CN112605039A - Cleaning method for removing metal conductive film on surface of molybdenum material - Google Patents
Cleaning method for removing metal conductive film on surface of molybdenum material Download PDFInfo
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- CN112605039A CN112605039A CN202011444307.2A CN202011444307A CN112605039A CN 112605039 A CN112605039 A CN 112605039A CN 202011444307 A CN202011444307 A CN 202011444307A CN 112605039 A CN112605039 A CN 112605039A
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- molybdenum material
- molybdenum
- soaking
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 145
- 239000011733 molybdenum Substances 0.000 title claims abstract description 145
- 239000000463 material Substances 0.000 title claims abstract description 113
- 238000004140 cleaning Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 16
- 239000002184 metal Substances 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 89
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 84
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000002791 soaking Methods 0.000 claims abstract description 71
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000005488 sandblasting Methods 0.000 claims abstract description 48
- 238000001035 drying Methods 0.000 claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 28
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 27
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000010926 purge Methods 0.000 claims abstract description 13
- 239000013072 incoming material Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 15
- 238000007689 inspection Methods 0.000 claims description 12
- 238000005422 blasting Methods 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 230000002950 deficient Effects 0.000 claims description 6
- 239000010408 film Substances 0.000 claims 6
- 238000007654 immersion Methods 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 abstract description 7
- 231100000719 pollutant Toxicity 0.000 abstract description 7
- 230000004580 weight loss Effects 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract 1
- 238000005468 ion implantation Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
Classifications
-
- 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
- B08B3/02—Cleaning by the force of jets or sprays
-
- 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
- B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
- B24C1/00—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods
- B24C1/08—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods for polishing surfaces, e.g. smoothing a surface by making use of liquid-borne abrasives
- B24C1/086—Descaling; Removing coating films
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention relates to a cleaning method for removing a metal conductive film on the surface of a molybdenum material, which comprises the following steps: checking incoming materials; washing with pure water; soaking in hydrochloric acid; soaking in oxalic acid; surface sand blasting; soaking in nitric acid and hydrofluoric acid; soaking in pure water; ultrasonic cleaning; purging with nitrogen; and (5) drying. According to the method, hydrochloric acid is adopted for soaking, most deposited pollutants on the surface of the molybdenum material part can be removed conveniently, a sand blasting machine is used for performing sand blasting on the molybdenum material part, an oxide layer on the surface of the molybdenum material part can be removed conveniently, the molybdenum material part is soaked in a mixed solution of nitric acid and hydrofluoric acid, trace metals stained on the surface of the molybdenum material part can be removed, ultrasonic cleaning and nitrogen are used for cleaning the surface of the molybdenum material part, particle pollutants on the surface of the molybdenum material part are greatly reduced, the single weight loss of the molybdenum material part is reduced by adopting the method, the loss of a base material of the molybdenum material part is reduced, the use times of the molybdenum material part are increased, and the use cost of a client is reduced.
Description
Technical Field
The invention relates to the technical field of cleaning of precision spare parts of semiconductor equipment, in particular to a cleaning method for removing a metal conductive film on the surface of a molybdenum material.
