CN101381866A - Method for preparing ion polymer-metal composite material - Google Patents
Method for preparing ion polymer-metal composite material Download PDFInfo
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- CN101381866A CN101381866A CNA2008101507836A CN200810150783A CN101381866A CN 101381866 A CN101381866 A CN 101381866A CN A2008101507836 A CNA2008101507836 A CN A2008101507836A CN 200810150783 A CN200810150783 A CN 200810150783A CN 101381866 A CN101381866 A CN 101381866A
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Abstract
The invention discloses a method for preparing an ionomer-metallic composite material, which adopts a Nafion-117 type ion-exchange film as a matrix material, uses [Pd(NH3) 2]Cl2 as a main salt, and adopts the chemical plating method to prepare a Pb metal type IPMC material. The process flow is divided into four parts: (1) the surface contact areas for ions to penetrate and reduction reaction are increased through sanding and roughening the ion-exchange film; (2) a pretreated Nafion film is impregnated for Pb ion exchange, a strong reducing agent reduces Pb ions, and a Pb metal layer is formed on the surface of the ion-exchange film; (3) secondary reduction is carried out by the improved chemical Pb plating method to thicken electrodes on the surface of a sandwich layer material; and (4) the material is subjected to post-treatment. The method has low cost, and experiments show that the IPMC material prepared has good performance, so that the ionomer-metallic composite material has high promotion value.
Description
Technical field
The present invention relates to a kind of preparation method of ion polymer-metal composite material, particularly a kind of preparation method who makes electrode layer and the membrane-bound ion polymer-metal composite material of ion-exchange based on electroless plating.
Background technology
Ion polymer-metal composite material (IPMC) is a kind of ionic electroactive polymer, have light weight, snappiness good, be swift in response and the bidirectional reversible function of sensing-actuating, can be used for making electromechanical transducing devices such as driving mechanism to replace traditional piezoelectric ceramics, is that recent two decades emerges and has the novel intelligent material of very big application potential.The IPMC material mainly is made up of ion-exchange membrane core material and metal electrode layer material, make electrode layer and ion-exchange membrane combination by physics or chemical process, wherein platinum is the most extensive as the research of electrode, the basic Study on Preparation of Pt-Nafion type IPMC material is comparatively ripe, and U.S. M.Shahinpoor has applied for this preparation method's patent (patent No. 6109852).Platinum electrode type IPMC material mainly adopts electroless plating to prepare, and the platinum salt that uses in the electroless plating process is quite expensive, comparatively speaking, selects palladium as electrode materials, and preparation cost will reduce a lot, but platinum genotype IPMC material technology and be not suitable for metallic palladium.As the IPMC of electrode materials certain research is arranged also with metals such as Ag, Cu and Ni in addition, but these materials this in powering up effect down, be easy to oxidation and make material property very unstable.
Summary of the invention
The palladium and the platinum character that are all platinum metals are similar, but palladium salt is cheap relatively and density is littler, is fit to very much do electrode materials.The purpose of this invention is to provide a kind ofly with the novel process of palladium as electrode preparation IPMC material, can effectively reduce IPMC material cost of manufacture, performance is also comparatively stable and good simultaneously.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of preparation method of ion polymer-metal composite material comprises the steps:
1) pre-treatment of base material: as base material, this base material alligatoring and cleaning, acidifying, deionization poach are washed with ion-exchange membrane Nafion film;
2) chemical palladium-plating comprises reduction for the first time and reduction for the second time;
The concrete technical process of reductive for the first time is:
1. adopt dichloro two ammoniums to close palladium [Pd (NH
3)
2] Cl
2Salts solution as once reducing plating bath, the concentration of pressing 1.5-2g/L is with [Pd (NH
3)
2] Cl
2Be mixed in the deionized water, and dropwise add 25% ammoniacal liquor stirred solution and all dissolve, pretreated Nafi on film is put into the palladium salts solution soak and carry out ion-exchange an evening until palladium salt;
