CN116786810A - Chromium powder for sputtering target and preparation method thereof - Google Patents
Chromium powder for sputtering target and preparation method thereof Download PDFInfo
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- CN116786810A CN116786810A CN202310846955.8A CN202310846955A CN116786810A CN 116786810 A CN116786810 A CN 116786810A CN 202310846955 A CN202310846955 A CN 202310846955A CN 116786810 A CN116786810 A CN 116786810A
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 238000005477 sputtering target Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000746 purification Methods 0.000 claims abstract description 61
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 37
- 239000011651 chromium Substances 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 33
- 239000001257 hydrogen Substances 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000010298 pulverizing process Methods 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 22
- 239000000843 powder Substances 0.000 description 14
- 239000003792 electrolyte Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000013077 target material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000012216 screening Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- -1 data storage Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
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- Chemical & Material Sciences (AREA)
- 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 application belongs to the technical field of powder metallurgy materials and preparation thereof, and particularly relates to chromium powder for a sputtering target and a preparation method thereof. The application discloses chromium powder for a sputtering target and a preparation method thereof, wherein the purity of the chromium powder is more than 99.95 percent, the O content in the chromium powder is less than 150ppm, and the S content in the chromium powder is less than 30ppm. The preparation method of the chromium powder for the sputtering target comprises the following steps: and (3) purification: purifying the chromium slices; crushing: and crushing the purified chromium slices to obtain the chromium powder. The chromium powder prepared by the application has the characteristics of purity of more than 99.95%, low gas impurity content and adjustable particle size distribution.
Description
Technical Field
The application belongs to the technical field of powder metallurgy materials and preparation thereof, and particularly relates to chromium powder for a sputtering target and a preparation method thereof.
Background
Along with the rapid development of coating technology, chromium targets have been widely used in the fields of decorative coating, optical coating, data storage, coating of automobile parts and the like. Wherein high-purity chromium targets are needed for high-end semiconductors, chips, precision electronic products, automobile piston rings and optical material coating films. The raw material for preparing the high-purity chromium target is the chromium powder with high purity and low gas impurity content, the purity of which is more than 99.95 percent. The chemical composition requirements of the high purity, low gas content chromium powder are shown in table 1.
TABLE 1 high purity chromium powder chemical composition
Under vacuum condition, electrolytic chromium flakes with a purity of 99.95% can be obtained by contact with a suitable thermal deposition surface, i.e. electrolytic method, but the gas impurity O content reaches more than 5000ppm and the S content reaches more than 200ppm. Firstly, the electrolytic chromium sheet must be purified to reduce O, S content; secondly, the electrolytic piece is crushed and pulverized to meet the requirement of high-purity low-gas chromium powder for target materials. There is no related patent for mass production of high-purity low-gas chromium powder for targets.
Disclosure of Invention
Aiming at the defects and the defects existing in the prior art, the application aims to provide chromium powder for a sputtering target and a preparation method thereof, wherein the chromium powder has the characteristics of purity of more than 99.95%, low gas impurity content and adjustable particle size distribution. The purity of the produced target material is more than 99.95%, the relative density is high, the content of gas impurities is low, and the structure is uniform.
The technical scheme adopted for solving the technical problems is as follows:
a chromium powder for a sputtering target, the purity of the chromium powder is more than 99.95 percent (wherein, the purity is (1-sum of metal impurities) ×100 percent), the O content in the chromium powder is less than 150ppm, and the S content is less than 30ppm.
In the above chromium powder for sputtering target, as a preferred embodiment, the tap density of the chromium powder is greater than 4.0g/cm 3 The average particle size of the chromium powder is less than 80 mesh, preferably the average particle size of the chromium powder is greater than 325 mesh.
The preparation method of the chromium powder for the sputtering target comprises the following steps:
and (3) purification: purifying the chromium slices;
crushing: and crushing the purified chromium slices to obtain the chromium powder.
In the above method for producing chromium powder for a sputtering target, as a preferred embodiment, in the purifying step, the chromium flakes are electrolytic chromium flakes; preferably, the electrolytic chromium sheet is prepared by an electrolytic method.
