CN113290427A - Treatment method of high-purity nickel evaporation material - Google Patents
Treatment method of high-purity nickel evaporation material Download PDFInfo
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- CN113290427A CN113290427A CN202110565387.5A CN202110565387A CN113290427A CN 113290427 A CN113290427 A CN 113290427A CN 202110565387 A CN202110565387 A CN 202110565387A CN 113290427 A CN113290427 A CN 113290427A
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- cleaning
- evaporation material
- washing
- purity nickel
- pure water
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 248
- 239000000463 material Substances 0.000 title claims abstract description 124
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 124
- 238000001704 evaporation Methods 0.000 title claims abstract description 120
- 230000008020 evaporation Effects 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000004140 cleaning Methods 0.000 claims abstract description 147
- 238000005406 washing Methods 0.000 claims abstract description 90
- 239000002253 acid Substances 0.000 claims abstract description 63
- 238000000227 grinding Methods 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 67
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims description 16
- 239000003599 detergent Substances 0.000 claims description 11
- 238000005498 polishing Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000012459 cleaning agent Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims 1
- 238000002525 ultrasonication Methods 0.000 claims 1
- 230000003749 cleanliness Effects 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000007888 film coating Substances 0.000 abstract description 5
- 238000009501 film coating Methods 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 23
- 238000004544 sputter deposition Methods 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 230000002035 prolonged effect Effects 0.000 description 5
- 238000005477 sputtering target Methods 0.000 description 5
- 239000013077 target material Substances 0.000 description 5
- 238000005554 pickling Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- -1 and in the prior art Chemical compound 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013020 steam cleaning Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B31/00—Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor
- B24B31/02—Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor involving rotary barrels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B31/00—Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor
- B24B31/12—Accessories; Protective equipment or safety devices; Installations for exhaustion of dust or for sound absorption specially adapted for machines covered by group B24B31/00
-
- 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
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
Abstract
The invention provides a treatment method of a high-purity nickel evaporation material, which comprises the steps of sequentially carrying out first cleaning and first acid washing on the high-purity nickel evaporation material to obtain a pretreated high-purity nickel evaporation material; sequentially grinding, second cleaning, third cleaning and second acid cleaning the pretreated high-purity nickel evaporation material to obtain a ground high-purity nickel evaporation material; and drying the ground high-purity nickel evaporation material to obtain the cleaned high-purity nickel evaporation material, thereby effectively removing impurities and oxide layers on the surface of the high-purity nickel evaporation material, improving the cleanliness of the surface of the high-purity nickel evaporation material, contributing to improving the film coating performance and prolonging the service life.
Description
Technical Field
The invention relates to the technical field of semiconductor sputtering evaporation materials, in particular to a method for processing a high-purity nickel evaporation material.
Background
With the development of science and technology and modern society, thin film materials are more and more widely applied to the fields of information, new energy, electronics, flat panel display and the like, especially with the development of semiconductor process technology, the thin film materials become indispensable important components for civilization in modern society, and the quality requirement of sputtering target materials required for forming high-quality thin films is higher and higher, so that the preparation technology of the target materials with high quality requirement becomes very important.
Nickel is used as a common film material and is most widely applied to the fields in which almost all metal films are applied, and the requirements on the films in the fields of semiconductors, magnetic recording, flat panel display and the like are high, so that higher requirements are provided for metal targets. For example, nickel is required to have a high purity, typically greater than 99.99%, while the texture is required to be uniform with an average grain size typically less than 40 um. This ensures that a highly uniform and highly pure thin film is obtained, thereby ensuring the performance of the device.
However, impurities and stains and oxidation layers often exist on the surface of the high-purity nickel, and in the prior art, isopropanol and pure water are often adopted for ultrasonic cleaning or centrifugal grinding by a grinding machine, but the oxidation layers and impurities and stains still exist on the surface of the high-purity nickel after cleaning.
