CN111020577B - TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment - Google Patents
TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment Download PDFInfo
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- CN111020577B CN111020577B CN201911055808.9A CN201911055808A CN111020577B CN 111020577 B CN111020577 B CN 111020577B CN 201911055808 A CN201911055808 A CN 201911055808A CN 111020577 B CN111020577 B CN 111020577B
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
Abstract
The invention discloses a TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment, which is used for plating the surface of a titanium alloy material subjected to high-temperature diffusion welding through the steps of oil removal, oxide removal, alkaline washing activation, nickel preplating, chemical nickel plating, acid washing activation, flash gold plating, pulse gold plating and the like.
Description
Technical Field
The invention relates to the technical field of titanium alloy plating, in particular to a TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment.
Background
The TC4 titanium alloy treated by high-temperature diffusion welding (the temperature is 800-900 ℃, the vacuum degree is 8 multiplied by 10 < -3 > Pa) has changed surface texture structure and oxide composition, and a coating layer with good bonding force cannot be obtained on the titanium alloy by using the traditional titanium alloy plating process. In addition, in order to obtain a coating layer with good bonding force on the TC4 titanium alloy base material, the pretreatment process of the existing mature TC4 titanium alloy coating process generally uses strong acid, strong base, strong oxidant, fluoride and chromate, and the chemicals have great harm to the environment and cause great potential safety hazard to wastewater treatment and production safety of operators. The pretreatment process of the environmentally-friendly TC4 plating process has extremely strict operation conditions, long production period and extremely difficult realization of batch production.
Therefore, the TC4 titanium alloy surface plating green process aiming at the high-temperature diffusion welding treatment, which can be produced stably in batches, is environment-friendly and has good bonding force, is significant.
Disclosure of Invention
In order to solve the problems, the invention provides a TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment.
Specifically, the TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment comprises the following steps:
s1, oxide removal: removing oxides on the surface of the titanium alloy by sand blasting, and cleaning sand grains on the surface of the titanium alloy by compressed air;
s2, alkali washing activation: cleaning the titanium alloy by using a strong alkaline solution to ensure that the surface of the titanium alloy has activity;
s3, nickel preplating: putting the titanium alloy activated by alkali washing into a nickel pre-plating solution, and performing nickel pre-plating treatment on the titanium alloy for 60-150 s by using a current of 5-8A/dm 2;
s4, chemical nickel plating: carrying out chemical nickel plating treatment on the titanium alloy subjected to the nickel pre-plating treatment for more than 15 min;
s5, acid washing activation: washing and drying the titanium alloy subjected to the chemical nickel plating treatment with water, removing residual organic matters on the surface and grease brought in during the operation process, and washing the titanium alloy with sulfuric acid with the concentration of 70-200 g/L for 60-120 s;
s6, flash gold plating: carrying out flash gold plating treatment on the titanium alloy subjected to acid pickling and activating treatment for 0.5-1.5 min;
s7, pulse gold plating: performing pulse gold plating on the titanium alloy subjected to the flash gold plating treatment, wherein the current density is 1.5A-2.5/dm 2; the time is 15-20 min.
Further, the method also comprises a first ultrasonic chemical oil removal step: and performing first ultrasonic chemical degreasing on the titanium alloy before the step S1 to remove residual grease on the surface of the titanium alloy.
Further, the titanium alloy after the first ultrasonic chemical degreasing treatment is washed by water and dried at the temperature lower than 100 ℃.
Further, the method also comprises a second ultrasonic chemical oil removal step: and after the step S2, performing secondary ultrasonic chemical degreasing and water washing on the titanium alloy to remove grease brought in the sand blasting process and other operation processes on the surface of the titanium alloy.
Further, the nickel preplating solution comprises HCl with the concentration of 70-200 ml/L and NiCl with the concentration of 300-400 mg/L2。
Further, the water washing in step S5 includes tap water washing and ultrasonic ion water washing.
Further, the drying temperature in step S5 is lower than 150 ℃, and the drying time is 2 h.
Further, the method also comprises the following post-processing steps: and (3) sequentially carrying out tap water washing, ultrasonic deionized water washing and drying treatment on the titanium alloy subjected to the pulse gold plating treatment.
Further, the ultrasonic deionized water washing temperature is 80-90 ℃, and the time is 5-10 min; when drying, the oven is heated to 100 ℃, the titanium alloy parts are placed in the oven, the temperature is raised to 350 ℃ for drying, and the drying time is 20 min.
