CN106087009A - A kind of Graphene scaffold composite plating solution - Google Patents

A kind of Graphene scaffold composite plating solution Download PDF

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Publication number
CN106087009A
CN106087009A CN201610673563.6A CN201610673563A CN106087009A CN 106087009 A CN106087009 A CN 106087009A CN 201610673563 A CN201610673563 A CN 201610673563A CN 106087009 A CN106087009 A CN 106087009A
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deionized water
nickel
added
ethanol
standby
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CN201610673563.6A
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王世群
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention discloses a kind of Graphene scaffold composite plating solution, be made up of the raw material of following weight portion: aniline 6.8 9, Ammonium persulfate. 0.1 0.2, boric acid 50 60, sodium sulfate 12, potassium dihydrogen phosphate 0.3 0.5, nickel sulfate 220 250, Nickel dichloride. 40 50, sodium lauryl sulphate 0.2 0.3, ptfe emulsion 50 60, cationic surfactant FC1343 4, cerium oxide 2.5 3, zinc sulfate 1.3 1.6, polyvinyl alcohol 1.6 2, boron oxide 2.8 3, mullite 1.6 2, appropriate amount of ethanol, deionized water are appropriate;The present invention is far superior to conventional method of the prior art, and prepared electroplate liquid stability improves, and the quality of electroplate liquid is high, there is not decortication phenomenon, uniform color, and smooth surface is up-to-standard, is worthy to be popularized.