2. will rinse well through the Nafion film of ion-exchange, and put into the beaker that fills deionized water, and add the ammoniacal liquor of 5% (weight) by the minim of 15-20ml/L, stirring at low speed is heated to 40 ℃ with the beaker water-bath then;
3. the NaBH4 solution of Dropwise 5 % (weight) reduces the palladium ion on the Nafion film again, so just forms the metallic palladium layer on Nafion film surface, becomes the Pd-Nafion film;
4. clean after reduction is finished, and be immersed in the HCl solution of 0.2mol/L, in order to carrying out the reduction second time;
The concrete technical process of reductive for the second time is:
1. prepare the secondary reduction plating bath, this plating bath comprises the palladium salt [Pd (NH of 1-1.5g/L
3)
2] Cl
2, the ammoniacal liquor of 25% (weight) of 80g/L and the Na of 8g/L
2EDTA (disodium ethylene diamine tetraacetate), and heating in water bath to 40 ℃;
2. the Pd-Nafion film after will once reducing is put into the secondary reduction plating bath after cleaning, and stirring at low speed; The hydrazine solution of preparation 10% (weight) concentration splashes in the reduction plating bath, splashes at least three times, and 1 hour pitch time, and bath temperature raises 10 ℃ one by one until 60 ℃; The amount of splashing into is 0.5-1ml/L at every turn;
3. splash into take a morsel after the 4 hours NaBH of plating bath Dropwise 5 % (weight) of hydrazine solution for the last time
4Solution is judged the reduction terminal point, and the back electroless plating that reacts completely finishes and takes out and clean;
3) material aftertreatment: comprise driving ion-exchange and cutting:
1. drive ion-exchange: the Pd-Nafion acidization after at first will reducing for the second time, clean then, if the driving ion is M
N+, then use band M ionic alkaline solution or salts solution to soak more than 8 hours;
2. cutting: the Pd-Nafion film after the reduction cuts into the sample of normal size for the second time, and upper and lower palladium electrode is isolated.
In the such scheme, the NaBH of described Dropwise 5 %
4Solution makes the concrete technology of palladium ion reductive on the Nafion film be: the amount by 10-12ml/L begins to drip NaBH
4Solution, later on every half an hour, temperature raises 3 ℃, drips the NaBH of same amount
4Solution is raised to 60 ℃ up to temperature; Press the amount of 100-120ml/L at last and add NaBH4 solution, palladium ion is fully reduced.
Preparation technology's scheme of Pd-Nafion type IPMC of the present invention is an electrode materials with the metallic palladium, with Pd[(NH
3)
2] Cl
2Be main salt, Nafion-117 type ion-exchange membrane is prepared the comparatively good IPMC material of performance as body material.Ultimate principle of the present invention is earlier ion exchange membrane material to be immersed in the metallic palladium salts solution, makes palladium ion enter exchange membrane, uses strong reductant NaBH again
4With the palladium ion reduction, thereby form palladium electrode, adopt hydrazine to bathe plating then and thicken the palladium electrode layer on Nafion film surface; Use auxiliary reagent HCl, NaOH to be used for cleaning and driving ion exchange in addition.
The present invention catalytic film reaction is separated with hydrogen and the industrial Pd-electroplating process successful Application in purifying field in the IPMC material preparation, not only reduced the waste of palladium salt, lowered the precious metal cost, and make the IPMC material property not be subjected to preparation technology's influence, keep and same good and stable of Pt-Nafion type IPMC material.Its overlay coating is evenly fine and closely woven, and has good electrical conductivity.
Description of drawings
Fig. 1 prepares the structure iron of the Pd-Nafion type IPMC material of finishing for electroless plating.Wherein Fig. 1 a is a front view; Fig. 1 b is a side-view.Among the figure: 1, palladium electrode; 2, Nafion ion-exchange membrane.
Fig. 2 is Pd-Nafion type IPMC material displacement response under the effect of 2.5V step voltage.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
As shown in Figure 1, be that example illustrates preparation method of the present invention to prepare the IPMC material that size is about 5cm * 5cm:
1) preprocessing process:
As base material,, can adopt the sand papering alligatoring with Nafion ion-exchange membrane 2 because be the small area material preparation, with sand paper more than No. 600, Nafion film 2 surfaces of polishing gently.Make the surface evenly stressed during polishing as far as possible, do not exert oneself excessive otherwise can cause viscous deformation; Note at last observing coarse uniformity coefficient, under light, observe the surface and become muddy and do not have obvious bright spot, can think that polishing reaches even effect.