In the above-mentioned method for producing chromium powder for a sputtering target, as a preferred embodiment, in the purification step, the length of the chromium flakes is 2 to 80mm (e.g., 2 to 10mm, 20 to 40mm, 50 to 80 mm); preferably, the purity of the chromium flakes is 99.96% or more, the O content is less than 5500ppm, and the S content is less than 250ppm.
In the above method for producing chromium powder for a sputtering target, as a preferred embodiment, in the purifying step, the chromium flakes are purified by hydrogen gas which is introduced from the lower portion of the container containing the chromium flakes and flows out from the upper portion of the container containing the chromium flakes; preferably, the purification treatment is performed in a horizontal vacuum hydrogen furnace, and the hydrogen flow direction is lower in and upper out; because of low hydrogen density, the mode of lower inlet and upper outlet is more favorable for the smooth penetration of hydrogen through all original electrolytic chromium plates. Preferably, the chromium sheets are stacked, and gaps exist between the upper, lower, left and right adjacent chromium sheets so as to facilitate hydrogen circulation and deoxidation; if the length of the chromium sheet is too large, the circulation of hydrogen is not facilitated, and if the length of the chromium sheet is too small, the collection is not facilitated. The application adopts hydrogen for purification, and can avoid the problem that impurities are easy to be introduced when graphite powder and tin powder are used for purification.
In the above-mentioned method for producing chromium powder for a sputtering target, as a preferred embodiment, in the purification step, the purification treatment is performed under a negative pressure, preferably a negative hydrogen pressure condition, preferably the purification treatment is performed under a hydrogen pressure of 2000 to 10000Pa (e.g., 2000Pa, 3000Pa, 4000Pa, 5000Pa, 6000Pa, 7000Pa, 8000Pa, 9000 Pa).
In the above method for producing chromium powder for a sputtering target, as a preferred embodiment, in the purification step, the purification treatment is carried out at a temperature of 1350 to 1550 ℃ (e.g., 1350 ℃, 1390 ℃, 1430 ℃, 1470 ℃, 1510 ℃, 1550 ℃) for a time of 10 to 20 hours (e.g., 10 hours, 12 hours, 14 hours, 16 hours, 18 hours, 20 hours), preferably, the amount of hydrogen consumed for purifying the chromium sheet is 0.2 to 0.8m 3 Kg (e.g. 0.3 m) 3 /kg、0.4m 3 /kg、0.5m 3 /kg、0.6m 3 /kg、0.7m 3 /kg)。
In the above-described method for producing chromium powder for a sputtering target, as a preferred embodiment, in the pulverizing step, the pulverizing includes crushing and grinding; preferably, the chromium particles obtained after the crushing are smaller than 5mm (e.g. 0.5-1mm, 2-3mm, 4-5 mm); preferably, the grinding is an air flow mill or an impact mill, and the average particle size of the chromium powder obtained after the grinding is less than 80 mesh (e.g., 250-325 mesh, 150-200 mesh, 80-100 mesh), preferably, the average particle size of the chromium powder is greater than 325 mesh; if the average granularity of the chromium powder is larger than 80 meshes, the prepared target microstructure is coarse, and the difficulty of improving the density of the target preparation process is increased; if the average granularity of the chromium powder is smaller than 325 meshes, the chromium powder is difficult to crush, the requirement on crushing equipment is high, and the oxygen content is easy to increase again in the process of pulverizing.
In the above method for preparing chromium powder for a sputtering target, as a preferred embodiment, after the pulverizing step, the method further comprises a batch mixing step of: carrying out batch processing on the chromium powder, and then weighing and packaging; preferably, the batch-mixing treatment is carried out in a double cone mixer, preferably, the batch-mixing treatment is carried out under the protection of inert gas, and the time of the batch-mixing treatment is 2-5h (for example, 2.5h, 3h and 4.5 h).
Compared with the prior art, the application has the following beneficial effects:
(1) The chromium powder prepared by the application has the characteristics of purity of more than 99.95%, low gas impurity content and adjustable particle size distribution.