Description

A kind of Graphene scaffold composite plating solution
Technical field
The present invention relates to electroplate liquid technical field, particularly relate to a kind of Graphene scaffold composite plating solution.
Background technology
Electroplate also known as metal electrodeposition technology, be that workpiece is immersed in the solution containing slaine to be deposited, and to workpiece Apply negative charge, in surface of the work one layer of metal compact with workpiece of deposition or the process of alloy-layer.That electroplates is basic Principle is to make the metal ion in solution that reduction reaction to occur on solution and plating piece interface by various electric field actions, generates gold Belong to atom and be deposited on metal surface formation coating.Composite deposite is by by adding insoluble solid particle to plating solution In, make matrix metal co-deposit with solid particle, form a kind of process for modifying surface of composite deposite.Nickel coating because of It has the features such as excellent corrosion resistance, wearability and thickness of coating is uniform, obtains at aspects such as aviation, automobile, electronics, chemical industry To extensively application.But, nickel coating coefficient of friction is bigger.And politef is to be polymerized by tetrafluoroethylene monomer, performance Stable, in addition to there is splendid resistance to chemical corrosion, also there is the most heat-resisting, tolerance to cold, and the least friction Coefficient.By adding polytetrafluoroethylgranule granule in electroplate liquid, polytetrafluoroethylgranule granule is made to be distributed to along with the electro-deposition of nickel In nickel coating, the composite deposite prepared has significant antifriction effect.
In " research of NI-PTFE composite plating process " literary composition, author proposes by adding politef breast in electroplate liquid Liquid and FC134 cationic surfactant, be successfully prepared Ni/PTFE composite deposite, and test shows that coating surface is uniform, flat Whole, in terms of tribological property, the coefficient of friction of composite deposite is 0.218, is only about the 34% of nickel coating, but due to PTFE matter is soft, after entering in coating, makes composite deposite relatively nickel coating hardness reduce, and wear extent increased simultaneously.So In some field, this composite deposite can not meet demand.Rare earth element can significantly improve solid particle in functional composite material The performance such as content, hardness, wearability and high temperature oxidation resistance, a series of at chromium plating, thermo-chemical treatment, conversion film etc. at present Process for treating surface is applied.So the present invention will add the property such as hardness and the wearability of rare earth element raising composite deposite Can, expand application.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of Graphene scaffold composite plating solution.
The present invention is achieved by the following technical solutions:
A kind of Graphene scaffold composite plating solution, is made up of the raw material of following weight portion: aniline 6.8-9, Ammonium persulfate. 0.1-0.2, boric acid 50-60, sodium sulfate 1-2, potassium dihydrogen phosphate 0.3-0.5, nickel sulfate 220-250, Nickel dichloride. 40-50,12 Alkyl sodium sulfate 0.2-0.3, ptfe emulsion 50-60, cationic surfactant FC1343-4, cerium oxide 2.5-3, sulfur Acid zinc 1.3-1.6, polyvinyl alcohol 1.6-2, boron oxide 2.8-3, mullite 1.6-2, appropriate amount of ethanol, deionized water are appropriate.
Described a kind of Graphene scaffold composite plating solution, is made up of following concrete steps:
(1) zinc sulfate is added in the deionized water of 6-8 times amount stirring to dissolving, adds that polyvinyl alcohol is super to stir, will Cerium oxide, boron oxide and mullite are put in calcining furnace and to be calcined 1-2h at 500-55-DEG C, be added to while hot in ethanol soak until It is cooled to room temperature, then cleans up post-drying with deionized water and be ground into micropowder and be added in above-mentioned solution, heat while stirring, Until being dried;
(2) by DBSA, water, aniline and n-butyl alcohol according to mol ratio 1.5-2:10-14:1.0-1.4:0.8-1.2 Ratio is added in flask, is stirred vigorously and obtains transparent colourless emulsion, then equal with product mix and blend prepared by step (1) Even, Ammonium persulfate. deionized water dissolving is made the solution of 2mol/L, is then slowly dropped in flask, after dropping Reacting 5-7h under room temperature, the ethanol adding excess is slowly stirred 7-10min, filters, and product deionized water, ethanol are the most clear Wash, be subsequently placed in vacuum drying oven and at 60 DEG C, be dried 24h;
(3) being added to by boric acid in the deionized water of 60 DEG C, it is standby that stirring makes it dissolve, and adds sulfur when temperature of electroplating solution is 50 DEG C Acid nickel, Nickel dichloride. and sodium lauryl sulphate, use magnetic stirrer the most standby, adds polytetrafluoro in another container Vac emulsion and cationic surfactant FC134, be stirring evenly and then adding into product and surplus materials thereof prepared by step (2), Ultrasonic agitation is uniformly rear standby;
(4) standby product step (3) prepared is with 800r/min mix and blend 20-30min, the most auxiliary at 80kHz ultrasound wave It is transferred in electrolysis bath after helping concussion 30min, stands the granule removing particle diameter >=5 μm, i.e. can get electroplate liquid.
The invention have the advantage that the present invention to use in electroplate liquid and add ptfe emulsion raising nickel/polytetrafluoroethyl-ne The anti-attrition of alkene composite deposite and lubricity, improve the performance of single nickel coating, in order to improve composite deposite hardness and wear-resisting The problem that performance is the highest, uses nano-particle reinforcement coating, easily reunites because of nano-particle again and adhere to negative electrode table in electroplate liquid Face makes the problem that surface roughness increases, and uses polyaniline that granule is carried out coating modification, improves and easily reunites and to the moon between microgranule The tendency that pole springs up, and improve the performances such as the wearability of coating, hardness and high temperature oxidation resistance, also utilize modifying agent to oxygen Change boron modification, improve its characteristic being not readily dissolved in water, good dispersion, and improve the fire-resistant, ageing-resistant of coating and antioxidation Etc. performance;The present invention is far superior to conventional method of the prior art, and prepared electroplate liquid stability improves, the quality of electroplate liquid , there is not decortication phenomenon in height, uniform color, and smooth surface is up-to-standard, is worthy to be popularized.
Detailed description of the invention
A kind of Graphene scaffold composite plating solution, is made up of the raw material of following weight portion (kilogram): aniline 6.8, Ammonium persulfate. 0.1, boric acid 50, sodium sulfate 1, potassium dihydrogen phosphate 0.3, nickel sulfate 220, Nickel dichloride. 40, sodium lauryl sulphate 0.2, ptfe emulsion 50, cationic surfactant FC1343, cerium oxide 2.5, zinc sulfate 1.3, polyvinyl alcohol 1.6, Boron oxide 2.8, mullite 1.6, appropriate amount of ethanol, deionized water are appropriate.
Described a kind of Graphene scaffold composite plating solution, is made up of following concrete steps:
(1) zinc sulfate is added in the deionized water of 6 times amount stirring to dissolving, adds that polyvinyl alcohol is super to stir, by oxygen Change cerium, boron oxide and mullite are put into and are calcined 1h in calcining furnace at 500 DEG C, are added to while hot in ethanol soak until being cooled to room Temperature, then cleans up post-drying with deionized water and is ground into micropowder and is added in above-mentioned solution, heat while stirring, until dry Dry;
(2) DBSA, water, aniline and n-butyl alcohol are added to flask according to mol ratio 1.5:10:1.0:0.8 ratio In, it being stirred vigorously and obtain transparent colourless emulsion, the product mixing and stirring then prepared with step (1), by Ammonium persulfate. Make the solution of 2mol/L with deionized water dissolving, be then slowly dropped in flask, after dropping, at room temperature react 5h, The ethanol adding excess is slowly stirred 7min, filters, and product deionized water, ethanol clean repeatedly, is subsequently placed in vacuum and does Dry case is dried at 60 DEG C 24h;
(3) being added to by boric acid in the deionized water of 60 DEG C, it is standby that stirring makes it dissolve, and adds sulfur when temperature of electroplating solution is 50 DEG C Acid nickel, Nickel dichloride. and sodium lauryl sulphate, use magnetic stirrer the most standby, adds polytetrafluoro in another container Vac emulsion and cationic surfactant FC134, be stirring evenly and then adding into product and surplus materials thereof prepared by step (2), Ultrasonic agitation is uniformly rear standby;
(4) standby product step (3) prepared is with 800r/min mix and blend 20min, shakes at 80kHz ultrasonic assistant simultaneously It is transferred in electrolysis bath after swinging 30min, stands the granule removing particle diameter >=5 μm, i.e. can get electroplate liquid.
Plating piece carrying out plate previous series of processes and enters electroplating bath, nickel anode plating front surface activation processing, afterwards according to preparation Electroplate liquid carry out electroplating processes, bath temperature is 45 DEG C, and electric current density is 9A/dm2, and coating is carried out performance test, result As follows:
Outward appearance: smooth even, coefficient of friction: 0.23, wear extent (500g, 200r/min, mm3): 2.48 × 10-2, porosity (individual/cm2): 0.9, adhesion: do not peel off, salt fog (120 hours): without significant change.

