CN106099145B - The preparation method and its preparation facilities of one proton exchanging film fuel battery and membrane electrode - Google Patents
The preparation method and its preparation facilities of one proton exchanging film fuel battery and membrane electrode Download PDFInfo
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- CN106099145B CN106099145B CN201610727327.8A CN201610727327A CN106099145B CN 106099145 B CN106099145 B CN 106099145B CN 201610727327 A CN201610727327 A CN 201610727327A CN 106099145 B CN106099145 B CN 106099145B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M2008/1095—Fuel cells with polymeric electrolytes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The present invention provides the preparation methods and its preparation facilities of a kind of Proton Exchange Membrane Fuel Cells of fine tubular structure and membrane electrode.Tube-shaped proton exchanging film material is prepared with proton exchange membrane resin solution;It is equipped with cathode and anode catalyst pulp;Using anode, cathode inks, anode and cathode Catalytic Layer is prepared in the heating tube outer surface peace plate surface for posting PTFE film respectively;Tube-shaped proton exchanging film is covered in above-mentioned heating tube outer surface;Plate collapses in the outer surface of heating tube;Entirety is fitted into tubular type pressure apparatus;Under certain temperature and pressure, hot pressing obtains fine tubulose membrane electrode of fuel batter with proton exchange film;It is fitted into after cutting in fuel cell fixture and obtains tubular proton exchange membrane fuel cell.When the Proton Exchange Membrane Fuel Cells with microcapillary structure works, the fuel gas (hydrogen) and oxidant (air or oxygen) of reaction have respectively entered pipe internal channel and pipe outer wall, and contacted with catalyst, electrochemical reaction occurs and produces electricl energy.
Description
Technical field
The invention belongs to fuel cell preparation fields, and in particular to a kind of microminiature has the proton friendship of fine tubular structure
Change the preparation method and its preparation facilities of membrane cell and membrane electrode.
Background technique
In the latest 20 years, it since Proton Exchange Membrane Fuel Cells has the characteristics that energy efficiency height, cleanliness without any pollution, and obtains
It obtained extensive research concern and rapidly developed.Proton Exchange Membrane Fuel Cells can be applied to power battery and the distribution of electric car
Formula power station, while the emphasis of exploitation is also become in terms of microminiature, it is mainly used for such as mobile phone, laptop portable electric
Source.However, the characteristics of compact battery has its own, if minimizing fuel cell using traditional battery material and structure
There is very big difficulty, it is therefore desirable to be innovated.
The core component of Proton Exchange Membrane Fuel Cells is membrane electrode, usually applies catalysis in the two sides of proton exchange membrane
There are gas diffusion layers and bipolar plates in layer, Catalytic Layer two sides, form " sandwich " structure.In terms of small fuel cell, power is close
Degree is far below large-scale bipolar plate structure fuel cell.There are some new technology roads at the small-sized aspect of fuel cell at present
Line is mainly based upon mechanical micro Process and microelectric technique.Wherein more representational is to process skill using semi-conductor silicon chip
Art, the technology use porous silicon chip made from microelectric technique as battery support, and the metals such as copper or gold are sputtered on silicon wafer
Thin layer enhances conductive capability, reduces the size of battery in this way, improves the power density of battery, convenient for batch production.But
It is at present no matter from technical standpoint or from cost consideration, there are still many problems, and power density is still reached to less than business
The requirement of change.
Summary of the invention
The purpose of the invention is to make up the deficiencies in the prior art, providing a kind of microminiature has fine tubular structure
Proton Exchange Membrane Fuel Cells and membrane electrode preparation method and its preparation facilities, the microminiature fuel cell provided is using micro-
Thin tube-like proton exchange membrane substantially increases specific surface area, increases catalytic reaction zone domain, reduces battery volume, shortens biography
Guiding path is conducive to mass transfer.Aqueous vapor shortened channel is conducive to simplify the water management of fuel cell generation.