CN109930162A discloses a cleaning method for recovering sputtering target, which comprises separating the old sputtering aluminum target face plate and back plate by using a grinder; placing the separated sputtering aluminum target panel in a container of an acid solution, wherein the mass concentration of the acid solution is 10-75%; after the dissolution is finished, taking out the sputtering aluminum target panel, immersing the sputtering aluminum target panel into a sodium hydroxide solution, and neutralizing the acid solution on the surface of the target; the mass concentration of the sodium hydroxide solution is 10-20%; after the acid-base neutralization is finished, taking out the sputtering aluminum target panel and immersing the sputtering aluminum target panel into pure water; taking out from the pure water, and observing whether the residual attachments exist or not by naked eyes; drying in a greenhouse without the deposit finally yielded a clean aluminum target, but no cleaning of high-purity nickel was involved.
CN112267099A discloses a method for cleaning the surface of a target, which comprises the following steps: and cleaning the surface of the target material with flowing water, wiping, and then sequentially carrying out ultrasonic vibration cleaning, jet cleaning and blowing and drying to obtain the cleaned target material, wherein the cleaning of high-purity nickel is not involved.
CN101724818B discloses a cleaning method for copper or copper alloy sputtering target, which has at least two cleaning stages, including: in the first cleaning stage, a first cleaning agent solution is used for cleaning the copper or copper alloy sputtering target material for at least one time; and in the second cleaning stage, the copper or copper alloy sputtering target is cleaned at least once by using a second cleaning agent solution. The cleaning method can also comprise a preheating procedure before the first cleaning stage and a steam cleaning stage after the second cleaning stage, but the cleaning of high-purity nickel is not involved.
Therefore, it is necessary to develop a method for cleaning a high purity nickel evaporation material, which is easy to operate and has a good cleaning effect.
Disclosure of Invention
In order to solve the technical problems, the invention provides a treatment method of a high-purity nickel evaporation material, which comprises the steps of sequentially carrying out a plurality of cleaning and pickling processes and matching with a grinding process, so that impurities and an oxidation layer on the surface of the high-purity nickel evaporation material are effectively removed, the cleanliness of the surface of the high-purity nickel evaporation material is improved, the improvement of film coating performance is facilitated, and the service life is prolonged.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a treatment method of a high-purity nickel evaporation material, which comprises the following steps:
(1) sequentially carrying out first cleaning and first acid washing on the high-purity nickel evaporation material to obtain a pretreated high-purity nickel evaporation material;
(2) sequentially grinding, second cleaning, third cleaning and second acid cleaning the pretreated high-purity nickel evaporation material obtained in the step (1) to obtain a ground high-purity nickel evaporation material;
(3) and (3) drying the ground high-purity nickel evaporation material obtained in the step (2) to obtain a cleaned high-purity nickel evaporation material.
The invention carries out pretreatment on the high-purity evaporation material, then carries out grinding and further cleaning processes, and effectively removes impurities and oxide layers on the surface of the high-purity nickel evaporation material in a mode of matching cleaning, pickling and grinding, improves the cleanliness of the surface of the high-purity nickel evaporation material, is beneficial to improving the film coating performance, and can repeatedly use grinding particles, thereby saving the cost.
Preferably, the purity of the high-purity nickel evaporation material is more than or equal to 99.9 wt%, and for example, the purity can be 99.9 wt%, 99.91 wt%, 99.92 wt%, 99.93 wt%, 99.94 wt%, 99.95 wt%, 99.96 wt%, 99.97 wt%, 99.98 wt%, 99.99 wt%, and the like.
The high-purity nickel generally refers to a nickel material with the purity of more than or equal to 99.9 wt%.
Preferably, the average particle size of the high-purity nickel evaporation material is 10-50 mm, and for example, the average particle size may be 10mm, 15mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45mm, 50mm, or the like.
Preferably, the first washing of step (1) includes washing in a detergent and pure water in this order under the first ultrasonic.
Preferably, the detergent comprises a liquid detergent.
The detergent of the present invention is not particularly limited, and various kinds of detergents known to those skilled in the art can be used.
The evaporation material is washed in the pure water after being washed in the detergent, so that bubbling can be increased, the flow of liquid can be increased, the buoyancy of bubbles can be more fully utilized to drive the evaporation material to roll in the liquid, and the evaporation material is more fully washed.