Background
The core spare parts of ion implantation process cavities in semiconductor processing equipment and photoelectric processing equipment are easy to deposit pollutants on the surfaces of molybdenum parts in the using process and need to be cleaned and regenerated periodically. The traditional cleaning method of the molybdenum component in the ion implantation equipment only uses sand blasting operation to remove the surface film layer, the method has single process and convenient operation, but can not completely remove deposited pollutants on the surface of the molybdenum component, and can not meet the use requirement for the ion implantation cavity with higher requirement on particle pollutants.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a cleaning method for removing a metal conductive film on the surface of a molybdenum material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a cleaning method for removing a metal conductive film on the surface of a molybdenum material comprises the following steps:
(1) inspection of incoming material
Carrying out appearance inspection on the molybdenum component to be cleaned, and confirming whether the molybdenum component is defective or not;
(2) rinsing with pure water
The molybdenum material part is washed completely by using a water gun, and a loose film layer on the surface of the molybdenum material part is removed;
(3) soaking in hydrochloric acid
Soaking the part to be cleaned in a hydrochloric acid solution, wherein the volume ratio of hydrochloric acid to water in the hydrochloric acid solution is 1:1, soaking for more than 1 hour, removing a film layer attached to the surface of the molybdenum part, taking out, immediately washing with pure water, and washing for 3 minutes;
(4) soaking in oxalic acid
Soaking the molybdenum material part soaked and washed by the hydrochloric acid in the step (3) into oxalic acid solution, wherein the volume ratio of oxalic acid to water in the oxalic acid solution is 1:2, soaking for 10 minutes, removing a residual film layer on the surface of the molybdenum material part, taking out, immediately washing by using pure water, and washing for 3 minutes;
(5) surface blasting
Carrying out sand blasting treatment on the molybdenum material part cleaned in the step (4) by adopting a sand blasting machine, wherein the sand blasting time is 3-5 minutes, and removing an oxide layer on the surface of the molybdenum material part, wherein the parameters of the sand blasting machine are as follows: the pressure is 4-5kg/cm2The distance between the sand blasting gun head and the part is 15-20 cm, the angle is 60-90 degrees, and the sand blasting medium is silicon oxide;
(6) nitric acid and hydrofluoric acid soak
Immersing the molybdenum material part subjected to sand blasting into a mixed solution of nitric acid and hydrofluoric acid, wherein the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution of nitric acid and hydrofluoric acid is 1:1:98, soaking for 3-5 minutes, then immediately taking out, and washing by using pure water;
(7) soaking in pure water
Soaking the molybdenum material part cleaned in the step (6) in pure water for more than 30 minutes, and then blowing water traces on the surface of the part by using compressed air;
(8) ultrasonic cleaning
Transferring the molybdenum material part subjected to water stain drying in the step (7) to a 100-grade clean room, then putting the molybdenum material part into an ultrasonic cleaning tank, cleaning for 30 minutes, turning the part once every 15 minutes, wherein the ultrasonic frequency is 40KHz, the ultrasonic power density is 8-12W/square inch, and pure water in the cleaning tank is kept overflowing;
(9) nitrogen purging
Performing surface purging on the molybdenum component subjected to ultrasonic cleaning in the step (8) by using nitrogen with the purity of 99.999 percent to remove water marks on the surface of the molybdenum component;
(10) drying
And (4) transferring the molybdenum material component purged in the step (9) to a clean drying oven, drying for 3 hours, and taking out the molybdenum material component after the molybdenum material component is naturally cooled.
Preferably, the soaking temperature of the hydrochloric acid solution in the step (3) is 20-40 ℃.
Preferably, the soaking temperature of the oxalic acid solution in the step (4) is 20-40 ℃.
Preferably, the particle size of the silica in the step (5) is 0.03 to 0.5 mm.
Preferably, the roughness of the silicon oxide in the step (5) is required to be 0.5 to 1.0 μm.
Preferably, the overflow flow rate of the pure water in the cleaning tank in the step (8) is 20L/min.
Preferably, the drying temperature of the drying oven in the step (10) is 150 ℃.
The invention has the beneficial effects that: the invention provides a cleaning method for removing a metal conductive film on the surface of a molybdenum material, which is convenient to remove most deposited pollutants on the surface of a molybdenum material part by adopting hydrochloric acid soaking, and does not damage the molybdenum material component, the molybdenum material component is subjected to sand blasting treatment by using a sand blasting machine, so that an oxide layer on the surface of the molybdenum material component is convenient to remove, the molybdenum material component is soaked in a mixed solution of nitric acid and hydrofluoric acid, can remove trace metal stained on the surface of the molybdenum material component, uses ultrasonic cleaning and nitrogen to clean the surface of the molybdenum material component, greatly reduces particle pollutants on the surface of the molybdenum material component, by setting reasonable cleaning parameters and reagent proportion, the method reduces the single weight loss of the molybdenum component, reduces the loss of the base material of the molybdenum component, increases the use times of the molybdenum component and reduces the use cost of a client.
