KR20240085393A - Manufacturing method for Catalyst electrode using electrospray - Google Patents
Manufacturing method for Catalyst electrode using electrospray Download PDFInfo
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- KR20240085393A KR20240085393A KR1020220170196A KR20220170196A KR20240085393A KR 20240085393 A KR20240085393 A KR 20240085393A KR 1020220170196 A KR1020220170196 A KR 1020220170196A KR 20220170196 A KR20220170196 A KR 20220170196A KR 20240085393 A KR20240085393 A KR 20240085393A
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- catalyst
- electrode
- carbon paper
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- 239000003054 catalyst Substances 0.000 title claims abstract description 71
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 33
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 239000000446 fuel Substances 0.000 claims abstract description 9
- 238000007787 electrohydrodynamic spraying Methods 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002861 polymer material Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 108091003079 Bovine Serum Albumin Proteins 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229940098773 bovine serum albumin Drugs 0.000 description 2
- 239000012018 catalyst precursor Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000000840 electrochemical analysis Methods 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical group S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000000970 chrono-amperometry Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/886—Powder spraying, e.g. wet or dry powder spraying, plasma spraying
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8605—Porous electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8668—Binders
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
-
- Z05E30/00—
Abstract
본 발명은 연료전지나 배터리 등에 적용되는 촉매전극의 제조 기술에 관한 것으로, 촉매를 포함하는 용액을 전기분무 방식으로 카본페이퍼에 코팅하는 단계를 포함하는 촉매전극 제조방법에 관한 것이다.
이러한 본 발명에 의하면 카본페이퍼에 전기전도성을 갖는 촉매가 고르게 코팅되어 우수한 전기화학적 성능을 가진 촉매전극을 얻을 수 있다. 또한 본 발명에 의한 촉매전극을 연료전지 및 배터리 등 다양한 분야에 적용할 수 있게 된다. The present invention relates to a manufacturing technology for catalytic electrodes applied to fuel cells, batteries, etc., and to a method for manufacturing a catalytic electrode including the step of coating a solution containing a catalyst on carbon paper by electrospraying.
According to the present invention, a catalyst electrode having excellent electrochemical performance can be obtained by evenly coating carbon paper with an electrically conductive catalyst. Additionally, the catalyst electrode according to the present invention can be applied to various fields such as fuel cells and batteries.
Description
본 발명은 연료전지나 배터리 등에 적용되는 촉매전극의 제조 기술에 관한 것으로, 보다 상세하게는 카본페이퍼를 지지체로 하는 코팅 효율과 안정성이 우수한 촉매전극의 제조방법에 관한 것이다. The present invention relates to a manufacturing technology for catalytic electrodes applied to fuel cells, batteries, etc., and more specifically, to a method for manufacturing a catalytic electrode with excellent coating efficiency and stability using carbon paper as a support.
연료전지나 배터리 또는 각종 센서의 전극은 촉매층과 촉매층을 지지해 주는 지지체로 구성되어 있다. 지지체로 보통 다공성 카본페이퍼(carbon paper)나 카폰펠트(carbon felt)가 쓰이지만, 상대적으로 낮은 압축변형률과 강한 강도를 가지는 카본페이퍼의 사용이 일반적이다. 지지체는 촉매층을 지지해 주는 역할 외에도 반응기체나 액체를 촉매층으로 확산시켜주는 확산층(diffusion layer), 촉매층에서 발생한 전류를 분리판으로 이동시켜 주는 집전체(current collector), 생성된 물 등이 촉매층 밖으로 유출되게 하는 통로 등의 역할도 수행한다. 따라서 지지체는 수분에 의한 flooding이 일어나지 않도록 polytetrafluoroethylene(PTFE; Teflon) 등으로 발수처리(hydrophobic coating) 하는 것이 바람직하고, 반응기체가 잘 통과하도록 50~90%의 기공율을 가져야 한다. 또한 그 위에 코팅된 촉매층이 전해질 막과 잘 접촉되어 접촉저항이 최소화 되도록 평탄하여야 하며 발생한 전류를 잘 집전하도록 전기전도도가 높아야 한다. The electrodes of fuel cells, batteries, or various sensors are composed of a catalyst layer and a support that supports the catalyst layer. Porous carbon paper or carbon felt is usually used as a support, but carbon paper, which has a relatively low compressive strain and strong strength, is commonly used. In addition to supporting the catalyst layer, the support serves as a diffusion layer that diffuses the reaction gas or liquid into the catalyst layer, a current collector that moves the current generated in the catalyst layer to the separator plate, and a current collector that moves the generated water, etc. out of the catalyst layer. It also performs the role of a conduit for outflow. Therefore, it is desirable for the support to be hydrophobically coated with polytetrafluoroethylene (PTFE; Teflon) to prevent flooding by moisture, and it should have a porosity of 50 to 90% to allow the reaction gas to easily pass through. In addition, the catalyst layer coated on top must be flat to ensure good contact with the electrolyte membrane to minimize contact resistance, and must have high electrical conductivity to properly collect the generated current.