In order to reach the purpose of the present invention, technical solution is as follows:A kind of fine tubular proton exchange membrane fuel cell and film
The preparation method of electrode, which is characterized in that including step:
1), using proton exchange membrane resin solution, application template method prepares tube-shaped proton exchanging film material;
2) cathode inks, Anode inks, are equipped with;
3), using Anode inks, anode catalyst layer is prepared in the heating tube outer surface for posting PTFE film, uses yin
Electrode catalyst slurry prepares cathode catalysis layer in the planar surface for posting PTFE film;
4), tube-shaped proton exchanging film is covered in the heating tube outer surface for being prepared with anode catalyst layer;
5), the plate for being prepared with cathode catalysis layer is collapsed in the outer surface of step 4) tube-shaped proton exchanging film afterwards;
6), the tubular type pressure apparatus for thering is the heating tube of plate to be fitted into step 5 volume;
It 7) will include, that the temperature control system of electrically heated rod and thermocouple is fitted into heating tube hollow space, and passes through
The screw torque of tubular type pressure apparatus is controlled to control pressure, controls temperature between 100 DEG C~150 DEG C, pressure 0.05~
Between 0.1MPa, hot pressing obtains fine tubulose membrane electrode of fuel batter with proton exchange film;
8) tubulose membrane electrode, is cut into required size, is fitted into fuel cell fixture and obtains tube-shaped proton exchanging film
Fuel cell or battery pile.Preferably, proton exchange membrane resin solution is Nafion solution of the concentration in 1wt%~10wt%.
Preferably, the template for preparing tube-shaped proton exchanging film is column glass template, column glass template outer diameter
Between 0.5mm~2mm, length prepares the tubulose in the step 4) between 1cm~10cm, using the tape casting
Proton exchange membrane, prepared tube-shaped proton exchanging film internal diameter is between 0.5mm~2mm, and length is between 1cm~10cm.
Preferably, provisioned catalyst pulp is the mixture of catalyst, proton exchange membrane resin solution and dispersing agent,
It is carried out using ultrasonic disperse and paddling process evenly dispersed;It is equipped in catalyst pulp, catalyst used is business Pt/C catalysis
Agent, for Pt content between 20wt%~60wt%, resin solution used is the resin solution of corresponding proton exchange membrane;Dispersion used
Agent is the mixing of one or more of deionized water, ethyl alcohol, isopropanol, and dispersing agent adds volume and addition proton exchange membrane tree
The volume ratio of lipoprotein solution is 10:1~20:Between 1;During catalyst pulp is equipped with:In catalyst and proton exchange membrane resin solution
The mass ratio of dried resin is 3:1~4:Between 1.
Preferably, it is prepared respectively using spread coating or spray coating method in the heating tube outer surface peace plate surface for posting PTFE film
Anode and cathode Catalytic Layer, catalyst loading is in 0.1~0.5mg/cm2Between, pipe outside diameter is heated between 0.5mm~2mm,
Length is between 1cm~10cm, and sheet width is between 0.5mm~2mm, and length is between 1cm~10cm.
Preferably, in the step 5), the specific steps are:The plate of cathode catalysis layer is prepared with along wide
Degree direction, catalyst inwardly collapse into tubulose, and cover in the outer surface of tube-shaped proton exchanging film.Preferably, step
8) tubulose membrane electrode is cut into size of the length between 1mm~10mm in.Tubulose membrane electrode is cut into required size after sunlight,
It is fitted into fuel cell fixture and obtains tubulose proton
Exchange film fuel battery.When the Proton Exchange Membrane Fuel Cells with microcapillary structure works, the fuel of reaction
Gas (hydrogen) and oxidant (air or oxygen) have respectively entered pipe internal channel and pipe outer wall, and contact with catalyst, and electricity occurs
It chemically reacts and produces electricl energy.
A kind of preparation facilities of fine tubular proton exchange membrane fuel cell and membrane electrode, which is characterized in that including tubular type
Pressure apparatus, heating tube and plate, heating tube is for making anode catalyst layer, and heating tube is cylindrical structure, and heating tube
Center tool
There is hollow space, plate is flat shape and can collapse, and plate is for making cathode catalysis layer, tubular type pressure dress
There is the outwardly extending compression piece of two panels on the side wall set, compress on piece and spiral shell is installed
Two panels can be compressed piece and is tightly pressed together by bolt, bolt, and the center of tubular type pressure apparatus has cavity.Preferably,
It is characterized in that, tubular type pressure apparatus internal diameter is 0.5mm~2mm, and length is 1cm~10cm.
The device have the advantages that:Using fine tubular fuel cell and membrane electrode of the invention preparation method and
Its preparation facilities realizes the preparation of micro-tubular structure Proton Exchange Membrane Fuel Cells.It is big by using fine tube-shaped proton exchanging film
Specific surface area is improved greatly, catalytic reaction zone domain is increased, reduces battery volume, shortens conducting path, be conducive to mass transfer.
