CN109440146A - A kind of silver based on no cyanogen system-titanium carbide composite deposite and preparation method thereof - Google Patents
A kind of silver based on no cyanogen system-titanium carbide composite deposite and preparation method thereof Download PDFInfo
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- CN109440146A CN109440146A CN201811435163.7A CN201811435163A CN109440146A CN 109440146 A CN109440146 A CN 109440146A CN 201811435163 A CN201811435163 A CN 201811435163A CN 109440146 A CN109440146 A CN 109440146A
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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
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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Abstract
The present invention relates to electrical contact protective materials technical fields more particularly to a kind of silver based on no cyanogen system-titanium carbide composite deposite and preparation method thereof.The present invention provides a kind of preparation methods of the silver based on no cyanogen system-titanium carbide composite deposite, comprising the following steps: step 1: preparing composite plating bath, nano silicon carbide titanium valve and evenly dispersed is added in the composite plating bath;The composite plating bath includes AgNO3Solution, Na2S2O3Solution, K2S2O5Solution, CH3COONH4Solution and CH5N3S solution it is one or more;Step 2: copper sheet substrate being respectively put into deionized water, acetone and dehydrated alcohol and impregnates and is cleaned by ultrasonic clean and be soaked in dehydrated alcohol spare as substrate;Step 3: being electroplated in the composite plating bath that the copper sheet substrate that step 2 is obtained is put into step 1.The present invention provides a kind of functional coatings based on the preparation of no cyanogen system, are difficult to meet environmental requirements for solving silver plated contact, and hardness, wear-resisting and anti-corrosion etc. the poor technical problem of performances.
Description
Technical field
The present invention relates to electrical contact protective materials technical field more particularly to a kind of silver-titanium carbides based on no cyanogen system
Composite deposite and preparation method thereof.
Background technique
Isolated switchgear in recent years at the scene operation in most important problem be exactly heating defect, one side heating defect
It will cause the decline of through-current capability, if on the other hand handled not in time, it will bring bigger harm.Switch touching hair
Heat problem is mainly increased, caused by kwh loss increasing due to the contact resistance between dynamic/static contact, and causes the raised original of resistance
Because mainly contact fingertip clamping force becomes smaller, the electric conductivity of contact surface itself is bad, contact surface is since divide-shut brake number increases
The abrasion of generation rises contact resistance, even contact surface is corrosion-resistant and the coating that conducts electricity very well is worn away completely.Cause
The main reason for silver plated contact heating defect is the abrasion of silver coating caused by a large amount of divide-shut brake mechanically actuated, even polishing leakage
Copper and silver coating are corroded during military service, and corrosion forms poorly conductive especially in industrial sulfur-bearing atmospheric environment
Vulcanization silverskin.Carrying out changed handling to silvering is to improve one kind simply effective side of its wear-resisting property and corrosion resisting property
Method.But this modification should not influence the excellent conduction of silvering itself and heating conduction.It, can to improve silvering wearability
Consider to introduce the component such as graphite etc. with self-lubricating property in silvering, or introduces wear-resisting particle, such as carbide ceramics
Particle.There is titanium carbide high rigidity, strong wear-resisting characteristic can be mentioned by dispersion-strengtherning mechanism when it is distributed in silver matrix
The hardness of high silver matrix, while the ability of titanium carbide itself resistance skimming wear is also very strong, can help the entirety for improving material
Wearability reduces the generation of abrasive dust, therefore undoubtedly has important theory and reality using titanium carbide modified by nano particles silvering
Border meaning.
Therefore, silver plated contact is difficult to meet environmental requirements, and hardness, wear-resisting and anti-corrosion etc. performances are poor becomes this
Field technical staff technical problem urgently to be resolved.
Summary of the invention
The present invention provides a kind of functional coatings based on the preparation of no cyanogen system, are difficult to meet for solving silver plated contact
Environmental requirement, and hardness, wear-resisting and anti-corrosion etc. the poor technical problem of performances.
The present invention provides a kind of preparation methods of the silver based on no cyanogen system-titanium carbide composite deposite, including following step
It is rapid:
Step 1: preparing composite plating bath, nano silicon carbide titanium valve and evenly dispersed is added in the composite plating bath;
The composite plating bath includes AgNO3Solution, Na2S2O3Solution, K2S2O5Solution, CH3COONH4Solution and CH5N3S is molten
Liquid it is one or more;
Step 2: copper sheet substrate being respectively put into deionized water, acetone and dehydrated alcohol and impregnates and is cleaned by ultrasonic completely simultaneously
It is soaked in dehydrated alcohol spare as substrate;
Step 3: being electroplated in the composite plating bath that the copper sheet substrate that step 2 is obtained is put into step 1.
