CN102337526B - Preparation method of nickel electrode made of piezoelectric composite material - Google Patents
Preparation method of nickel electrode made of piezoelectric composite material Download PDFInfo
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- CN102337526B CN102337526B CN 201110271920 CN201110271920A CN102337526B CN 102337526 B CN102337526 B CN 102337526B CN 201110271920 CN201110271920 CN 201110271920 CN 201110271920 A CN201110271920 A CN 201110271920A CN 102337526 B CN102337526 B CN 102337526B
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Abstract
The invention discloses a preparation method of a nickel electrode made of a piezoelectric composite material. The nickel electrode is prepared by using a chemical plating method. The preparation method comprises steps of roughening, sensitizing and activating the piezoelectric composite material, and putting the piezoelectric composite material in a nickel plating liquid to be plated with nickel to obtain the nickel electrode, wherein the activating solution used in the activation procedure is a palladium salt activating solution or nickel salt activating solution, the palladium salt activating solution is prepared by dissolving PdCl2 in certain hydrochloric acid, the PdCl2 content is 0.3-0.5 g/L and the content of the concentrated HCl is 9.9-11 ml/L; the nickel salt activating solution is prepared by dissolving nickel acetate and sodium borohydride in absolute methanol, the content of the nickel acetate is 64-68 g/L, and the content of the sodium borohydride is 64-68 g/L. The invention has the advantages of high nickel plating speed, easiness in regulating and controlling the thickness of a plating layer, uniform and dense thickness of the plating layer of a nickel plate, strong combination force of the plating layer, good uniformity and wearing resistance, remarkable erosion resistance, excellent welding property and long service life, so that the application demand of the composite material is met.
Description
Technical field
The present invention relates to a kind of on piezo-electricity composite material the method for nickel coating electrode, be specifically related to a kind of method that adopts electroless plating nickel coating electrode on the piezo-electricity composite material components and parts.
Background technology
Piezo-electricity composite material refers to be combined according to certain mode of communicating and a kind of novel material with piezoelectric effect of consisting of by at least a piezoelectric phase material and non-piezoelectric phase material.The Some features such as the propagation medium couplings such as piezo-electricity composite material has that specific acoustic resistance is low, Yi Yushui and tissue, low mechanical quality factor, the sensitive figure of merit of high hydrostatic pressure, temperature stability are good are widely applied aspect the underwater sound, ultrasonic, electroacoustic and other.Because piezo-electricity composite material is that ceramic piezoelectric ceramics and organism material polymers are composited, if make electrode have good adhesion strength at piezoelectric ceramics and polymkeric substance simultaneously, and it is very difficult to reach uniformity consistency, thereby has limited the use range of piezo-electricity composite material.Therefore development is suitable for the electrode of piezo-electricity composite material, makes the good piezoelectric property of its performance, and applying of piezo-electricity composite material had very important significance.
At present, what the preparation method of piezoelectric ceramics electrode generally adopted is burning infiltration silver, and this method maturing temperature is 800 ℃, and the non-piezoelectric phase polymkeric substance in the piezo-electricity composite material can not bear so high temperature.Therefore, this method is not suitable for the making of piezo-electricity composite material electrode.Adopt of the electrode method of preparation piezo-electricity composite material is coated with silver slurry, metal spraying technique etc. more at present, adopt the electrode bonding strength and the lack of homogeneity that are coated with silver-colored paste-making method preparation, and metal spraying raw materials technology and apparatus expensive makes product cost too high, lose the market competitiveness.
Chemical plating technology is not need impressed current, the material surface with autocatalysis activity by solution in the metal deposition process that carries out of chemical reduction reaction.The coating that adopts chemical plating technology to obtain also has the following advantages: (1) is no matter the body form complicated coating that can both obtain uniformity how; (2) deposition coating has unique chemistry, physical and mechanical property; (3) coating is at the material surface strong adhesion, and coating is fine and closely woven, and big area plating qualification rate is high; (4) less investment, simple and easy to do, processing method is simple, and production is originally low, to the less pollution of environment.Because the above advantage of electroless plating, it has become metal and the metallized effective means of nonmetallic surface, and a large amount of research has also been passed through in its technical process.But, electroless plating be yet there are no report for the preparation of the electrode of piezo-electricity composite material, piezo-electricity composite material is comprised of piezoelectric ceramics and polymkeric substance, the two adopts the method for general nonmetallic surface electroless plating can not generate normal coating, polymkeric substance can't adhesive electrodes, therefore must just can make these two kinds of differing materials have close autocatalysis activity by a kind of chemical plating method new, that be fit to piezo-electricity composite material of research and probe, thereby obtain the coating of uniformity.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nickel electrode made of piezoelectric composite material, present method is improved the technique of existing chemical nickel plating method, make pottery and polymkeric substance energy while plated with nickel in the piezo-electricity composite material, it is even to form electrode materials and layer electrodes.
