CN102592699A - Ag/Cr2O3 composite film for contact point and preparation and application thereof - Google Patents

Ag/Cr2O3 composite film for contact point and preparation and application thereof Download PDF

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CN102592699A
CN102592699A CN201110388963XA CN201110388963A CN102592699A CN 102592699 A CN102592699 A CN 102592699A CN 201110388963X A CN201110388963X A CN 201110388963XA CN 201110388963 A CN201110388963 A CN 201110388963A CN 102592699 A CN102592699 A CN 102592699A
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composite membrane
composite
electric contact
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CN102592699B (en
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彭晓
张洪亮
王福会
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Institute of Metal Research of CAS
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Abstract

The invention relates to the technology of composite film preparation, in particular to an Ag/Cr2O3 composite film for a contact point and a preparation and an application thereof. The composite film comprises an Ag base body and Cr2O3 particles dissipated in the Ag base body; and by mass percentage, the content of Cr2O3 particles is 1.5-15.0 percent, and the rest is Ag. The composite film can be prepared through two steps: firstly, an Ag/Cr composite coating with dissipated Cr particles is prepared on an Ag-based Cu base body through an Ag-Cr particle coelectrodeposition method; and secondly, through the in-situ internal oxidation of Cr particles, the Cr particles in the Ag/Cr composite coating are subjected to oxidation to generate Cr2O3 particles which are uniformly dissipated in the Ag base body so as to obtain the Ag/Cr2O3 composite film. The composite film provided by the invention has a simple and mature technology, and is easy to popularize. Compared with an Ag/3.9Cr2O3 composite film prepared by a composite galvanic deposit method, as well as a common Ag/MexOy contact point material prepared by an alloy internal oxidation method and reported in the literature, the Ag/4.0Cr2O3 composite film has fair density and resistivity, as well as obviously higher rigidity.

Description

A kind of electric contact is used Ag/Cr 2O 3Composite membrane and preparation thereof and application
Technical field
The present invention relates to the composite membrane technology of preparing, more particularly, relate to a kind of electric contact and use Ag/Cr 2O 3Composite membrane and preparation thereof and application.
Background technology
Ag/Me xO y(Me is a metal, like Cd, Zn etc.) type electric contact material is owing to having higher hardness, good anti-melting welding and arc resistant ablation property and low and stable contact resistance is widely used in the low-voltage electrical apparatus field.Wherein the Ag/CdO electric contact material is called as " omnipotent contact " owing to have excellent comprehensive performances, uses very extensive.Yet the Cd steam that produces because of its arcing is poisonous, is forbidden in household electrical appliance and car electrics, using by developed countries such as America and Europes.Therefore, the new Ag/Me of research xO yThe type electric contact material is extensively paid close attention to, and the compound electric contact of this that reported has Ag/SnO with material system 2, Ag/ZnO and Ag/CuO etc.But up to the present, the problem of alternative Ag/CdO is not effectively solved yet.
Ag/Me xO yType electric contact material powder metallurgic method commonly used and the preparation of alloy inner oxidation method.Compare the Ag/Me of internal oxidation preparation with powder metallurgic method xO yType electric contact material hardness is high and wear-resisting, simultaneously high the and anti-arc erosion of density.But the alloy inner oxidation method also has its shortcoming, and promptly material surface and interior oxidation tissue are difficult to reach even.It mainly shows both ways, and the one, inner oxide is prone to generate at crystal boundary; The 2nd, the size of inner oxide particle increases with depth of internal oxidation.The main cause that causes these two phenomenons to produce is that metal M e has certain solubility in Ag.Therefore select to be used to prepare Ag/Me with the immiscible metal of Ag xO yThe type electric contact material can be avoided the generation of the problems referred to above.
The present invention reports that a kind of electric contact uses Ag/Cr 2O 3The preparation of composite membrane and application.At first, adopt method preparation Ag/Cr composite deposite on the Cu matrix that soaks the Ag bottoming of Ag and Cr particle coelectrodeposition.Can know by the Ag-Cr binary phase diagraml; The mutual solubility of Ag and Cr is very little; And do not form any intermetallic compound between the two, counterdiffusion takes place in hardly under the high temperature, yet O has higher solubility and diffusion rate in Ag; Therefore oxidation in the original position of Cr particle can take place in above-mentioned Ag/Cr composite deposite under atmospheric atmosphere, thereby is converted into Ag/Cr 2O 3Composite membrane, this composite membrane has following characteristics.