Preferably, the power of the first ultrasonic wave is 200-300W, such as 200W, 210W, 220W, 230W, 240W, 250W, 260W, 270W, 280W, 290W or 300W.
Preferably, the time of washing in the detergent in the first washing is 2-10 min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10 min.
Preferably, the time for cleaning in pure water in the first cleaning is 2 to 10min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, or 10 min.
Preferably, the first acid washing includes washing in a nitric acid solution and pure water in this order.
Preferably, the concentration of the nitric acid solution is 62 to 68 wt%, and may be, for example, 62 wt%, 63 wt%, 64 wt%, 65 wt%, 66 wt%, 67 wt%, 68 wt%, or the like.
Preferably, the time for cleaning in the nitric acid solution in the first acid cleaning is 2 to 10min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, or 10 min.
Preferably, the time for cleaning in pure water in the first acid cleaning is 2 to 10min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, or 10 min.
Preferably, the cleaning in pure water in the first acid washing is performed under the second ultrasonic wave.
Preferably, the power of the second ultrasonic wave is 200-300W, such as 200W, 210W, 220W, 230W, 240W, 250W, 260W, 270W, 280W, 290W or 300W.
Preferably, said grinding of step (2) comprises performing in a centrifugal grinder.
The grinding is carried out in order to remove an oxide layer and impurities on the surface of the high-purity nickel evaporation material, so that the cleanliness of the high-purity nickel evaporation material can be improved.
Preferably, the second cleaning includes cleaning in pure water and a polishing liquid in this order under the third ultrasonic.
Preferably, the power of the third ultrasonic wave is 200-300W, such as 200W, 210W, 220W, 230W, 240W, 250W, 260W, 270W, 280W, 290W or 300W.
Preferably, the time for cleaning in pure water in the second cleaning is 2 to 10min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, or 10 min.
Preferably, the time for cleaning in the polishing solution in the second cleaning is 2 to 10min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, or 10 min.
Preferably, the abrasive liquid comprises a hand sanitizer.
The hand sanitizer of the present invention is not particularly limited and hand sanitizers of the type well known to those skilled in the art may be used.
Preferably, the volume ratio of the hand sanitizer to the pure water in the grinding liquid is 1 (45-55).
Preferably, the third washing comprises washing in isopropanol under a fourth ultrasound.
Preferably, the power of the fourth ultrasonic wave is 200-300W, such as 200W, 210W, 220W, 230W, 240W, 250W, 260W, 270W, 280W, 290W or 300W.
Preferably, the time of the third cleaning is 2-10 min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10 min.
Preferably, the second acid washing comprises washing in a hydrochloric acid solution and pure water in sequence.
Preferably, the concentration of the hydrochloric acid solution is 38 to 42 wt%, for example, 38 wt%, 39 wt%, 40 wt%, 41 wt%, 42 wt%, or the like.
Preferably, the time for cleaning in hydrochloric acid solution in the second acid cleaning is 2-10 min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10 min.
Preferably, the time for cleaning in pure water in the second acid cleaning is 2 to 10min, for example, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min, or 10 min.
Preferably, the second acid washing in pure water washing is performed under fifth ultrasonic.
Preferably, the power of the fifth ultrasonic wave is 200-300W, such as 200W, 210W, 220W, 230W, 240W, 250W, 260W, 270W, 280W, 290W, 300W, and the like.
Preferably, the temperature for drying in step (3) is 100-120 ℃, for example, 100 ℃, 102 ℃, 104 ℃, 106 ℃, 108 ℃, 110 ℃, 112 ℃, 114 ℃, 116 ℃, 118 ℃ or 120 ℃ and the like.
Preferably, the drying time is 30-50 min, for example, 30min, 32min, 34min, 36min, 38min, 40min, 42min, 44min, 46min, 48min or 50 min.
