CN114182217A - Low-oxygen chromium target and manufacturing method thereof - Google Patents
Low-oxygen chromium target and manufacturing method thereof Download PDFInfo
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- CN114182217A CN114182217A CN202210145047.1A CN202210145047A CN114182217A CN 114182217 A CN114182217 A CN 114182217A CN 202210145047 A CN202210145047 A CN 202210145047A CN 114182217 A CN114182217 A CN 114182217A
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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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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
Abstract
The invention discloses a low-oxygen chromium target and a manufacturing method thereof, and the low-oxygen chromium target comprises the following steps: firstly, carrying out hydrogen reduction treatment on pure chromium powder with a certain granularity; filling and compacting the reduced pure chromium powder into a mold, and placing the pure chromium powder and the mold into a closed high-pressure container filled with a liquid medium for pre-compression treatment to obtain a chromium metal block; thirdly, placing the chromium metal block in hot isostatic pressing equipment for secondary pressing to obtain a chromium target blank; fourthly, annealing the obtained chromium target blank; fifthly, screening out qualified chromium target blanks by utilizing a nondestructive testing process, and then adding the qualified chromium target blanks into the required size by utilizing a machine to obtain the finished chromium target. The method can obtain the isotropic chromium target with low oxygen, high purity, nearly compact and fine and uniform crystal grains, can meet the technical requirement of physical vapor deposition in the photoelectric industry, and can be repeatedly utilized through a special plastic mold, thereby obviously improving the production efficiency and reducing the manufacturing cost of the chromium target.
Description
Technical Field
The invention belongs to the technical field of manufacturing of targets used in photoelectric industries such as TFT-LCD, IC, PCB and the like, and particularly relates to a low-oxygen chromium target and a manufacturing method thereof.
Background
In recent years, the photoelectric industry such as global panel display, touch control, circuit board and semiconductor manufacturing has been rapidly developed and shifted to the home. The chromium film has the advantages of excellent oxidation resistance, light transmission stability, thermal stability and the like, and is widely applied to shading materials and electrode materials in the photoelectric industry. The chromium film in the photoelectric industry is generally manufactured by a physical vapor deposition process such as magnetron sputtering or vacuum evaporation. In the physical vapor deposition process, parameters such as the purity, the density, the grain size and the like of the target have obvious influence on the deposition efficiency, the deposition speed and the film forming quality.
The common chromium target manufacturing method mainly comprises two process routes of vacuum melting and powder metallurgy. The chromium target manufactured by the vacuum melting process inevitably has metallurgical defects such as component segregation, loose shrinkage cavity and the like, and the relative density of the finished target is low, so that the high-standard requirement of the photoelectric industry on the target cannot be met. Compared with a vacuum melting process, the target material manufactured by the powder metallurgy process has high purity, the relative density is close to the theoretical density, and the grain size is controllable, so that the powder metallurgy process gradually replaces the vacuum melting process to become a mainstream process route in the field of chromium target manufacturing. In summary, how to provide a process route that can satisfy the physical property requirements of chromium target such as purity, density and grain size, and simultaneously can improve the production efficiency and reduce the production cost is a problem that needs to be solved by those skilled in the art.
In view of the above, the present inventors propose a low-oxygen chromium target and a method for manufacturing the same to solve the problems of the prior art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a low-oxygen chromium target and a manufacturing method thereof, wherein the manufacturing method can meet the requirements of industries (TFT-LCD, IC, PCB and other photoelectric industries) on the purity, density, grain size and other related performances of the chromium target, and can improve the production efficiency of the target and reduce the production cost.
The purpose of the invention is solved by the following technical scheme:
a manufacturing method of a low-oxygen chromium target mainly comprises the following steps:
step one, carrying out hydrogen reduction treatment on pure chromium powder with a certain particle size;
filling and compacting the pure chromium powder subjected to reduction treatment in the step one into a mold, and then placing the pure chromium powder and the mold into a closed high-pressure container filled with a liquid medium for pre-compression treatment to obtain a chromium metal block;
thirdly, placing the chromium metal block obtained in the second step into hot isostatic pressing equipment for secondary pressing to obtain a chromium target blank;
step four, annealing heat treatment is carried out on the chromium target blank obtained in the step three, so that residual stress generated in the multiple pressing process is eliminated, and the stress induced crack source is reduced;
and fifthly, carrying out full-width flaw detection treatment on the chromium target blank subjected to heat treatment in the fourth step by using a nondestructive detection process, screening out qualified chromium target blanks, and machining the qualified chromium target blanks into required sizes by using a machine to obtain finished chromium targets.
Further, the granularity of the pure chromium powder in the first step is 15-212 mu m, and the purity is more than or equal to 99%.
Further, the temperature of the hydrogen reduction treatment in the first step is set to 900-1300 ℃, and the time is set to 120-300 min.