The present invention is achieved by the following measures:
A kind of preparation method of nickel electrode made of piezoelectric composite material, it is characterized in that: adopt the method preparation of electroless plating, piezo-electricity composite material is put into nickel-plating liquid carry out nickel plating after alligatoring, sensitization, activation, obtain nickel electrode, activating used activation solution is palladium salt activation solution or nickel salt activation solution, wherein, palladium salt activation solution is with PdCl
2Soluble in water formulated with concentrated hydrochloric acid, PdCl
2Content is that 0.3-0.5g/L, dense HCl content are 9.9-11ml/L; The nickel salt activation solution is nickelous acetate and sodium borohydride to be dissolved in the anhydrous methanol formulated, and the content of nickelous acetate is 64-68g/L, and the content of sodium borohydride is 64-68g/L.
In the used palladium salt activation solution, PdCl
2Optimum content is 0.4g/L, and is in the used nickel salt activation solution, best when the concentration of nickelous acetate and sodium borohydride is identical.
Used nickel-plating liquid is the aqueous solution, and its composition is NiSO
47H
2O, NaC
6H
5O
72H
2O, NaH
2PO
2H
2O, NH
4Cl and BSO additive, wherein, NiSO
47H
2O concentration is 15-25g/L, NaC
6H
5O
72H
2O content is 9-15g/L, NaH
2PO
2H
2O content is 18-30g/L, NH
4Cl content is 30 g/L, and the BSO additive level is 0.08-0.2g/L, and nickel-plating liquid is reconciled pH to 8-11 with ammoniacal liquor, preferably transfers to 9-9.6.
The compound method of nickel-plating liquid is: take by weighing each composition by proportioning, then with NaH
2PO
2H
2O and NH
4Cl mixes, and is made into B solution, with NiSO
47H
2O, BSO additive and NaC
6H
5O
72H
2O mixes, and is made into A solution; B solution is slowly splashed in the A solution, reconcile pH with ammoniacal liquor, and get final product.
The used coarsening solution of alligatoring is density 1.0-1.5g/cm
3The mixing mineral acid and the mixed solution of water, its volume ratio 1:2-1:4, used mineral acid comprises hydrochloric acid, sulfuric acid, nitric acid, perchloric acid etc.
The used sensitizing solution of sensitization is SnCl
22H
2The aqueous solution of O and concentrated hydrochloric acid, SnCl
22H
2The content of O in water is 26-35g/L, and the content of dense HCl in water is 45-55ml/L.
Piezo-electricity composite material of the present invention consist of piezoelectric ceramics and polymkeric substance, described polymkeric substance comprises Resins, epoxy, silica gel, high-temp glue etc.
Concrete, present method may further comprise the steps:
(1) piezo-electricity composite material with desired size adds in the coarsening solution, processes 5-30min under the room temperature, then piezo-electricity composite material is put into boiling water and cleans, to remove coarsening solution;
(2) piezo-electricity composite material after the alligatoring is put into sensitizing solution, process 3-15min under the room temperature, then use washed with de-ionized water;
(3) piezo-electricity composite material after the sensitization is put into activation solution and carry out activation treatment, use washed with de-ionized water after processing; Adopting the treatment condition of palladium salt activation solution is to process 3-15min under the room temperature, and the treatment condition that adopt the nickel salt activation solution are the 20-40 ℃ of lower 30-50min of processing;
(4) piezo-electricity composite material after will activating is put into nickel-plating liquid, carries out nickel plating under 25-50 ℃, and constantly stirs, and stops nickel plating when coating reaches thickness, and the nickel dam that the matrix material both sides are unnecessary removes, and get final product.
In the aforesaid method, temperature is lower and different according to thickness of coating and temperature different for plating time, and nickel plating speed is less, and spended time is longer, generally can reach thickness requirement at 3-15min, can adjust as required when actually operating.