As a preferred technical solution of the present invention, the processing method includes the steps of:
(1) sequentially carrying out first cleaning and first acid washing on a high-purity nickel evaporation material with the average particle size of 10-50 mm and the purity of more than or equal to 99.9 wt% to obtain a pretreated high-purity nickel evaporation material, wherein the first cleaning comprises sequentially cleaning in a cleaning agent for 2-10 min and in pure water for 2-10 min under first ultrasonic with the power of 200-300W; the first acid washing comprises sequentially washing in a nitric acid solution with the concentration of 62-68 wt% for 2-10 min and in pure water for 2-10 min, wherein the washing in the pure water in the first acid washing needs to be carried out under second ultrasonic with the power of 200-300W;
(2) sequentially carrying out grinding, second cleaning, third cleaning and second acid cleaning on the pretreated high-purity nickel evaporation material obtained in the step (1) in a centrifugal grinder to obtain the ground high-purity nickel evaporation material, wherein the second cleaning comprises sequentially cleaning in pure water for 2-10 min and in grinding liquid for 2-10 min under third ultrasonic with the power of 200-300W, and the volume ratio of the hand sanitizer to the pure water in the grinding liquid is 1 (45-55); the third cleaning comprises cleaning in isopropanol for 2-10 min under fourth ultrasonic with the power of 200-300W; the second acid washing comprises washing in a hydrochloric acid solution with the concentration of 38-42 wt% for 2-10 min and washing in pure water for 2-10 min in sequence, and the washing in the pure water in the second acid washing needs to be carried out under fifth ultrasonic with the power of 200-300W;
(3) and (3) drying the ground high-purity nickel evaporation material obtained in the step (2) for 30-50 min at 100-120 ℃ to obtain the cleaned high-purity nickel evaporation material.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) according to the treatment method of the high-purity nickel evaporation material, provided by the invention, through sequentially carrying out a plurality of cleaning and pickling processes and matching with a grinding process, impurities and an oxidation layer on the surface of the high-purity nickel evaporation material are effectively removed, the cleanliness of the surface of the high-purity nickel evaporation material is improved, the coating performance is improved, the service life is prolonged, the service life of the cleaned high-purity nickel evaporation material is more than or equal to 2014 kW.h, and the service life of the cleaned high-purity nickel evaporation material is more than or equal to 2058 kW.h under the optimal selection condition;
(2) the method for treating the high-purity nickel evaporation material provided by the invention is simple in operation steps and easy to implement.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
First, an embodiment
Example 1
The embodiment provides a method for processing a high-purity nickel evaporation material, which comprises the following steps:
(1) sequentially carrying out first cleaning and first acid washing on a high-purity nickel evaporation material with the average particle size of 30mm and the purity of 99.9 wt% to obtain a pretreated high-purity nickel evaporation material, wherein the first cleaning comprises sequentially cleaning in a cleaning agent for 6min and cleaning in pure water for 6min under first ultrasonic with the power of 250W; the first acid washing comprises washing in 65 wt% nitric acid solution for 6min and washing in pure water for 6min, wherein the washing in pure water in the first acid washing needs to be carried out under second ultrasonic with the power of 250W;
(2) sequentially carrying out grinding, second cleaning, third cleaning and second acid cleaning on the pretreated high-purity nickel evaporation material obtained in the step (1) in a centrifugal grinder to obtain the ground high-purity nickel evaporation material, wherein the second cleaning comprises sequentially cleaning in pure water for 6min and cleaning in grinding liquid for 6min under third ultrasonic with the power of 250W, and the volume ratio of the hand sanitizer to the pure water in the grinding liquid is 1: 50; the third cleaning comprises cleaning in isopropanol for 6min under fourth ultrasonic with the power of 250W; the second acid washing comprises washing in a hydrochloric acid solution with the concentration of 40 wt% for 6min and washing in pure water for 6min in sequence, and the washing in the pure water in the second acid washing needs to be carried out under fifth ultrasonic with the power of 250W;
(3) and (3) drying the ground high-purity nickel evaporation material in the step (2) for 40min at 110 ℃ to obtain the cleaned high-purity nickel evaporation material.
The type of the hand sanitizer in the embodiment is a semille worker hand sanitizer.