Also can use blasting craft, then with sand-blasting gun or other sand-blast device with 2sec/cm
2Speed polishing Nafion film surface.This method is more suitable for the big area material preparation.The alligatoring purpose is the contact area that increases ion infiltration and reduction reaction, and electrode better and through the Nafion film after the roughening is combined.
Material after the alligatoring should be after being heated to 60 ℃ ultrasonic cleaning 20 minutes, remove its surface particles; Take out the Nafion acid then and wash, remove foreign ion by acidification; The hydrochloric acid soln that uses is about 150ml, 2mol/L, and the pickling time is 40 minutes; Boil in deionized water at last and wash, remove unnecessary hydrochloric acid and other impurity, the time is about 30 minutes; Can be kept in the deionized water through pretreated Nafion film.
2) reduction for the first time:
Reduction is in order to make Nafion film 2 surface deposition layer of metal Catalytic Layer for the first time, is the chemical reaction basis of chemical palladium-plating in the secondary reduction.Earlier pretreated Nafion film is immersed in [Pd (NH
3)
2] Cl
2In the salts solution, infiltrate ion-exchange membrane through the ion-exchange palladium ion, (the present invention advises adopting NaBH to use strong reductant again
4) make it reduction, so just form the metallic palladium layer on the ion-exchange membrane surface.
[Pd (the NH that needs in the reduction
3)
2] Cl
2Salt calculates according to the plating palladium amount of single face 2mg/cm2, and the ion-exchange membrane of 5cm * 5cm size needs the 100mg palladium, converts [Pd (NH to
3)
2] Cl
2The about 0.2g of the quality of salt.
1. load weighted salt is mixed with the 150ml deionized water, and dropwise add 25% ammoniacal liquor stirred solution and all dissolve until palladium salt, the about altogether 10ml of dropping ammonia puts into the palladium salts solution with pretreated Nafion film and soaks an evening.
2. will rinse well with deionized water through the Nafion film of ion-exchange, put into the beaker that fills the 180ml deionized water, drip 3ml, 5% ammoniacal liquor, install the water-bath platform then, and adjust rotating speed and be about 120 rev/mins, be heated to 40 ℃.
3. begin to splash into 2ml, 5% NaBH
4Solution, later on every half an hour, temperature raises 3 ℃, drips 2ml, 5% NaBH
4Solution is raised to 60 ℃ up to temperature.
4. add 20ml, 5% NaBH4 solution at last, palladium ion is fully reduced.
5. reduction is used washed with de-ionized water after finishing, and is immersed in the HCl solution of 150ml, 0.2mol/L, takes out after 8 hours and carries out next step reduction.
3) secondary reduction:
After once reducing, Nafion film surface has deposited the thin metallic palladium layer of one deck, in order to improve electrode characteristic, need thicken electrode layer.The present invention is with reference to industrial Pd-electroplating process prescription, and in conjunction with the characteristics of IPMC material preparation, research summary has gone out a kind of feasible preparation scheme by experiment.Specific operation process is as follows:
1. prepare the secondary plating bath: palladium salt dosage is 0.16g, ammoniacal liquor and Na
2The EDTA usage quantity is respectively 12g and 1.2g, is mixed with the 150ml plating bath after the weighing, installs the water-bath platform, with plating bath heating in water bath to 40 ℃.
2. the material after will once reducing is put into plating bath after with washed with de-ionized water, adjusts about 60 rev/mins of rotating speed, and the hydrazine solution 25ml of preparation 10% splashes into 0.1ml (about);
3. temperature is elevated to 50 ℃ after 1 hour, splashes into the 0.1ml hydrazine solution once more;
4. after 1 hour, be warmed up to 60 ℃, splash into the 0.1ml hydrazine solution once more; The NaBH of plating bath Dropwise 5 % took a morsel after 4 hours
4Solution is judged the reduction terminal point, and the back electroless plating that reacts completely finishes and takes out and clean.
4) material aftertreatment:
1. drive ion-exchange: the IPMC material after at first will cleaning is immersed among the HCl of 100ml, 0.1mol/L, removes foreign ion, soaks 3 hours at the HCl of new 100ml, 0.1mol/L solution after 3 hours again, uses washed with de-ionized water then.In the NaOH of 200ml, 0.1mol/L solution soaking more than 8 hours.