종래 카본페이퍼에 촉매층을 결합시키는 방법으로 딥 코팅(dip coating), 브러싱(brushing), 스프레이(spray coating), 드롭 캐스팅(drop casting) 등이 제시된 바 있다(비특허문헌 참조). 그러나 이러한 코팅 방법들은 손실되는 촉매의 양이 많으며, 카본페이퍼 표면에 촉매가 고르게 코팅되지 않는다는 단점이 있다. 촉매가 불균일하게 분산되면 반응에 참여하는 촉매의 면적이 줄어들며, 전해액과 촉매, 전극이 만나는 삼상계면이 제대로 형성되지 못해 전극의 전체적인 전기화학적 반응이 감소되는 문제가 발생한다. Conventional methods for bonding a catalyst layer to carbon paper include dip coating, brushing, spray coating, and drop casting (see non-patent literature). However, these coating methods have the disadvantage that a large amount of catalyst is lost and the catalyst is not evenly coated on the surface of the carbon paper. If the catalyst is unevenly dispersed, the area of the catalyst participating in the reaction is reduced, and the three-phase interface where the electrolyte, catalyst, and electrode meet is not properly formed, which reduces the overall electrochemical reaction of the electrode.
등록특허 10-1301613은 카본페이퍼에 탄소나노튜브를 성장시킨 다음 그 위에 스퍼터링으로 촉매(여기서는 철(Fe))를 증착하고 소결하여 고분자 전해질 연료전지용 철 촉매를 제조하는 방법을 제시하고 있다. 이에 의하면 촉매가 고르고 안정적으로 코팅되지만 비교적 복잡한 공정(스퍼터링)과 고온(850~1050℃) 처리가 필요하다는 단점이 있다. Registered patent 10-1301613 proposes a method of producing an iron catalyst for a polymer electrolyte fuel cell by growing carbon nanotubes on carbon paper and then depositing a catalyst (here, iron (Fe)) on it by sputtering and sintering. According to this, the catalyst is coated evenly and stably, but it has the disadvantage of requiring a relatively complicated process (sputtering) and high temperature (850~1050℃) treatment.
등록특허 10-1799384는, 다공성 내열합금 지지체에 전기분무방식으로 촉매 전구체막을 형성한 다음 열처리 환원하여 촉매 전구체를 촉매로 변환시키는 방법을 제시하고 있다. 그러나 상기 선행기술문헌은 카본페이퍼가 아닌 내열합금을 지지체로 채택한 것이고 역시 고온(400~600℃)으로 열처리해야 하는 문제가 있다. Registered Patent No. 10-1799384 proposes a method of forming a catalyst precursor film on a porous heat-resistant alloy support by electrospraying and then converting the catalyst precursor into a catalyst by heat treatment and reduction. However, the prior art literature adopts heat-resistant alloy rather than carbon paper as a support, and there is a problem that it must be heat treated at high temperature (400-600°C).
본 발명은 탄소 가닥으로 이뤄진 카본페이퍼에 촉매를 저온에서 간편하고 고르게 코팅하는 방법을 제공하는 것을 목적으로 한다. The purpose of the present invention is to provide a method of simply and evenly coating a catalyst on carbon paper made of carbon strands at low temperature.