(2) The application adopts a negative pressure purification process, the hydrogen flow direction is a mode of lower inlet and upper outlet, and the hydrogen consumption for purification is 0.2-0.8m 3 And/kg, the consumed hydrogen amount is small, and the advantages are remarkable.
(3) The purity of the target material produced by the chromium powder prepared by the application is more than 99.95 percent, the relative density is high, the gas impurity content is low, the structure is uniform, and the chromium powder is suitable for coating applications such as high-end semiconductors, precise electronic products, automobile piston rings and the like.
Drawings
FIG. 1 is a morphology diagram of the high purity low gas chromium powder produced in example 1 of the present application.
FIG. 2 is a photograph of a microstructure of a target material produced by the chromium powder produced in example 1 of the present application.
Detailed Description
The present application will be further described with reference to the following examples, which are presented by way of illustration of the application and not limitation, in order to highlight the objects, technical solutions and advantages of the application. The technical scheme of the application is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.
The measurement method of each parameter in the following examples is as follows:
measuring the density of the target material by adopting an Archimedes drainage method; tap density is measured by adopting GB/T5162-2006 of determination of tap density of metal powder; the microstructure was analyzed using a metallographic microscope.
Example 1:
the purity of the original electrolytic chromium sheet used in this example is preferably 99.96% or more, the O content is 5200ppm, and the S content is 190ppm.
The preparation method of the high-purity low-gas chromium powder comprises the following steps:
step one, screening the original electrolyte sheets with the components, wherein the length of the screened electrolyte sheets is 20-50mm;
step two, placing the screened electrolytic piece into a tungsten crucible mold for purification treatment, wherein the purification treatment is performed under the negative pressure condition, namely, the purification treatment is performed under the hydrogen pressure of 3000Pa, the purification treatment temperature is 1400 ℃, the purification treatment time is 12 hours, and the hydrogen consumption for the electrolytic chromium piece purification treatment is 0.5m 3 Kg (gaps exist between adjacent electrolytic chromium plates to ensure smooth gas circulation).
And thirdly, crushing and pulverizing the purified electrolyte sheet. The crushed particles are 2-3mm, and then the crushed particles are put into an air flow mill for grinding, and the average particle size of the ground powder is 150-100 meshes.
And fourthly, putting the ground powder into a double-cone mixer for batch mixing. And mixing under the protection of argon for 3 hours.
The high-purity low-gas chromium tap density obtained by the method reaches 4.1g/cm < 3 >, the average particle size of the powder is 140 meshes, and the chemical components of the powder meet the requirement of a target material. The chromium target prepared by the powder has the characteristics of high purity, high density (the density is more than 7.14g/cm < 3 >), no air holes, uniform structure and uniform grains. The particle size composition of the powder is shown in Table 2, the chemical composition of the powder is shown in Table 3, the morphology of the powder is shown in FIG. 1, and the microstructure of the target prepared from the powder is shown in FIG. 2.
TABLE 2 high purity low gas chromium powder particle size distribution
| Number of meshes | +60 | -60～+100 | -100～+140 | -140～+200 | -200～+325 | -325 |
| Percentage (wt%) | 0 | 3.5 | 42.1 | 29.1 | 18.7 | 6.6 |
TABLE 3 high purity low gas chromium powder chemical composition
Example 2
This embodiment mainly describes the deaeration effect by negative pressure purification. The purity of the original electrolytic chromium plate is preferably 99.96% or more, the O content is 5500ppm, and the S content is 200ppm.
