CN103801289B - A kind of preparation method of fuel-cell catalyst - Google Patents

A kind of preparation method of fuel-cell catalyst Download PDF

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CN103801289B
CN103801289B CN201410093341.8A CN201410093341A CN103801289B CN 103801289 B CN103801289 B CN 103801289B CN 201410093341 A CN201410093341 A CN 201410093341A CN 103801289 B CN103801289 B CN 103801289B
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catalyst
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CN103801289A (en
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程立明
魏广科
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Jiangsu hydrogen power new energy Co., Ltd.
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Jiangsu Lv Yao Fuel Cell System Manufacturing Co Ltd
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    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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Abstract

The invention discloses a kind of preparation method of fuel-cell catalyst, comprise preparation four-in-one mould release membrance, vacuum magnetic-control sputtering graphite linings, vacuum magnetic-control sputtering noble metal catalyst, carrier of separating film, pulverize the step of carrier film and carbonization.The present invention adopts vacuum sputtering to be splashed in carrier film by graphite and noble metal catalyst, improve the adhesive force of metal platinum on graphite support particles, improve catalyst life, catalyst activity is strengthened, catalytic efficiency is high, thus reduce the use of fuel cell noble metal, greatly reduce the production cost of fuel cell.Meanwhile, production technology of the present invention is simple, and production efficiency is high, is applicable to producing fuel-cell catalyst in enormous quantities, has and significance fuel cell industrialization.

Description

A kind of preparation method of fuel-cell catalyst
Technical field
The present invention relates to field of fuel cell technology, be specifically related to a kind of preparation method of fuel-cell catalyst.
Background technology
Efficient as one, the eco-friendly TRT of fuel cell, in base station power, middle-size and small-size power station, electric motor car, stand-by power supply, portable power supplies etc., has broad application prospects.Fuel cell can be divided into Proton Exchange Membrane Fuel Cells, DMFC, alkaline fuel cell, SOFC, fuse salt fuel cell, microbiological fuel cell, biological fuel cell etc.Fuel cell is primarily of compositions such as end plate, collector plate, bipolar plates, membrane electrodes, and wherein membrane electrode is the core component of fuel cell, and catalyst is the cardiac component of membrane electrode.The catalyst of current comparative maturity is mainly carrier with carbon dust, loaded metal platinum.
Describe VulcanXC-72R carbon black in patent CN102810677A be carrier carry Pt catalyst (catalyst 1) and Ketjen carbon black for year Pt catalyst (catalyst 2) used in combination, add conventional Pt/C(VulcanXC-72R carbon black) specific area of catalyst, improve catalyst activity.But the Pt/C(Ketjen carbon black added) the Ketjen carbon black-supported specific area that uses of catalyst is large, particle diameter is little, difficulties in dispersion, ratio in Catalytic Layer shared by effecting reaction region is lower, the utilization rate of noble metal is also lower, and catalyst also more easily moves and reunites, along with the carrying out of electrochemical reaction simultaneously, the catalytic effect of catalyst weakens gradually, and battery efficiency reduces gradually.
Carbon dust is also the common carrier in fuel cell, adopts carbon dust to be that carrier mainly contains following shortcoming at present:
(1) metal platinum particles and carbon carrier adhesive force can reduce thereupon the use of battery, finally cause the generation of catalyst agglomeration phenomenon, cause the minimizing in membrane electrode life-span;
(2) the electrochemical corrosion resistant performance of carbon carrier can be more and more weak along with the use of battery, and last carbon carrier is etched electrochemically, and causes Catalytic Layer to be subsided, and causes membrane electrode hydraulic performance decline;
(3) surface area of carbon carrier is less, affects the speed of gas-liquid-solid three reaction, the contact surface of catalyst platinum atom and hydrogen is reduced, the catalytic efficiency of metal platinum can not be made to improve, cause the waste of noble metal platinum to a certain extent;
(4) because catalyst efficiency is lower, in order to reach the power density of demand, the consumption of meeting larger catalyst, and then increase the thickness of Catalytic Layer, add the internal resistance of membrane electrode, reduce the performance of membrane electrode, and then cause the power output of pile to decline.
