CN111485239A - Chemical deplating liquid for deplating nickel layer on surface of diamond and deplating method thereof - Google Patents
Chemical deplating liquid for deplating nickel layer on surface of diamond and deplating method thereof Download PDFInfo
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- CN111485239A CN111485239A CN201910084089.7A CN201910084089A CN111485239A CN 111485239 A CN111485239 A CN 111485239A CN 201910084089 A CN201910084089 A CN 201910084089A CN 111485239 A CN111485239 A CN 111485239A
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- China
- Prior art keywords
- deplating
- diamond
- sulfuric acid
- hydrogen peroxide
- nickel layer
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- 239000010432 diamond Substances 0.000 title claims abstract description 46
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 44
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 20
- 239000000126 substance Substances 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 title claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 50
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims abstract 4
- 238000003756 stirring Methods 0.000 claims description 34
- 239000004576 sand Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims 1
- 238000007772 electroless plating Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000002344 surface layer Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 230000007794 irritation Effects 0.000 abstract description 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 abstract 1
- 239000002341 toxic gas Substances 0.000 abstract 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 15
- 238000005303 weighing Methods 0.000 description 9
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
Classifications
-
- 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
- C23F1/30—Acidic compositions for etching other metallic material
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Carbon And Carbon Compounds (AREA)
- Detergent Compositions (AREA)
Abstract
The invention belongs to the technical field of chemical deplating, and particularly relates to a chemical deplating solution for deplating a nickel layer on the surface of diamond and a deplating method thereof. The stripping solution of the invention comprises sulfuric acid and hydrogen peroxide, does not contain nitric acid, and avoids generating NO and NO in the stripping reaction2The plating stripping process has no irritation and toxic smell when the plating stripping process is carried out by toxic gases, and the plating stripping process is very environment-friendly; does not contain cyanide, can reduce environmental pollution, effectively protects the health and safety of operators, and is beneficial to enterprises to carry out large-scale deplating. The deplating method provided by the invention can remove the metal on the surface layer of the diamond at room temperature, and can completely remove the metal coating on the surface of the diamond.
Description
Technical Field
The invention belongs to the technical field of chemical deplating, and particularly relates to a chemical deplating solution for deplating a nickel layer on the surface of diamond and a deplating method thereof.
Background
The diamond wire is a novel cutting tool put into production in recent years, is formed by uniformly fixing diamond particles on a rigid steel wire substrate according to a certain distribution density, and is mainly applied to cutting hard and brittle materials such as photovoltaic silicon materials, sapphires and the like at present.
However, in the production process of the diamond wire, the quality of the nickel layer on the surface of the diamond is deteriorated due to factors such as friction, corrosion and the like, and the diamond cannot be continuously used for production. In order to improve the process flow, save the cost and reasonably utilize resources, the part of the diamond needs to be recycled and deplated (the incomplete metal layer on the surface of the diamond is removed), so that the diamond can be plated again.
The conventional deplating method for diamond adopts direct immersion in nitric acid, and the method can generate a large amount of NO and NO2And the like, seriously harms the safety of human bodies and causes environmental pollution, and is not suitable for large-scale production.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a chemical stripping solution for stripping a nickel layer on the surface of diamond and a stripping method thereof.
In order to achieve the technical purpose, the invention adopts the following technical scheme: the chemical stripping liquid for stripping the nickel layer on the surface of the diamond comprises sulfuric acid and hydrogen peroxide, wherein the volume ratio of the sulfuric acid to the hydrogen peroxide is (2-8): 3-10.
Preferably, the volume ratio of the sulfuric acid to the hydrogen peroxide is 3.5-5.5: 4-8.
The method for deplating the nickel layer on the surface of the diamond comprises the following steps:
step one, recovering residual diamonds in a diamond wire production line, and cleaning to obtain recovered wet sand;
step two, taking the collected wet sand and putting the collected wet sand into a stirring container, adding pure water and starting stirring, wherein the stirring speed is 50-500 rpm;
step three, keeping the stirring state, adding sulfuric acid into the stirring container added with the recovered wet sand and the pure water in the step two, wherein the volume ratio of the sulfuric acid to the pure water is (2-8): 20;
step four, keeping the stirring state, gradually dropwise adding hydrogen peroxide into the stirring container added with the recovered wet sand, the pure water and the sulfuric acid in the step three, wherein the volume ratio of the hydrogen peroxide to the pure water is 3-10: 20, dropwise adding hydrogen peroxide for 10-90 min;
and step five, after dropwise adding hydrogen peroxide and continuously stirring for a period of time, stopping stirring, completing reaction, cleaning and detecting the diamond, and completing deplating of the nickel layer on the surface of the diamond.
Preferably, in the second step, the stirring speed is 150-350 rpm.
