CN110565129A - Electroplating formula of nonmagnetic nickel-phosphorus alloy and continuous electroplating process thereof - Google Patents
Electroplating formula of nonmagnetic nickel-phosphorus alloy and continuous electroplating process thereof Download PDFInfo
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- CN110565129A CN110565129A CN201910904675.1A CN201910904675A CN110565129A CN 110565129 A CN110565129 A CN 110565129A CN 201910904675 A CN201910904675 A CN 201910904675A CN 110565129 A CN110565129 A CN 110565129A
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- Prior art keywords
- nickel
- phosphorus alloy
- phosphorus
- electroplating
- formula
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- 229910001096 P alloy Inorganic materials 0.000 title claims abstract description 39
- 238000009713 electroplating Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 21
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 title claims description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 12
- 239000011574 phosphorus Substances 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004327 boric acid Substances 0.000 claims abstract description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 6
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims abstract description 6
- CGHIBGNXEGJPQZ-UHFFFAOYSA-N 1-hexyne Chemical compound CCCCC#C CGHIBGNXEGJPQZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 150000002009 diols Chemical class 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims description 30
- 238000005406 washing Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000005238 degreasing Methods 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 description 9
- 238000009472 formulation Methods 0.000 description 5
- KDOWHHULNTXTNS-UHFFFAOYSA-N hex-3-yne-2,5-diol Chemical compound CC(O)C#CC(C)O KDOWHHULNTXTNS-UHFFFAOYSA-N 0.000 description 5
- 230000005389 magnetism Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004685 neutron diffraction pattern Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
the invention relates to the field of continuous electroplating, and discloses an electroplating formula of a nonmagnetic nickel ~ phosphorus alloy and a continuous electroplating process thereof, wherein the electroplating formula comprises 500ml/l of nickel sulfamate, 8g/l of nickel chloride, 40g/l of boric acid, 17g/l of phosphoric acid and 1.2g/l of 3 ~ hexyne ~ 2, 5 ~ diol, and the mass percentage of phosphorus in a nickel ~ phosphorus alloy coating electroplated by using the formula is 11 ~ 16%.
Description
Technical Field
The invention relates to the field of continuous electroplating, in particular to an electroplating formula of a nonmagnetic nickel-phosphorus alloy and a continuous electroplating process thereof.
background
The nickel-phosphorus alloy has the advantages of compact plating layer, corrosion resistance, wear resistance, excellent magnetism, optics, electricity and the like, is widely applied to products such as automobiles, communication, aviation, consumer electronics and the like, and is realized by adopting a chemical plating mode for a long time, but the chemical plating operation parameters are difficult to adjust, the quality is unstable, the yield is low, the productivity is low, chemical nickel needs to be re-bathed every five production periods (about two continuous production days), the technical difficulty of recovering phosphorus in scrapped plating liquid is high, and the trouble is brought to wastewater treatment, so the production cost is high.
Disclosure of Invention
the purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides an electroplating formula of a nonmagnetic nickel-phosphorus alloy and a continuous electroplating process thereof, wherein the mass percent of phosphorus in a nickel-phosphorus alloy coating electroplated by using the electroplating formula and the electroplating process can reach more than 11 percent to form an amorphous coating, and the compactness, the corrosion resistance and the magnetism of the amorphous coating are superior to those of chemical plating.
the technical scheme includes that the non ~ magnetic nickel ~ phosphorus alloy electroplating formula comprises 450 ~ 550ml/l of nickel sulfamate, 6 ~ 12g/l of nickel chloride, 35 ~ 45g/l of boric acid, 17g/l of phosphoric acid and 1.2g/l of 3 ~ hexyne ~ 2, 5 ~ diol, and the mass percentage of phosphorus in the nickel ~ phosphorus alloy electroplated by the formula is 11 ~ 16%.