Detailed Description
The invention is further illustrated by the following examples:
a cleaning method for removing a metal conductive film on the surface of a molybdenum material comprises the following steps:
(1) inspection of incoming material
Carrying out appearance inspection on the molybdenum component to be cleaned, and confirming whether the molybdenum component is defective or not;
(2) rinsing with pure water
The molybdenum material part is washed completely by using a water gun, and a loose film layer on the surface of the molybdenum material part is removed;
(3) soaking in hydrochloric acid
Soaking the part to be cleaned in a hydrochloric acid solution, wherein the volume ratio of hydrochloric acid to water in the hydrochloric acid solution is 1:1, soaking for more than 1 hour, removing a film layer attached to the surface of the molybdenum part, taking out, immediately washing with pure water, and washing for 3 minutes;
(4) soaking in oxalic acid
Soaking the molybdenum material part soaked and washed by the hydrochloric acid in the step (3) into oxalic acid solution, wherein the volume ratio of oxalic acid to water in the oxalic acid solution is 1:2, soaking for 10 minutes, removing a residual film layer on the surface of the molybdenum material part, taking out, immediately washing by using pure water, and washing for 3 minutes;
(5) surface blasting
Carrying out sand blasting treatment on the molybdenum material part cleaned in the step (4) by adopting a sand blasting machine, wherein the sand blasting time is 3-5 minutes, and removing an oxide layer on the surface of the molybdenum material part, wherein the parameters of the sand blasting machine are as follows: the pressure is 4-5kg/cm2The distance between the sand blasting gun head and the part is 15-20 cm, the angle is 60-90 degrees, and the sand blasting medium is silicon oxide;
(6) nitric acid and hydrofluoric acid soak
Immersing the molybdenum material part subjected to sand blasting into a mixed solution of nitric acid and hydrofluoric acid, wherein the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution of nitric acid and hydrofluoric acid is 1:1:98, soaking for 3-5 minutes, then immediately taking out, and washing by using pure water;
(7) soaking in pure water
Soaking the molybdenum material part cleaned in the step (6) in pure water for more than 30 minutes, and then blowing water traces on the surface of the part by using compressed air;
(8) ultrasonic cleaning
Transferring the molybdenum material part subjected to water stain drying in the step (7) to a 100-grade clean room, then putting the molybdenum material part into an ultrasonic cleaning tank, cleaning for 30 minutes, turning the part once every 15 minutes, wherein the ultrasonic frequency is 40KHz, the ultrasonic power density is 8-12W/square inch, and pure water in the cleaning tank is kept overflowing;
(9) nitrogen purging
Performing surface purging on the molybdenum component subjected to ultrasonic cleaning in the step (8) by using nitrogen with the purity of 99.999 percent to remove water marks on the surface of the molybdenum component;
(10) drying
And (4) transferring the molybdenum material component purged in the step (9) to a clean drying oven, drying for 3 hours, and taking out the molybdenum material component after the molybdenum material component is naturally cooled.
Preferably, the soaking temperature of the hydrochloric acid solution in the step (3) is 20-40 ℃.
Preferably, the soaking temperature of the oxalic acid solution in the step (4) is 20-40 ℃.
Preferably, the particle size of the silica in the step (5) is 0.03 to 0.5 mm.
Preferably, the roughness of the silicon oxide in the step (5) is required to be 0.5 to 1.0 μm.
Preferably, the overflow flow rate of the pure water in the cleaning tank in the step (8) is 20L/min.
Preferably, the drying temperature of the drying oven in the step (10) is 150 ℃.
The cleaning method is suitable for the field of semiconductor integrated circuit manufacturing and the field of display panel manufacturing, and is used for cleaning molybdenum material spare parts of process equipment such as molybdenum electrodes, molybdenum anti-sticking plates, molybdenum filaments and the like in an ion implantation process, and the single weight loss of the molybdenum material parts is reduced by 80%.