Claims (2)

1. a Graphene scaffold composite plating solution, it is characterised in that be made up of the raw material of following weight portion: aniline 6.8-9, Ammonium persulfate. 0.1-0.2, boric acid 50-60, sodium sulfate 1-2, potassium dihydrogen phosphate 0.3-0.5, nickel sulfate 220-250, chlorine Change nickel 40-50, sodium lauryl sulphate 0.2-0.3, ptfe emulsion 50-60, cationic surfactant FC1343-4, Cerium oxide 2.5-3, zinc sulfate 1.3-1.6, polyvinyl alcohol 1.6-2, boron oxide 2.8-3, mullite 1.6-2, appropriate amount of ethanol, go from Sub-water is appropriate.
A kind of Graphene scaffold composite plating solution, it is characterised in that by following concrete steps system Prepare into:
(1) zinc sulfate is added in the deionized water of 6-8 times amount stirring to dissolving, adds that polyvinyl alcohol is super to stir, will Cerium oxide, boron oxide and mullite are put in calcining furnace and to be calcined 1-2h at 500-55-DEG C, be added to while hot in ethanol soak until It is cooled to room temperature, then cleans up post-drying with deionized water and be ground into micropowder and be added in above-mentioned solution, heat while stirring, Until being dried;
(2) by DBSA, water, aniline and n-butyl alcohol according to mol ratio 1.5-2:10-14:1.0-1.4:0.8-1.2 Ratio is added in flask, is stirred vigorously and obtains transparent colourless emulsion, then equal with product mix and blend prepared by step (1) Even, Ammonium persulfate. deionized water dissolving is made the solution of 2mol/L, is then slowly dropped in flask, after dropping Reacting 5-7h under room temperature, the ethanol adding excess is slowly stirred 7-10min, filters, and product deionized water, ethanol are the most clear Wash, be subsequently placed in vacuum drying oven and at 60 DEG C, be dried 24h;
(3) being added to by boric acid in the deionized water of 60 DEG C, it is standby that stirring makes it dissolve, and adds sulfur when temperature of electroplating solution is 50 DEG C Acid nickel, Nickel dichloride. and sodium lauryl sulphate, use magnetic stirrer the most standby, adds polytetrafluoro in another container Vac emulsion and cationic surfactant FC134, be stirring evenly and then adding into product and surplus materials thereof prepared by step (2), Ultrasonic agitation is uniformly rear standby;
(4) standby product step (3) prepared is with 800r/min mix and blend 20-30min, the most auxiliary at 80kHz ultrasound wave It is transferred in electrolysis bath after helping concussion 30min, stands the granule removing particle diameter >=5 μm, i.e. can get electroplate liquid.
CN201610673563.6A 2016-08-16 2016-08-16 A kind of Graphene scaffold composite plating solution Pending CN106087009A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114959811A (en) * 2022-05-31 2022-08-30 暨南大学 High-corrosion-resistance composite electroplating electrolyte and preparation method of coating thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104143372A (en) * 2014-07-30 2014-11-12 安徽状元郎电子科技有限公司 Modified mullite conducting silver paste and preparing method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104143372A (en) * 2014-07-30 2014-11-12 安徽状元郎电子科技有限公司 Modified mullite conducting silver paste and preparing method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
中国科学技术信息研究所: "《技术发展预测与评论(第一卷)》", 31 August 2003, 北京理工大学出版社 *
王博: "Ni-P-PTFE复合镀层工艺及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *
黄惠等: "《导电聚苯胺基复合阳极材料的制备》", 30 January 2016, 冶金工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114959811A (en) * 2022-05-31 2022-08-30 暨南大学 High-corrosion-resistance composite electroplating electrolyte and preparation method of coating thereof
CN114959811B (en) * 2022-05-31 2023-08-15 暨南大学 High corrosion-resistant composite electroplating electrolyte and preparation method of plating layer thereof

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Application publication date: 20161109