It is furthermore preferred that the partial size of the nano silicon carbide titanium valve is 50~100nm.
Preferably, the pH value of the composite plating bath is 5.0~6.0.
Preferably, the AgNO3The concentration of solution is 40~45gL-1。
Preferably, the Na2S2O3The concentration of solution is 200~250gL-1。
Preferably, the K2S2O5The concentration of solution is 40~45gL-1。
Preferably, the CH3COONH4The concentration of solution is 20~30gL-1。
Preferably, the CH5N3The concentration of S solution is 0.6~0.8gL-1。
Preferably, the current density of the plating is 2.5~5.0mAcm-2。
Preferably, the temperature of the plating is 25~45 DEG C.
The present invention also provides a kind of composite deposites based on no cyanogen system silver-titanium carbide, by above-mentioned based on no cyanogen body
It is that silver-titanium carbide composite deposite preparation method is made.
It is furthermore preferred that the composite deposite based on no cyanogen system silver-titanium carbide with a thickness of 10~15 μm.
Silver and titanium carbide composite deposite and preparation method thereof provided by the invention based on no cyanogen system, has overcome cyanogen plating
The pollution problem of silver process, and stable composite plating bath can be obtained, preparation process is simple, easy to control, low in cost, is suitble to criticize
Amount production, obtained composite deposite crystallize careful, surfacing, have that hardness is high, wearability is good, good conductivity, not easy to change
The advantages that, the application in electrical contact protective materials field can be better meet.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is silver-titanium carbide composite deposite surface scanning electron microscope (SEM) photograph in the embodiment of the present invention 1;
Fig. 2 is the first scanning electron microscope (SEM) photograph of silver-titanium carbide composite deposite cross section in the embodiment of the present invention 1;
Fig. 3 is the second scanning electron microscope (SEM) photograph of silver-titanium carbide composite deposite cross section in the embodiment of the present invention 1.
Specific embodiment
The embodiment of the invention provides a kind of functional coatings based on the preparation of no cyanogen system, for solving silver plated contact hardly possible
To meet environmental requirements, and hardness, wear-resisting and anti-corrosion etc. the poor technical problem of performances.
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with the present invention
Attached drawing in embodiment, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that disclosed below
Embodiment be only a part of the embodiment of the present invention, and not all embodiment.Based on the embodiments of the present invention, this field
Those of ordinary skill's all other embodiment obtained without making creative work, belongs to protection of the present invention
Range.
Embodiment 1
Substrate uses high-purity oxygen-free copper piece, and substrate is polishing to 1000# using sand paper first, is then used respectively in ultrasound
Deionized water, dehydrated alcohol, acetone clean 3~5min, are immersed in spare in dehydrated alcohol.The formula that electroplate liquid uses are as follows: 40
~45gL-1AgNO3, 200~250gL-1Na2S2O3, 40~45gL-1K2S2O5, 20~30gL-1CH3COONH4、0.6
~0.8gL-1CH5N3S, using deionized water dissolving chemicals wiring solution-forming, adjusting bath pH value is 5.4~5.8.Matching
1.8gL is added in good plating solution-1Nano silicon carbide titanium valve (partial size: 50~100nm), magnetic agitation 2.5 hours.It will be beaten through machinery
Copper sheet substrate is put into matter before plating as cathode as anode, copper sheet substrate by the high purity graphite plate for grinding and cleaning up
30~60s is impregnated in the dilution heat of sulfuric acid that amount score is 10% and is washed with deionized water, and is removed oxide on surface, is carried out later
Composite plating operation controls technological parameter: current density 5.0mAcm using constant current mode-2, electrodeposition temperature is 30 DEG C,
Electro-deposition pH be 5.0~6.0, electrodeposition time 0.5 hour, magnetic stirring apparatus rotor speed 1000rmin-1.After the completion of plating
With deionized water repeated flushing plated item, after drying, silver-titanium carbide composite deposite is obtained.