Aqueous vapor shortened channel is conducive to simplify the water management of fuel cell generation.Microminiature proton exchange is greatly improved to realize
Membrane cell power generation performance improves volume and quality specific power and simplifies the purpose of battery system management.These performances
It improves, it will be so that fuel cell more has competitiveness in portable electric source domain.At present for portable power, whether hand
Machine or laptop, the service life of battery are to restrict its critical issue for further developing and influencing its competitiveness.Match
With suitable hydrogen source, the fuel cell of high-energy density will use the time with longer than lithium ion battery, and not need
Charging, it is only necessary to it replaces hydrogen source (hydrogen container or other), it is more convenient to use.
Method described in the invention patent is not limited only to the preparation of Nafion membrane and membrane electrode in citing, according to this patent
Provided method can be expanded to the fuel cell membrane electrode preparation based on other business proton exchange membrane.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of heating tube in preparation facilities of the present invention.
Fig. 2 is the structural schematic diagram of plate in preparation facilities of the present invention.
Fig. 3 is that heating tube winds the structural schematic diagram after plate;
Fig. 4 is the structural schematic diagram of tubular type pressure apparatus.
Specific embodiment
The present invention will be further described below with reference to examples, but protection scope of the present invention is not limited solely to implement
Example.
In conjunction with shown in Fig. 1-Fig. 4,
A kind of preparation facilities of fine tubular proton exchange membrane fuel cell and membrane electrode, including tubular type pressure apparatus 3, plus
Heat pipe 1 and plate 2.
For heating tube 1 for making anode catalyst layer, heating tube 1 is cylindrical structure, and during the center of heating tube has
Empty part 1-1, hollow space 1-1 are for placing the temperature control systems such as electrically heated rod and thermocouple.
Plate 2 is flat shape and can collapse that plate 2 is for making cathode catalysis layer, the side wall of tubular type pressure apparatus 3
It is upper that there is the outwardly extending compression piece 3-3 of two panels, it compresses on piece and bolt 3-2 is installed, two panels can be compressed piece and is pressed on by bolt
Together, the center of tubular type pressure apparatus 3 has cavity 3-1, controls pressure by control bolt torque.It, will be in Fig. 3 when assembly
The heating tube for being wound with plate is placed in cavity 3-1, screwing bolts, and the side wall of tubular type pressure apparatus applies heating tube and plate
Pressure.
Embodiment 1:
1. prepared by tube-shaped proton exchanging film:The Nafion solution 2ml that concentration is 5wt% is weighed, with outer diameter is 2mm, length
It is template for the column glass of 2cm, the tape casting is used to prepare the tube-shaped proton exchanging film that internal diameter is 2cm for 2mm, length;
2. prepared by anode catalyst layer slurry:0.4mg60%Pt/C catalyst is weighed to be put into small beaker, be added 2ml go from
Sub- water simultaneously stirs, and 2mg5%Nafion solution is added in whipping process, is uniformly mixed after agitated, sonic oscillation mixing
Anode catalyst layer slurry;
3. prepared by cathode catalysis layer slurry:The 0.4mg60%Pt/C catalyst that weighs similar with step 2 is put into small beaker,
2ml deionized water is added and stirs, 2.6mg5%Nafion solution, agitated, sonic oscillation mixing are added in whipping process
Uniformly mixed cathode catalysis layer slurry is obtained afterwards;
4. prepared by anode side catalyst layer:Using outer surface to post the outer diameter of PTFE film as 2mm, length is 2cm in Fig. 1
Shown in heating tube, the anode catalyst layer slurry configured in step 2 is sprayed under the conditions of 100 DEG C using the method for spraying
It is applied to the outer surface of heating tube, the loading of Pt/C catalyst is 0.5mg/cm2, anode side catalyst layer is completed to prepare;5.
The preparation of cathode side catalyst layer:The plate matched in Fig. 2 that the width for posting PTFE film is 2cm for 2mm, length is used, with step 4 class
Seemingly, the cathode catalysis layer slurry configured in step 3 PTFE has been sprayed under the conditions of 100 DEG C using the method for spraying
The planar surface of pad pasting, the loading of Pt/C catalyst are 0.5mg/cm2, cathode side catalyst layer is completed to prepare;
6. the set of tube-shaped proton exchanging film obtained in step 1 is prepared in step 4 outside the heating tube of anode catalyst layer
Surface;
7. the plate for being prepared with cathode catalysis layer obtained in step 5 is prolonged width direction, catalyst inwardly collapses into pipe
Shape, and cover in the outer surface of step 6;
8. temperature control system (including electrically heated rod and thermocouple) to be fitted into the hollow portion of heating tube in step 6
Point;
9. being fitted into step 8 with tubular type pressure apparatus shown in Fig. 4, tubular type pressure apparatus internal diameter is 2mm, and length is
2cm;
10. hot pressing obtains fine tubulose membrane electrode of fuel batter with proton exchange film under the conditions of 140 DEG C, 0.05MPa;
11. the tubulose membrane electrode that step 10 Len got is 2cm is cut into tubulose membrane electrode 4 that length is 5mm, it is complete
At the preparation of microminiature membrane electrode of fuel batter with proton exchange film.