1) Cr that gives birth in 2O 3Particle is nontoxic, and has good electrical conductivity (room temperature resistivity is 13 Ω m).
2) Cr is converted into Cr 2O 3,, can significantly improve the hardness of composite membrane because of volumetric expansion produces bigger compression.
3) this electric contact material is by " Cu matrix+Ag/Cr 2O 3Composite membrane " form, compare with Ag base electric contact material commonly used at present, have province Ag advantage.
In sum, this electric contact material system can not only satisfy uses required electricity and mechanical performance, also can greatly reduce preparation cost.
Summary of the invention:
The present invention is exactly to the problems referred to above, provides a kind of electric contact to use Ag/Cr 2O 3Composite membrane and preparation thereof and application.
To achieve these goals, the present invention adopts following technical scheme:
A kind of electric contact is used Ag/Cr 2O 3Composite membrane: it is by Ag matrix and disperse Cr wherein 2O 3Particle is formed, by mass percentage, and Cr 2O 3Granule content is 1.5%-15.0%, and all the other are Ag.
Electric contact is used Ag/Cr 2O 3The preparation method of composite membrane: preparation is carried out in two steps,
1) at first adopt the method for Ag and Cr particle coelectrodeposition on the Cu matrix that soaks the Ag bottoming, to prepare the Ag/Cr composite deposite that the Cr particle dispersion distributes; By mass percentage, the Cr granule content is 1.0%-10.0% in the Ag/Cr composite deposite, and all the other are Ag.
2), make the Cr particulate oxidation in the Ag/Cr composite deposite generate Cr then through oxidation in the original position of Cr particle 2O 3Thereby particle and even dispersion obtain Ag/Cr in the Ag matrix 2O 3Composite membrane.By mass percentage, Ag/Cr 2O 3Cr in the composite membrane 2O 3Granule content is 1.5%-15.0%, and all the other are Ag.
Soak the Ag bottoming in the step 1) before the Cu matrix coelectrodeposition earlier.Soak consisting of of Ag liquid: thiocarbamide 180-220g/l, AgNO 310-20g/l, solvent are water.Soak Ag liquid pH value and be 3-5, temperature 15-35 ℃, time 30-180s obtains pure Ag prime coat.
Stir up and down with the speed of 60-180rpm through porous plate when coelectrodeposition prepares the Ag/Cr composite deposite and make the Cr particle suspending in deposit fluid, Cr particle size 10nm-2 μ m, addition 10-150g/l.Deposit fluid is formed as follows: Na 2S 2O 3180g/l-220g/l, AgNO 330g/l-50g/l, K 2S 2O 530g/l-50g/l, solvent are water.Deposit fluid pH value is 4-6, temperature 15-45 ℃, and current density 0.3-1.5A/dm 2, time 0.5-5h.
The thickness of prepared Ag/Cr composite deposite is 10-200 μ m, and concrete thickness can be controlled through changing the realization of depositing current density and time as required, and its sedimentation time reduces with the increase of current density.Like current density at 0.5A/dm 2The time, deposition 4h, thickness can reach 75 μ m.
Step 2) oxidizing process adopts air atmosphere, temperature 500-750 ℃, time 0.5-5h in.Make the degree of depth of oxidation in the Ag/Cr composite deposite be lower than thickness of coating through the controlled oxidation parameter, influence the adhesion of composite membrane to avoid oxygen to be penetrated into the Cu matrix.Ag/Cr 2O 3The thickness of composite membrane is 5-190 μ m, and concrete thickness can be realized controlled through setting oxidizing temperature and time.Like 500 ℃ of oxidation 4h, thickness can reach 28 μ m.To obtaining certain thickness Ag/Cr 2O 3Composite membrane, oxidization time raises with temperature and obviously reduces.
Said Ag/Cr 2O 3The application of composite membrane." Cu matrix+the Ag/Cr that obtains 2O 3Composite membrane " system can be used as the electric contact of electric elements such as relay, circuit breaker, contactor and travel switch.