the invention also provides a continuous electroplating process of the nonmagnetic nickel ~ phosphorus alloy, which comprises the following steps of oil removal, acid pickling and nickel ~ phosphorus plating, wherein the formula of the nonmagnetic nickel ~ phosphorus alloy is used for electroplating, the temperature is controlled to be 60 ℃, the pH value is 1.5 ~ 2, and the current density is 8 ~ 10 ASD.
further, in the oil removing step, the operation specifically comprises the following operations of ultrasonic oil removal at the bath solution temperature of 60 ℃, current density of 8 ~ 15ASD, electrolytic oil removal of alkaline oil removal powder in water solution → normal temperature water washing → hot water washing at 40 ~ 50 ℃.
further, the pickling step specifically comprises the following operations of soaking 8 ~ 20S in 20% sulfuric acid → washing with water at normal temperature → washing with hot water at 40 ~ 50 ℃.
Has the advantages that: the process can obtain amorphous nickel-phosphorus alloy coating with phosphorus mass percentage up to more than 11% by setting parameters of various components in degreasing, pickling, nickel-phosphorus plating and nickel-phosphorus plating liquid medicine and using phosphoric acid with valence state of +5 and a semigloss agent of 3-hexyne-2, 5-diol in a matching way, wherein nickel is one of paramagnetic substances, when the phosphorus content in the phosphorus-nickel alloy reaches more than 11%, the nickel-phosphorus structure has no symmetry and periodic repeatability, and an electron diffraction pattern, a neutron diffraction pattern and an X-ray diffraction pattern of the nickel-phosphorus alloy consist of wider corona and dispersive rings, so that the nickel-phosphorus alloy coating forms amorphous isotropy and has the characteristic of no magnetism. The amorphous nickel-phosphorus alloy coating is characterized in that: 1. non-magnetic; 2. the compactness and the corrosion resistance are better than those of chemical nickel; 3. excellent wear-resisting, magnetism, optics, mechanics advantage; the use of 3-hexyne-2, 5-diol in the electroplating formula ensures that the nickel-phosphorus plating layer has luster (or semi-luster) and the appearance of the plating layer is beautiful, smooth and beautiful. Compared with the traditional chemical nickel plating mode, the nickel-phosphorus alloy plating layer electroplated by the process has stable quality, high yield, low electroplating cost, less phosphorus emission and more environmental protection, all the defects of the chemical nickel-phosphorus alloy plating are solved, the phosphorus content can reach more than 11 percent to form an amorphous nickel-phosphorus alloy plating layer, and the compactness, the corrosion resistance and the magnetism of the amorphous nickel-phosphorus alloy plating layer are superior to those of the chemical plating.
drawings
FIG. 1 is a flow chart of an electroplating process of a nonmagnetic nickel-phosphorus alloy;
FIG. 2 is a photograph of a 2000-fold scanning electron microscope of a nickel-phosphorus alloy coating obtained by the electroplating formulation and process of embodiment 1;
FIG. 3 is a 30-fold scanning electron microscope photograph of a nickel-phosphorus alloy coating obtained by the electroplating formulation and process of embodiment 1;
FIG. 4 is an EDS test pattern of the nickel-phosphorus alloy plating in box 1 of FIG. 3;
FIG. 5 is an EDS test pattern of the nickel-phosphorous alloy coating in box 2 of FIG. 3.
Detailed Description
the present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
the embodiment provides an electroplating formula of a nonmagnetic nickel-phosphorus alloy, which comprises 500ml/l of nickel sulfamate, 8g/l of nickel chloride, 40g/l of boric acid, 17g/l of phosphoric acid and 1.2g/l of 3-hexyne-2, 5-diol.