Surface microscopic topographic is carried out to the coating that the present embodiment obtains and constituent analysis, the surface that Fig. 1 gives coating are swept
Electronic Speculum (SEM) pattern is retouched, dark areas is titanium carbide accumulation regions in figure, and light tone region is silver matrix, it can be seen that in Copper base material table
The coating prepared on face is composite deposite of the nano titanium carbide Dispersed precipitate in silver matrix.Fig. 2 is the cross section of above-mentioned coating
SEM shape appearance figure, as seen from the figure, the silver-based coating surface are fine and close, and are well combined with Copper base material.Meanwhile it being dissipated using X-ray energy
It penetrates spectrum (EDS) and line scanning constituent analysis has been carried out to plating layer cross section, section component distributing is as shown in figure 3, can show that silver-based plates
Carbonization Ti content is 2.6at.% in layer, remaining is silver.Also the hardness of above-mentioned coating is measured, HV hardness number is 133.
Embodiment 2
The present embodiment uses operation similar to Example 1, and 2.6gL is added in the plating solution prepared-1Nano titanium carbide
Powder (partial size: 50~100nm), current density 3.75mAcm-2, silver-titanium carbide composite deposite is prepared, in composite deposite
Carbonization Ti content is 3.4at.%, remaining is silver, and the HV hardness of coating is 139, the surface of coating and cross-sectional morphology with reality
It is similar to apply example 1.
Embodiment 3
The present embodiment uses operation similar to Example 1, and 3.5gL is added in the plating solution prepared-1Nano titanium carbide
Powder (partial size: 50~100nm), current density 2.5mAcm-2, silver-titanium carbide composite deposite is prepared, in composite deposite
Carbonization Ti content is 4.2at.%, remaining is silver, and the HV hardness of coating is 142, the surface of coating and cross-sectional morphology with reality
It is similar to apply example 1.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features;And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite, which comprises the following steps:
Step 1: preparing composite plating bath, nano silicon carbide titanium valve and evenly dispersed is added in the composite plating bath;
The composite plating bath includes AgNO3Solution, Na2S2O3Solution, K2S2O5Solution, CH3COONH4Solution and CH5N3S solution
It is one or more;
Step 2: copper sheet substrate is respectively put into deionized water, acetone and dehydrated alcohol impregnate and be cleaned by ultrasonic it is clean and by its
It is soaked in dehydrated alcohol spare as substrate;
Step 3: being electroplated in the composite plating bath that the copper sheet substrate that step 2 is obtained is put into step 1.
2. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the pH value of the composite plating bath is 5.0~6.0.
3. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the AgNO3The concentration of solution is 40~45gL-1。
4. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the Na2S2O3The concentration of solution is 200~250gL-1。
5. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the K2S2O5The concentration of solution is 40~45gL-1。
6. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the CH3COONH4The concentration of solution is 20~30gL-1。
7. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the CH5N3The concentration of S solution is 0.6~0.8gL-1。
8. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the current density of the plating is 2.5~5.0mAcm-2。
9. a kind of preparation method of the silver based on no cyanogen system-titanium carbide composite deposite according to claim 1, feature
It is, the temperature of the plating is 25~45 DEG C.
10. a kind of composite deposite based on no cyanogen system silver-titanium carbide, which is characterized in that by claim 1~9 any one
The preparation method based on no cyanogen system silver-titanium carbide composite deposite is made.
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Cited By (3)
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CN110923785A (en) * | 2019-12-11 | 2020-03-27 | 哈尔滨东大高新材料股份有限公司 | Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition |
CN110983393A (en) * | 2019-12-27 | 2020-04-10 | 广东电网有限责任公司电力科学研究院 | Silver-niobium carbide composite coating and preparation method thereof |
CN111235608A (en) * | 2020-03-10 | 2020-06-05 | 国网浙江省电力有限公司电力科学研究院 | Cyanide-free silver-based composite plating solution, silver-based composite plating layer and preparation method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110923785A (en) * | 2019-12-11 | 2020-03-27 | 哈尔滨东大高新材料股份有限公司 | Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition |
CN110923785B (en) * | 2019-12-11 | 2022-04-22 | 哈尔滨东大高新材料股份有限公司 | Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition |
CN110983393A (en) * | 2019-12-27 | 2020-04-10 | 广东电网有限责任公司电力科学研究院 | Silver-niobium carbide composite coating and preparation method thereof |
CN111235608A (en) * | 2020-03-10 | 2020-06-05 | 国网浙江省电力有限公司电力科学研究院 | Cyanide-free silver-based composite plating solution, silver-based composite plating layer and preparation method thereof |
CN111235608B (en) * | 2020-03-10 | 2021-02-12 | 国网浙江省电力有限公司电力科学研究院 | Cyanide-free silver-based composite plating solution, silver-based composite plating layer and preparation method thereof |
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Application publication date: 20190308 |