Preferably, in the third step, the volume ratio of the sulfuric acid to the pure water is 3.5-5.5: 20.
preferably, in the fourth step, the volume ratio of the hydrogen peroxide to the pure water is 4-8: 20.
preferably, the total time from the start of the addition of sulfuric acid in step three to the stop of stirring in step five is not less than 2 hours.
The sulfuric acid in the deplating method provided by the invention provides an acidic system, and the oxydol can fully and completely exert the oxidation performance under the acidic condition, and Ni + H is reacted2SO4+H2O2→NiSO4+2H2O, thereby completely removing the nickel layer.
The method for stripping the nickel metal on the surface layer of the diamond can strip the nickel metal on the surface layer of the diamond at room temperature, has no irritation and toxic smell in the stripping process, is very environment-friendly, and can thoroughly strip the metal coating on the surface of the diamond. The invention solves the problem of toxic and carcinogenic substances (such as NO and NO) existing in the chemical deplating method in the conventional technology2And the like), simplifies the preparation of the chemical deplating solution (only containing common sulfuric acid and hydrogen peroxide, and no other additives), is more beneficial to large-scale deplating production, reduces the production procedures and cost, and can recover the solution after deplating.
Drawings
The drawings are only for purposes of illustrating and explaining the present invention and are not to be construed as limiting the scope of the present invention. Wherein:
FIG. 1 is a microscope image of diamond before deplating;
FIG. 2 is a microscope image of diamond after deplating.
Detailed Description
In order to make the technical problems, aspects, and advantages of the present invention more comprehensible, the present invention will be described in further detail with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Collecting and cleaning residual diamond on a production line, weighing 2kg of recovered wet sand by using an electronic balance, putting the recovered wet sand into a 15L stirring container, pouring 2L of pure water, starting stirring at the speed of 50rpm, adding 200m of L sulfuric acid into a reactor, weighing 300m of L hydrogen peroxide, adjusting the pump speed, and finishing the adding within 10 min.
Example 2
Collecting and cleaning residual diamond on a production line, weighing 2kg of recovered wet sand by using an electronic balance, putting the recovered wet sand into a 15L stirring container, pouring 2L of pure water, starting stirring at the speed of 500rpm, adding 800m of L sulfuric acid into a reactor, weighing 1000m of L hydrogen peroxide, adjusting the pump speed, and finishing the adding for 90 min.
Example 3
Collecting and cleaning residual diamond on a production line, weighing 2kg of recovered wet sand by using an electronic balance, putting the weighed recovered wet sand into a 15L stirring container, pouring 2L of pure water, starting stirring at the speed of 150rpm, adding 350m of L of sulfuric acid into a reactor, weighing 400m of L of hydrogen peroxide, adjusting the pump speed, and finishing the adding for 30 min.
Example 4
Collecting and cleaning residual diamond on a production line, weighing 2kg of recovered wet sand by using an electronic balance, putting the recovered wet sand into a 15L stirring container, pouring 2L of pure water, starting stirring at the stirring speed of 350rpm, adding 550m of L of sulfuric acid into a reactor, measuring 800m of L of hydrogen peroxide, adjusting the pump speed, and finishing the adding for 60 min.
Example 5
Collecting and cleaning residual diamond on a production line, weighing 2kg of recovered wet sand by using an electronic balance, putting the weighed recovered wet sand into a 15L stirring container, pouring 2L of pure water, starting stirring at the speed of 250rpm, adding 400m of L of sulfuric acid into a reactor, weighing 500m of L of hydrogen peroxide, adjusting the pump speed, and finishing the adding within 45 min.
Performance testing
Counting the time for 120min from the addition of the sulfuric acid, recording the odor of the generated irritant gas in the deplating process, and stopping stirring when the time is up. And cleaning and drying the diamond, and observing the surface condition of the diamond by using a microscope.
Referring to fig. 1 and 2, all of the embodiments of examples 1 to 5 were able to remove the diamond coating layer cleanly from the results of microscopic observation.
| Examples | Odor size | Stripping of the coating |
| 1 | In | All are |
| 2 | Small | All are |
| 3 | Small | All are |
| 4 | Small | All are |
| 5 | Small | All are |
The above description is only an exemplary embodiment of the present invention, and is not intended to limit the scope of the present invention. Any equivalent changes and modifications that can be made by one skilled in the art without departing from the spirit and principles of the invention shall fall within the protection scope of the invention.
Claims (7)
1. The chemical deplating liquid for deplating the nickel layer on the surface of the diamond is characterized in that: the catalyst comprises sulfuric acid and hydrogen peroxide, wherein the volume ratio of the sulfuric acid to the hydrogen peroxide is (2-8): 3-10.