Example 1
A cleaning method for removing a metal conductive film on the surface of a molybdenum material comprises the following steps:
(1) inspection of incoming material
Carrying out appearance inspection on the molybdenum component to be cleaned, and confirming whether the molybdenum component is defective or not;
(2) rinsing with pure water
The molybdenum material part is washed completely by using a water gun, and a loose film layer on the surface of the molybdenum material part is removed;
(3) soaking in hydrochloric acid
Soaking the part to be cleaned in a hydrochloric acid solution, wherein the volume ratio of hydrochloric acid to water in the hydrochloric acid solution is 1:1, the soaking time is more than 1 hour, the soaking temperature is 20 ℃, a film layer attached to the surface of the molybdenum part is removed, the part is immediately washed by pure water after being taken out, and the washing time is 3 minutes;
(4) soaking in oxalic acid
Soaking the molybdenum material part soaked and washed by the hydrochloric acid in the step (3) into oxalic acid solution, wherein the volume ratio of oxalic acid to water in the oxalic acid solution is 1:2, soaking for 10 minutes at the soaking temperature of 20 ℃, removing a residual film layer on the surface of the molybdenum material part, taking out, immediately washing by pure water, and washing for 3 minutes;
(5) surface blasting
Carrying out sand blasting treatment on the molybdenum material part cleaned in the step (4) by adopting a sand blasting machine, wherein the sand blasting time is 3 minutes, and removing an oxide layer on the surface of the molybdenum material part, wherein the parameters of the sand blasting machine are as follows: the pressure was 4kg/cm2The distance between the sand blasting gun head and the part is 15 cm, the angle is 60 degrees, the sand blasting medium is silicon oxide, the grain size of the silicon oxide is 0.03 mm, and the roughness requirement of the silicon oxide is 0.5 micron;
(6) nitric acid and hydrofluoric acid soak
Immersing the molybdenum material part subjected to sand blasting into a mixed solution of nitric acid and hydrofluoric acid, wherein the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution of nitric acid and hydrofluoric acid is 1:1:98, soaking for 3 minutes, then immediately taking out, and washing by using pure water;
(7) soaking in pure water
Soaking the molybdenum material part cleaned in the step (6) in pure water for more than 30 minutes, and then blowing water traces on the surface of the part by using compressed air;
(8) ultrasonic cleaning
Transferring the molybdenum material part subjected to water stain drying in the step (7) to a 100-grade clean room, then putting the molybdenum material part into an ultrasonic cleaning tank, cleaning for 30 minutes, turning the part once every 15 minutes, wherein the ultrasonic frequency is 40KHz, the ultrasonic power density is 8W/square inch, pure water in the cleaning tank keeps overflowing, and the overflow flow is 20L/min;
(9) nitrogen purging
Performing surface purging on the molybdenum component subjected to ultrasonic cleaning in the step (8) by using nitrogen with the purity of 99.999 percent to remove water marks on the surface of the molybdenum component;
(10) drying
And (4) transferring the molybdenum material component purged in the step (9) to a clean drying oven, drying at 150 ℃ for 3 hours, and taking out the molybdenum material component after the molybdenum material component is naturally cooled.
Example 2
A cleaning method for removing a metal conductive film on the surface of a molybdenum material comprises the following steps:
(1) inspection of incoming material
Carrying out appearance inspection on the molybdenum component to be cleaned, and confirming whether the molybdenum component is defective or not;
(2) rinsing with pure water
The molybdenum material part is washed completely by using a water gun, and a loose film layer on the surface of the molybdenum material part is removed;
(3) soaking in hydrochloric acid
Soaking the part to be cleaned in a hydrochloric acid solution, wherein the volume ratio of hydrochloric acid to water in the hydrochloric acid solution is 1:1, the soaking time is more than 1 hour, the soaking temperature is 40 ℃, a film layer attached to the surface of the molybdenum part is removed, the part is immediately washed by pure water after being taken out, and the washing time is 3 minutes;
(4) soaking in oxalic acid
Soaking the molybdenum material part soaked and washed by the hydrochloric acid in the step (3) into oxalic acid solution, wherein the volume ratio of oxalic acid to water in the oxalic acid solution is 1:2, soaking for 10 minutes at the soaking temperature of 40 ℃, removing a residual film layer on the surface of the molybdenum material part, taking out, immediately washing by using pure water, and washing for 3 minutes;
(5) surface blasting
Carrying out sand blasting treatment on the molybdenum component cleaned in the step (4) by adopting a sand blasting machine, wherein the sand blasting time is 5 minutes, and removing an oxide layer on the surface of the molybdenum component, wherein the parameters of the sand blasting machine are as follows: the pressure was 5kg/cm2The distance between the sand blasting gun head and the part is 20 cm, the angle is 90 degrees, the sand blasting medium is silicon oxide, the silicon oxideThe grain size is 0.5 mm, and the roughness of the silicon oxide is required to be 1.0 micron;
(6) nitric acid and hydrofluoric acid soak
Immersing the molybdenum material part subjected to sand blasting into a mixed solution of nitric acid and hydrofluoric acid, wherein the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution of nitric acid and hydrofluoric acid is 1:1:98, soaking for 5 minutes, then immediately taking out, and washing by using pure water;
(7) soaking in pure water
Soaking the molybdenum material part cleaned in the step (6) in pure water for more than 30 minutes, and then blowing water traces on the surface of the part by using compressed air;
(8) ultrasonic cleaning
Transferring the molybdenum material part subjected to water stain drying in the step (7) to a 100-grade clean room, then putting the molybdenum material part into an ultrasonic cleaning tank, cleaning for 30 minutes, turning the part once every 15 minutes, wherein the ultrasonic frequency is 40KHz, the ultrasonic power density is 12W/square inch, pure water in the cleaning tank keeps overflowing, and the overflow flow is 20L/min;
(9) nitrogen purging
Performing surface purging on the molybdenum component subjected to ultrasonic cleaning in the step (8) by using nitrogen with the purity of 99.999 percent to remove water marks on the surface of the molybdenum component;
(10) drying
And (4) transferring the molybdenum material component purged in the step (9) to a clean drying oven, drying at 150 ℃ for 3 hours, and taking out the molybdenum material component after the molybdenum material component is naturally cooled.