Graphene has the material with carbon element being less than 10 layers of graphitic molecules layer structure, and specific area is high, and show very strong quantum effect, has good electronic conduction ability.Patent CN101814607A discloses a kind of preparation method of used in proton exchange membrane fuel cell platinum/graphen catalyst, it adopts Graphene to be carrier, with sodium borohydride or ethylene glycol for reducing agent, by graphite oxide and chloroplatinic acid Gong global, obtain a kind of used in proton exchange membrane fuel cell platinum/graphen catalyst.The method increase the stability of catalyst, but complex technical process, length consuming time.
Patent CN102000590B discloses the preparation method of a kind of fuel cell Graphene/FePt nanocatalyst; it take natural flake graphite as raw material; be oxidized by Hummers method and obtained graphite oxide; by graphite oxide, etc. the chloroplatinic acid of amount of substance together with ferric nitrate ultrasonic dissolution in deionized water; add hydrazine hydrate and regulate pH value of solution to 10 ~ 10.5 with ammoniacal liquor; oil bath heating at 120 DEG C; back flow reaction 2.5 ~ 3h under nitrogen protection; collecting precipitation also washs, and obtains Graphene/FePt nanocatalyst after drying.The method decreases the load capacity of noble metal platinum in fuel-cell catalyst to a certain extent, reduces the production cost of fuel cell.
Magnetron sputtering technique is widely used in field of film preparation, it utilizes magnetic field and electronic reciprocal effect, electronics is run in the shape of a spiral at target near surface, thus increases the probability that electronic impact argon gas produces ion, the ion produced hits target surface thus sputters target under electric field action.
Summary of the invention
Goal of the invention: for solving the technical problem existed in prior art, the present invention proposes a kind of preparation method of fuel-cell catalyst, can reduce catalyst amount, saves battery cost, reduces Catalytic Layer thickness, improves battery performance.
Technology contents: for realizing above-mentioned technical purpose, the present invention proposes a kind of preparation method of fuel-cell catalyst, comprises the steps:
A, prepare carrier film with adhesive layer: apply one deck silicone oil release layer respectively in two sides of release basement membrane, then a silicone oil release layer surface applies one deck adhesive layer more wherein;
B, vacuum magnetic-control sputtering graphite linings: preparation density is greater than 1.8g/cm 3, the nano-graphite target embryo that purity is greater than 99.99%, by vacuum magnetic-control sputtering technology, the nano-graphite target embryo of preparation is splashed to the adhesive layer surface of carrier film, form one deck graphite linings on carrier film surface, sputtering layer thickness is 10 ~ 30nm;
C, vacuum magnetic-control sputtering noble metal catalyst: produce platinum target embryo by pressurization fusion casting, make the density of platinum target embryo be greater than 20.5g/cm 3, purity is greater than 99.99%, and the graphite linings of carrier film sputters this platinum target embryo by vacuum magnetic-control sputtering technology, obtains the carrier film being loaded with noble metal catalyst, sputtering layer thickness is 1 ~ 3nm;
D, carrier of separating film: utilize stripping machine the carrier film being loaded with noble metal catalyst obtained in step C to be peeled off from release basement membrane; Cut into slices after rolling, obtain the carrier film section that section area is less than or equal to 4 square centimeters; The section of this carrier film is placed in cleaning agent and carries out ultrasonic cleaning, wash the adhesive layer on film surface, after having cleaned, at 100 ~ 120 DEG C, carry out vacuum drying;
E, pulverizing: use micropowder grinding that the carrier film obtained in step e section is ground into the particle of 0.2-3 μm;
F, carbonization: the particle obtained in step e is put into retort, under the protection of argon gas or nitrogen, at 600 DEG C ~ 1300 DEG C, carbonization obtains fuel-cell catalyst in 30 ~ 120 minutes.
Wherein, the making material of described release basement membrane is selected from PET(PETG), PVC(polyvinyl chloride), PC(Merlon), PEN(PEN), PA(polyamide) and PI(polyimides) in any one, be preferably PET film.