Embodiment 2:
1. prepared by tube-shaped proton exchanging film:The Nafion solution 3ml that concentration is 5.5wt% is weighed, with outer diameter is 1mm, length
The column glass that degree is 1cm is template, and the tape casting is used to prepare the tube-shaped proton exchanging film that internal diameter is 1cm for 1mm, length;
2. prepared by anode catalyst layer slurry:It weighs 0.08mg40%Pt/C catalyst to be put into small beaker, 1ml ethyl alcohol is added
And stir, 0.5mg5%Nafion solution is added in whipping process, is obtained after agitated, sonic oscillation mixing uniformly mixed
Anode catalyst layer slurry;
3. prepared by cathode catalysis layer slurry:The 0.08mg40%Pt/C catalyst that weighs similar with step 2 is put into small beaker,
1ml ethyl alcohol is added and stirs, 0.56mg5%Nafion solution is added in whipping process, after agitated, sonic oscillation mixing
To uniformly mixed cathode catalysis layer slurry;
4. prepared by anode side catalyst layer:Using outer surface to post the outer diameter of PTFE film as 1mm, length is 1cm in Fig. 1
Shown in heating tube, the anode catalyst layer slurry configured in step 2 is sprayed under the conditions of 90 DEG C using the method for spraying
It is applied to the outer surface of heating tube, the loading of Pt/C catalyst is 0.4mg/cm2, anode side catalyst layer is completed to prepare;
5. prepared by cathode side catalyst layer:Using the width for posting PTFE film for 1mm, length is 1cm with flat in Fig. 2
Plate, it is similar with step 4, utilize the method for spraying under the conditions of 90 DEG C by it in cathode catalysis layer slurry configured in step 3
It is sprayed at the planar surface of PTFE pad pasting, the loading of Pt/C catalyst is 0.4mg/cm2, urged to prepare and complete cathode side
Change layer;
6. the set of tube-shaped proton exchanging film obtained in step 1 is prepared in step 4 outside the heating tube of anode catalyst layer
Surface;
7. the plate for being prepared with cathode catalysis layer obtained in step 5 is prolonged width direction, catalyst inwardly collapses into pipe
Shape, and cover in the outer surface of step 6;
8. temperature control system (including electrically heated rod and thermocouple) to be fitted into the hollow portion of heating tube in step 6
Point;
9. being fitted into step 8 with tubular type pressure apparatus shown in Fig. 4, tubular type pressure apparatus internal diameter is 1mm, and length is
1cm;
10. hot pressing obtains fine tubulose membrane electrode of fuel batter with proton exchange film under the conditions of 140 DEG C, 0.06MPa;
11. the tubulose membrane electrode that step 10 Len got is 1cm is cut into tubulose membrane electrode 5 that length is 2mm, it is complete
At the preparation of microminiature membrane electrode of fuel batter with proton exchange film.
It should be noted that after sunlight:Above embodiments are only to illustrate the present invention and not limit technology described in the invention
Scheme, therefore, although this specification is referring to above-mentioned each embodiment, the present invention has been described in detail, this
Field it is to be appreciated by one skilled in the art that still can modify to the present invention or equivalent replacement, and all do not depart from this
The technical solution and its improvement of the spirit and scope of invention, should all cover within the scope of the claims of the present invention.