Further, the mold used in the second step is a plastic elastic mold.
Further, the pressure during pre-pressing treatment in the second step is set to be 90-160 MPa, and the time is set to be 150-400 min.
Further, the third step of hot isostatic pressing is carried out in an inert atmosphere, and after the hot isostatic pressing is finished, argon gas is used for gas cooling.
Further, the specific parameters of the step three hot isostatic pressing treatment are as follows: the pressure is set to be 90-160 MPa, the temperature is set to be 1150-1600 ℃, the temperature rise rate is set to be 3-6 ℃/min, and the pressure maintaining time is set to be 3-15 h.
Furthermore, the annealing temperature in the fourth step is set to be 1000-1400 ℃, the heat preservation time is set to be 20-80 min, and the annealing is carried out in a gas cooling mode.
Further, the nondestructive testing process in the fifth step is mainly to perform flaw detection screening on the manufactured chromium target by using ultrasonic nondestructive testing.
The low-oxygen chromium target is manufactured by the manufacturing method, and the oxygen increment from the original powder to the finished target material of the low-oxygen chromium target is less than or equal to 100 ppm.
Compared with the prior art, the invention has the following beneficial effects:
compared with the prior chromium target manufacturing technology, the low-oxygen chromium target and the manufacturing method thereof have the following advantages: firstly, purifying chromium powder by using a hydrogen reduction method to reduce the content of impurity elements; the method comprises the steps of carrying out pre-pressing forming on chromium powder by utilizing a one-step pre-pressing forming technology to form a chromium metal block, and then carrying out near-net forming on a chromium target blank by utilizing a hot isostatic pressing forming process to further improve the density of the target. The chromium powder can form residual stress in the target after one-step prepressing forming technology and hot isostatic pressing forming, so that the probability of the initiation of defects such as cracks in the target is increased, and the quality of the target is further improved by adopting an annealing process in a post-treatment procedure. In addition, the chromium target manufactured by the method has uniform grain size, and because the powder is pre-pressed and molded by using the one-time liquid high-pressure preforming technology, the links of sheath manufacturing, powder degassing, sheath seal welding leak detection, sheath removal and the like are omitted in the hot isostatic pressing process, and meanwhile, the plastic elastic die can be repeatedly utilized, so that the production efficiency is obviously improved, and the manufacturing cost of the target is reduced.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a block flow diagram of a method of manufacture of the present invention;
FIG. 2 is a microstructure of a chromium target produced in example 1 of the present invention;
FIG. 3 is a microstructure of a chromium target produced in example 2 of the present invention.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus consistent with certain aspects of the invention, as detailed in the appended claims.
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings and examples.
Referring to fig. 1, the method for manufacturing a low-oxygen chromium target of the present invention specifically includes the following steps:
step one, carrying out hydrogen reduction treatment on pure chromium powder with a certain particle size;
specifically, pure chromium powder (the shape of the powder is flaky powder or spherical powder) with the particle size of 15-212 microns and the purity of more than or equal to 99% (for example, the purity of the chromium powder can be 99%, 99.5%, 99.9%, 99.99% or 99.999%, but not limited to the listed values) is reduced by hydrogen for 120-300 min at the temperature of 900-1300 ℃, so that the content of impurity elements is reduced, and the purity of the chromium powder is further improved.
Filling and compacting the pure chromium powder subjected to reduction treatment in the step one into a mold, and then placing the pure chromium powder and the mold into a closed high-pressure container filled with a liquid medium for pre-compression treatment to obtain a chromium metal block;
specifically, the pre-pressing treatment parameters are that the pressure is set to be 90-160 MPa, the time is set to be 150-400 min, the plastic elastic mold is adopted as the rubber mold, the mold can be repeatedly utilized for many times, the production efficiency is obviously improved, and the target manufacturing cost is reduced.
Thirdly, placing the chromium metal block obtained in the second step into hot isostatic pressing equipment for secondary pressing to obtain a chromium target blank;
specifically, the hot isostatic pressing is carried out in an inert atmosphere, a sheath is not needed, links such as sheath preparation, powder degassing, sheath seal welding leak detection, sheath removal and the like are omitted, and the time for manufacturing the chromium target is saved; the specific treatment parameters in the hot isostatic pressing process are as follows: setting the pressure to be 90-160 MPa, setting the temperature to be 1150-1600 ℃, setting the temperature rise rate to be 3-6 ℃/min, and setting the pressure maintaining time to be 3-15 h; and after the hot isostatic pressing is finished, cooling by adopting argon gas. According to the invention, the density of the chromium target blank is improved by reasonably setting the specific parameters of hot isostatic pressing, so that the problem that the density of the target material cannot reach the standard due to the fact that the requirement of volume diffusion of chromium powder cannot be met when the hot isostatic pressing temperature is too low can be avoided; when the temperature is too high, recrystallization can occur, and the crystal grains can grow gradually along with the hot isostatic pressing process, so that the crystal grain size of the finished target is too large, which exceeds the specification of YS/T1220-2018 on the crystal grain size of the chromium target, and the sputtering rate in the subsequent film preparation process is reduced.
