CN101165219A - Method for control size of electroforming nickel crystal in nickel sulphate electroforming liquid - Google Patents
Method for control size of electroforming nickel crystal in nickel sulphate electroforming liquid Download PDFInfo
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- CN101165219A CN101165219A CNA2007101200645A CN200710120064A CN101165219A CN 101165219 A CN101165219 A CN 101165219A CN A2007101200645 A CNA2007101200645 A CN A2007101200645A CN 200710120064 A CN200710120064 A CN 200710120064A CN 101165219 A CN101165219 A CN 101165219A
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- deionized water
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Abstract
The present invention is nickel sulfate electroforming process capable of controlling the size of electroformed nickel crystal, and belongs to the field of electroforming technology. The technological process includes the steps of compounding electroforming fluid, pre-treatment of cathode material and nickel electrolyzing anode, electroforming, and cathode demolding. The present invention is superior in that the size of electroformed nickel crystal and thus the performance of electroformed nickel may be controlled easily and effectively.
Description
Technical field
The invention belongs to the electroforming preparing technical field, a kind of method of controlling the electroformed nickel grain-size in the single nickel salt electroforming solution particularly is provided, be used to control the electroformed nickel grain-size and then obtain different processing characteristicies, is a kind of practical technique easily and effectively.
Background technology
Because electroformed nickel compares with other electroforming material, not only have excellent in chemical, machining property and mechanical property and also can be used for the high-precision component of electroforming (Liu Renzhi. the nickel electroforming. practical galvanoplastics .2006,9; 242-243.).It is stable inadequately that but electroforming at present also exists the electroformed layer performance, the undesirable deficiency that waits of intensity under the normal temperature.By famous Hall-Petch formula, the grain size of the performance of metallic substance and material structure has substantial connection as can be known, and obtained widely confirming, for example from grain-size to the influence of pure iron mechanical property (Sun Maocai. flow of metal. Metal Mechanic Property .2003 (6); 46-47.) can find out increase along with grain-size, the yield strength of pure iron, tensile strength, unit elongation all have significant increase.Electroformed nickel is the important materials of the broken first key position-cavity liner of preparation, test show the grain-size of the shaped charge action of electroformed nickel cavity liner and material have confidential relation (Yang Feng, Tian Wenhuai etc. the variation of electroformed nickel cavity liner microstructure and property after anneal. Arms Material and science .2005 (11); 6-29.), control electroforming pure nickel grain-size can significantly improve the shaped charge action of electroforming pure nickel cavity liner at 1-5 μ m.The grain-size of material is also more and more paid attention to by people the influence of some properties of material, for example grain-size to the influence of nanocrystalline cobalt friction wear performance (Wang Liping, Gao Yan etc. grain-size is to the influence of nanocrystalline cobalt friction wear performance. sufacing .2005,2; 1-34.) etc.
At present domestic patent about the electroforming aspect is mainly concentrated electrocasting method and preparation, to the present patent that does not also have in this respect of grain-size how to control electroforming material.
Summary of the invention
The object of the present invention is to provide a kind of in the single nickel salt electroforming solution method of control electroformed nickel grain-size, problem such as it is stable inadequately to solve electroformed nickel settled layer performance, and intensity is undesirable under the normal temperature.Can make things convenient for, effectively control the grain size of electroformed nickel and then the performance of control electroformed nickel by the present invention.Technology of the present invention is:
(1) joins electroforming solution: the deionized water that in the electrotyping bath that cleans up with deionized water, adds electrotyping bath volume 1/3-2/3, regulate stir speed (S.S.) (20-80r/min) and be heated to 45-55 ℃, insulation 1-2h, in electrotyping bath, add 250-350g/L six hydration nickel sulfate, 42-55g/L nickelous chloride, 0.05-2g/L asccharin successively.