Design philosophy of the present invention is: the mutual solubility of Ag and Cr is very little, and does not form any intermetallic compound between the two, and counterdiffusion takes place hardly for they under the high temperature, yet O has higher solubility and diffusion rate in Ag.Therefore, adopt the method for Ag and Cr particle coelectrodeposition that oxidation in the original position of Cr particle can take place under atmospheric atmosphere at the Ag/Cr composite deposite for preparing on the Cu matrix, thereby be converted into Ag/Cr 2O 3Composite membrane.Owing to produce compression in the interior oxidizing process in the composite membrane, its hardness is obviously improved, and the Cr of interior life 2O 3Particle is nontoxic, and has good electrical conductivity (room temperature resistivity is 13 Ω m).Simultaneously, " Cu matrix+Ag/Cr 2O 3Composite membrane " the electric contact system compares with Ag base electric contact material at present commonly used, has province Ag advantage.
Beneficial effect of the present invention:
1.Ag/Cr 2O 3The composition of composite membrane, thickness can be realized through composition, thickness and the oxidizing condition of control Ag/Cr composite deposite.And the composition of Ag/Cr composite deposite is relevant with the technological parameters such as content, sedimentation time and current density of Cr particle in the tank liquor with thickness.
2. composite membrane and basal body binding force are good.Soak the adhesion that the Ag layer can significantly improve Ag/Cr composite deposite and matrix before the electro-deposition, can make Ag/Cr composite deposite depth of internal oxidation be lower than thickness of coating, influence whole serviceability to avoid oxygen to be penetrated into the Cu matrix through the controlled oxidation parameter.
3. technology is simple, cost is low.The present invention adopts coelectrodeposition and inner oxidation method, and technology is simple, adopts Cu to do matrix and can significantly reduce material cost, therefore, is of wide application.
Accompanying drawing (table) explanation
Fig. 1-1 soaks the surface topography photo of Ag prime coat for the embodiment of the invention.
Fig. 1-2 soaks the surface topography photo after (technological parameter is with the Ag process of soaking among the embodiment) in deposit fluid for pure Cu sample.
Fig. 2 is the cross section light microscopic photo of embodiment of the invention coelectrodeposition Ag/2.4Cr composite deposite.
Fig. 3 is that embodiment of the invention coelectrodeposition Ag/2.4Cr composite deposite is at 500 ℃ of airborne oxidation kinetics curves.
Fig. 4 is the cross section light microscopic photo (wherein " I ", " II " and " III " represent pure Ag layer, interior zoneofoxidation and original composite deposite respectively) behind the oxidation 4h in 500 ℃ of air of embodiment of the invention coelectrodeposition Ag/2.4Cr composite deposite.
Table 1 is embodiment of the invention Ag/4.0Cr 2O 3Composite membrane and Comparative examples A g/3.9Cr 2O 3Composite membrane and the Ag/Me commonly used that adopts the inner oxidation method preparation xO yThe numerical value of density, hardness and the resistivity of type electric contact material (like Ag/12CdO).
Embodiment
Embodiment: with Ag/4.0Cr 2O 3Composite membrane be prepared as example, the preparation method is following:
1) pretreatment of base material
Pure Cu base material is processed into the sample of 15 * 10 * 2mm size, with 800 #Silicon carbide paper pre-grinding dries up after the ultrasonic cleaning in acetone.
2) step 1: coelectrodeposition
Soak Ag earlier before the Cu matrix coelectrodeposition, soak Ag liquid and form as follows: thiocarbamide 200g/l, AgNO 315g/l, solvent are water.The pH value is 4 (using concentration to regulate as the hydrochloric acid of 50vol%).Soak 25 ℃ of Ag liquid temps, time 120s.Obtain pure Ag prime coat.
With average particle size particle size is that the Cr particle of 30nm is immersed in the sodium thiosulfate type deposit fluid, so that Dispersion of Particles, the addition of Cr particle is 80g/l.Deposit fluid is formed as follows: Na 2S 2O 3200g/l, AgNO 340g/l, K 2S 2O 540g/l, solvent are water.Deposit fluid pH value is 5.Stirring up and down with the speed of 120rpm through porous plate in the coelectrodeposition process fully is suspended in the tank liquor nanometer Cr particle.Technological parameter is: 25 ℃ of temperature, current density 0.5A/dm 2, time 4h.By mass percentage, the Cr granule content is 2.4% in the prepared Ag/Cr composite deposite, and all the other are Ag, count Ag/2.4Cr.
