CN103938192A - Chemical deposition preparation method of piezoelectric composite metal electrode - Google Patents
Chemical deposition preparation method of piezoelectric composite metal electrode Download PDFInfo
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- CN103938192A CN103938192A CN201410142316.4A CN201410142316A CN103938192A CN 103938192 A CN103938192 A CN 103938192A CN 201410142316 A CN201410142316 A CN 201410142316A CN 103938192 A CN103938192 A CN 103938192A
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Abstract
The invention relates to a chemical deposition preparation method of a piezoelectric composite metal electrode. The chemical deposition preparation method particularly aims at a PZT ceramic and polymer coexisting composite material and comprises the following preparation steps: preparing a piezoelectric composite, cleaning, removing oil, wetting, carrying out primary coarsening, reducing, carrying out secondary coarsening, activating a colloid target, peptizing, carrying out chemical plating and passivating. According to the chemical deposition preparation method, a metal coating chemically deposited on the surface of the piezoelectric composite has a bright surface, is fine in crystallization, can uniformly cover the surfaces of ceramics and polymers and has good binding force with the ceramics and polymers. An adopted medium and low temperature technology is capable of ensuring that the piezoelectric composite metal electrode is free of deformation and material separation. The chemical deposition preparation method does not need expensive equipment and is low in cost and suitable for large scale production.
Description
Technical field
The present invention relates to piezo-electricity composite material metal electrode electroless plating preparation method, belong to composite electrode research and development field.
Background technology
Pb-based lanthanumdoped zirconate titanates (PZT) ceramic/polymer composite has that piezo-electric modulus is high, density is low, specific acoustic resistance is low and the feature such as mechanical quality is good, as element of transducer, dominate always in the fields such as underwater acoustic transducer, biomedical imaging, ultrasonic engineering.In piezo-electricity composite material transverter, the impact of electrode pair components and parts performance and used life is very big.Therefore, develop and a kind ofly on matrix material, obtain that bonding force is good, the preparation method of the metal electrode that is evenly distributed, become the key of transducing components and parts performance superperformance.
At present, the general Magnetron Sputtering Thin Film deposition technique that adopts of piezo-electricity composite material electrode preparation.Document 1
[1]disclose a kind of magnetron sputtering and prepared the method for composite electrode, but this technology has the following disadvantages: (1) is high to equipment and site requirements; (2) the raw-material utilization ratio of electrode and production efficiency are lower; (3) electrode obtaining and the bonding force of piezo-electricity composite material are poor.
Traditional wet-chemical deposition techniques, can obtain on complex-shaped part that bonding force is good, the coating of uniformity, and the method technique is simple simultaneously, and cost is low.In matrix material, not only contain Pb-based lanthanumdoped zirconate titanates (PZT) pottery but also contain organic polymer.For polymer materials, adopt conventional wet-chemical deposition techniques, its preprocessing process need to pass through a few to tens of minutes roughening treatment of 60~75 DEG C.After polymer materials roughening treatment, piezo-electricity composite material easily produces PZT pottery and polymkeric substance disengaging in distortion, matrix material.Publication number is 102337526 patent of invention
[2]application discloses a kind of preparation method of nickel electrode made of piezoelectric composite material, the method adopts normal temperature mixing mineral acid (hydrochloric acid, sulfuric acid, nitric acid and perchloric acid etc.) alligatoring, carry out again sensitization, activation and the processing of chemical deposited nickel film, obtain the nickel electrode of piezo-electricity composite material.But mineral acid only can alligatoring PZT pottery, cannot carry out effective alligatoring to polymer materials.Therefore,, by the method alligatoring piezo-electricity composite material, nickel film and the PZT pottery of electroless plating can obtain good bonding force, cannot obtain good bonding force with polymer materials.
1. Wan Yuanyuan, Li Li, Wang Likun, Qin Lei, the preparation [J] of Wei's army .1-3 type piezo-electricity composite material electrode. functional materials, 2007,38 (02), 738-740.
2. Cheng Xin, Zhang Ying, Huang Shifeng, Sun Min, Zhou Meijuan, Hao Chao. a kind of preparation method [P] .CN102337526. of nickel electrode made of piezoelectric composite material
Summary of the invention
The object of the invention is to avoid weak point in background technology, invent a kind of piezo-electricity composite material metal electrode electroless plating preparation method.