전술한 목적을 달성하기 위한 본 발명은, 촉매를 포함하는 용액을 전기분무 방식으로 카본페이퍼에 코팅하는 단계를 포함하는 촉매전극 제조방법에 관한 것이다.The present invention for achieving the above-described object relates to a method for manufacturing a catalyst electrode including the step of coating a solution containing a catalyst on carbon paper by electrospraying.
본 발명에서 상기 용액은 촉매와 카본페이퍼의 결합력을 증진시키는 고분자 물질을 함유는 것이 바람직하다. 하기 실시예에서는 결합력 증진 고분자 물질로 듀폰사의 나피온을 이용하였는데, 이에 한정되는 것은 아니고 예를 들면 생체모사 단백질의 종류인 Polydopamine 또는 BSA(Bovine Serum Albumin) 등과 같은 접착기능이 있는 고분자물질을 채택할 수도 있다. In the present invention, the solution preferably contains a polymer material that improves the bonding force between the catalyst and the carbon paper. In the following examples, DuPont's Nafion was used as a bonding strength enhancing polymer material, but it is not limited to this, and for example, a polymer material with an adhesive function such as Polydopamine or BSA (Bovine Serum Albumin), a type of biomimetic protein, can be used. It may be possible.
본 발명에서 상기 용액의 용매는 물, 및 물과 혼화 가능한 유기용매로 이루질 수 있다. 이때 제1용매인 탈이온수는 촉매잉크 내의 고분자 화합물과 촉매가 고르게 분산되어 코팅이 균일하게 이루어질 수 있도록 하는 역할을 하며, 제2용매인 휘발성 용매는 촉매층 형성 시 빠른 건조 및 이에 의한 기체확산층(카본전극)에 기공을 적절하게 형성할 수 있도록 한다. 촉매 이외의 촉매층에 영향을 주는 물질이 모두 제2용매와 함께 배출·제거된다. 하기 실시예에서는 자기 얼룩을 남기지 않고 쉽게 증발하며 반응성이 적절한 이소프로필 알코올을 제2용매로 선정하였는데, 이에 제한되는 것은 아니다. In the present invention, the solvent of the solution may be water or an organic solvent miscible with water. At this time, the first solvent, deionized water, plays a role in ensuring that the polymer compounds and catalysts in the catalyst ink are evenly dispersed to ensure uniform coating, and the second solvent, a volatile solvent, dries quickly when forming the catalyst layer and thereby creates a gas diffusion layer (carbon). electrode) to properly form pores. All substances that affect the catalyst layer other than the catalyst are discharged and removed along with the second solvent. In the following examples, isopropyl alcohol, which evaporates easily without leaving self-stains and has appropriate reactivity, was selected as the second solvent, but is not limited thereto.
본 발명에서 상기 촉매는, 연료전지, 배터리 또는 센서 등 용도에 대응되는 것으로서, 하기 실시예에서는 MoS2를 예시적으로 사용하였는데, 이에 제한되는 것은 아니며 전압을 인가했을 때, 대전될 수 있는 파우더 형태의 다양한 화합물을 촉매로 선택할 수 있다. In the present invention, the catalyst corresponds to uses such as fuel cells, batteries, or sensors. MoS 2 was used as an example in the following examples, but is not limited thereto and is in the form of a powder that can be charged when a voltage is applied. A variety of compounds can be selected as catalysts.
본 발명에서 촉매를 포함하는 용액(이하 '촉매용액'이라 함)은 균일하게 혼합되는 것이 바람직하다. 하기 실시예에서는 균일 혼합을 위해 초음파진동기를 활용하였는데, 이외에 다른 균질장치를 이용할 수도 있을 것이다. In the present invention, it is preferable that the solution containing the catalyst (hereinafter referred to as 'catalyst solution') is uniformly mixed. In the following examples, an ultrasonic vibrator was used for uniform mixing, but other homogenization devices may also be used.