Example 2
The embodiment provides a method for processing a high-purity nickel evaporation material, which comprises the following steps:
(1) sequentially carrying out first cleaning and first acid washing on a high-purity nickel evaporation material with the average particle size of 10mm and the purity of 99.99 wt% to obtain a pretreated high-purity nickel evaporation material, wherein the first cleaning comprises sequentially cleaning in a cleaning agent for 2min and cleaning in pure water for 2min under first ultrasonic with the power of 200W; the first acid washing comprises washing in nitric acid solution with the concentration of 62 wt% for 10min and washing in pure water for 10min in sequence, wherein the washing in the pure water in the first acid washing needs to be carried out under second ultrasonic with the power of 200W;
(2) sequentially carrying out grinding, second cleaning, third cleaning and second acid cleaning on the pretreated high-purity nickel evaporation material obtained in the step (1) in a centrifugal grinder to obtain the ground high-purity nickel evaporation material, wherein the second cleaning comprises sequentially cleaning in pure water for 2min and cleaning in grinding liquid for 2min under third ultrasonic with the power of 200W, and the volume ratio of the hand sanitizer to the pure water in the grinding liquid is 1: 45; the third cleaning comprises cleaning in isopropanol for 10min under fourth ultrasound with power of 200W; the second acid washing comprises washing in a hydrochloric acid solution with the concentration of 38 wt% for 2min and washing in pure water for 2min in sequence, wherein the washing in the pure water in the second acid washing needs to be carried out under fifth ultrasonic with the power of 200W;
(3) and (3) drying the ground high-purity nickel evaporation material in the step (2) for 30min at 120 ℃ to obtain the cleaned high-purity nickel evaporation material.
The type of the hand sanitizer in the embodiment is a semille worker hand sanitizer.
Example 3
The embodiment provides a method for processing a high-purity nickel evaporation material, which comprises the following steps:
(1) sequentially carrying out first cleaning and first acid washing on a high-purity nickel evaporation material with the average particle size of 50mm and the purity of 99.9 wt% to obtain a pretreated high-purity nickel evaporation material, wherein the first cleaning comprises sequentially cleaning in a cleaning agent for 10min and cleaning in pure water for 10min under first ultrasonic with the power of 300W; the first acid washing comprises washing in a nitric acid solution with the concentration of 68 wt% for 2min and washing in pure water for 2min in sequence, wherein the washing in the pure water in the first acid washing needs to be carried out under second ultrasonic with the power of 300W;
(2) sequentially carrying out grinding, second cleaning, third cleaning and second acid cleaning on the pretreated high-purity nickel evaporation material obtained in the step (1) in a centrifugal grinder to obtain the ground high-purity nickel evaporation material, wherein the second cleaning comprises sequentially cleaning in pure water for 10min and in grinding liquid for 10min under third ultrasonic with the power of 300W, and the volume ratio of the hand sanitizer to the pure water in the grinding liquid is 1: 55; the third cleaning comprises cleaning in isopropanol for 2min under fourth ultrasound with power of 300W; the second acid washing comprises washing in a hydrochloric acid solution with the concentration of 42 wt% for 10min and washing in pure water for 10min in sequence, and the washing in the pure water in the second acid washing needs to be carried out under fifth ultrasonic with the power of 300W;
(3) and (3) drying the ground high-purity nickel evaporation material in the step (2) for 50min at 100 ℃ to obtain the cleaned high-purity nickel evaporation material.
The type of the hand sanitizer in the embodiment is a semille worker hand sanitizer.
Example 4
This example provides a method for treating a high purity nickel evaporation material, which is different from example 1 only in that the concentration of the nitric acid solution in step (1) is 60 wt%, and the rest is the same as example 1.
Example 5
This example provides a method for treating a high purity nickel evaporation material, which is different from example 1 only in that the concentration of the nitric acid solution in step (1) is 70 wt%, and the rest is the same as example 1.
Example 6
This example provides a method for treating a high purity nickel evaporation material, which is different from example 1 only in that the volume ratio of the hand cleanser to the pure water in the polishing slurry is 1:40, and the rest is the same as example 1.