The technical scheme that technical solution problem of the present invention adopts is: a kind of electroless plating preparation method of piezo-electricity composite material metal electrode, is undertaken by being prepared as follows order:
Activation → dispergation → electroless plating → the passivation of piezo-electricity composite material → cleaning → oil removing → hydrophilic → mono-step alligatoring → reduction → bis-step alligatoring → colloidal palladium.Between each step of preparation order, successively use tap water and washed with de-ionized water clean.
Its concrete steps are:
1. clean: piezo-electricity composite material is successively clean with tap water and washed with de-ionized water.The object of cleaning is the pollutent that clean composite material surface adheres to.
2. oil removing: in 30~40 DEG C of degreasing fluids, oil removing 5~10 minutes.Degreasing fluid is prepared by following formula rate: anhydrous sodium carbonate (Na
2cO
3) 40-60g/L, sodium phosphate (Na
3pO
412H
2o) 40-60g/L, sodium hydroxide (NaOH) 10~50g/L, water glass (Na
2siO
39H
2o) 5~20g/L, OP-10 emulsifying agent 1~3ml/L.The object of oil removing is to remove saponified oil and the mineral oil of composite material surface.
3. hydrophilic: in 30~40 DEG C of hydrophilic liquid, to stir and soak 3~5 minutes.Hydrophilic liquid is prepared with volume ratio by following formula: acetonitrile (C
2h
3n) 10~20%, methylene dichloride (CH
2cl
2) 5~10%, DMF (C
3h
7nO) 70~85%.Hydrophilic object is to improve the wetting ability of composite material surface.
4. a step alligatoring: in 40~50 DEG C of one step coarsening solution, soak 2~3 minutes.One step coarsening solution is prepared by following formula rate: chromic anhydride (CrO
3) 350~400g/L, sulfuric acid (H
2sO
4) 250~300ml/L, hydrofluoric acid (HF40%) 4~10ml/L.The object of one step alligatoring is main etching and micro-alligatoring organic polymer, and organic polymer surface hydrophilicity is improved.
5. reduction: in reduced liquid, soak at room temperature 0.5-1.5 minute.Reduced liquid is prepared by following formula rate: Sodium Pyrosulfite (Na
2s
2o
6) 5~20g/L.The object of reduction is, is trivalent chromium by the hexavalent chrome reduction that is attached to composite material surface.
6. two step alligatoring: in two step coarsening solutions, soak under normal temperature 3~5 minutes.Two step coarsening solutions are prepared by following formula rate: hydrofluoric acid (HF40%) 100~250ml/L, ammonium bifluoride (NH
4hF
2) 10~20g/L.The object of two step alligatoring is main etching and micro-alligatoring PZT pottery, and ceramic surface wetting ability is improved.
7. colloidal palladium activation: in colloidal palladium solution, soak at 30~35 DEG C 3~5 minutes.Colloidal pd activation solution is prepared by following formula rate: dichloro diamino palladium (Pd (NH
3)
2cl
2) 0.05~1.0g/L, tin protochloride (SnCl
22H
2o) 8~16g/L, hydrochloric acid 10~60ml/L, sodium stannate (Na
2snO
33H
2o) 0.4-0.8g/L, sodium-chlor (NaCl) 100~150g/L.The object of colloidal palladium activation is, makes composite material surface adhesion palladium colloid.
8. dispergation: separate in glue, soak at 45-55 DEG C 2~3 minutes.Separate glue and press the preparation of row formula rate: sulfuric acid (H
2sO
4) 150~250ml/L.The object of dispergation is, composite material surface exposed have the nanoparticle palladium of catalytic activity.
9. electroless plating: in electroless plating copper solutions, electroless plating 10~60 minutes at 30~40 DEG C.Electroless plating solution is prepared by following formula rate: copper sulfate (CuSO
45H
2o) 10~15g/L, disodium ethylene diamine tetraacetate (EDTA2Na) 29~44g/L, oxoethanoic acid (C
2h
2o
3) 7~12g/L, yellow prussiate of potash 10~20mg/L, a, a '-dipyridyl 10~30mg/L, pH13-14.The object of electroless plating is, deposits copper coating at composite material surface.Copper coating surface-brightening and crystallization be careful, can be covered in equably pottery and polymer surfaces, all have good bonding force with pottery and polymkeric substance.