The preparation method of the high-purity low-gas chromium comprises the following steps:
step one, screening the original electrolyte sheets with the components, wherein the length of the screened electrolyte sheets is 20-50mm;
step two, placing the screened electrolytic piece into a tungsten crucible mold for purification treatment, wherein the purification treatment is performed under the negative pressure condition, namely, the purification treatment is performed under the hydrogen pressure of 2500Pa, the purification treatment temperature is 1460 ℃, the purification treatment time is a variable, and the purification treatment time corresponds to the hydrogen consumption amount (under a certain hydrogen pressure) of purifying each kilogram of electrolytic chromium pieceThe longer the time under force, the more hydrogen is consumed, unit m 3 /kg。
And thirdly, crushing and pulverizing the purified electrolyte sheet. The crushed particles are 2-3mm, and then the crushed particles are put into an air flow mill for grinding, and the average particle size of the ground powder is 150-100 meshes. The powder purification effect is shown in Table 4.
TABLE 4 high purity low gas chromium powder gas content
| Purification treatment time | Hydrogen amount (m) 3 /kg) | O(ppm) | S(ppm) |
| 10h | 0.3 | 130 | 26 |
| 13h | 0.4 | 110 | 20 |
| 16h | 0.5 | 87 | 13 |
| 20h | 0.6 | 62 | 10 |
| 26h | 0.8 | 55 | 8 |
Example 3
The purity of the original electrolytic chromium plate is preferably 99.96% or more, the O content is 5500ppm, and the S content is 200ppm.
The preparation method of the high-purity low-gas chromium comprises the following steps:
step one, screening the original electrolyte sheets with the components, wherein the length of the screened electrolyte sheets is 20-50mm;
and step two, placing the screened electrolyte sheet into a tungsten crucible mold for purification treatment, wherein the purification treatment is performed under the negative pressure condition, namely, the purification treatment is performed under 4000Pa hydrogen pressure, the purification treatment time is 15h, and the purification treatment temperature is 1350 ℃.
And thirdly, crushing and pulverizing the purified electrolyte sheet. The crushed particles are 2-3mm, and then the crushed particles are put into an air flow mill for grinding, and the average particle size of the ground powder is 150-100 meshes. The powder purification effect is shown in Table 5.
Example 4
The procedure was the same as in example 3, except that the purification treatment temperature was 1400 ℃. The purification effect of the obtained chromium powder is shown in Table 5.
Example 5
The procedure was the same as in example 3, except that the purification treatment temperature was 1450 ℃. The purification effect of the obtained chromium powder is shown in Table 5.
Example 6
The procedure was the same as in example 3, except that the purification treatment temperature was 1500 ℃. The purification effect of the obtained chromium powder is shown in Table 5.
Example 7
The procedure was the same as in example 3, except that the purification treatment temperature was 1550 ℃. The purification effect of the obtained chromium powder is shown in Table 5.
Table 5 gas content in the high purity low gas chromium powder obtained
| Examples | Purification temperature (. Degree. C.) | O(ppm) | S(ppm) |
| Example 3 | 1350 | 105 | 21 |
| Example 4 | 1400 | 96 | 16 |
| Example 5 | 1450 | 58 | 9 |
| Example 6 | 1500 | 65 | 11 |
| Example 7 | 1550 | 98 | 14 |
As can be seen from the results of the above examples, the chromium powder satisfies the requirements of less than 150ppm of gas content O and less than 30ppm of S at 1350-1550 ℃ in the purification treatment, but has more preferable effect at 1450 ℃.
Comparative example 1
The domestic patent CN1102872C discloses a chromium purification method, which adopts a positive pressure purification method, and the hydrogen pressure is 55x10 7 Under Pa, the hydrogen consumption is 5.17m 3 The O content of 233ppm can be met only when per kg, and the application has the obvious advantages of smaller hydrogen consumption when the negative pressure purification treatment is adopted.
Comparative example 2
The procedure was the same as in example 1, except that the hydrogen pressure during the purification treatment was 1500pa and the purification treatment time was 35 hours, and the purification effect was as follows: the O content is 280ppm, the S content is 45ppm, and the requirements cannot be met.
While the basic principles, principal features and advantages of the present application have been described in the foregoing examples, it will be appreciated by those skilled in the art that the present application is not limited by the foregoing examples, but is merely illustrative of the principles of the application, and various changes and modifications can be made without departing from the scope of the application, which is defined by the appended claims.