2. The electroless plating solution for nickel layer plating on diamond surfaces according to claim 1, wherein: the volume ratio of the sulfuric acid to the hydrogen peroxide is 3.5-5.5: 4-8.
3. The method for deplating the nickel layer on the surface of the diamond is characterized by comprising the following steps:
step one, recovering residual diamonds in a diamond wire production line, and cleaning to obtain recovered wet sand;
step two, taking the collected wet sand and putting the collected wet sand into a stirring container, adding pure water and starting stirring, wherein the stirring speed is 50-500 rpm;
step three, keeping the stirring state, adding sulfuric acid into the stirring container added with the recovered wet sand and the pure water in the step two, wherein the volume ratio of the sulfuric acid to the pure water is (2-8): 20;
step four, keeping the stirring state, gradually dropwise adding hydrogen peroxide into the stirring container added with the recovered wet sand, the pure water and the sulfuric acid in the step three, wherein the volume ratio of the hydrogen peroxide to the pure water is 3-10: 20, dropwise adding hydrogen peroxide for 10-90 min;
and step five, after dropwise adding hydrogen peroxide and continuously stirring for a period of time, stopping stirring, completing reaction, cleaning and detecting the diamond, and completing deplating of the nickel layer on the surface of the diamond.
4. A method of deplating a nickel layer from a diamond surface as claimed in claim 3, wherein: in the second step, the stirring speed is 150-350 rpm.
5. A method of deplating a nickel layer from a diamond surface as claimed in claim 3, wherein: in the third step, the volume ratio of the sulfuric acid to the pure water is 3.5-5.5: 20.
6. the method for deplating the nickel layer on the surface of the diamond according to claim 5, wherein: in the fourth step, the volume ratio of the hydrogen peroxide to the pure water is 4-8: 20.
7. a method of deplating a nickel layer from a diamond surface as claimed in claim 3, wherein: and (4) starting timing from the addition of the sulfuric acid in the step three, and stopping stirring in the step five for no less than 2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910084089.7A CN111485239A (en) | 2019-01-29 | 2019-01-29 | Chemical deplating liquid for deplating nickel layer on surface of diamond and deplating method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910084089.7A CN111485239A (en) | 2019-01-29 | 2019-01-29 | Chemical deplating liquid for deplating nickel layer on surface of diamond and deplating method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111485239A true CN111485239A (en) | 2020-08-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910084089.7A Pending CN111485239A (en) | 2019-01-29 | 2019-01-29 | Chemical deplating liquid for deplating nickel layer on surface of diamond and deplating method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111485239A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116043227A (en) * | 2022-12-06 | 2023-05-02 | 洛阳吉瓦新材料科技有限公司 | Environment-friendly silicon carbide deplating production device and method |
| CN116445747A (en) * | 2023-03-22 | 2023-07-18 | 湖北绿钨资源循环有限公司 | Method for separating and recovering tungsten and nickel resources from tungsten wire waste for photovoltaic use |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1302979A2 (en) * | 2001-10-15 | 2003-04-16 | Shinko Electric Industries Co. Ltd. | Method of forming through-hole or recess in silicon substrate |
| CN101829964A (en) * | 2010-04-28 | 2010-09-15 | 江西赛维Ldk太阳能高科技有限公司 | Diamond wire and preparation method thereof |
| CN103924245A (en) * | 2014-04-10 | 2014-07-16 | 北京工业大学 | Chemical stripping solution and stripping method |
| CN107460492A (en) * | 2017-07-14 | 2017-12-12 | 镇江仁德新能源科技有限公司 | A kind of diamond cutting secant decoating liquid and its method |
-
2019
- 2019-01-29 CN CN201910084089.7A patent/CN111485239A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1302979A2 (en) * | 2001-10-15 | 2003-04-16 | Shinko Electric Industries Co. Ltd. | Method of forming through-hole or recess in silicon substrate |
| CN101829964A (en) * | 2010-04-28 | 2010-09-15 | 江西赛维Ldk太阳能高科技有限公司 | Diamond wire and preparation method thereof |
| CN103924245A (en) * | 2014-04-10 | 2014-07-16 | 北京工业大学 | Chemical stripping solution and stripping method |
| CN107460492A (en) * | 2017-07-14 | 2017-12-12 | 镇江仁德新能源科技有限公司 | A kind of diamond cutting secant decoating liquid and its method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116043227A (en) * | 2022-12-06 | 2023-05-02 | 洛阳吉瓦新材料科技有限公司 | Environment-friendly silicon carbide deplating production device and method |
| CN116445747A (en) * | 2023-03-22 | 2023-07-18 | 湖北绿钨资源循环有限公司 | Method for separating and recovering tungsten and nickel resources from tungsten wire waste for photovoltaic use |
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Application publication date: 20200804 |
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