The used BSO additive of the present invention is the electroless plating common additives, and its main chemical compositions is asccharin, formal name used at school o-benzoic sulfimide, elementary brightening agent.
The present invention adopts scientific and rational nickel plating technology that piezo-electricity composite material is carried out the nickel plating operation, can plate simultaneously electrode on piezoelectric ceramics and polymkeric substance, for use facilitates.Sum up through great many of experiments, when nickel plating, adopt 25-50 ℃ temperature range, nickel plating speed is fast in this scope, and coating is even.Fig. 1 is bath temperature on plating the impact of speed, as can be seen from the figure, and along with the speed of the rising nickel plating of temperature also increases.Fig. 2,3,4 is respectively 3000 times of SEM figure at 30 ℃, 40 ℃, 50 ℃ lower nickel plating gained nickel dams, and as can be seen from the figure, the nickel dam among Fig. 2,3,4 all is attached on the piezoelectric ceramics and polymkeric substance of piezo-electricity composite material.Nickel dam arrangement regulation among Fig. 3, and Fig. 2 and 4 has accumulation, agglomeration to occur.This shows that nickel plating speed can not be only seen in the selection of temperature, also will consider the performance of gained coating comprehensively.In addition, the pH of nickel-plating liquid is also most important to the formation of coating.Fig. 5 and 6 is respectively 3000 times of SEM images of pH8.0,9.2 o'clock gained coating, as can be seen from the figure, the nickel dam during pH8.0 has accumulation, agglomeration to occur, and arrange comparison rule, evenly of nickel dam during pH9.0, this shows that pH changes performance on coating also large impact.
In order to make the heterogeneity in the piezo-electricity composite material plate simultaneously electrode, the present invention improves chemical plating technology, and activating process has been carried out selection, optimization, adopts palladium salt activation solution and nickel salt activation solution that material is activated.Palladium salt activation method is to use the reductive agent such as tin protochloride that palladium ion is reduced to palladium metal, makes its deposition or is adsorbed on matrix surface, and it has the characteristics such as activation effect is good, technique is simple, is the metal activation liquid that industrial value is arranged at present most.The nickel salt activation method is by selecting suitable reductive agent, with the reduction of the metal ion in the nickel salt solution, thereby obtains metallic particles, and the palladium activation method cost that no-palladium activating technique is more traditional is low, pollute the advantages such as little, has boundless Research Prospects.By these two kinds of activation methods, make piezoelectric ceramics and polymkeric substance have close catalytic activity, thereby can on two kinds of different non-metallic material, plate simultaneously electrode by the method for electroless plating, and coating is even, bonding force is strong.In addition, also nickel-plating liquid is improved in Ni-Speed, make the nickel plating temperature gentle, plating time is fast, and thickness of coating is easy to control, and bath life is long.
Except above-mentioned improvement, roughening process has been carried out selection, optimization, what the present invention used in roughening process is that density is about 1.0-1.5g/cm
3(preferred 1.2g/cm
3) the mixing inorganic acid solution.The roughening processes such as mixing solutions, phosphoric acid, sodium hydroxide of mixing solutions, chromium trioxide and the hydrofluoric acid of the aqueous solution, hydrofluoric acid and nitric acid of the hydrofluoric acid that generally uses now or sulfuric acid have been abandoned.The coarsening solution that this technique is used have cost lower, pollute less, the advantage such as low temperature (less energy-consumption), coarsening solution are stable.
The present invention does not need expensive device, can be at complex components surface deposition nickel, the speed of nickel plating is fast, the thickness of coating easy-regulating, gained nickel electrode thickness of coating even compact, binding force of cladding material is strong, and homogeneity is good, and wear resistance is good, etch resistant properties is good, weldability is good, and long service life can satisfy the demand that matrix material is used.
Description of drawings
Fig. 1 is that bath temperature is to plating the curve of speed;
3000 times of SEM images of gained coating when Fig. 2 is 30 ℃;
3000 times of SEM images of gained coating when Fig. 3 is 40 ℃;
3000 times of SEM images of gained coating when Fig. 4 is 50 ℃;
3000 times of SEM images of gained coating when Fig. 5 is pH=8.0;
3000 times of SEM images of gained coating when Fig. 6 is pH=9.2;
Fig. 7 is 5000 times of SEM images of embodiment 1 gained coating;
Fig. 8 is 5000 times of SEM images of no-palladium activating coating.