이상과 같은 본 발명에 의한 촉매전극은 다량의 촉매가 카본페이퍼의 탄소 가닥 표면에 고르고 견고하게 코팅되어 있어, 연료전지, 배터리 또는 센서 등의 전극으로 활용될 수 있다. The catalyst electrode according to the present invention as described above has a large amount of catalyst coated evenly and firmly on the surface of the carbon strands of carbon paper, so it can be used as an electrode for fuel cells, batteries, or sensors.
본 발명에 의한 촉매전극 제작을 위해 전기분무장치를 활용하게 된다. 전기분무장치의 구체적인 구성과 작동방법 등은 종래 널리 알려져 있는 것이므로 전기분무장치 자체에 대한 설명은 생략한다.An electrospray device is used to manufacture the catalyst electrode according to the present invention. Since the specific configuration and operating method of the electrospray device are widely known, description of the electrospray device itself will be omitted.
이상과 같이 본 발명에 의하면 카본페이퍼에 전기전도성을 갖는 촉매가 고르게 코팅되어 우수한 전기화학적 성능을 가진 촉매전극을 얻을 수 있다. As described above, according to the present invention, a catalyst electrode having excellent electrochemical performance can be obtained by evenly coating carbon paper with an electrically conductive catalyst.
또한 본 발명에 의한 촉매전극을 연료전지 및 배터리 등 다양한 분야에 적용할 수 있게 된다. Additionally, the catalyst electrode according to the present invention can be applied to various fields such as fuel cells and batteries.
도 1은 본 발명에 의한 전기분무 방법을 사용하는 장치에 대한 모식도.
도 2는 본 발명의 실시예에 의한 촉매전극 표면의 SEM 사진.
도 3은 본 발명의 실시예 및 비교예에 의한 촉매전극의 전기화학적 성능을 보여주는 그래프.
도 4는 본 발명의 실시예에 의한 촉매전극의 시간에 따른 전기화학적 성능의 안정성을 보여주는 그래프.1 is a schematic diagram of a device using the electrospray method according to the present invention.
Figure 2 is an SEM photograph of the surface of a catalyst electrode according to an example of the present invention.
Figure 3 is a graph showing the electrochemical performance of catalyst electrodes according to examples and comparative examples of the present invention.
Figure 4 is a graph showing the stability of electrochemical performance over time of a catalyst electrode according to an embodiment of the present invention.
이하 첨부된 도면과 실시예를 들어 본 발명을 보다 상세히 설명한다. 그러나 이러한 도면과 실시예는 본 발명의 기술적 사상의 내용과 범위를 쉽게 설명하기 위한 예시일 뿐, 이에 의해 본 발명의 기술적 범위가 한정되거나 변경되는 것은 아니다. 이러한 예시에 기초하여 본 발명의 기술적 사상의 범위 안에서 다양한 변형과 변경이 가능함은 당업자에게는 당연할 것이다.Hereinafter, the present invention will be described in more detail with reference to the attached drawings and examples. However, these drawings and examples are merely examples for easily explaining the content and scope of the technical idea of the present invention, and the technical scope of the present invention is not limited or changed thereby. Based on these examples, it will be obvious to those skilled in the art that various modifications and changes are possible within the scope of the technical idea of the present invention.
[실시예][Example]
1. 촉매 잉크의 준비1. Preparation of catalyst ink
다음 표와 같은 조성을 상온에서 초음파진동기로 5분간 교반하여 촉매 잉크를 준비하였다.Catalyst ink was prepared by stirring the composition shown in the following table for 5 minutes at room temperature with an ultrasonic vibrator.
MoS2(Aldrich chemistry, 1317-33-5 MoS2)은 전기전도성 파우더인데, 촉매 역할을 한다.MoS 2 (Aldrich chemistry, 1317-33-5 MoS 2 ) is an electrically conductive powder that acts as a catalyst.
