot 1200 DEG C of insulations after 3 hours, obtain the slab of 210*175*35.5mm specification;
(4) heat treatment: the slab after forging is put into Muffle furnace, 1280 DEG C of insulations 24 hours;
(5) rolling: the Muffle furnace slab after a heat treatment being put into steel rolling heating, carry out hot rolling 1200 DEG C of insulations after 1 hour, pass deformation controls about 20%, obtains the slab of 450*176*16.5mm specification; Then naturally cool to room temperature also at room temperature cold rolling, time cold rolling, pass deformation is 10%, and total deformation is 54%, and the specification of cold rolling rear slab is 980*177*7.6mm;
(6) secondary heat treatment: Muffle furnace put into by the slab that rolling is good, 1050 DEG C of insulations 50 minutes, air cooling of coming out of the stove;
(7) machined: by the Ni-W-Cr alloy slab after secondary heat treatment by dimensional requirement machined, first Linear cut becomes the disk of given size, then become to meet the Ni-W-Cr alloy target material of dimensional accuracy with lathe car.
Alloy target material end properties prepared by the present embodiment is see table 1.
Embodiment 3
Ni-W-Cr alloy disks prepared by the present embodiment is made up of following element by atomic percent: Ni:81%, W:5%, Cr:14%.
The specification of alloy disks prepared by the present embodiment is Φ 170 × 6.35mm.
Manufacture method is as follows:
(1) prepare burden: by the designing requirement of above-mentioned alloy target material composition take the nickel of 99.95%, the High Pure Chromium of 99.95% and 99.95% high-purity tungsten bar;
(2) melting, ingot casting: the nickel weighed up, chromium and tungsten metal derby are put into vacuum induction melting furnace, by normal smelting process smelt (namely smelting by technique well known in the art) wherein melting time vacuum degree control at 0.1Pa, smelting temperature controls 1650 ~ 1700 DEG C (the present embodiment controls at about 1680 DEG C), wherein refining time is 10min, and cast temperature is 1530 DEG C;
(3) forge: melting gained ingot blank is put into Muffle furnace, carry out forge hot 1050 DEG C of insulations after 2 hours, obtain the slab of 215*174*35.5mm specification;
(4) heat treatment: the slab after forging is put into Muffle furnace, 1200 DEG C of insulations 12 hours;
(5) rolling: the Muffle furnace slab after a heat treatment being put into steel rolling heating, carry out hot rolling 1050 DEG C of insulations after 1.5 hours, pass deformation controls about 25%, obtains the slab of 445*176*17mm specification; Then naturally cool to room temperature also at room temperature cold rolling, time cold rolling, pass deformation is 10%, and total deformation is 55%, and the specification of cold rolling rear slab is 1010*176*7.5mm;
(6) secondary heat treatment: Muffle furnace put into by the slab that rolling is good, 900 DEG C of insulations 120 minutes, air cooling of coming out of the stove;
(7) machined: by the Ni-W-Cr alloy slab after secondary heat treatment by dimensional requirement machined, first Linear cut becomes the disk of given size, then become to meet the Ni-W-Cr alloy target material of dimensional accuracy with lathe car.
Alloy target material end properties prepared by the present embodiment is see table 1.
Embodiment 4
Ni-W-Cr alloy disks prepared by the present embodiment is made up of following element by atomic percent: Ni:72%, W:8%, Cr:20%.
The specification of alloy disks prepared by the present embodiment is Φ 170 × 6.35mm.
Manufacture method is as follows:
(1) prepare burden: by the designing requirement of above-mentioned alloy target material composition take the nickel of 99.95%, the High Pure Chromium of 99.95% and 99.95% high-purity tungsten bar;
(2) melting, ingot casting: the nickel weighed up, chromium and tungsten metal derby are put into vacuum induction melting furnace, by normal smelting process smelt (namely smelting by technique well known in the art) wherein melting time vacuum degree control at 0.1Pa, smelting temperature controls 1650 ~ 1700 DEG C (the present embodiment controls at about 1680 DEG C), wherein refining time is 12min, and cast temperature is 1580 DEG C;
(3) forge: melting gained ingot blank is put into Muffle furnace, carry out forge hot 1100 DEG C of insulations after 3 hours, obtain the slab of 220*175*35.5mm specification;
(4) heat treatment: the slab after forging is put into Muffle furnace, 1250 DEG C of insulations 36 hours;
(5) rolling: the Muffle furnace slab after a heat treatment being put into steel rolling heating, carry out hot rolling 1200 DEG C of insulations after 1.5 hours, pass deformation controls about 25%, obtains the slab of 450*175*17.3mm specification; Then naturally cool to room temperature also at room temperature cold rolling, time cold rolling, pass deformation is 10%, and total deformation is 54%, and the specification of cold rolling rear slab is 1020*175*7.6mm;
(6) secondary heat treatment: Muffle furnace put into by the slab that rolling is good, 1000 DEG C of insulations 70 minutes, air cooling of coming out of the stove;
(7) machined: by the Ni-W-Cr alloy slab after secondary heat treatment by dimensional requirement machined, first Linear cut becomes the disk of given size, then become to meet the Ni-W-Cr alloy target material of dimensional accuracy with lathe car.