Embodiment
The present invention will be further elaborated below by specific embodiment, should be understood that, following explanation only is in order to explain the present invention, its content not to be limited.
All used pharmaceutical chemicalss of the present invention all can have been bought in market, and its source does not repeat them here, below among the embodiment used concentrated hydrochloric acid be the hydrochloric acid of 37wt%.Used coarsening solution is by density 1.0-1.5g/cm
3The mixing mineral acid and water 1:2-4 is formulated by volume, described mineral acid comprises sulfuric acid, hydrochloric acid, nitric acid, perchloric acid etc., blending ratio is to reach density 1.0-1.5g/cm
3Be advisable.
Resins, epoxy, high-temp glue and silica gel used among the following embodiment all can have been bought in market, and used Resins, epoxy comprises Racemic glycidol amine epoxy resin and line style aliphatic category Resins, epoxy, and all energy should be in the present invention for the model of having bought on the market.
Adopt palladium salt activation solution to carry out electroless plating reaction
Embodiment 1
Used solution is as follows:
Prepare each solution according to following method:
Coarsening solution: mineral acid and distilled water are prepared in proportion.
Sensitizing solution: with SnCl
22H
2O and concentrated hydrochloric acid and distilled water are prepared in proportion, the dissolution process heat treated.
Activation solution: with PdCl
2Be dissolved in the hydrochloric acid after the dilution and be made into the dissolution process heat treated.
Nickel-plating liquid: a, the various pharmaceutical chemicalss that will calculate weighing are used respectively an amount of dissolved in distilled water;
B, with NaH
2PO
2H
2O and NH
4Cl solution mixes, and is made into B liquid;
C, with NiSO
47H
2O, BSO additive and NaC
6H
5O
72H
2Each solution of O mixes successively, is made into A liquid;
D, under constantly stirring, slowly B liquid is added A liquid;
E, with distilled water diluting to prescribed volume on the lower side, transfer PH to specialized range with ammoniacal liquor.
After solution preparation is good, adopt the method for chemical nickel plating, 1-3 piezo-electricity composite material and 2-2 type piezo-electricity composite material are carried out nickel plating, the piezoelectric ceramics in the used piezo-electricity composite material is: PMN-ZT or PZT, polymkeric substance is AB-grouting resin, high-temp glue or silica gel, and its step is as follows:
(1) alligatoring: piezo-electricity composite material is put into processed 15min in the coarsening solution at normal temperatures, the sample after the alligatoring is placed on after the flowing water flushing boils 5min in the boiling water to remove the alligatoring raffinate fully;
(2) sensitization: take out after at room temperature processing 5min, use washed with de-ionized water;
(3) activation: stir also under the room temperature and constantly stir substrate, take out behind the 5min, use washed with de-ionized water;
(4) electroless plating: sample is 30 ℃ of lower 8min that process in nickel-plating liquid, constantly stir to make coating even;
(5) trimming: after coating reaches thickness, adopt the mode of polishing to remove at piezo-electricity composite material side electrode.
The nickel electrode coating of all types of materials that obtain by aforesaid method is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, and welding lead is firm.The type that can get thus piezo-electricity composite material does not affect the enforcement of electroless plating, and piezoelectric ceramics commonly used and polymkeric substance all can adopt this mode plated electrode.
Embodiment 2
Used solution is as follows:
Method according to embodiment 1 prepares required solution, adopt the method for chemical nickel plating that 1-3 piezo-electricity composite material and 2-2 type piezo-electricity composite material are carried out nickel plating, piezoelectric ceramics in the used piezo-electricity composite material is: PMN-ZT or PZT, polymkeric substance is Resins, epoxy, high-temp glue or silica gel, method such as embodiment 1.Sample is 37 ℃ of lower electrodes that obtain in nickel-plating liquid.The electrode obtained coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, the firm difficult drop-off of welding lead.
Embodiment 3
Used solution is as follows:
Method according to embodiment 1 prepares required solution, adopt the method for chemical nickel plating that 1-3 piezo-electricity composite material and 2-2 type piezo-electricity composite material are carried out nickel plating, piezoelectric ceramics in the used piezo-electricity composite material is: PMN-ZT, PZT, polymkeric substance is AB-grouting resin, high-temp glue or silica gel, method such as embodiment 1.Sample is 25 ℃ of lower electrodes that obtain in nickel-plating liquid.The electrode obtained coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, and welding lead is firm.