2. 촉매 코팅2. Catalyst coating
도 1에 개념적으로 도시된 것과 같은 전기분무장치를 활용하여 카본페이퍼(Toray, Toray Carbon Paper 060, Wet Proofed)에 위에서 준비된 촉매 잉크를 전기분무하여 코팅하였다. 전기분무 조건은 다음 표와 같다. 표에서 접지면적은 카본페이퍼 이면에 접착된 전도성 테이프(3M, 구리테이프)의 면적이다.Using an electrospray device as conceptually shown in Figure 1, the catalyst ink prepared above was electrosprayed and coated on carbon paper (Toray, Toray Carbon Paper 060, Wet Proofed). Electrospray conditions are as shown in the table below. In the table, the ground area is the area of the conductive tape (3M, copper tape) attached to the back of the carbon paper.
이어서 40℃의 대류 오븐에 전기분무된 카본페이퍼를 10분 동안 건조하여 실시예 촉매전극(촉매가 전기분무 코팅된 카본페이퍼)을 제작하였다.Next, the electrosprayed carbon paper was dried in a convection oven at 40°C for 10 minutes to produce an example catalyst electrode (carbon paper coated with electrospray catalyst).
15kV의 전압으로 촉매 잉크를 0.5 mL/분의 속도로 10분에 걸쳐 천천히 분무하였다. 이때 방울의 크기는 인가하는 전압에 따라 변동될 수 있다. 수동분무한 것을 제외하고는 동일한 방법으로 비교예 촉매전극(촉매가 수동분무 코팅된 카본페이퍼)을 준비하였다.The catalyst ink was sprayed slowly over 10 minutes at a rate of 0.5 mL/min with a voltage of 15 kV. At this time, the size of the droplet may vary depending on the applied voltage. A comparative catalyst electrode (carbon paper coated with a manual spray coating) was prepared in the same manner except that it was manually sprayed.
3. 제작된 촉매전극의 특성 분석3. Characteristic analysis of the manufactured catalyst electrode
(1) 촉매전극의 SEM 사진 (1) SEM photo of catalyst electrode
제작된 촉매전극의 표면을 SEM으로 관찰하였다(도 2 참조). 도면에서 (A)가 비교예, (B)가 실시예이다.The surface of the manufactured catalyst electrode was observed using SEM (see Figure 2). In the drawing, (A) is a comparative example and (B) is an example.
수동분무에 의한 전극인 비교예를 보면 약 8.6 ㎛ 직경의 탄소가닥에 약 1 ㎛ 이하의 작은 파티클들이 불균일하게 부착된 반면, 전기분무에 의한 전극인 실시예의 경우 같은 탄소 가닥에 약 2 ㎛의 크기를 갖는 파티클이 고르고 견고하게 부착되었다. 같은 양의 촉매가 사용되었으나 탄소가닥에 부착된 촉매 파티클의 양은 확연하게 다르다는 것을 알 수 있다.Looking at the comparative example, which is an electrode made by manual spraying, small particles of about 1 ㎛ or less were attached unevenly to a carbon strand with a diameter of about 8.6 ㎛, while in the example of an electrode made by electrospraying, small particles of about 2 ㎛ in size were attached to the same carbon strand. Particles with were evenly and firmly attached. Although the same amount of catalyst was used, the amount of catalyst particles attached to the carbon strands was clearly different.
(2) 촉매전극의 수소 생성반응(2) Hydrogen production reaction at the catalyst electrode
황산 0.1 M 내에서 수소 생성반응에 대한 특성을 분석하여 도 3에 나타내었다.The characteristics of the hydrogen production reaction in 0.1 M sulfuric acid were analyzed and shown in Figure 3.
실험은 삼전극 시스템 하에서 진행되었으며, H-cel을 사용하여 수소 생산량을 확인하였다. 기준전극은 Ag/AgCl을 상대전극은 백금 메쉬로 된 전극을 사용하였다. 작업전극은 수동분무로 촉매를 코팅한 카본페이퍼 전극(비교예)과 위에서 설명된 방법으로 제작된 카본페이퍼 전극(실시예)으로 전기화학적 분석을 진행하였다. 분석 방법은 선형주사전위법(Linear Sweep Voltammetry)을 이용하였으며, 0V ~ -0.85V 범위에서 진행하였다.The experiment was conducted under a three-electrode system, and hydrogen production was confirmed using H-cel. Ag/AgCl was used as the reference electrode, and a platinum mesh electrode was used as the counter electrode. Electrochemical analysis was performed using the working electrode as a carbon paper electrode coated with a catalyst by manual spraying (comparative example) and a carbon paper electrode manufactured using the method described above (example). The analysis method used Linear Sweep Voltammetry and was conducted in the range of 0V to -0.85V.