The invention has the beneficial effects that: (1) the process can obtain a coating layer with good bonding force on the TC4 titanium alloy base material treated by high-temperature diffusion welding.
(2) Compared with the traditional titanium alloy plating process, the process does not introduce dangerous chemicals such as strong oxidant, fluoride, chromate and the like, and is safe and environment-friendly.
(3) Compared with the traditional titanium alloy plating process, the process has the advantages of simple and convenient operation, shorter process route and less time consumption, and can be used for batch production.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
A TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment comprises the following specific process steps:
example one
1) Ultrasonic chemical degreasing
Can remove the residual oil stain of the surface machining and ensure the continuity of the water film in 30s on the surface of the material after washing.
2) Cleaning of
Running tap water was subjected to two-stage water washing for 15s per stage.
3) Drying by baking
Baking at 100 deg.C or below until the residual water on the surface of the material is dried.
4) Sand spray-drying
And removing oxide on the surface of the material by sand blasting to increase the surface roughness of the material.
5) Compressed air blows off residual sand grains
The pressure of compressed air is required to be 0.4-0.6 MPa, the compressed air is required to be free of oil and water, and sand grains remained on the surface of the material are cleaned.
6) Ultrasonic chemical degreasing
The grease brought in the sand blasting process and other operation processes of the material surface can be removed, and the water film continuity in the material surface 30s after water washing is ensured.
7) Washing with water
Two stages of tap water cleaning, 15s each.
8) Alkali washing activation
And (3) cleaning by using a strong alkaline solution to generate certain activity on the surface of the material.
9) Pre-nickel plating
HCl：70ml/L；
NiCl2：300g/L；
Current density: 3A/dm 2;
temperature: normal temperature;
time: 60s to 150 s.
10) Electroless nickel plating
And (3) carrying out high-temperature chemical nickel plating with medium phosphorus (containing 6-9 percent of phosphorus), wherein the nickel content is 5.6-6 g/L, the pH is controlled to be 4.6-4.9, the temperature is controlled to be 85-91 ℃, and the plating is carried out for more than 15 min.
11) Cleaning of
(a) Washing and cleaning with tap water: two-stage cleaning, 15s for each stage;
(b) ultrasonic deionized water washing: and 5 min.
12) Drying
Baking at 150 deg.C for 2 hr, and air cooling.
13) Ultrasonic chemical degreasing
Removing residual organic matters after nickel plating and grease brought in by other operation processes. And the water film in the cleaned 30s after oil removal is ensured not to break continuously.
14) Acid washing activation
The pickling solution comprises the following components: 70g/L of sulfuric acid; temperature: normal temperature; time: 60s to 120 s.
15) Flash gold plating
0.1-3 g/L of gold, 140-180 g/L of anhydrous sodium sulfite, 80-100 g/L of potassium citrate, 8-10 of pH and 1-2A/dm of current density2The temperature is 45-50 ℃, the time is 0.5-1.5 min, and the plating time is as follows: 0.5-1.5 min.
16) Pulse gold plating
10-15g/L of Au, 140-180 g/L of sodium sulfite, 80-100 g/L of potassium citrate, 60-100g/L of potassium chloride, 40-60 ℃, 8-10 of pH and 0.3A/dm of current density2Plating time: 15-20 min.
17) Washing with water
And two-stage cleaning, wherein each stage of cleaning is performed for 15s by using tap water.
18) Ultrasonic deionized water washing
Temperature: 80-90 ℃; time: 5-10 min.
19) Drying by baking
(a) The temperature is 350 ℃ (the oven is heated to 100 ℃ and the parts are put in, and the temperature is raised to 350 ℃);
(b) time: 20 min;
(c) and cooling the part along with the furnace.
Example two
1) Ultrasonic chemical degreasing
Can remove the residual oil stain of the surface machining and ensure the continuity of the water film in 30s on the surface of the material after washing.
2) Cleaning of
Running tap water was subjected to two-stage water washing for 15s per stage.
3) Drying by baking
Baking at 100 deg.C or below until the residual water on the surface of the material is dried.
4) Sand spray-drying
And removing oxide on the surface of the material by sand blasting to increase the surface roughness of the material.
5) Compressed air blows off residual sand grains
The pressure of compressed air is required to be 0.4-0.6 MPa, the compressed air is required to be free of oil and water, and sand grains remained on the surface of the material are cleaned.
6) Ultrasonic chemical degreasing
The grease brought in the sand blasting process and other operation processes of the material surface can be removed, and the water film continuity in the material surface 30s after water washing is ensured.
7) Washing with water
Two stages of tap water cleaning, 15s each.