Embodiment 4
Used solution is as follows:
Method according to embodiment 1 prepares required solution, adopt the method for chemical nickel plating that 1-3 piezo-electricity composite material and 2-2 type piezo-electricity composite material are carried out nickel plating, piezoelectric ceramics in the used piezo-electricity composite material is: PMN-ZT, PZT, polymkeric substance is Resins, epoxy, high-temp glue or silica gel, method such as embodiment 1.Sample is 50 ℃ of lower electrodes that obtain in nickel-plating liquid.The electrode obtained coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, and welding lead is firm.
Adopt the nickel salt activation solution to carry out electroless plating reaction
Embodiment 5
Used solution is as follows:
Method preparation coarsening solution, sensitizing solution and nickel-plating liquid according to embodiment 1.The compound method of nickel salt activation solution is: the nickelous acetate of calculated amount and sodium borohydride are used respectively volume required half dissolve with methanol.Adopt the method for chemical nickel plating that 1-3 piezo-electricity composite material and 2-2 type piezo-electricity composite material are carried out nickel plating, piezoelectric ceramics is PMN-ZT, PZT in the used piezo-electricity composite material, polymkeric substance is AB-grouting resin, silica gel or high-temp glue, alligatoring, sensitization and nickel plating process such as embodiment 1, activation method is: sample is put into 37 ℃ of nickelous acetate solution, stir and constantly stir substrate, (sodium borohydride is reductive agent slowly to pour sodium borohydride solution behind the 10min into, reduced nickel simple substance), continue to stir and constantly stir substrate, take out behind the 20min, use washed with de-ionized water;
Gained nickel coating electrode coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, and welding lead is firm.
Embodiment 6
Used solution is as follows:
Method according to embodiment 5 prepares required solution, and 1-3 piezo-electricity composite material and 2-2 type piezo-electricity composite material carried out nickel plating, piezoelectric ceramics is PMN-ZT, PZT in the used piezo-electricity composite material, and polymkeric substance is Resins, epoxy, silica gel and high-temp glue, method such as embodiment 5.Sample is 42 ℃ of lower electrodes that obtain in nickel-plating liquid.The electrode obtained coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, and welding lead is firm.
Embodiment 7
Used solution is as follows:
Method according to embodiment 5 prepares required solution, and piezo-electricity composite material is carried out nickel plating, and used piezo-electricity composite material forms method such as embodiment 5 by piezoelectric ceramics and AB-grouting resin.Sample is 50 ℃ of lower electrodes that obtain in nickel-plating liquid.The electrode obtained coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, and welding lead is firm.
Embodiment 8
Used solution is as follows:
Method according to embodiment 5 prepares required solution, and piezo-electricity composite material is carried out nickel plating, and used piezo-electricity composite material forms method such as embodiment 5 by piezoelectric ceramics and AB-grouting resin.The electrode obtained coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, and welding lead is firm.
Embodiment 9
Used solution is as follows:
After solution preparation is good, 1-3 piezo-electricity composite material and 2-2 type piezo-electricity composite material are carried out nickel plating, piezoelectric ceramics is PMN-ZT, PZT in the used piezo-electricity composite material, and polymkeric substance is Resins, epoxy, silica gel or high-temp glue, method such as embodiment 5.Gained nickel coating electrode coating is even, and is strong with the piezo-electricity composite material bonding force, difficult drop-off, the firm difficult drop-off of welding lead.