3) step 2: interior oxidation
The internal oxidation process parameter is following: adopt air atmosphere, 500 ℃ of temperature, time 4h.By mass percentage, prepared Ag/Cr 2O 3Cr in the composite membrane 2O 3Granule content is 4.0%, and all the other are Ag, count Ag/4.0Cr 2O 3
Comparative example: to adopt Ag and Cr 2O 3The Cr that the method for particle (average grain diameter is greater than the nanometer Cr particle in the embodiment of the invention) coelectrodeposition prepares on the Cu base material 2O 3The Ag/Cr that particle dispersion distributes 2O 3Composite membrane is a comparative example.By mass percentage, prepared Ag/Cr 2O 3Cr in the composite membrane 2O 3Content is 3.9%, and all the other are Ag, count Ag/3.9Cr 2O 3
Analyzed and soaked Ag prime coat, Ag/2.4Cr composite deposite (before and after the oxidation) and Comparative examples A g/3.9Cr among the embodiment 2O 3The pattern of composite membrane.To embodiment A g/4.0Cr 2O 3Composite membrane and Comparative examples A g/3.9Cr 2O 3Performances such as the density of composite membrane, hardness and resistivity are measured, and with document in the Ag/Me commonly used of the employing inner oxidation method preparation reported xO yType electric contact material (like Ag/12CdO) compares.
(1) morphology analysis:
Fig. 1-1 is for soaking the surface topography photo of Ag prime coat in the embodiment of the invention.This Ag layer has covered whole C u matrix, and compact structure.
Fig. 1-2 is for putting into the Cu sample in the surface topography photo after electro-deposition Ag liquid soaks (technological parameter is with the Ag process of soaking of the embodiment of the invention).Compare with the Ag layer that soaks shown in Fig. 1-1, it is loose how empty to soak the Ag laminar surface that obtains at electro-deposition Ag liquid.This mainly be because the standard electrode potential of Cu (+0.339V) than Ag (+0.799V) negative, when Cu got in the deposit fluid that contains high concentration Ag salt, displacement reaction took place rapidly in the surface, generates loose Ag layer, the adhesion of it and matrix is poor; And when Cu get into by low concentration Ag salt and high concentration complexant forms soak in the Ag liquid time, displacement reaction is slower, surperficial generation one deck densification and the good Ag layer of adhesion.Can significantly improve the adhesion of Ag/Cr composite deposite with this Ag layer bottoming.
Fig. 2 is the cross section light microscopic photo of embodiment of the invention coelectrodeposition Ag/2.4Cr composite deposite.The thickness of coating is more even, and good with the Cu matrix bond.Grey Cr particle in the coating relatively is evenly distributed among the white Ag.Obviously greater than the average-size (30nm) of nanometer Cr particle, this is because due to some nanometer Cr particle agglomerations to the size of viewed Cr particle.
Fig. 3 is that embodiment of the invention coelectrodeposition Ag/2.4Cr composite deposite is at 500 ℃ of airborne oxidation kinetics curves.It is thus clear that along with the prolongation of oxidization time, weightening finish increases gradually.Behind the oxidation 4h, weightening finish is about 0.54mg/cm 2Because not oxidation of Ag, therefore weightening finish mainly is to form Cr because interior oxidation has taken place the Cr particle in the composite deposite 2O 3Cause.
Fig. 4 is embodiment of the invention coelectrodeposition Ag/2.4Cr composite deposite cross section light microscopic photo behind the oxidation 4h in 500 ℃ of air.Be that composite deposite obviously is divided into three layers of " I ", " II " and " III " from outside to inside with (Fig. 2) is visibly different before the oxidation.Outside " I " layer is the fine silver layer of contrast homogeneous, and it is to form to outdiffusion under the driving by the oxidation generation compression in the Cr particle of the Ag in the composite deposite.This pure Ag layer is prone to remove in practical application; A disperse some Dark grey particles that distributed can be known that by oxidation kinetics curve among Fig. 3 interior oxidation has taken place the Cr particle in the Ag/2.4Cr composite deposite in middle " II " layer, explains that " II " layer is internal oxidation layer, i.e. Ag/Cr 2O 3Composite membrane.The Cr of its Oxford gray 2O 3Particle is generated by oxidation in the Cr particle in the original composite deposite.To Ag/Cr 2O 3The cross section of composite membrane is carried out EDAX and is detected, and the result shows that the quality percentage composition of Cr in the composite membrane is 2.7% (to be converted to Cr 2O 3Content be 4.0%), a little more than original composite deposite, this mainly with composite deposite in Ag in oxidizing process, taken place relevant to outdiffusion; Inner " III " layer is unoxidized Ag/2.4Cr composite deposite, and it and Cu matrix bond are good.