The nickel-phosphorus alloy plating layer is electroplated by using the electroplating formula through the following continuous electroplating process (the process flow is shown in figure 1):
degreasing, namely ultrasonically degreasing the bath solution at the temperature of 60 ℃, → degreasing the bath solution at the temperature of 60 ℃, performing electrolysis on the bath solution at the current density of 8 ~ 15ASD, and performing alkaline degreasing powder in water solution, namely degreasing the bath solution at the temperature of 40 ~ 50 ℃, washing the bath solution at normal temperature, and washing the bath solution with hot water at the temperature of 40 ~ 50 ℃.
acid washing, namely soaking the steel plate in 20% sulfuric acid for 8 ~ 20S → washing with water at normal temperature → washing with hot water at 40 ~ 50 ℃.
and (3) nickel ~ phosphorus plating, wherein the electroplating formula for electroplating the nonmagnetic nickel ~ phosphorus alloy is adopted, the temperature is controlled to be 60 ℃, the pH value is 1.5 ~ 2, and the current density is 8 ~ 10ASD during electroplating.
As can be seen from fig. 2, the nickel-phosphorus alloy plating layer plated using the above plating formulation and plating process has a dense crystal.
as can be seen from fig. 3 to 5, in the nickel-phosphorus alloy plating layer, the mass percentage of phosphorus reached 15.268% at the 1 st point and 15.303% at the 2 nd point.
Embodiment 2:
The embodiment provides an electroplating formula of a nonmagnetic nickel-phosphorus alloy, which comprises 550ml/l of nickel sulfamate, 6g/l of nickel chloride, 35g/l of boric acid, 17g/l of phosphoric acid and 1.2g/l of 3-hexyne-2, 5-diol.
the nickel-phosphorus alloy plating layer is plated by using the above plating formulation through the same continuous plating process as that of embodiment 1, which is not described herein.
Embodiment 3:
The embodiment provides an electroplating formula of a nonmagnetic nickel-phosphorus alloy, which comprises 450ml/l of nickel sulfamate, 12g/l of nickel chloride, 45g/l of boric acid, 17g/l of phosphoric acid and 1.2g/l of 3-hexyne-2, 5-diol.
The nickel-phosphorus alloy plating layer is plated by using the above plating formulation through the same continuous plating process as that of embodiment 1, which is not described herein.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (4)
1. an electroplating formula of a nonmagnetic nickel ~ phosphorus alloy is characterized by comprising 450 ~ 550ml/l of nickel sulfamate, 6 ~ 12g/l of nickel chloride, 35 ~ 45g/l of boric acid, 17g/l of phosphoric acid and 1.2g/l of 3 ~ hexyne ~ 2, 5 ~ diol, wherein the mass percent of phosphorus in a nickel ~ phosphorus alloy coating electroplated by using the formula is 11 ~ 16%.
2. A continuous electroplating process of a nonmagnetic nickel-phosphorus alloy is characterized by comprising the following steps:
Oil removal
Acid pickling
the nickel-phosphorus plating method comprises the step of using the electroplating formula of the nonmagnetic nickel-phosphorus alloy in claim 1, wherein the temperature is controlled to be 60 ℃, the pH value is 1.5-2, and the current density is 8-10 ASD.
3. The continuous electroplating process of the nonmagnetic nickel-phosphorus alloy according to claim 2, characterized by comprising the following operations in the degreasing step:
ultrasonic degreasing at the bath solution temperature of 60 ℃, current density of 8 ~ 15ASD, electrolytic degreasing of alkaline degreasing powder aqueous solution → normal temperature washing → hot washing at 40 ~ 50 ℃.