The making material of described adhesive layer be selected from acrylic compounds, polyurethanes and silica type any one, be preferably silica type.
The thickness of described release basement membrane is 15 ~ 250 μm; The thickness of described silicone oil release layer is 1 ~ 5 μm; The thickness of described adhesive layer is 2 ~ 10 μm.Preferably, the thickness of described release basement membrane is 150 μm; The thickness of described silicone oil release layer is 3 μm; The thickness of described adhesive layer is 2 μm.
Wherein, in step B; the preparation method of graphite target embryo is as follows: 10 ~ 100 Nano graphite powders are mixed into phenolic resins powder; the weight ratio of Nano graphite powder and phenolic resins powder is 20:(1 ~ 5); under 320 ~ 370 DEG C of constant temperature; dispersed with stirring becomes lotion material; target idiosome is made by forming machine; the idiosome made is inserted mould; be semi-finished product target embryo at 500 ~ 1000 tons of forming under the pressure; semi-finished product target embryo is put into high temperature sintering furnace, and high temperature sintering 15 ~ 30 minutes under 1500 ~ 1700 DEG C of nitrogen or argon shield, makes nano-graphite target embryo.By high-pressure molding and high temperature sintering, contribute to improving graphite target density, improve sputtering uniformity.
Particularly, the vacuum magnetic-control sputtering technology described in step B or C is magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology.
Sputtering condition in step B or C is: pressure 0.5 ~ 3Pa; Sputtering power 5 ~ 20W/cm 2; Sputtering working gas is argon gas, gas flow 10 ~ 20mL/min per minute.
Cleaning agent described in step D is butanone or ethyl acetate.
Beneficial effect: compared with prior art, fuel-cell catalyst preparation method tool of the present invention has the following advantages:
(1) vacuum sputtering is adopted to be splashed in carrier film by graphite and noble metal catalyst, improve the adhesive force of metal platinum on graphite support particles, improve catalyst life, catalyst activity is strengthened, catalytic efficiency is high, thus reduce the use of fuel cell noble metal, greatly reduce the production cost of fuel cell.
(2) production technology is simple, and production efficiency is high, is applicable to producing fuel-cell catalyst in enormous quantities, has and significance fuel cell industrialization.
Accompanying drawing explanation
Fig. 1 is the structural representation of carrier film of the present invention.
Fig. 2 is the polarization curve of fuel-cell catalyst of the present invention.
Fig. 3 is the power density curve map of fuel-cell catalyst of the present invention.
Fig. 4 is the polarization curve of JohnsonMatthey catalyst.
Fig. 5 is the power density curve map of JohnsonMatthey catalyst.
Fig. 6 is vacuum magnetic-control sputtering schematic diagram.
Detailed description of the invention
In following examples the purchase source of material therefor and model as follows:
Platinum: (SUMITOMO CHEMICAL metal), vacuum magnetic-control sputtering equipment (Japanese ULVACspt500 type, platinum target).
embodiment 1the preparation of graphite target embryo and platinum target embryo.
The preparation of graphite target embryo: get commercially available 10 ~ 100 Nano graphite powder 20KG; be mixed into 1 ~ 5KG commercial phenolic resin powder; under 350 degrees Celsius of constant temperature; dispersed with stirring becomes lotion material; 20mm is made thick by forming machine; 125mm is wide; the long target idiosome of 600mm; the idiosome made is inserted mould, and be that 10 ~ 15mm is thick at 500 ~ 1000 tons of forming under the pressure, 125mm is wide; the semi-finished product target embryo that 600mm is long; semi-finished product target embryo is put into high temperature sintering furnace, and under 1600 degrees Celsius of nitrogen or argon shield, high temperature sintering 15 ~ 30 minutes, makes nano-graphite sputtering target material.By high-pressure molding and high temperature sintering, contribute to improving graphite target density, improve sputtering uniformity.