10. passivation: in passivating solution, passivation 1~5 minute under normal temperature.Passivating solution is prepared by following formula rate: Sodium orthomolybdate (Na
2moO
42H
2o) 1~5g/L, cerous nitrate (Ce (NO
3)
36H
2o) 0.5~2g/L, benzotriazole (BTA) 0.2~3g/L.The object of passivation is: the protection against corrosion and the anti-tarnishing ability that improve chemical plating copper layer.
In above steps, all use deionized water obtain solution.
Piezo-electricity composite material is after a step alligatoring and two step alligatoring, must control organic polymer material surface uniform and occur that diameter is less than the pit of 200nm, thereby make electroless plating layer and matrix material produce " anchor " effect, the metal electrode that guarantee obtains and the bonding force of matrix material are good.The better scope of pit is 60-150nm.
The piezo-electricity composite material that preparation method of the present invention is ceramic for PZT especially and epoxide resin polymer coexists, can all carry out even alligatoring to the polymkeric substance in matrix material and PZT pottery.By electroless plating, at the metal plating of piezo-electricity composite material surface deposition, surface-brightening and crystallization be careful, can be covered in equably pottery and polymer surfaces, all have good bonding force with pottery and polymkeric substance.Middle low temperature process used, can ensure that piezo-electricity composite material metal electrode is without being out of shape, departing from without material.Piezo-electricity composite material metal electrode prepared by electroless plating of the present invention, with low cost, without expensive device, can realize scale operation.
The copper electrode coating surface light and the crystallization that obtain piezo-electricity composite material by aforesaid method are careful, can be covered in equably pottery and polymer surfaces, have good protection against corrosion and anti-tarnishing ability, all have good bonding force with pottery and polymkeric substance.
In piezo-electricity composite material of the present invention, polymkeric substance is preferably epoxy resin material; Pottery is preferably Pb-based lanthanumdoped zirconate titanates (PZT) pottery.
Adopt the present invention to prepare metal electrode on piezo-electricity composite material surface.Low temperature technique in the present invention's process using used, can ensure that metal electrode production process piezo-electricity composite material is without departing from without mutual between distortion, polymkeric substance and pottery.The layer electrodes that obtains light and evenly, there is good bonding force with PZT pottery and polymer material substrate simultaneously.In addition, the present invention is without expensive device, with low cost, is applicable to scale operation.
Brief description of the drawings
Fig. 1 is piezo-electricity composite material metallograph;
Fig. 2 is the copper electrode metallograph of piezo-electricity composite material electroless plating;
Embodiment
Below by embodiment, the present invention will be further elaborated; it is to be understood that, following example is just to brief description of the present invention, instead of limitation of the present invention; any innovation and creation that do not exceed in connotation of the present invention, all fall within the scope of protection of the present invention.
Piezo-electricity composite material (Fig. 1) metal electrode is the disk that lead zirconate-titanate ceramic and epoxide resin polymer are composited, and disk diameter is about 5cm.
Undertaken by being prepared as follows order: piezo-electricity composite material is cleaned, be placed in 35 DEG C of degreasing fluids, oil removing 10 minutes; At 35 DEG C in hydrophilic liquid, hydrophilic treatment 5 minutes; In 45 DEG C of one step coarsening solution, soak 2 minutes; In reduced liquid, soak at room temperature 1 minute; In two step coarsening solutions, under normal temperature, soak 3 minutes; In 35 DEG C of colloidal palladium solution, soak 3 minutes; Separate in glue, soak 2 minutes for 50 DEG C; In 40 DEG C of electroless plating copper solutionss, electroless plating 30 minutes; In passivating solution, passivation 5 minutes under normal temperature.
Solution formula that above-mentioned operation is used is as follows:
1, degreasing fluid is prepared by following recipe ratio:
2, hydrophilic liquid is prepared by following recipe ratio:
Acetonitrile (C
2h
3n) 15%,
Methylene dichloride (CH
2cl
2) 10%,
DMF (C
3h
7nO) 75%.
3, coarsening solution is prepared by following recipe ratio:
Chromic anhydride (CrO
3) 350g/L,
Sulfuric acid (H
2sO
4) 250ml/L,
Hydrofluoric acid (HF40%) 5ml/L.