2. cutting process: after the cutting of IPMC edge of materials, be cut into the shape of actual needs again.The purpose of cutting process is that upper/lower electrode is isolated, and cuts into the sample of normal size, and the Pd-Nafion type IPMC material sample of final preparation as shown in Figure 1.
The IPMC material of 5cm * 5cm that prepared of the present invention is formed cuts into the 5.5cm*1cm*0.2mm sample, and is mounted to cantilever beam structures, and it is 4.9cm*1cm*0.2mm that back material Free Transform portion size is installed.Between two electrodes of material, add voltage, under the 2.5V step voltage, during material end Free Transform, its tip displacement response as shown in Figure 2, can find to power up the about 13mm of back material maximum distortion, be about 26% of length of material, compare with the Pt-Nafion type performance for preparing in the patent of M.Shahinpoor, deformation performance will be got well.
Claims (3)
1, a kind of preparation method of ion polymer-metal composite material is characterized in that, comprises the steps:
1) pre-treatment of base material: as base material, this base material roughening and cleaning, acidifying, deionization poach are washed with ion-exchange membrane Nafion film;
2) chemical palladium-plating comprises reduction for the first time and reduction for the second time;
The concrete technical process of reductive for the first time is:
1. adopt dichloro two ammoniums to close palladium [Pd (NH
3)
2] Cl
2Salts solution as once reducing plating bath, the concentration of pressing 1.5-2g/L is with [Pd (NH
3)
2] Cl
2Be mixed in the deionized water, and dropwise add 25% ammoniacal liquor stirred solution and all dissolve, pretreated Nafion film is put into the palladium salts solution soak and carry out ion-exchange an evening until palladium salt;
2. will rinse well through the Nafion film of ion-exchange, and put into the beaker that fills deionized water, and add 5% ammoniacal liquor by the minim of 15-20ml/L, stirring at low speed is heated to 40 ℃ with the beaker water-bath then;
3. the NaBH of Dropwise 5 % again
4Solution makes the palladium ion reduction on the Nafion film, so just forms the metallic palladium layer on Nafion film surface, becomes the Pd-Nafion film;
4. clean after reduction is finished, and be immersed in the HCl solution of 0.2mol/L, in order to carrying out the reduction second time;
The concrete technical process of reductive for the second time is:
1. prepare the secondary reduction plating bath, this plating bath comprises the palladium salt [Pd (NH of 1-1.5g/L
3)
2] Cl
2, 25% the ammoniacal liquor of 80g/L and the disodium ethylene diamine tetraacetate Na of 8g/L
2EDTA, and heating in water bath to 40 ℃;
2. the Pd-Nafion film after will once reducing is put into the secondary reduction plating bath after cleaning, and stirring at low speed; Prepare the hydrazine solution of 10% concentration, splash in the reduction plating bath, splash at least three times, 1 hour pitch time, and bath temperature raises 10 ℃ one by one until 60 ℃; The amount of splashing into is 0.5-1ml/L at every turn;
3. splash into take a morsel after the 4 hours NaBH of plating bath Dropwise 5 % of hydrazine solution for the last time
4Solution is judged the reduction terminal point, and the back electroless plating that reacts completely finishes and takes out and clean;
3) material aftertreatment: comprise driving ion-exchange and cutting:
1. drive ion-exchange: the Pd-Nafion acidization after at first will reducing for the second time, clean then, if the driving ion is M
N+, n=1,2,3,4 then uses band M ionic alkaline solution or salts solution to soak more than 8 hours;
2. cutting: the Pd-Nafion film after the reduction cuts into the sample of required size for the second time, and upper and lower palladium electrode is isolated.
2, the preparation method of ion polymer-metal composite material as claimed in claim 1 is characterized in that, the NaBH of described Dropwise 5 %
4Solution makes the concrete technology of palladium ion reductive on the Nafion film be: the amount by 10-12ml/L begins to drip NaBH4 solution, and later on every half an hour, temperature raises 3 ℃, drips the NaBH4 solution of same amount, is raised to 60 ℃ up to temperature; Press the amount of 100-120ml/L at last and add NaBH4 solution, palladium ion is fully reduced.
3, the preparation method of ion polymer-metal composite material as claimed in claim 1 is characterized in that, described driving ion M
N+Be sodium ion.
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