The deionized water that in the Glass Containers that cleans up with deionized water, adds electrotyping bath volume 1/5-2/5, be stirred and heated to boiling, add 25-40g/L boric acid and boil 20-40min, add the 0.02-1g/L sodium lauryl sulphate then, after treating that sodium lauryl sulphate is fully dissolved, the liquid for preparing in the Glass Containers is poured in the electrotyping bath.The deionized water that reinjects is filled it up with electrotyping bath.Fully stir, be incubated 6-14h at 45-55 ℃.
(2) cathode material, the pre-treatment of electrolytic nickel anode: cathode material is through (240
#→ 400
#→ 600
#) silicon carbide waterproof abrasive paper polishing → deionization washing → nitric acid passivation → deionization washing → drying; The electrolytic nickel anode cleans in boiling water → deionization washing → hydrochloric acid activation → deionization washing with brush.
(3) electroforming: the sulphuric acid soln with 3-8% is regulated pH=3.5-4.5, and anode electrolysis nickel plate is put into the anode basket and connected circuit, regulates current density 1-7A/dm
2, holding current density constant, the electroforming of not cutting off the power supply.
(4) the negative electrode demoulding: the mechanical external force demoulding (knocking) → deionization washing → drying with hammer.Can get the electroformed nickel of various grain sizes by this Fang Fang and electroforming flow process.
The invention has the advantages that: the present invention can make things convenient for, effectively control the grain size of electroformed nickel and then the performance of control electroformed nickel.
Description of drawings
Fig. 1 is the electroformed nickel plate surface topography SEM photo that utilizes the technology of the present invention preparation, and asccharin content is 0.1g/L, and the mensuration by grain fineness number The grain size as can be known is about 3.5 μ m.
Fig. 2 is the electroformed nickel plate surface topography SEM photo that utilizes the technology of the present invention preparation, and asccharin content is 0.2g/L, and the mensuration by grain fineness number The grain size as can be known is about 2.0 μ m.
Fig. 3 is the electroformed nickel plate surface topography SEM photo that utilizes the technology of the present invention preparation, and asccharin content is 0.4g/L, and the mensuration by grain fineness number The grain size as can be known is about 1.2 μ m.
Embodiment
Six hydration nickel sulfate electroforming solution preparation: add the 1L deionized water in volume is the beaker of 2L, stirs (40r/min) and be heated to 50 ℃, insulation 1h adds six hydration nickel sulfate, the 94.8g nickelous chloride of 562g successively.Getting 400mL beaker deionized water rinsing, drying, add the 400mL deionized water, be stirred and heated to boiling, add 56g boric acid and boil half an hour, add the 0.8g sodium lauryl sulphate then, treat that sodium lauryl sulphate is fully dissolved after, it is slowly poured in the six hydration nickel sulfate solution, add the 0.2g asccharin, add deionized water again to solution 2L.Fully stir, be incubated (50 ℃) 12h.
The pre-treatment of negative electrode, anode material: with used negative electrode stainless steel 240
#→ 400
#→ 600
#The polishing of silicon carbide waterproof abrasive paper is rinsed well with deionized water, puts into nitric acid and carries out surface passivation in 10 minutes.Anode electrolysis nickel plate with the careful clean surface of toothbrush, is put into sheet nickel hydrochloric acid then and made its surface active in 15 minutes.
Electroforming: the sulphuric acid soln with 5% is regulated pH=4.0, and anode electrolysis nickel plate is put into the anode basket and connected circuit, and the adjusting current density is 5A/dm
2, the holding current density constant, electroforming 6h does not cut off the power supply.
The demoulding: take out anode and carry out the demoulding (rapping) with hammer.To gained electroformed nickel sample clean, drying.
In above-mentioned 2L solution, regulate asccharin content and be respectively 0.4g, 0.8g.Repeat above process.Electroformed nickel plate sample to different asccharin content of add (0.1g/L, 0.2g/L, 0.4g/) carries out surperficial sem analysis.Result such as Fig. 1-3.