Alloy target material end properties prepared by the present embodiment is see table 1.
Comparative example 1
The alloy target material composition of preparation is identical with embodiment 1 with size.
Preparation method: except not carrying out a heat treatment step, other operating procedures are identical with embodiment 1.
The alloy target material end properties that this comparative example obtains is see table 1.As can be seen from Fig. 3, there is more serious component segregation in target finished product.
Comparative example 2
The alloy target material composition of preparation is identical with embodiment 1 with size.
Preparation method: except not carrying out hot rolling process, other operating procedures are identical with embodiment 1, namely directly carry out cold rolling after a heat treatment.
The alloy target material end properties that this comparative example obtains is see table 1.
Comparative example 3
The alloy target material composition of preparation is identical with embodiment 1 with size.
Preparation method: except not carrying out a heat treatment and hot rolling process, other operating procedures are identical with embodiment 1, namely directly carry out cold rolling after forge hot.
The alloy target material end properties that this comparative example obtains is see table 1.
The properties of product table of table 1 embodiment of the present invention
The method of testing of properties of product described in table 1 is as follows:
Composition tolerances is that alloy component analysis adopts energy dispersion X-ray spectrometer (EDX) or Xray fluorescence spectrometer (XRF) by obtaining after alloy component analysis is carried out in the different parts sampling of same finished product target.
The mensuration of purity adopts ICP or GDMS method to measure.
Mean grain size is by GB/T6394-2002(mean grain size grading (resection)) calculate.
Should be appreciated that the purposes of these embodiments is only not intended to for illustration of the present invention limit the scope of the invention.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various change, amendment and/or modification to the present invention, and these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (6)
1. a manufacture method for Ni-W-Cr alloy target material, is characterized in that, comprises batching step successively, melting, ingot casting stage, forging step, a heat treatment step, and milling step, secondary heat treatment step and machined manufacture a finished product step, wherein:
In described melting, ingot casting stage, described melting adopts vacuum induction melting, and wherein refining time is 10 ~ 15 minutes; Cast when alloy liquid temperature reaches more than liquidus curve 50 ~ 100 DEG C;
In described forging step, carry out forging to obtain forging stock after ingot casting is incubated 2 ~ 4 hours under 1050 ~ 1250 DEG C of conditions;
In a described heat treatment step, forging stock is incubated under 1200 DEG C ~ 1320 DEG C conditions and within 12 ~ 36 hours, heat-treats;
In described milling step, carry out hot rolling after the slab after a heat treatment is incubated 1 ~ 1.5 hour under 1050 ~ 1250 DEG C of conditions, be then cooled to room temperature and carry out cold rolling at ambient temperature, described cold rolling total deformation is more than 50%;
In described secondary heat treatment step, the slab obtained after cold rolling is incubated 30 ~ 120 minutes, air cooling of coming out of the stove under 900 DEG C ~ 1100 DEG C conditions.
2. manufacture method according to claim 1, is characterized in that, the Ni-W-Cr alloy target material of described method manufacture is made up of following element by atomic percent: Cr4-20%, W5-15%, Ni65 ~ 91%.
3. manufacture method according to claim 2, is characterized in that, the Ni-W-Cr alloy target material of described method manufacture is made up of following element by atomic percent: Cr8-15%, W7-12%, Ni75 ~ 85%.
4. manufacture method according to claim 1, is characterized in that, in described milling step, the slab after a heat treatment is put into the Muffle furnace of steel rolling heating to be incubated 1 ~ 1.5 hour under 1100 ~ 1200 DEG C of conditions.
5. manufacture method according to claim 1, is characterized in that, the purity of the raw metal used in described batching step is more than 99.95%.
6. manufacture method according to claim 1, is characterized in that, in described milling step, described cold rolling total deformation is 50-60%.
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| CN111411266A (en) * | 2020-05-08 | 2020-07-14 | 中国华能集团有限公司 | Preparation process of nickel-based high-tungsten polycrystalline superalloy |
| CN114752816A (en) * | 2022-03-15 | 2022-07-15 | 北京科技大学 | Die alloy for isothermal forging and preparation method thereof |
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| CN111411266A (en) * | 2020-05-08 | 2020-07-14 | 中国华能集团有限公司 | Preparation process of nickel-based high-tungsten polycrystalline superalloy |
| CN111411266B (en) * | 2020-05-08 | 2021-03-16 | 中国华能集团有限公司 | Preparation process of nickel-based high-tungsten polycrystalline superalloy |
| CN114752816A (en) * | 2022-03-15 | 2022-07-15 | 北京科技大学 | Die alloy for isothermal forging and preparation method thereof |
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