Claims (10)
1. The chromium powder for the sputtering target is characterized in that the purity of the chromium powder is more than 99.95 percent, the O content in the chromium powder is less than 150ppm, and the S content in the chromium powder is less than 30ppm.
2. The chromium powder for a sputtering target according to claim 1, wherein the tap density of the chromium powder is greater than 4.0g/cm 3 The average particle size of the chromium powder is less than 80 mesh, preferably the average particle size of the chromium powder is greater than 325 mesh.
3. A method for producing the chromium powder for a sputtering target according to any one of claims 1 to 2, characterized by comprising:
and (3) purification: purifying the chromium slices;
crushing: and crushing the purified chromium slices to obtain the chromium powder.
4. A production method according to claim 3, wherein in the purification step, the chromium sheet is an electrolytic chromium sheet; preferably, the electrolytic chromium sheet is prepared by an electrolytic method.
5. A production method according to claim 3, wherein in the purification step, the length of the chromium flakes is 2 to 80mm; preferably, the purity of the chromium flakes is 99.96% or more, the O content is less than 5500ppm, and the S content is less than 250ppm.
6. The production method according to claim 3, wherein in the purification step, the chromium sheet is subjected to purification treatment with hydrogen gas, the hydrogen gas is introduced from a lower portion of a container accommodating the chromium sheet and flows out from an upper portion of the container accommodating the chromium sheet; preferably, the purification treatment is performed in a horizontal vacuum hydrogen furnace, and the hydrogen flow direction is lower in and upper out.
7. A method of preparation according to claim 3, characterized in that in the purification step the purification treatment is carried out under negative pressure, preferably under negative hydrogen pressure, preferably under a hydrogen pressure of 2000-10000 Pa.
8. A method according to claim 3, wherein the temperature of the purification treatment is 1350-1550 ℃, and the time of the purification treatment is 10-20 hours; preferably, the amount of hydrogen consumed in the purification treatment of the chromium sheet is 0.2 to 0.8m 3 /kg。
9. A production method according to claim 3, wherein in the pulverizing step, the pulverization includes crushing and grinding; preferably, the chromium particles obtained after the crushing are smaller than 5mm; preferably, the grinding is an air flow mill or an impact mill, and the average particle size of the chromium powder obtained after the grinding is less than 80 mesh, preferably the average particle size of the chromium powder is more than 325 mesh.
10. A method of manufacture according to claim 3, wherein after the comminuting step, the method of manufacture further comprises a batch step of: carrying out batch processing on the chromium powder, and then weighing and packaging; preferably, the batch mixing treatment is carried out in a double cone mixer, preferably, the batch mixing treatment is carried out under the protection of inert gas, and the time of the batch mixing treatment is 2-5h.
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| CN102784919A (en) * | 2011-05-16 | 2012-11-21 | 湖南省益浩新材料有限公司 | Method for preparing high-purity superfine chromium powder |
| CN102814501A (en) * | 2012-09-14 | 2012-12-12 | 苏州晶纯新材料有限公司 | Preparation method of ultralow-oxygen chromium powder |
| JP2015196885A (en) * | 2014-04-02 | 2015-11-09 | 株式会社エンハンストマテリアル | Manufacturing method of ultra-low oxygen/ultra-high pure chromium target and ultra-low oxygen/ultra-high pure chromium target |
| CN107385240A (en) * | 2017-07-25 | 2017-11-24 | 北京兴荣源科技有限公司 | It is a kind of can mass production electrolysis chromium piece degasification technique |
| CN107904410A (en) * | 2017-11-03 | 2018-04-13 | 中信锦州金属股份有限公司 | A kind of compound degasser prepares the production method of high temperature alloy and the special high-purity metal chromium of target |
| CN112589099A (en) * | 2020-12-15 | 2021-04-02 | 江苏应用元素科技有限公司 | Method for reducing production cost of multi-arc chromium target |
| CN114713834A (en) * | 2022-03-09 | 2022-07-08 | 自贡硬质合金有限责任公司 | High-purity molybdenum powder for sputtering target and preparation method thereof |
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