Example 7
This example provides a method for treating a high purity nickel evaporation material, which is different from example 1 only in that the volume ratio of the hand cleanser to the pure water in the polishing slurry is 1:50, and the rest is the same as example 1.
Example 8
This example provides a method for treating a high purity nickel evaporation material, which is different from example 1 only in that the concentration of the hydrochloric acid solution of step (2) is 35 wt%, and the rest is the same as example 1.
Example 9
This example provides a method for treating a high purity nickel evaporation material, which is different from example 1 only in that the concentration of the hydrochloric acid solution of step (2) is 45 wt%, and the rest is the same as example 1.
Second, comparative example
Comparative example 1
This comparative example provides a method of treating a high purity nickel evaporation material, which is different from example 1 only in that the first cleaning is not performed, and the rest is the same as example 1.
Comparative example 2
This comparative example provides a method of treating a high purity nickel evaporation material, which is different from example 1 only in that the first acid washing is not performed, and the rest is the same as example 1.
Comparative example 3
This comparative example provides a method of treating a high purity nickel evaporation material, which is different from example 1 only in that grinding is not performed, and the rest is the same as example 1.
Comparative example 4
This comparative example provides a method of treating a high purity nickel evaporation material, which is different from example 1 only in that the second washing is not performed, and the rest is the same as example 1.
Comparative example 5
This comparative example provides a method of treating a high purity nickel evaporation material, which is different from example 1 only in that the third cleaning is not performed, and the rest is the same as example 1.
Comparative example 6
This comparative example provides a method of treating a high purity nickel evaporation material, which differs from example 1 only in that a second acid wash is not performed, and is otherwise the same as example 1.
Third, test and results
The method for testing the service life of the washed high-purity nickel evaporation material comprises the following steps: the cleaned high-purity nickel evaporation material is applied to the process of semiconductor sputtering coating.
The test results of the above examples and comparative examples are shown in table 1.
TABLE 1
| Service life of high-purity nickel evaporation material after cleaning (kW. h) | |
| Example 1 | 2462 |
| Example 2 | 2458 |
| Example 3 | 2464 |
| Example 4 | 2024 |
| Example 5 | 2017 |
| Example 6 | 2020 |
| Example 7 | 2014 |
| Example 8 | 2006 |
| Example 9 | 2018 |
| Comparative example 1 | 1842 |
| Comparative example 2 | 1788 |
| Comparative example 3 | 1744 |
| Comparative example 4 | 1828 |
| Comparative example 5 | 1954 |
| Comparative example 6 | 1854 |
From table 1, the following points can be seen:
(1) the invention provides a treatment method of a high-purity nickel evaporation material, which is characterized in that through sequentially carrying out a plurality of cleaning and pickling processes and matching with a grinding process, impurities and an oxidation layer on the surface of the high-purity nickel evaporation material are effectively removed, the cleanliness of the surface of the high-purity nickel evaporation material is improved, the coating performance is improved, and the service life is prolonged, specifically, the service life of the cleaned high-purity nickel evaporation material is more than or equal to 2014 kW.h, and under the optimal selection condition, the service life of the cleaned high-purity nickel evaporation material is more than or equal to 2058 kW.h;
(2) as can be seen from the combination of the embodiment 1 and the embodiments 4 to 5, the concentration of the nitric acid solution in the step (1) in the embodiment 1 is 65 wt%, compared with the concentrations of the nitric acid solutions in the steps (1) in the embodiments 4 to 5 of 60 wt% and 70 wt%, the service life of the high-purity nickel evaporation material after cleaning in the embodiment 1 is 2462kW · h, and the service lives of the high-purity nickel evaporation materials after cleaning in the embodiments 4 to 5 are 2024kW · h and 2017kW · h, respectively, which shows that the concentration of the nitric acid solution in the step (1) is controlled within a certain range, so that the cleanliness of the surface of the high-purity nickel evaporation material can be improved, the film plating performance can be improved, and the service life can be further prolonged;