4. The continuous electroplating process of the nonmagnetic nickel-phosphorus alloy according to claim 2, characterized in that the pickling step specifically comprises the following operations:
soaking in 20% sulfuric acid for 8 ~ 20S → washing with water at normal temperature → washing with hot water at 40 ~ 50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910904675.1A CN110565129B (en) | 2019-09-24 | 2019-09-24 | Electroplating formula of nonmagnetic nickel-phosphorus alloy and continuous electroplating process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910904675.1A CN110565129B (en) | 2019-09-24 | 2019-09-24 | Electroplating formula of nonmagnetic nickel-phosphorus alloy and continuous electroplating process thereof |
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| CN110565129A true CN110565129A (en) | 2019-12-13 |
| CN110565129B CN110565129B (en) | 2020-06-05 |
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| CN201910904675.1A Active CN110565129B (en) | 2019-09-24 | 2019-09-24 | Electroplating formula of nonmagnetic nickel-phosphorus alloy and continuous electroplating process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112064073A (en) * | 2020-08-04 | 2020-12-11 | 深圳市生利科技有限公司 | Nickel alloy electroplating solution and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3677913A (en) * | 1971-04-01 | 1972-07-18 | M & T Chemicals Inc | Nickel plating |
| JPS5770286A (en) * | 1980-10-22 | 1982-04-30 | Dainippon Printing Co Ltd | Plating bath composition and plating method |
| US4345007A (en) * | 1975-12-17 | 1982-08-17 | General Electric Company | Electro-deposition of a nonmagnetic conductive coating for memory wire protection |
| BG52096A (en) * | 1980-10-31 | 1996-09-30 | Armjanov | Method for the application of complex coating including magnetic layer on an aluminium alloy substrate |
| CN1783217A (en) * | 2004-11-30 | 2006-06-07 | 富士通株式会社 | Method of forming NiP nonmagnetic film and method of manufacturing magnetic head using the film |
| CN101343760A (en) * | 2008-08-28 | 2009-01-14 | 南平市同创电子有限公司 | Microelectron packaging metal cover plate electroplating nickel phosphor alloy production technology |
| CN101730759A (en) * | 2007-06-18 | 2010-06-09 | 维尔英科有限公司 | Method for improving cathode morphology |
-
2019
- 2019-09-24 CN CN201910904675.1A patent/CN110565129B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3677913A (en) * | 1971-04-01 | 1972-07-18 | M & T Chemicals Inc | Nickel plating |
| US4345007A (en) * | 1975-12-17 | 1982-08-17 | General Electric Company | Electro-deposition of a nonmagnetic conductive coating for memory wire protection |
| JPS5770286A (en) * | 1980-10-22 | 1982-04-30 | Dainippon Printing Co Ltd | Plating bath composition and plating method |
| BG52096A (en) * | 1980-10-31 | 1996-09-30 | Armjanov | Method for the application of complex coating including magnetic layer on an aluminium alloy substrate |
| CN1783217A (en) * | 2004-11-30 | 2006-06-07 | 富士通株式会社 | Method of forming NiP nonmagnetic film and method of manufacturing magnetic head using the film |
| CN101730759A (en) * | 2007-06-18 | 2010-06-09 | 维尔英科有限公司 | Method for improving cathode morphology |
| CN101343760A (en) * | 2008-08-28 | 2009-01-14 | 南平市同创电子有限公司 | Microelectron packaging metal cover plate electroplating nickel phosphor alloy production technology |
Non-Patent Citations (1)
| Title |
|---|
| 李雪城 等: "脉冲电铸非晶态镍磷合金试验研究", 《电加工与模具》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112064073A (en) * | 2020-08-04 | 2020-12-11 | 深圳市生利科技有限公司 | Nickel alloy electroplating solution and application thereof |
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| CN110565129B (en) | 2020-06-05 |
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Effective date of registration: 20231108 Address after: 523000 No. 2, Yinhu Third Road, shishuikou, Qiaotou town, Dongguan City, Guangdong Province Patentee after: DONGGUAN STANDARD ELECTRONIC MATERIAL CO.,LTD. Address before: Room 393, No. 68, Dongcheng Section, Yunhe West 1st Road, Dongcheng Street, Dongguan City, Guangdong Province, 523000 Patentee before: Dongguan Guanxing Intellectual Property Agency Co.,Ltd. Effective date of registration: 20231108 Address after: Room 393, No. 68, Dongcheng Section, Yunhe West 1st Road, Dongcheng Street, Dongguan City, Guangdong Province, 523000 Patentee after: Dongguan Guanxing Intellectual Property Agency Co.,Ltd. Address before: 223005 Huaian 1 Jiangsu economic and Technological Development Zone Patentee before: HUAIYIN INSTITUTE OF TECHNOLOGY |