Claims (1)
1. the method for a control electroformed nickel grain-size in the single nickel salt electroforming solution is characterized in that technology is:
(1) joins electroforming solution: the deionized water that in the electrotyping bath that cleans up with deionized water, adds electrotyping bath volume 1/3-2/3, regulate stir speed (S.S.) 20-80r/min, be heated to 45-55 ℃, insulation 1-2h, in electrotyping bath, add 250-350g/L six hydration nickel sulfate, 42-55g/L nickelous chloride, 0.05-2g/L asccharin successively;
The deionized water that in the Glass Containers that cleans up with deionized water, adds electrotyping bath volume 1/5-2/5, be stirred and heated to boiling, add 25-40g/L boric acid and boil 20-40min, add the 0.02-1g/L sodium lauryl sulphate then, after treating the sodium lauryl sulphate dissolving, the liquid for preparing in the Glass Containers is poured in the electrotyping bath; Inject deionized water and fill it up with electrotyping bath; Stir, be incubated 6-14h at 45-55 ℃;
(2) cathode material, the pre-treatment of electrolytic nickel anode: cathode material is through 240
#→ 400
#→ 600
#Silicon carbide waterproof abrasive paper polishing → deionization washing → nitric acid passivation → deionization washing → drying; The electrolytic nickel anode cleans in boiling water → deionization washing → hydrochloric acid activation → deionization washing with brush;
(3) electroforming: the sulphuric acid soln with 3-8% is regulated pH=3.5-4.5, and anode electrolysis nickel plate is put into the anode basket and connected circuit, regulates current density 1-7A/dm
2, the holding current density constant;
(4) the negative electrode demoulding: knock the demoulding → deionization washing → drying with hammer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101200645A CN101165219A (en) | 2007-08-08 | 2007-08-08 | Method for control size of electroforming nickel crystal in nickel sulphate electroforming liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101200645A CN101165219A (en) | 2007-08-08 | 2007-08-08 | Method for control size of electroforming nickel crystal in nickel sulphate electroforming liquid |
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| CN101165219A true CN101165219A (en) | 2008-04-23 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104805476A (en) * | 2015-04-21 | 2015-07-29 | 柳州凡一科技有限公司 | Electroplating solution for base plate of rice transplanter |
| CN104862748A (en) * | 2015-05-29 | 2015-08-26 | 中国科学院金属研究所 | Crystalline grain scale gradient metallic nickel and controllable preparation method thereof |
| CN105220184A (en) * | 2015-08-11 | 2016-01-06 | 模德模具(苏州工业园区)有限公司 | A kind of Nickel Electroforming Electrolyte Solution and preparation method thereof |
| CN106283129A (en) * | 2016-10-08 | 2017-01-04 | 贵州大学 | For fracture or the electroplate liquid of crackle quick electronickelling and technique and device |
| CN113551963A (en) * | 2021-08-18 | 2021-10-26 | 山西太钢不锈钢股份有限公司 | Method for preparing metallographic specimen of stainless steel ultrathin precise strip steel cross section |
-
2007
- 2007-08-08 CN CNA2007101200645A patent/CN101165219A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104805476A (en) * | 2015-04-21 | 2015-07-29 | 柳州凡一科技有限公司 | Electroplating solution for base plate of rice transplanter |
| CN104862748A (en) * | 2015-05-29 | 2015-08-26 | 中国科学院金属研究所 | Crystalline grain scale gradient metallic nickel and controllable preparation method thereof |
| CN105220184A (en) * | 2015-08-11 | 2016-01-06 | 模德模具(苏州工业园区)有限公司 | A kind of Nickel Electroforming Electrolyte Solution and preparation method thereof |
| CN106283129A (en) * | 2016-10-08 | 2017-01-04 | 贵州大学 | For fracture or the electroplate liquid of crackle quick electronickelling and technique and device |
| CN113551963A (en) * | 2021-08-18 | 2021-10-26 | 山西太钢不锈钢股份有限公司 | Method for preparing metallographic specimen of stainless steel ultrathin precise strip steel cross section |
| CN113551963B (en) * | 2021-08-18 | 2024-05-28 | 山西太钢不锈钢股份有限公司 | Method for preparing metallographic specimen of stainless steel ultrathin precise strip steel cross section |
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Open date: 20080423 |