(2) performance test and analysis
1) method of testing
1. hardness test: grind off embodiment of the invention Ag/4.0Cr 2O 3Behind the pure Ag layer on composite membrane surface, adopt HV-1000 type microhardness testers to measure embodiment A g/4.0Cr 2O 3Composite membrane and Comparative examples A g/3.9Cr 2O 3The hardness of composite membrane.Used experiment load is 10g, and the load time is 10s.Choose 5 points and carry out hardness test, results averaged respectively being coated with to keep at a certain distance away on the layer cross section.
2. density measurement: after grinding off Cu matrix (comprising unoxidized Ag/2.4Cr composite deposite among the embodiment), through measuring embodiment of the invention Ag/4.0Cr 2O 3Composite membrane and Comparative examples A g/3.9Cr 2O 3The volume and weight of composite membrane calculates its density.
3. resistivity measurement: adopt YB2511A type Estimate of Resistance for DC Low Resistance tester to measure embodiment of the invention Ag/4.0Cr 2O 3Composite membrane and Comparative examples A g/3.9Cr 2O 3The resistivity of composite membrane.Earlier two composite membranes are cut into strip (the length and width height is respectively l, a and b) before measuring, respectively testing equipment are inserted at its two ends then, conditioning equipment when applying certain voltage U, shows a certain electric current I.Resistance R=the U/I of composite membrane, electricalresistivity=RS/l, wherein S is the cross-sectional area (a * b) of rectangular sample.
Table 1
Figure BDA0000114299390000051
2) test result and analysis
Table 1 has been enumerated embodiment of the invention Ag/4.0Cr 2O 3Composite membrane and Comparative examples A g/3.9Cr 2O 3The Ag/Me commonly used of the employing alloy inner oxidation method preparation of reporting in composite membrane and the document xO yThe numerical value of the performances such as density, hardness and resistivity of type electric contact material (like Ag/12CdO).Thus it is clear that, with Comparative examples A g/3.9Cr of the present invention 2O 3Composite membrane and these several kinds Ag/Me commonly used xO yThe type electric contact material is compared, embodiment of the invention Ag/4.0Cr 2O 3The density of composite membrane is suitable, resistivity lower (except that Ag/12CdO), and hardness is higher.
Embodiment of the invention Ag/4.0Cr 2O 3The hardness of composite membrane is higher than Comparative examples A g/3.9Cr of the present invention 2O 3The reason of composite membrane mainly is the Cr among the former 2O 3Particle oxidation in the Cr particle in-situ forms, and because of volumetric expansion produces bigger compression, can significantly improve the hardness of composite membrane.
Embodiment of the invention Ag/4.0Cr 2O 3These several kinds Ag/Me commonly used that the hardness of composite membrane is enumerated in the table 1 xO yThe reason of type electric contact material mainly contained two: one, and the former grain size is less than the latter.When the thin brilliant coat of metal temperature of prepared by electrodeposition was increased to 500 ℃, its grain size generally still was a submicron order.Normally first molten alloy of alloy inner oxidation method and then oxidation, the Ag/Me that therefore prepares xO yThe grain size of type electric contact material is generally micron order.According to the refined crystalline strengthening principle, crystal grain is thin more, and the intensity of material and hardness are just high more; The 2nd, the average grain diameter of contained oxide particle is less than the latter among the former.Ag/4.0Cr 2O 3Cr in the composite membrane 2O 3The average grain diameter of particle is a nanoscale, and is evenly distributed.And the average grain diameter of oxide particle is about 500nm-1 μ m in the commercial electric contact material of these several kinds employing internal oxidations preparation, and skewness.Based on the dispersion-strengtherning principle, particle is tiny more, and it is even more to distribute, and strengthening effect is good more, and hardness is just high more.