Example 3
A cleaning method for removing a metal conductive film on the surface of a molybdenum material comprises the following steps:
(1) inspection of incoming material
Carrying out appearance inspection on the molybdenum component to be cleaned, and confirming whether the molybdenum component is defective or not;
(2) rinsing with pure water
The molybdenum material part is washed completely by using a water gun, and a loose film layer on the surface of the molybdenum material part is removed;
(3) soaking in hydrochloric acid
Soaking the part to be cleaned in a hydrochloric acid solution, wherein the volume ratio of hydrochloric acid to water in the hydrochloric acid solution is 1:1, the soaking time is more than 1 hour, the soaking temperature is 30 ℃, a film layer attached to the surface of the molybdenum part is removed, the part is immediately washed by pure water after being taken out, and the washing time is 3 minutes;
(4) soaking in oxalic acid
Soaking the molybdenum material part soaked and washed by the hydrochloric acid in the step (3) into oxalic acid solution, wherein the volume ratio of oxalic acid to water in the oxalic acid solution is 1:2, soaking for 10 minutes at the soaking temperature of 30 ℃, removing a residual film layer on the surface of the molybdenum material part, taking out, immediately washing by pure water, and washing for 3 minutes;
(5) surface blasting
Carrying out sand blasting treatment on the molybdenum material part cleaned in the step (4) by adopting a sand blasting machine, wherein the sand blasting time is 3-5 minutes, and removing an oxide layer on the surface of the molybdenum material part, wherein the parameters of the sand blasting machine are as follows: the pressure was 4kg/cm2The distance between the sand blasting gun head and the part is 19 cm, the angle is 70 degrees, the sand blasting medium is silicon oxide, the grain size of the silicon oxide is 0.3 mm, and the roughness requirement of the silicon oxide is 0.8 micron;
(6) nitric acid and hydrofluoric acid soak
Immersing the molybdenum material part subjected to sand blasting into a mixed solution of nitric acid and hydrofluoric acid, wherein the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution of nitric acid and hydrofluoric acid is 1:1:98, soaking for 4 minutes, then immediately taking out, and washing by using pure water;
(7) soaking in pure water
Soaking the molybdenum material part cleaned in the step (6) in pure water for more than 30 minutes, and then blowing water traces on the surface of the part by using compressed air;
(8) ultrasonic cleaning
Transferring the molybdenum material part subjected to water stain drying in the step (7) to a 100-grade clean room, then putting the molybdenum material part into an ultrasonic cleaning tank, cleaning for 30 minutes, turning the part once every 15 minutes, wherein the ultrasonic frequency is 40KHz, the ultrasonic power density is 11W/square inch, pure water in the cleaning tank keeps overflowing, and the overflow flow is 20L/min;
(9) nitrogen purging
Performing surface purging on the molybdenum component subjected to ultrasonic cleaning in the step (8) by using nitrogen with the purity of 99.999 percent to remove water marks on the surface of the molybdenum component;
(10) drying
And (4) transferring the molybdenum material component purged in the step (9) to a clean drying oven, drying at 150 ℃ for 3 hours, and taking out the molybdenum material component after the molybdenum material component is naturally cooled.