The preparation of platinum target embryo: produce platinum target embryo by pressurization fusion casting, be of a size of 300 × 100 × 2mm, make the density of platinum target embryo be greater than 20.5g/cm 3, purity is greater than 99.99%.
embodiment 2
A preparation method for fuel-cell catalyst, comprises the steps:
(1) preparation is with the carrier film of adhesive layer: apply one deck silicone oil release layer respectively in two sides of the release basement membrane of PET (thickness is 150 μm), thickness is 3 μm, then a silicone oil release layer surface applies one deck adhesive layer more wherein, and the material of adhesive layer is silica gel, and thickness is 2 μm, obtain carrier film, as shown in Figure 1, wherein, 1-1 is release basement membrane, 1-2 is silicone oil release layer, and 1-3 is adhesive layer;
(2) vacuum magnetic-control sputtering graphite linings: under the pressure of 1Pa, graphite target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed on the adhesive layer of carrier film, the adhesive layer of carrier film sputters easy layer graphite linings, sputtering layer thickness is 15nm, and sputtering power is 10W/cm 2, sputtering working gas is argon gas, gas flow 15ml/min;
(3) vacuum magnetic-control sputtering noble metal catalyst: under the pressure of 1Pa, platinum target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed in the graphite linings of carrier film, sputtering layer thickness is 2nm, and sputtering power is 15W/cm 2, sputtering working gas is argon gas, and gas flow 15ml/min obtains the carrier film sputtering noble metal catalyst;
As shown in Figure 6, wherein, 1 is carrier film to the principle of Vacuum Magnetic sputtering, and 2 is nano-graphite target embryo, and 3 is platinum target embryo, and 4 is vacuum chamber, and 5 is deflector roll.First the carrier film 1 processed is drawn the vacuum cavity 4 being from left to right introduced into sputtering graphite linings through deflector roll 5, carry out sputtering graphite linings, then enter splash-proofing sputtering metal platinum layer vacuum cavity 4, carry out splash-proofing sputtering metal platinum layer on the surface of graphite linings.Catalyst film after having sputtered draws through deflector roll 5, then carries out rolling, proceeds to subsequent processing after rolling completes.
(4) carrier of separating film: utilize stripping machine to have the carrier film of noble metal catalyst to peel off from release basement membrane the sputtering obtained in step (3); Cut into slices after rolling, obtain the carrier film section that section area is less than or equal to 4 square centimeters; The film section this being loaded with catalyst is placed in ethyl acetate carries out ultrasonic cleaning, washes the adhesive layer on film surface, carries out vacuum drying after having cleaned at 120 DEG C.
(5) pulverize: use micropowder grinding that the carrier film obtained in step (4) section is ground into the particle of 0.5 micron;
(6) particle after pulverizing in step (5) is put into retort, under the protection of argon gas or nitrogen, at 1100 DEG C, carbonization obtains fuel-cell catalyst in 100 minutes.
embodiment 3
A preparation method for fuel-cell catalyst, comprises the steps:
(1) preparation is with the carrier film of adhesive layer: apply one deck silicone oil release layer respectively in two sides of the release basement membrane of PET (thickness is 100 μm), thickness is 3 μm, then a silicone oil release layer surface applies one deck adhesive layer more wherein, and the material of adhesive layer is acrylic compounds glue, and thickness is 5 μm, obtain carrier film, as shown in Figure 1, wherein, 1-1 is release basement membrane, 1-2 is silicone oil release layer, and 1-3 is adhesive layer;
(2) vacuum magnetic-control sputtering graphite linings: under the pressure of 1Pa, graphite target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed on the adhesive layer of carrier film prepared by step (1), adhesive layer sputters one deck graphite linings, sputtering layer thickness is 20nm, and sputtering power is 15W/cm 2, sputtering working gas is argon gas, gas flow 20ml/min;
(3) vacuum magnetic-control sputtering noble metal catalyst: under the pressure of 1Pa, platinum target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed in the graphite linings of carrier film prepared by step (2), sputtering layer thickness is 3nm, and sputtering power is 15W/cm 2, sputtering working gas is argon gas, and gas flow 15ml/min obtains the carrier film sputtering noble metal catalyst;
(4) carrier of separating film: utilize stripping machine to have the carrier film of noble metal catalyst to peel off from release basement membrane the sputtering obtained in step (3); Cut into slices after rolling, obtain the carrier film section that section area is less than or equal to 4 square centimeters; The film section this being loaded with catalyst is placed in ethyl acetate carries out ultrasonic cleaning, washes the adhesive layer on film surface, carries out vacuum drying after having cleaned at 120 DEG C.