8) Alkali washing activation
And (3) cleaning by using a strong alkaline solution to generate certain activity on the surface of the material.
9) Pre-nickel plating
HCl：９０ml/L；
NiCl2：３５０g/L；
Current density: 5A/dm 2;
temperature: normal temperature;
time: 60s to 150 s.
10) Electroless nickel plating
And (3) carrying out high-temperature chemical nickel plating with medium phosphorus (containing 6-9 percent of phosphorus), wherein the nickel content is 5.6-6 g/L, the pH is controlled to be 4.6-4.9, the temperature is controlled to be 85-91 ℃, and the plating is carried out for more than 15 min.
11) Cleaning of
(a) Washing and cleaning with tap water: two-stage cleaning, 15s for each stage;
(b) ultrasonic deionized water washing: and 5 min.
12) Drying
Baking at 150 deg.C for 2 hr, and air cooling.
13) Ultrasonic chemical degreasing
Removing residual organic matters after nickel plating and grease brought in by other operation processes. And the water film in the cleaned 30s after oil removal is ensured not to break continuously.
14) Acid washing activation
The pickling solution comprises the following components: 150 g/L of sulfuric acid; temperature: normal temperature; time: 60s to 120 s.
15) Flash gold plating
0.1-3 g/L of gold, 140-180 g/L of anhydrous sodium sulfite, 80-100 g/L of potassium citrate, 8-10 of pH and 1-2A/dm of current density2The temperature is 45-50 ℃, the time is 0.5-1.5 min, and the plating time is as follows: 0.5-1.5 min.
16) Pulse gold plating
10-15g/L of Au, 140-180 g/L of sodium sulfite, 80-100 g/L of potassium citrate, 60-100g/L of potassium chloride, 40-60 ℃, 8-10 of pH and 0.3A/dm of current density2Plating time: 15-20 min.
17) Washing with water
And two-stage cleaning, wherein each stage of cleaning is performed for 15s by using tap water.
18) Ultrasonic deionized water washing
Temperature: 80-90 ℃; time: 5-10 min.
19) Drying by baking
(a) The temperature is 350 ℃ (the oven is heated to 100 ℃ and the parts are put in, and the temperature is raised to 350 ℃);
(b) time: 20 min;
(c) and cooling the part along with the furnace.
EXAMPLE III
1) Ultrasonic chemical degreasing
Can remove the residual oil stain of the surface machining and ensure the continuity of the water film in 30s on the surface of the material after washing.
2) Cleaning of
Running tap water was subjected to two-stage water washing for 15s per stage.
3) Drying by baking
Baking at 100 deg.C or below until the residual water on the surface of the material is dried.
4) Sand spray-drying
And removing oxide on the surface of the material by sand blasting to increase the surface roughness of the material.
5) Compressed air blows off residual sand grains
The pressure of compressed air is required to be 0.4-0.6 MPa, the compressed air is required to be free of oil and water, and sand grains remained on the surface of the material are cleaned.
6) Ultrasonic chemical degreasing
The grease brought in the sand blasting process and other operation processes of the material surface can be removed, and the water film continuity in the material surface 30s after water washing is ensured.
7) Washing with water
Two stages of tap water cleaning, 15s each.
8) Alkali washing activation
And (3) cleaning by using a strong alkaline solution to generate certain activity on the surface of the material.
9) Pre-nickel plating
HCl：１１０ml/L；
NiCl2：４００g/L；
Current density: 8A/dm 2;
temperature: normal temperature;
time: 60s to 150 s.
10) Electroless nickel plating
And (3) carrying out high-temperature chemical nickel plating with medium phosphorus (containing 6-9 percent of phosphorus), wherein the nickel content is 5.6-6 g/L, the pH is controlled to be 4.6-4.9, the temperature is controlled to be 85-91 ℃, and the plating is carried out for more than 15 min.
11) Cleaning of
(a) Washing and cleaning with tap water: two-stage cleaning, 15s for each stage;
(b) ultrasonic deionized water washing: and 5 min.
12) Drying
Baking at 150 deg.C for 2 hr, and air cooling.
13) Ultrasonic chemical degreasing
Removing residual organic matters after nickel plating and grease brought in by other operation processes. And the water film in the cleaned 30s after oil removal is ensured not to break continuously.
14) Acid washing activation
The pickling solution comprises the following components: 200g/L of sulfuric acid; temperature: normal temperature; time: 60s to 120 s.