4, reduced liquid is prepared by following recipe ratio:
Sodium Pyrosulfite (Na
2s
2o
6) 5g/L.
5, two step coarsening solutions are prepared by following recipe ratio:
Hydrofluoric acid (HF40%) 200ml/L,
Ammonium bifluoride (NH
4hF
2) 20g/L.
6, colloidal palladium liquid is prepared by following recipe ratio:
7, dispergation
Sulfuric acid (H
2sO
4) 250ml/L.
8, electroless plating solution is prepared by following recipe ratio:
9, passivating solution is prepared by following recipe ratio:
Sodium orthomolybdate (Na
2moO
42H
2o) 2g/L,
Cerous nitrate (Ce (NO
3)
36H
2o) 1g/L,
Benzotriazole (BTA) 2g/L.
The copper electrode coating of the piezo-electricity composite material obtaining by aforesaid method, surface-brightening and crystallization be careful, can be covered in equably pottery and polymer surfaces (Fig. 2); Piezo-electricity composite material metal electrode is without departing from without mutual between distortion, pottery and polymkeric substance; Bonding force test shows that coating is without peeling, and bonding force is good.
Bonding force testing method: a kind of viscose band (the adhesion strength value of adhesive tape is approximately that the width of every 25mm is 8N) is sticked on coating, with rubber cylinder roll extrusion in the above, to remove the air filled cavity in adhesive surface.After the 10s of interval, use perpendicular to the pulling force of coating and make tape stripping, coating is good without peeling description taken in conjunction power.The present invention obtains piezo-electricity composite material metal electrode coating through above-mentioned testing method, and coating is without peeling, and binding force of cladding material is good.
Claims (3)
1. an electroless plating preparation method for piezo-electricity composite material metal electrode, comprises the steps: piezo-electricity composite material → cleaning → oil removing → hydrophilic → step alligatoring → reduction → bis-step alligatoring → colloidal palladium activation → dispergation → electroless plating → passivation, wherein:
(1) degreasing fluid composition and condition: anhydrous sodium carbonate (Na
2cO
3) 40-60g/L, sodium phosphate (Na
3pO
412H
2o) 40-60g/L, sodium hydroxide (NaOH) 10~50g/L, water glass (Na
2siO
39H
2o) 5~20g/L, OP-10 emulsifying agent 1~3ml/L, 30~40 DEG C, 5~10 minutes;
(2) hydrophilic liquid composition and condition: acetonitrile (C
2h
3n) 10~20%, methylene dichloride (CH
2cl
2) 5~10%, DMF (C
3h
7nO) 70~85%, 30~40 DEG C, 3~5 minutes;
(3) one step coarsening solution composition and conditions: chromic anhydride (CrO
3) 350~400g/L, sulfuric acid (H
2sO
4) 250~300ml/L, hydrofluoric acid (HF40%) 4~10ml/L, 40~50 DEG C, 2~3 minutes;
(4) reduced liquid composition and condition: Sodium Pyrosulfite (Na
2s
2o
6) 5~20g/L, room temperature, 0.5-1.5 minute;
(5) two step coarsening solution composition and conditions: hydrofluoric acid (HF40%) 100~250ml/L, ammonium bifluoride (NH
4hF
2) 10~20g/L, room temperature, 3~5 minutes;
(6) colloidal palladium solution composition and condition: dichloro diamino palladium (Pd (NH
3)
2cl
2) 0.05~1.0g/L, tin protochloride (SnCl
22H
2o) 8~16g/L, hydrochloric acid 10~60ml/L, sodium stannate (Na
2snO
33H
2o) 0.4-0.8g/L, sodium-chlor (NaCl) 100~150g/L, 30~35 DEG C, 3~5 minutes;
(7) separate glue composition and condition: sulfuric acid (H
2sO
4) 150~250ml/L, 45-55 DEG C, 2~3 minutes;
(8) chemical depositing copper solution composition and condition: copper sulfate (CuSO
45H
2o) 10~15g/L, disodium ethylene diamine tetraacetate (EDTA2Na) 29~44g/L, oxoethanoic acid (C
2h
2o
3) 7~12g/L, yellow prussiate of potash 10~20mg/L, a, a '-dipyridyl 10~30mg/L, pH13-14,30~40 DEG C, 10~60 minutes;
(9) passivating solution composition and condition: Sodium orthomolybdate (Na
2moO
42H
2o) 1~5g/L, cerous nitrate (Ce (NO
3)
36H
2o) 0.5~2g/L, benzotriazole (BTA) 0.2~3g/L, room temperature, 1~5 minute.