(5) pulverize: use micropowder grinding that the carrier film obtained in step (4) section is ground into the particle of 1.0 microns;
(6) particle after pulverizing in step (5) is put into retort, under the protection of argon gas or nitrogen, at 1200 DEG C, carbonization obtains fuel-cell catalyst in 120 minutes.
embodiment 4
A preparation method for fuel-cell catalyst, comprises the steps:
(1) preparation is with the carrier film of adhesive layer: apply one deck silicone oil release layer respectively in two sides of the release basement membrane of PEN (thickness is 200 μm), thickness is 4 μm, then a silicone oil release layer surface applies one deck adhesive layer more wherein, and the material of adhesive layer is polyurethane material, and thickness is 8 μm, obtain carrier film, as shown in Figure 1, wherein, 1-1 is release basement membrane, 1-2 is silicone oil release layer, and 1-3 is adhesive layer;
(2) vacuum magnetic-control sputtering graphite linings: under the pressure of 2Pa, graphite target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed on the adhesive layer of carrier film prepared by step (1), the adhesive layer of carrier film sputters one deck graphite linings, sputtering layer thickness is 25nm, and sputtering power is 20W/cm 2, sputtering working gas is argon gas, gas flow 20ml/min;
(3) vacuum magnetic-control sputtering noble metal catalyst: under the pressure of 2Pa, platinum target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed in the graphite linings of carrier film prepared by step (2), sputtering layer thickness is 1.5nm, and sputtering power is 20W/cm 2, sputtering working gas is argon gas, and gas flow 20ml/min obtains the carrier film sputtering noble metal catalyst;
(4) carrier of separating film: utilize stripping machine to have the carrier film of noble metal catalyst to peel off from release basement membrane the sputtering obtained in step (3); Cut into slices after rolling, obtain the carrier film section that section area is less than or equal to 4 square centimeters; The film section this being loaded with catalyst is placed in butanone carries out ultrasonic cleaning, washes the adhesive layer on film surface, carries out vacuum drying after having cleaned at 120 DEG C.
(5) pulverize: use micropowder grinding that the carrier film obtained in step (4) section is ground into the particle of 1.5 microns;
(6) particle after pulverizing in step (5) is put into retort, under the protection of argon gas or nitrogen, at 1300 DEG C, carbonization obtains fuel-cell catalyst in 120 minutes.
embodiment 5
A preparation method for fuel-cell catalyst, comprises the steps:
(1) preparation is with the carrier film of adhesive layer: apply one deck silicone oil release layer respectively in two sides of the release basement membrane of PA (thickness is 80 μm), thickness is 3 μm, then a silicone oil release layer surface applies one deck adhesive layer more wherein, and the material of adhesive layer is acrylic acid, and thickness is 5 μm, obtain carrier film, as shown in Figure 1, wherein, 1-1 is release basement membrane, 1-2 is silicone oil release layer, and 1-3 is adhesive layer;
(2) vacuum magnetic-control sputtering graphite linings: under the pressure of 1.5Pa, graphite target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed on the adhesive layer of carrier film 1, adhesive layer sputters one deck graphite linings, sputtering layer thickness is 15nm, and sputtering power is 15W/cm 2, sputtering working gas is argon gas, gas flow 20ml/min;
(3) vacuum magnetic-control sputtering noble metal catalyst: under the pressure of 2Pa, platinum target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed in the graphite linings of carrier film prepared by step (2), sputtering layer thickness is 2nm, and sputtering power is 20W/cm 2, sputtering working gas is argon gas, and gas flow 20ml/min obtains the carrier film sputtering noble metal catalyst;
(4) carrier of separating film: utilize stripping machine to have the carrier film of noble metal catalyst to peel off from release basement membrane the sputtering obtained in step (3); Cut into slices after rolling, obtain the carrier film section that section area is less than or equal to 4 square centimeters; The film section this being loaded with catalyst is placed in ethyl acetate carries out ultrasonic cleaning, washes the adhesive layer on film surface, carries out vacuum drying after having cleaned at 120 DEG C.