Claims (8)
1. a kind of preparation method of fine tubular proton exchange membrane fuel cell, which is characterized in that including step:
1), using proton exchange membrane resin solution, application template method prepares tube-shaped proton exchanging film;
2) cathode inks, Anode inks, are equipped with;
3), using Anode inks, anode catalyst layer is prepared in the heating tube outer surface for posting PTFE film, is urged using cathode
Agent slurry prepares cathode catalysis layer in the planar surface for posting PTFE film;
4), tube-shaped proton exchanging film is covered in the heating tube outer surface for being prepared with anode catalyst layer;
5), the plate for being prepared with cathode catalysis layer is collapsed in the outer surface of step 4) tube-shaped proton exchanging film afterwards;
6), the heating tube that step 5 volume has plate is assembled in tubular type pressure apparatus;
It 7) will include, that the temperature control system of electrically heated rod and thermocouple is fitted into heating tube hollow space, and passes through control
The screw torque of tubular type pressure apparatus controls pressure, controls temperature between 100 DEG C~150 DEG C, pressure 0.05~
Between 0.1MPa, hot pressing obtains fine tubulose membrane electrode of fuel batter with proton exchange film;
8) tubulose membrane electrode, is cut into required size, is fitted into fuel cell fixture and obtains tube-shaped proton exchanging film fuel
Battery or battery pile.
2. the preparation method of fine tubular proton exchange membrane fuel cell according to claim 1, which is characterized in that proton
Exchange membrane resin solution is Nafion solution of the concentration in 1wt%~10wt%.
3. the preparation method of fine tubular proton exchange membrane fuel cell according to claim 1, which is characterized in that preparation
The template of tube-shaped proton exchanging film is column glass template, and column glass template outer diameter is between 0.5mm~2mm, and length is in 1cm
Between~10cm, the tube-shaped proton exchanging film in the step 4), prepared tube-shaped proton exchanging film are prepared using the tape casting
Internal diameter is between 0.5mm~2mm, and length is between 1cm~10cm.
4. the preparation method of fine tubular proton exchange membrane fuel cell according to claim 1, which is characterized in that matched
Standby catalyst pulp is the mixture of catalyst, proton exchange membrane resin solution and dispersing agent, uses ultrasonic disperse and stirring
Method carries out evenly dispersed;
Be equipped in catalyst pulp, catalyst used is business Pt/C catalyst, Pt content between 20wt%~60wt%,
Resin solution used is the resin solution of corresponding proton exchange membrane;Dispersing agent used is deionized water, ethyl alcohol, one in isopropanol
Kind or several mixing, dispersing agent add volume and add the volume ratio of proton exchange membrane resin solution 10:1~20:1 it
Between;
During catalyst pulp is equipped with:The mass ratio of dried resin is 3 in catalyst and proton exchange membrane resin solution:1~4:1 it
Between.
5. the preparation method of fine tubular proton exchange membrane fuel cell according to claim 1, which is characterized in that use
Spread coating or spray coating method prepare anode and cathode Catalytic Layer in the heating tube outer surface peace plate surface for posting PTFE film respectively, urge
Agent loading is in 0.1~0.5mg/cm2Between, heat pipe outside diameter between 0.5mm~2mm, length 1cm~10cm it
Between, sheet width is between 0.5mm~2mm, and length is between 1cm~10cm.
6. the preparation method of fine tubular proton exchange membrane fuel cell according to claim 1, which is characterized in that in institute
It states in step 5), the specific steps are:The plate for being prepared with cathode catalysis layer collapses into tubulose, cathode catalysis layer position in the width direction
It covers in the medial surface of plate, and by the plate after in a tubular form in the outer surface of tube-shaped proton exchanging film.
7. the preparation method of fine tubular proton exchange membrane fuel cell according to claim 1, which is characterized in that step
8) tubulose membrane electrode is cut into size of the length between 1mm~10mm in.
8. a kind of preparation method of fine tubular proton exchange membrane fuel cell according to claim 1 prepares fine tubulose
The device of Proton Exchange Membrane Fuel Cells, which is characterized in that including tubular type pressure apparatus (3), heating tube (1) and plate (2), add
Heat pipe is for making anode catalyst layer, and heating tube is cylindrical structure, and the center of heating tube has hollow space (1-1),
Plate is flat shape and can collapse that plate has two on the side wall of tubular type pressure apparatus (3) for making cathode catalysis layer
The outwardly extending compression piece (3-3) of piece compresses on piece and is equipped with bolt (3-2), and two panels can be compressed piece and is tightly pressed together by bolt,
The center of tubular type pressure apparatus (3) has cavity (3-1);The tubular type pressure apparatus internal diameter is 0.5mm~2mm, length 1cm
~10cm.
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US10632447B2 (en) * | 2018-08-28 | 2020-04-28 | Molecule Works Inc. | Reactor for hydrothermal growth of structured materials |
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CN113488674B (en) * | 2021-07-07 | 2022-06-17 | 哈尔滨工业大学(深圳) | Assembling method of cylindrical self-breathing fuel cell |
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