본 그래프의 의미는 같은 전압내에서 비교예와 비교할 경우 실시예의 전류가 더 높은 것을 알 수 있는데, 이는 실시예에 의한 전극이 더 우수한 성능을 보인다고 할 수 있다.The meaning of this graph is that the current of the example is higher when compared to the comparative example within the same voltage, which means that the electrode according to the example shows better performance.
(3) 촉매전극의 안정성 (3) Stability of catalyst electrode
0.95 V(vs RHE) 내에서 24시간 동안 수소 생성반응에 대한 안정성을 확인하였다.The stability of the hydrogen production reaction was confirmed for 24 hours within 0.95 V (vs RHE).
위 (1)과 동일하게 삼전극 시스템 하에서 진행되었으며, H-cel을 사용하여 수소 생산량을 확인하였다. 기준전극은 Ag/AgCl을 상대전극은 백금 메쉬로 된 전극을 사용하였다. 작업전극은 수동분무로 촉매를 코팅한 카본페이퍼 전극(비교예)과 위에서 설명된 방법으로 제작된 카본페이퍼 전극(실시예)으로 전기화학적 분석을 진행하였다. 분석 방법은 시간대 전류법(ChronoAmperometry)을 이용하였으며, -0.95V에서 24시간 동안 측정하며 안정성을 확인하였다(도 4 참조). It was conducted under the same three-electrode system as (1) above, and hydrogen production was confirmed using H-cel. Ag/AgCl was used as the reference electrode and a platinum mesh electrode was used as the counter electrode. Electrochemical analysis was performed using the working electrode as a carbon paper electrode coated with a catalyst by manual spraying (comparative example) and a carbon paper electrode manufactured using the method described above (example). ChronoAmperometry was used as the analysis method, and stability was confirmed by measuring at -0.95V for 24 hours (see Figure 4).
그 결과, 실시예는 24시간 동안 안정적으로 전류를 유지하는 것을 확인할 수 있지만, 비교예는 대략 12시간이 지난 후 전류가 급격하게 떨어지는 것을 확인할 수 있다. 이는 실시예 전극의 성능이 안정적으로 지속되는 것을 보여준다.As a result, it can be seen that the Example maintains a stable current for 24 hours, but in the Comparative Example, it can be seen that the current drops rapidly after approximately 12 hours. This shows that the performance of the example electrode continues stably.
Claims (5)
A catalyst electrode manufacturing method comprising the step of coating a solution containing a catalyst on carbon paper by electrospraying.
상기 용액은 촉매와 카본페이퍼의 결합력을 증진시키는 고분자 물질을 함유하는 것을 특징으로 하는 촉매전극 제조방법.
In claim 1,
A method of manufacturing a catalyst electrode, characterized in that the solution contains a polymer material that improves the bonding force between the catalyst and carbon paper.
상기 용액의 용매는 물, 및 물과 혼화 가능한 유기용매로 이루어지는 것을 특징으로 하는 촉매전극 제조방법.
In claim 1 or 2,
A catalyst electrode manufacturing method, characterized in that the solvent of the solution consists of water and an organic solvent miscible with water.
상기 촉매는 MoS2인 것을 특징으로 하는 촉매전극 제조방법.
In claim 1 or 2,
A catalyst electrode manufacturing method, characterized in that the catalyst is MoS 2 .
상기 촉매전극은 연료전지, 배터리 또는 센서의 전극으로 활용되는 것을 특징으로 하는 촉매전극 제조방법.In claim 1 or 2,
A method of manufacturing a catalyst electrode, characterized in that the catalyst electrode is used as an electrode for a fuel cell, battery, or sensor.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| KR20240085393A true KR20240085393A (en) | 2024-06-17 |
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