Step four, carrying out annealing heat treatment on the chromium target blank obtained in the step three, and eliminating residual stress generated in the multiple pressing process and reducing a stress induced crack source;
specifically, the annealing temperature is set to 1000-1400 ℃, the heat preservation time is set to 20-80 min, and the annealing is carried out in a gas cooling mode.
Step five, carrying out full-width flaw detection treatment on the chromium target blank subjected to heat treatment in the step four by utilizing a nondestructive detection process, screening out qualified chromium target blanks, and machining the qualified chromium target blanks into required sizes by utilizing a machine to obtain finished chromium targets;
specifically, nondestructive testing is carried out on the annealed chromium target blank by utilizing ultrasonic nondestructive testing equipment, the target with defects is detected, screened and removed, the qualified chromium target blank is left, and the qualified chromium target blank is machined into a required size by utilizing processes such as wire cutting, turning and the like, so that the finished chromium target is obtained.
In order to further verify the efficacy of the manufacturing method of the present invention, the inventors made the following specific examples:
example 1
1) Reducing and purifying flaky pure chromium powder with the particle size of 15-106 microns and the purity of 99.95% under the protection of hydrogen, wherein the reduction temperature is 1300 ℃, and the reduction time is 120 min;
2) filling the pure chromium powder reduced in the step 1) into a plastic elastic die, compacting for 6 times, and maintaining the pressure at 160MPa for 150min to obtain a medium-density chromium metal block;
3) carrying out hot isostatic pressing secondary densification treatment on the chromium metal block obtained in the step 2), wherein the temperature is 1600 ℃, the pressure is 90MPa, and the time is 3h, the whole process is carried out in an inert atmosphere, so that inclusion is prevented from being introduced in the hot isostatic pressing process, and argon is adopted for air cooling after the hot isostatic pressing is finished;
4) annealing the chromium target blank subjected to the hot isostatic pressing in the step 3), wherein the annealing temperature is 1400 ℃, and the heat preservation time is 20 min;
5) and carrying out nondestructive testing on the annealed chromium target blank by using ultrasonic nondestructive testing equipment, screening out the qualified chromium target blank, and machining the qualified chromium target blank into the required size by using a wire cutting or turning machine to obtain the finished chromium target.
The chromium target produced according to the above example had a purity of 99.955% and a density of 99.95% and a microstructure pattern as shown in FIG. 2, with an average grain size of 68.6 μm, which increased the oxygen content of the chromium target by 80ppm after hot isostatic pressing compared to the original powder.
Example 2
1) Reducing and purifying flaky pure chromium powder with the particle size of 106-150 mu m and the purity of 99.999% under the protection of hydrogen, wherein the reduction temperature is 1150 ℃, and the reduction time is 210 min;
2) filling the pure chromium powder reduced in the step 1) into a plastic elastic die, compacting for 7 times, and maintaining the pressure at 130MPa for 270min to obtain a medium-density chromium metal block;
3) carrying out hot isostatic pressing secondary densification treatment on the chromium metal block obtained in the step 2), wherein the temperature is 1350 ℃, the pressure is 100MPa, the time is 9h, the whole process is carried out in an inert atmosphere, inclusions are prevented from being introduced in the hot isostatic pressing process, and after the hot isostatic pressing is finished, the chromium metal block is cooled to 200 ℃ by using argon gas and then taken out for air cooling;
4) annealing the chromium target blank subjected to the hot isostatic pressing in the step 3), wherein the annealing temperature is 1200 ℃, and the heat preservation time is 50 min;
5) and carrying out nondestructive testing on the annealed chromium target blank by using ultrasonic nondestructive testing equipment, screening out the qualified chromium target blank, and machining the qualified chromium target blank into the required size by using a wire cutting or turning machine to obtain the finished chromium target.
The chromium targets produced according to the above examples had a purity of 99.99% and a density of 99.95% and the microstructure shown in FIG. 3 shows an average grain size of 121.7 μm, which is a 42ppm increase in oxygen content after hot isostatic pressing of the chromium targets compared to the original powder.