(5) pulverize: use micropowder grinding that the carrier film obtained in step (4) section is ground into the particle of 2 microns;
(6) particle after pulverizing in step (5) is put into retort, under the protection of argon gas or nitrogen, at 1300 DEG C, carbonization obtains fuel-cell catalyst in 120 minutes.
embodiment 6
A preparation method for fuel-cell catalyst, comprises the steps:
(1) preparation is with the carrier film of adhesive layer: apply one deck silicone oil release layer respectively in two sides of the release basement membrane of PI (thickness is 50 μm), thickness is 2 μm, then a silicone oil release layer surface applies one deck adhesive layer more wherein, and the material of adhesive layer is acrylic acid, and thickness is 3 μm, obtain carrier film, as shown in Figure 1, wherein, 1-1 is release basement membrane, 1-2 is silicone oil release layer, and 1-3 is adhesive layer;
(2) vacuum magnetic-control sputtering graphite linings: under the pressure of 1.5Pa, graphite target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed on the adhesive layer of carrier film, make the adhesive layer of carrier film sputters one deck graphite linings, sputtering layer thickness is 12nm, and sputtering power is 20W/cm 2, sputtering working gas is argon gas, gas flow 15ml/min;
(3) vacuum magnetic-control sputtering noble metal catalyst: under the pressure of 1.5Pa, platinum target embryo embodiment 1 prepared by magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology is splashed in the graphite linings of carrier film, sputtering layer thickness is 2nm, and sputtering power is 20W/cm 2, sputtering working gas is argon gas, and gas flow 15ml/min obtains the carrier film sputtering noble metal catalyst;
(4) carrier of separating film: utilize stripping machine to have the carrier film of noble metal catalyst to peel off from release basement membrane the sputtering obtained in step (3); Cut into slices after rolling, obtain the carrier film section that section area is less than or equal to 4 square centimeters; The film section this being loaded with catalyst is placed in ethyl acetate carries out ultrasonic cleaning, washes the adhesive layer on film surface, carries out vacuum drying after having cleaned at 120 DEG C.
(5) pulverize: use micropowder grinding that the carrier film obtained in step (4) section is ground into the particle of 0.8 micron;
(6) particle after pulverizing in step (5) is put into retort, under the protection of argon gas or nitrogen, at 800 DEG C, carbonization obtains fuel-cell catalyst in 120 minutes.
embodiment 7catalytic performance is tested.
The testing procedure of catalyst catalytic performance is as follows:
(1) catalyst embodiment of the present invention 1 prepared mixes according to the ratio that mass ratio is 7:3 with nafion solution (du pont company), and adds appropriate ethanol and disperse, and is mixed with catalyst pulp;
(2) catalyst pulp will prepared, is coated in the both sides of 211 proton membranes respectively, and coated weight is according to two-sided platinum carrying capacity 0.25mg/cm 2standard carry out, make CCM;
(3) cut the area of one piece of 5*5cm from ready-made CCM, be placed on inside membrane electrode performance test fixture, carry out catalyst performance test;
(4) fuel cell special electronic load (150V/600W, Nanjing Zhong Yingrui instrument Electronics Co., Ltd.) is used to test, test condition: Hydrogen Vapor Pressure 40KPa, air 10 ~ 20KPa, room temperature 20 ± 2 DEG C.The polarization curve of detecting catalyst and power density curve, result as shown in Figures 2 and 3.
Use JohnsonMatthey catalyst sample as a comparison, concrete test operating procedure is also identical, and result as shown in Figure 4 and Figure 5.Contrast finds that the catalyst performance prepared by the present invention will exceed at least 70% than commercially available JohnsonMatthey catalyst performance by experiment.