15) Flash gold plating
0.1-3 g/L of gold, 140-180 g/L of anhydrous sodium sulfite, 80-100 g/L of potassium citrate, 8-10 of pH and 1-2A/dm of current density2The temperature is 45-50 ℃, the time is 0.5-1.5 min, and the plating time is as follows: 0.5-1.5 min.
16) Pulse gold plating
10-15g/L of Au, 140-180 g/L of sodium sulfite, 80-100 g/L of potassium citrate, 60-100g/L of potassium chloride, 40-60 ℃, 8-10 of pH and 0.3A/dm of current density2Plating time: 15-20 min.
17) Washing with water
And two-stage cleaning, wherein each stage of cleaning is performed for 15s by using tap water.
18) Ultrasonic deionized water washing
Temperature: 80-90 ℃; time: 5-10 min.
19) Drying by baking
(a) The temperature is 350 ℃ (the oven is heated to 100 ℃ and the parts are put in, and the temperature is raised to 350 ℃);
(b) time: 20 min;
(c) and cooling the part along with the furnace.
Claims (8)
1. The TC4 titanium alloy surface plating process after high-temperature diffusion welding treatment is characterized by comprising the following steps of:
s1, oxide removal: removing oxides on the surface of the titanium alloy by sand blasting, and cleaning sand grains on the surface of the titanium alloy by compressed air;
s2, alkali washing activation: cleaning the titanium alloy by using a strong alkaline solution to ensure that the surface of the titanium alloy has activity;
s3, nickel preplating: putting the titanium alloy activated by alkali washing into a nickel pre-plating solution, and performing nickel pre-plating treatment on the titanium alloy for 60-150 s by using a current of 5-8A/dm 2, wherein the nickel pre-plating solution comprises HCl with the concentration of 70-110 ml/L and NiCl with the concentration of 300-400 g/L2；
S4, chemical nickel plating: carrying out chemical nickel plating treatment on the titanium alloy subjected to the nickel pre-plating treatment for more than 15 min;
s5, acid washing activation: washing and drying the titanium alloy subjected to the chemical nickel plating treatment with water, removing residual organic matters on the surface and grease brought in during the operation process, and washing the titanium alloy with sulfuric acid with the concentration of 70-200 g/L for 60-120 s;
s6, flash gold plating: carrying out flash gold plating treatment on the titanium alloy subjected to acid pickling and activating treatment for 0.5-1.5 min;
s7, pulse gold plating: performing pulse gold plating on the titanium alloy subjected to the flash gold plating treatment, wherein the current density is 1.5A-2.5/dm 2; the time is 15-20 min;
and the method also comprises a post-treatment drying treatment step, wherein during drying, the drying oven is heated to 100 ℃, the titanium alloy part is placed in the drying oven, the temperature is raised to 350 ℃ for drying, and the drying time is 20 min.
2. The TC4 titanium alloy surface plating process after the high-temperature diffusion welding treatment according to claim 1, characterized by further comprising a first ultrasonic chemical degreasing step: and performing first ultrasonic chemical degreasing on the titanium alloy before the step S1 to remove residual grease on the surface of the titanium alloy.
3. The TC4 titanium alloy surface plating process after the high-temperature diffusion welding treatment according to claim 2, wherein the titanium alloy after the first ultrasonic chemical degreasing treatment is washed with water and dried at a temperature lower than 100 ℃.
4. The TC4 titanium alloy surface plating process after the high-temperature diffusion welding treatment according to claim 1, characterized by further comprising a second ultrasonic chemical degreasing step: and after the step S2, performing secondary ultrasonic chemical degreasing and water washing on the titanium alloy to remove grease brought in the sand blasting process and other operation processes on the surface of the titanium alloy.
5. The TC4 titanium alloy surface plating process after the high-temperature diffusion welding treatment according to claim 1, wherein the water washing in the step S5 comprises tap water washing and ultrasonic ion water washing.
6. The TC4 titanium alloy surface plating process after the high-temperature diffusion welding treatment as claimed in claim 1, wherein the drying temperature in the step S5 is lower than 150 ℃, and the drying time is 2 h.
7. The TC4 titanium alloy surface plating process after the high-temperature diffusion welding treatment according to claim 1, characterized by further comprising a post-treatment step: and (3) sequentially carrying out tap water washing, ultrasonic deionized water washing and drying treatment on the titanium alloy subjected to the pulse gold plating treatment.
8. The TC4 titanium alloy surface plating process after the high-temperature diffusion welding treatment according to claim 7, wherein the ultrasonic deionized water washing temperature is 80-90 ℃ and the time is 5-10 min.
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