Claims (5)
1. the preparation method of a nickel electrode made of piezoelectric composite material, it is characterized in that: adopt the method preparation of electroless plating, piezo-electricity composite material is put into nickel-plating liquid carry out nickel plating after alligatoring, sensitization, activation, obtain nickel electrode, described piezo-electricity composite material consist of piezoelectric ceramics and polymkeric substance, described polymkeric substance comprises Resins, epoxy or silica gel;
The used coarsening solution of alligatoring is density 1.0-1.5g/cm
3The mixing mineral acid and the mixed solution of water, mix the volume ratio 1:2-4 of mineral acid and water;
The used sensitizing solution of sensitization is SnCl
22H
2The aqueous solution of O and concentrated hydrochloric acid, SnCl
22H
2The content of O in water is 26-35g/L, and the content of concentrated hydrochloric acid in water is 45-55ml/L;
Activating used activation solution is palladium salt activation solution or nickel salt activation solution, and wherein, palladium salt activation solution is with PdCl
2Soluble in water formulated with concentrated hydrochloric acid, PdCl
2Content is that 0.3-0.5g/L, concentrated hydrochloric acid content are 9.9-11ml/L; The nickel salt activation solution is nickelous acetate and sodium borohydride to be dissolved in the anhydrous methanol formulated, and the content of nickelous acetate is 64-68g/L, and the content of sodium borohydride is 64-68g/L;
Described nickel-plating liquid is the aqueous solution, and its composition is NiSO
47H
2O, NaC
6H
5O
72H
2O, NaH
2PO
2H
2O, NH
4Cl and BSO additive, wherein, NiSO
47H
2O concentration is 15-25g/L, NaC
6H
5O
72H
2O content is 9-15g/L, NaH
2PO
2H
2O content is 18-30g/L, NH
4Cl content is 30 g/L, and the BSO additive level is 0.08-0.2g/L, pH8-11;
The preparation method may further comprise the steps:
(1) piezo-electricity composite material is added in the coarsening solution, process 5-30min under the room temperature, then piezo-electricity composite material is put into boiling water and clean, to remove coarsening solution;
(2) piezo-electricity composite material after the alligatoring is put into sensitizing solution, process 3-15min under the room temperature, then use washed with de-ionized water;
(3) piezo-electricity composite material after the sensitization is put into activation solution and carry out activation treatment, use washed with de-ionized water after processing; Adopting the treatment condition of palladium salt activation solution is to process 3-15min under the room temperature, and the treatment condition that adopt the nickel salt activation solution are the 20-40 ℃ of lower 30min of processing;
(4) piezo-electricity composite material after will activating is put into nickel-plating liquid, carries out nickel plating under 25-50 ℃, and constantly stirs, and stops nickel plating when coating reaches thickness, and the nickel dam that the matrix material both sides are unnecessary removes, and get final product; The compound method of nickel-plating liquid is: take by weighing each composition by proportioning, then with NaH
2PO
2H
2O and NH
4Cl mixes, and is made into B solution, with NiSO
47H
2O, BSO additive and NaC
6H
5O
72H
2O mixes, and is made into A solution; B solution is slowly splashed in the A solution, reconcile pH with ammoniacal liquor, and get final product.
2. preparation method according to claim 1 is characterized in that: PdCl in the described palladium salt activation solution
2Content is 0.4g/L.
3. preparation method according to claim 1, it is characterized in that: nickelous acetate is identical with the concentration of sodium borohydride in the described nickel salt activation solution.
4. preparation method according to claim 1, it is characterized in that: nickel-plating liquid pH is 9-9.6.
5. preparation method according to claim 1, it is characterized in that: the nickel plating temperature is 35-45 ℃.
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| CN103242063B (en) * | 2013-05-10 | 2015-02-25 | 济南大学 | Preparation method of piezoelectric ceramic surface electrode |
| CN103938192B (en) * | 2014-04-10 | 2016-06-08 | 厦门大学 | The electroless plating preparation method of a kind of piezo-electricity composite material metal electrode |
| CN104911568B (en) * | 2015-07-06 | 2018-02-09 | 合肥学院 | A kind of method of selective chemical plating |
| CN105801172B (en) * | 2016-03-04 | 2018-01-09 | 济南大学 | A kind of preparation method of cement base piezoelectric composite material surface nickel electrode |
| CN105586581B (en) * | 2016-03-04 | 2017-12-12 | 济南大学 | A kind of method in cement base piezoelectric composite material chemical nickel plating on surface |
| CN110195167B (en) * | 2019-04-28 | 2020-08-18 | 中南大学 | Nickel alloy framework reinforced metal matrix composite material and preparation method thereof |
| CN110918980B (en) * | 2019-12-16 | 2021-09-24 | 北京工商大学 | Electromagnetic shielding composite material and preparation method thereof |
| CN111763931A (en) * | 2020-07-15 | 2020-10-13 | 上海大学 | Preparation method of nickel-plated glass microspheres and product |
| CN112831776A (en) * | 2021-02-08 | 2021-05-25 | 福州大学 | Method for metalizing 3-3 type ceramic-polymer dielectric composite material |
| CN113059155B (en) * | 2021-03-22 | 2022-05-13 | 东北大学 | Preparation method of nickel-coated graphite composite powder material for conductive silica gel |
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