Claims (7)

1. a preparation method for fuel-cell catalyst, is characterized in that, comprises the steps:
A, prepare carrier film (1) with adhesive layer: apply one deck silicone oil release layer (1-2) respectively in two sides of release basement membrane (1-1), then silicone oil release layer (1-2) surface applies one deck adhesive layer (1-3) more wherein, obtains carrier film (1);
B, vacuum magnetic-control sputtering graphite linings: preparation density is greater than 1.8g/cm 3the nano-graphite target embryo (2) that purity is greater than 99.99%, by vacuum magnetic-control sputtering technology, the nano-graphite target embryo (2) of preparation is splashed to adhesive layer (1-3) surface of carrier film (1), form one deck graphite linings on carrier film (1) surface, sputtering layer thickness is 10 ~ 30nm; Wherein, the preparation method of graphite target embryo is as follows: 10 ~ 100 Nano graphite powders are mixed into phenolic resins powder, the weight ratio of Nano graphite powder and phenolic resins powder is 20: (1 ~ 5), under 320 ~ 370 DEG C of constant temperature, dispersed with stirring becomes lotion material, target idiosome is made by forming machine, the idiosome made is inserted mould, be semi-finished product target embryo at 500 ~ 1000 tons of forming under the pressure, semi-finished product target embryo is put into high temperature sintering furnace, high temperature sintering 15 ~ 30 minutes under 1500 ~ 1700 DEG C of nitrogen or argon shield, makes nano-graphite target embryo;
C, vacuum magnetic-control sputtering noble metal catalyst: produce platinum target embryo (3) by pressurization fusion casting, make the density of platinum target embryo (3) be greater than 20.5g/cm 3, purity is greater than 99.99%, and the graphite linings of carrier film (1) sputters this platinum target embryo (3) by vacuum magnetic-control sputtering technology, and obtain the carrier film (1) being loaded with noble metal catalyst, sputtering layer thickness is 1 ~ 3nm;
D, carrier of separating film (1): utilize stripping machine the carrier film (1) being loaded with noble metal catalyst obtained in step C to be peeled off from release basement membrane (1-1); Cut into slices after rolling, obtain the carrier film section that section area is less than or equal to 4 square centimeters; The section of this carrier film is placed in cleaning agent and carries out ultrasonic cleaning, wash the adhesive layer (1-3) on film surface, after having cleaned, at 100 ~ 120 DEG C, carry out vacuum drying;
E, pulverizing: use micropowder grinding that the carrier film obtained in step D section is ground into the particle of 0.2-3 μm;
F, carbonization: the particle obtained in step e is put into retort, under the protection of argon gas or nitrogen, at 600 DEG C ~ 1300 DEG C, carbonization obtains fuel-cell catalyst in 30 ~ 120 minutes.
2. the preparation method of fuel-cell catalyst according to claim 1, is characterized in that, the making material of described release basement membrane (1-1) be selected from PET, PVC, PC, PEN, PA and PI any one.
3. the preparation method of fuel-cell catalyst according to claim 1, is characterized in that, the making material of described adhesive layer (1-3) be selected from acrylic compounds, polyurethanes and silica type any one.
4. the preparation method of fuel-cell catalyst according to claim 1, is characterized in that, the thickness of described release basement membrane (1-1) is 15 ~ 250 μm; The thickness of described silicone oil release layer (1-2) is 1 ~ 5 μm; The thickness of described adhesive layer (1-3) is 2 ~ 10 μm.
5. the preparation method of fuel-cell catalyst according to claim 1, is characterized in that, the vacuum magnetic-control sputtering technology described in step B or C is magnetically controlled DC sputtering technology or medium frequency magnetron sputtering technology.
6. the preparation method of fuel-cell catalyst according to claim 1, is characterized in that, the sputtering condition in step B or C is: pressure 0.5 ~ 3Pa; Sputtering power 5 ~ 20W/cm 2; Sputtering working gas is argon gas, gas flow 10 ~ 20mL/min per minute.
7. the preparation method of fuel-cell catalyst according to claim 1, is characterized in that, the cleaning agent described in step D is butanone or ethyl acetate.
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Thin-film catalyst layers for polymer electrolyte fuel cell electrodes;M.S.WILSON等;《JOURNAL OF APPLIED ELECTROCHEMISTRY》;19921231;第22卷;第1-7页 *

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