Although embodiment of the invention Ag/4.0Cr 2O 3Contained Cr in the composite membrane 2O 3Amount be merely 4.0%, with the Ag/Me commonly used of the employing alloy inner oxidation method reported in document preparation xO yType electric contact material (like Ag/12CdO) is compared, and it has suitable density and resistivity and higher hardness.Simultaneously do matrix and also have province Ag advantage with Cu.

Claims (10)

1. an electric contact is used Ag/Cr 2O 3Composite membrane is characterized in that, composite membrane is by Ag matrix and disperse Cr wherein 2O 3Particle is formed, by mass percentage, and Cr 2O 3Granule content is 1.5%-15.0%, and all the other are Ag.
2. the said electric contact of claim 1 is used Ag/Cr 2O 3The preparation method of composite membrane is characterized in that, preparation is carried out in two steps:
(1) at first adopt the method for Ag and Cr particle coelectrodeposition on the Cu matrix that soaks the Ag bottoming, to prepare the Ag/Cr composite deposite that the Cr particle dispersion distributes;
(2), make the Cr particulate oxidation in the Ag/Cr composite deposite generate Cr then through oxidation in the original position of Cr particle 2O 3Thereby particle and even dispersion obtain Ag/Cr in the Ag matrix 2O 3Composite membrane.
3. use Ag/Cr according to the said electric contact of claim 2 2O 3The preparation method of composite membrane is characterized in that, the Ag/Cr composite deposite in the step 1), and by mass percentage, the Cr granule content is 1.0%-10.0%, all the other are Ag.
4. use Ag/Cr according to the said electric contact of claim 2 2O 3The preparation method of composite membrane is characterized in that, soaks the Ag bottoming in the step 1) before the Cu matrix coelectrodeposition earlier, soaks Ag liquid and consists of: thiocarbamide 180-220g/l, AgNO 310-20g/l, solvent is a water, soaking Ag liquid pH is 3-5, temperature 15-35 ℃, soak Ag time 30-180s, obtain pure Ag prime coat;
Stir up and down with the speed of 60-180rpm through porous plate when coelectrodeposition prepares the Ag/Cr composite deposite and make the Cr particle suspending in deposit fluid, Cr particle size 10nm-2 μ m, addition 10-150g/l, deposit fluid is formed as follows: Na 2S 2O 3180g/l-220g/l, AgNO 330g/l-50g/l, K 2S 2O 530g/l-50g/l, solvent are water, and deposit fluid pH is 4-6, temperature 15-45 ℃, and current density 0.3-1.5A/dm 2, time 0.5-5h.
5. use Ag/Cr according to the said electric contact of claim 2 2O 3The preparation method of composite membrane is characterized in that, the thickness of prepared Ag/Cr composite deposite is 10-200 μ m in the step 1).
6. use Ag/Cr according to the said electric contact of claim 2 2O 3The preparation method of composite membrane is characterized in that step 2) in Ag/Cr 2O 3Composite membrane, by mass percentage, Cr 2O 3Granule content is 1.5%-15.0%, and all the other are Ag.
7. use Ag/Cr according to the said electric contact of claim 2 2O 3The preparation method of composite membrane is characterized in that step 2) in method through interior oxidation, adopt air atmosphere, temperature 500-750 ℃, time 0.5-5h.
8. use Ag/Cr according to the said electric contact of claim 2 2O 3The preparation method of composite membrane is characterized in that step 2) the middle Ag/Cr for preparing 2O 3The thickness of composite membrane is 5-190 μ m.
9. the said electric contact of claim 1 is used Ag/Cr 2O 3The application of composite membrane is characterized in that, Cu matrix+Ag/Cr 2O 3Composite membrane is as the electric contact of electric elements.
10. use Ag/Cr according to the said electric contact of claim 9 2O 3The application of composite membrane is characterized in that, electric elements comprise relay, circuit breaker, contactor or travel switch.
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CN109023454B (en) * 2018-09-18 2020-04-07 蒙城繁枫真空科技有限公司 Method for electroplating Cr-Ag alloy coating by using double-cation ionic liquid

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