(3) as can be seen from the combination of examples 1 and 6 to 7, the volume ratio of the hand washing solution to the pure water in the polishing solution of example 1 is 1:50, and compared with the volume ratios of the hand washing solution to the pure water in the polishing solutions of examples 4 to 5, which are 1:40 and 1:50, respectively, the service life of the high-purity nickel evaporation material after cleaning in example 1 is 2462kW · h, and the service lives of the high-purity nickel evaporation materials after cleaning in examples 6 to 7 are 2020kW · h and 2014kW · h, respectively, which indicates that the present invention can control the volume ratio of the hand washing solution to the pure water in the polishing solution within a certain range, thereby improving the cleanliness of the surface of the high-purity nickel evaporation material, contributing to the improvement of the film plating performance, and further prolonging the service life;
(4) as can be seen from the combination of the embodiment 1 and the embodiments 8 to 9, the concentration of the hydrochloric acid solution in the step (2) in the embodiment 1 is 40 wt%, and compared with the concentrations of the hydrochloric acid solutions in the steps (2) in the embodiments 8 to 9 of 35 wt% and 45 wt%, the service life of the high-purity nickel evaporation material cleaned in the embodiment 1 is 2462kW · h, and the service lives of the high-purity nickel evaporation materials cleaned in the embodiments 8 to 9 are 2006kW · h and 2018kW · h, respectively, which shows that the concentration of the hydrochloric acid solution in the step (2) is controlled within a certain range, so that the cleanliness of the surface of the high-purity nickel evaporation material can be improved, the film plating performance can be improved, and the service life can be further prolonged;
(5) it can be seen from the combination of example 1 and comparative examples 1 to 6 that the first cleaning, the first acid cleaning, the polishing, the second cleaning, the third cleaning and the second acid cleaning were sequentially performed in example 1, and the service life of the high purity nickel evaporation material after cleaning in example 1 was 2462kW · h compared to the case where the first cleaning, the first acid cleaning, the polishing, the second cleaning, the third cleaning and the second acid cleaning were not performed in comparative examples 1 to 6, the service lives of the high-purity nickel evaporation materials cleaned in the comparative examples 1 to 6 are 1842 kW.h, 1788 kW.h, 1744 kW.h, 1828 kW.h, 1954 kW.h and 1854 kW.h respectively, therefore, the method sequentially carries out the first cleaning, the first acid washing, the grinding, the second cleaning, the third cleaning and the second acid washing on the high-purity nickel evaporation material, can improve the surface cleanliness of the high-purity nickel evaporation material, is favorable for improving the film coating performance, and prolongs the service life.
In conclusion, the invention provides a treatment method of a high-purity nickel evaporation material, which effectively removes impurities and an oxidation layer on the surface of the high-purity nickel evaporation material, improves the cleanliness of the surface of the high-purity nickel evaporation material, is beneficial to improving the film coating performance and prolonging the service life, the service life of the cleaned high-purity nickel evaporation material is more than or equal to 2014 kW.h, and under the optimal condition, the service life of the cleaned high-purity nickel evaporation material is more than or equal to 2058 kW.h.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The method for processing the high-purity nickel evaporation material is characterized by comprising the following steps of:
(1) sequentially carrying out first cleaning and first acid washing on the high-purity nickel evaporation material to obtain a pretreated high-purity nickel evaporation material;
(2) sequentially grinding, second cleaning, third cleaning and second acid cleaning the pretreated high-purity nickel evaporation material obtained in the step (1) to obtain a ground high-purity nickel evaporation material;
(3) and (3) drying the ground high-purity nickel evaporation material obtained in the step (2) to obtain a cleaned high-purity nickel evaporation material.
2. The process of claim 1, wherein the purity of the high purity nickel evaporation material is greater than or equal to 99.9 wt%;
preferably, the average particle size of the high-purity nickel evaporation material is 10-50 mm.
3. The treatment method according to claim 1 or 2, wherein the first washing of step (1) comprises washing in a detergent and pure water in this order under first ultrasonication;
preferably, the detergent comprises a liquid detergent;
preferably, the power of the first ultrasonic wave is 200-300W;
preferably, the time of washing in the detergent in the first washing is 2-10 min;
preferably, the time for cleaning in pure water in the first cleaning is 2-10 min.