The invention has been described in an illustrative manner, and it is to be understood that the invention is not limited to the specific embodiments described above, but is intended to cover various modifications, which may be made by the methods and technical solutions of the invention, or may be applied to other applications without modification.
Claims (7)
1. A cleaning method for removing a metal conductive film on the surface of a molybdenum material is characterized by comprising the following steps:
(1) inspection of incoming material
Carrying out appearance inspection on the molybdenum component to be cleaned, and confirming whether the molybdenum component is defective or not;
(2) rinsing with pure water
The molybdenum material part is washed completely by using a water gun, and a loose film layer on the surface of the molybdenum material part is removed;
(3) soaking in hydrochloric acid
Soaking the part to be cleaned in a hydrochloric acid solution, wherein the volume ratio of hydrochloric acid to water in the hydrochloric acid solution is 1:1, soaking for more than 1 hour, removing a film layer attached to the surface of the molybdenum part, taking out, immediately washing with pure water, and washing for 3 minutes;
(4) soaking in oxalic acid
Soaking the molybdenum material part soaked and washed by the hydrochloric acid in the step (3) into oxalic acid solution, wherein the volume ratio of oxalic acid to water in the oxalic acid solution is 1:2, soaking for 10 minutes, removing a residual film layer on the surface of the molybdenum material part, taking out, immediately washing by using pure water, and washing for 3 minutes;
(5) surface blasting
Carrying out sand blasting treatment on the molybdenum material part cleaned in the step (4) by adopting a sand blasting machine, wherein the sand blasting time is 3-5 minutes, and removing an oxide layer on the surface of the molybdenum material part, wherein the parameters of the sand blasting machine are as follows: the pressure is 4-5kg/cm2The distance between the sand blasting gun head and the part is 15-20 cm, the angle is 60-90 degrees, and the sand blasting medium is silicon oxide;
(6) nitric acid and hydrofluoric acid soak
Immersing the molybdenum material part subjected to sand blasting into a mixed solution of nitric acid and hydrofluoric acid, wherein the volume ratio of nitric acid to hydrofluoric acid to water in the mixed solution of nitric acid and hydrofluoric acid is 1:1:98, soaking for 3-5 minutes, then immediately taking out, and washing by using pure water;
(7) soaking in pure water
Soaking the molybdenum material part cleaned in the step (6) in pure water for more than 30 minutes, and then blowing water traces on the surface of the part by using compressed air;
(8) ultrasonic cleaning
Transferring the molybdenum material part subjected to water stain drying in the step (7) to a 100-grade clean room, then putting the molybdenum material part into an ultrasonic cleaning tank, cleaning for 30 minutes, turning the part once every 15 minutes, wherein the ultrasonic frequency is 40KHz, the ultrasonic power density is 8-12W/square inch, and pure water in the cleaning tank is kept overflowing;
(9) nitrogen purging
Performing surface purging on the molybdenum component subjected to ultrasonic cleaning in the step (8) by using nitrogen with the purity of 99.999 percent to remove water marks on the surface of the molybdenum component;
(10) drying
And (4) transferring the molybdenum material component purged in the step (9) to a clean drying oven, drying for 3 hours, and taking out the molybdenum material component after the molybdenum material component is naturally cooled.
2. The method for cleaning the molybdenum material surface with the metal conductive thin film according to claim 1, wherein the soaking temperature of the hydrochloric acid solution in the step (3) is 20-40 ℃.
3. The method as claimed in claim 1, wherein the immersion temperature of the oxalic acid solution in the step (4) is 20-40 ℃.
4. The method as claimed in claim 1, wherein the silicon oxide in step (5) has a particle size of 0.03-0.5 mm.
5. The cleaning method for removing the metal conductive film on the surface of the molybdenum material as claimed in claim 1, wherein the roughness of the silicon oxide in the step (5) is required to be 0.5-1.0 μm.
6. The method as claimed in claim 1, wherein the overflow rate of pure water in the cleaning tank in the step (8) is 20L/min.
7. The method for cleaning the molybdenum material surface with the metal conductive film as claimed in claim 1, wherein the drying temperature of the drying oven in the step (10) is 150 ℃.
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