Example 3
1) Reducing and purifying flaky pure chromium powder with the particle size of 150-212 mu m and the purity of 99.9% under the protection of hydrogen, wherein the reduction temperature is 900 ℃, and the reduction time is 300 min;
2) filling the pure chromium powder reduced in the step 1) into a plastic elastic die, compacting for 5 times, and maintaining the pressure at 90MPa for 400min to obtain a medium-density chromium metal block;
3) carrying out hot isostatic pressing secondary densification treatment on the chromium metal block manufactured in the step 2), wherein the temperature is 1150 ℃, the pressure is 160MPa, the time is 15h, the whole process is carried out in an inert atmosphere, inclusion is prevented from being introduced in the hot isostatic pressing process, and argon is adopted for air cooling after the hot isostatic pressing is finished;
4) annealing the chromium target blank subjected to the hot isostatic pressing in the step 3), wherein the annealing temperature is 1000 ℃, and the heat preservation time is 80 min;
5) and carrying out nondestructive testing on the annealed chromium target blank by using ultrasonic nondestructive testing equipment, screening out the qualified chromium target blank, and machining the qualified chromium target blank into the required size by using a wire cutting or turning machine to obtain the finished chromium target.
The chromium target prepared according to the above examples had a purity of 99.99%, a density of 99.85% and an average grain size of 175.4 μm, and the oxygen content of the chromium target after hot isostatic pressing increased by 40ppm compared to the original powder.
In conclusion, the invention firstly utilizes the one-time liquid high-pressure preforming technology to perform the chromium powder in a pre-pressing manner, so that the links of sheath preparation, powder degassing, sheath seal welding leak detection, sheath removal and the like are omitted in the hot isostatic pressing process, and meanwhile, the special plastic mould can be repeatedly utilized, thereby obviously improving the production efficiency and reducing the manufacturing cost of the chromium target. By adopting the technical scheme, the isotropic chromium target with low oxygen, high purity, nearly compact and fine and uniform crystal grains can be obtained, the requirements of physical vapor deposition technology in the photoelectric industries such as TFT-LCD, IC, PCB and the like can be met, and the oxygen increment from powder to the finished chromium target is less than or equal to 100 ppm.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
It is to be understood that the present invention is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (10)
1. A method for manufacturing a low-oxygen chromium target, which is characterized by mainly comprising the following steps:
step one, carrying out hydrogen reduction treatment on pure chromium powder with a certain particle size;
filling and compacting the pure chromium powder subjected to reduction treatment in the step one into a mold, and then placing the pure chromium powder and the mold into a closed high-pressure container filled with a liquid medium for pre-compression treatment to obtain a chromium metal block;
thirdly, placing the chromium metal block obtained in the second step into hot isostatic pressing equipment for secondary pressing to obtain a chromium target blank;
step four, carrying out annealing heat treatment on the chromium target blank obtained in the step three, and eliminating residual stress generated in the multiple pressing process and reducing a stress induced crack source;
and fifthly, carrying out full-width flaw detection treatment on the chromium target blank subjected to heat treatment in the fourth step by using a nondestructive detection process, screening out qualified chromium target blanks, and machining the qualified chromium target blanks into required sizes by using a machine to obtain finished chromium targets.
2. The method for manufacturing a low-oxygen chromium target according to claim 1, wherein the grain size of the pure chromium powder in the first step is 15-212 μm, and the purity is not less than 99%.
3. The method for producing a low-oxygen chromium target according to claim 1, wherein the temperature for the hydrogen reduction treatment in the first step is set to 900 to 1300 ℃ for 120 to 300 min.
4. The method for manufacturing a low-oxygen chromium target according to claim 1, wherein the mold used in the second step is a plastic elastic mold.
5. The method for producing a low-oxygen chromium target according to claim 1, wherein the pressure during the preliminary press treatment in the second step is set to 90 to 160MPa, and the time is set to 150 to 400 min.
6. The method of claim 1, wherein the third step of hot isostatic pressing is performed in an inert atmosphere, and after the hot isostatic pressing is completed, the target is cooled by argon gas.
7. The method for manufacturing a low-oxygen chromium target according to claim 1, wherein the specific parameters of the three-step hot isostatic pressing treatment are as follows: the pressure is set to be 90-160 MPa, the temperature is set to be 1150-1600 ℃, and the pressure maintaining time is set to be 3-15 h.
8. The method for manufacturing a low-oxygen chromium target according to claim 1, wherein the annealing temperature in the fourth step is set to 1000 to 1400 ℃, the holding time is set to 20 to 80min, and the annealing is followed by air cooling.
9. The method for manufacturing a low-oxygen chromium target according to claim 1, wherein the nondestructive testing process in the fifth step is mainly to perform flaw detection screening on the manufactured chromium target by using ultrasonic nondestructive testing.
10. A low-oxygen chromium target, characterized in that the low-oxygen chromium target is manufactured by the manufacturing method of any one of claims 1 to 9, and the oxygen increment of the low-oxygen chromium target from original powder to a finished target material is less than or equal to 100 ppm.
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2022
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Application publication date: 20220315 |