2. the electroless plating preparation method of a kind of piezo-electricity composite material metal electrode as claimed in claim 1, it is characterized in that: piezo-electricity composite material, after a step alligatoring and two step alligatoring, is controlled organic polymer material surface uniform and occurred that diameter is less than the pit of 200nm.
3. the electroless plating preparation method of a kind of piezo-electricity composite material metal electrode as claimed in claim 1, is characterized in that: described chemical plating copper layer surface-brightening, can be covered in equably pottery and polymer surfaces, all have good bonding force with pottery and polymkeric substance.
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Cited By (10)
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CN105586581A (en) * | 2016-03-04 | 2016-05-18 | 济南大学 | Method for chemical nickel-plating on surface of cement-based piezoelectric composite |
CN105951142A (en) * | 2016-05-19 | 2016-09-21 | 南通柏源汽车零部件有限公司 | Pretreatment technology for electroplating of automobile door handle |
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CN110134276A (en) * | 2019-04-30 | 2019-08-16 | 西安交通大学 | Two-dimentional P4X2Profile material is used as the purposes of piezoelectric material |
CN110813201A (en) * | 2019-11-07 | 2020-02-21 | 苏州天承化工有限公司 | Concentrated palladium colloid and preparation method and application thereof |
CN111635261A (en) * | 2020-06-30 | 2020-09-08 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material and preparation method thereof |
CN115896760A (en) * | 2022-09-15 | 2023-04-04 | 深圳市生利科技有限公司 | Pre-electroplating pretreatment process and application thereof |
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CN1047419A (en) * | 1989-05-16 | 1990-11-28 | 四川大学 | The production technology of electrode of piezoelectric ceramic device |
CN1057300A (en) * | 1991-05-29 | 1991-12-25 | 抚顺石油学院 | There are not lead-in wire Leaded Ceramic Disc Capacitor topochemistry nickel plating or copper method |
CN102337526A (en) * | 2011-09-15 | 2012-02-01 | 济南大学 | Preparation method of nickel electrode made of piezoelectric composite material |
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CN106567058B (en) * | 2015-10-09 | 2019-03-19 | 凯基有限公司 | Chromium-free environment-friendly metal-coated membrane structural system |
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 |
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CN107326347A (en) * | 2017-07-04 | 2017-11-07 | 西北工业大学 | Hard PMI foam integrated waveguide surface chemical plating copper methods |
CN107326347B (en) * | 2017-07-04 | 2019-09-20 | 西北工业大学 | Hard PMI foam integrated waveguide surface chemical plating copper method |
CN107680957A (en) * | 2017-10-27 | 2018-02-09 | 镇江佳鑫精工设备有限公司 | A kind of anti-interference semiconductor structure |
CN109894611B (en) * | 2019-03-29 | 2022-02-08 | 南京邮电大学 | Chemical plating Cu-Fe-Co-based composite corrosion-resistant wave-absorbing material and preparation method and application thereof |
CN109894611A (en) * | 2019-03-29 | 2019-06-18 | 南京邮电大学 | A kind of Electroless Cu Plating iron cobalt-based composite anticorrosive absorbing material and its preparation method and application |
CN110134276A (en) * | 2019-04-30 | 2019-08-16 | 西安交通大学 | Two-dimentional P4X2Profile material is used as the purposes of piezoelectric material |
CN110134276B (en) * | 2019-04-30 | 2020-12-15 | 西安交通大学 | Use of two-dimensional P4X 2-type material as piezoelectric material |
CN110813201B (en) * | 2019-11-07 | 2021-09-28 | 苏州天承化工有限公司 | Concentrated palladium colloid and preparation method and application thereof |
CN110813201A (en) * | 2019-11-07 | 2020-02-21 | 苏州天承化工有限公司 | Concentrated palladium colloid and preparation method and application thereof |
CN111635261A (en) * | 2020-06-30 | 2020-09-08 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material and preparation method thereof |
CN115896760A (en) * | 2022-09-15 | 2023-04-04 | 深圳市生利科技有限公司 | Pre-electroplating pretreatment process and application thereof |
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