4. The treatment method according to any one of claims 1 to 3, wherein the first acid washing comprises washing in a nitric acid solution and pure water in this order;
preferably, the concentration of the nitric acid solution is 62-68 wt%;
preferably, the time for cleaning in the nitric acid solution in the first acid washing is 2-10 min;
preferably, the time for cleaning in pure water in the first acid cleaning is 2-10 min;
preferably, the cleaning in pure water in the first acid washing is carried out under second ultrasonic wave;
preferably, the power of the second ultrasonic wave is 200-300W.
5. The process of any one of claims 1 to 4, wherein the grinding of step (2) comprises performing in a centrifugal grinder.
6. The treatment method according to any one of claims 1 to 5, wherein the second cleaning comprises cleaning in pure water and a polishing liquid in this order under third ultrasonic sound;
preferably, the power of the third ultrasonic wave is 200-300W;
preferably, the time for cleaning in pure water in the second cleaning is 2-10 min;
preferably, the cleaning time in the grinding fluid in the second cleaning is 2-10 min;
preferably, the abrasive liquid comprises a hand wash;
preferably, the volume ratio of the hand sanitizer to the pure water in the grinding liquid is 1 (45-55).
7. The process of any one of claims 1 to 6, wherein the third washing comprises washing in isopropanol under fourth ultrasound;
preferably, the power of the fourth ultrasonic wave is 200-300W;
preferably, the time of the third cleaning is 2-10 min.
8. The process according to any one of claims 1 to 7, wherein the second acid washing comprises washing in a hydrochloric acid solution and pure water in this order;
preferably, the concentration of the hydrochloric acid solution is 38-42 wt%;
preferably, the time for cleaning in the hydrochloric acid solution in the second acid cleaning is 2-10 min;
preferably, the time for cleaning in pure water in the second acid cleaning is 2-10 min;
preferably, the second acid washing in pure water washing is performed under fifth ultrasonic waves;
preferably, the power of the fifth ultrasonic wave is 200-300W.
9. The treatment method according to any one of claims 1 to 7, wherein the temperature of the drying in the step (3) is 100 to 120 ℃;
preferably, the drying time is 30-50 min.
10. The treatment method according to any one of claims 1 to 7, characterized in that it comprises the following steps:
(1) sequentially carrying out first cleaning and first acid washing on a high-purity nickel evaporation material with the average particle size of 10-50 mm and the purity of more than or equal to 99.9 wt% to obtain a pretreated high-purity nickel evaporation material, wherein the first cleaning comprises sequentially cleaning in a cleaning agent for 2-10 min and in pure water for 2-10 min under first ultrasonic with the power of 200-300W; the first acid washing comprises sequentially washing in a nitric acid solution with the concentration of 62-68 wt% for 2-10 min and in pure water for 2-10 min, wherein the washing in the pure water in the first acid washing needs to be carried out under second ultrasonic with the power of 200-300W;
(2) sequentially carrying out grinding, second cleaning, third cleaning and second acid cleaning on the pretreated high-purity nickel evaporation material obtained in the step (1) in a centrifugal grinder to obtain the ground high-purity nickel evaporation material, wherein the second cleaning comprises sequentially cleaning in pure water for 2-10 min and in grinding liquid for 2-10 min under third ultrasonic with the power of 200-300W, and the volume ratio of the hand sanitizer to the pure water in the grinding liquid is 1 (45-55); the third cleaning comprises cleaning in isopropanol for 2-10 min under fourth ultrasonic with the power of 200-300W; the second acid washing comprises washing in a hydrochloric acid solution with the concentration of 38-42 wt% for 2-10 min and washing in pure water for 2-10 min in sequence, and the washing in the pure water in the second acid washing needs to be carried out under fifth ultrasonic with the power of 200-300W;
(3) and (3) drying the ground high-purity nickel evaporation material obtained in the step (2) for 30-50 min at 100-120 ℃ to obtain the cleaned high-purity nickel evaporation material.
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Application publication date: 20210824 |