JP5272994B2 - Method for treating catalyst-carrying carbon and electrode for fuel cell - Google Patents
Method for treating catalyst-carrying carbon and electrode for fuel cell Download PDFInfo
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Description
本発明は、触媒担持カーボンの処理方法及び燃料電池用電極に関する。 The present invention relates to a method for treating catalyst-carrying carbon and a fuel cell electrode.
一般に、燃料電池用触媒として、カーボン粉末を担体とし、これに白金等の金属微粒子を担持させた触媒担持カーボンが知られている。この触媒担持カーボンを用いた燃料電池用電極は、触媒担持カーボンを電解質溶液等と混合して電極用ペーストを製造し、この電極用ペーストを用いて作製される。
ここで、一般に市販されている触媒等、その作製工程（主に乾燥工程）の影響により、かなり凝集した状態の触媒凝集体は、そのまま用いられると、電極用ペースト中での触媒の分散性が低く、触媒凝集体の内部まで電解質が浸透しにくい。このような触媒を用いて作製された電極は、全ての触媒が有効に機能できないため、電極の性能が低下してしまう。
In general, a catalyst-supporting carbon in which carbon powder is used as a carrier and metal fine particles such as platinum are supported thereon is known as a fuel cell catalyst. The fuel cell electrode using the catalyst-supporting carbon is manufactured by mixing the catalyst-supporting carbon with an electrolyte solution or the like to produce an electrode paste, and using the electrode paste.
Here, when the catalyst aggregate in a considerably aggregated state is used as it is due to the influence of the production process (mainly the drying process) such as a commercially available catalyst, the dispersibility of the catalyst in the electrode paste is reduced. It is low and the electrolyte hardly penetrates into the inside of the catalyst aggregate. Since the electrode produced using such a catalyst cannot function effectively for all catalysts, the performance of the electrode is degraded.
このような問題点を解決するため、触媒凝集体を電解質溶液等に混合した後に超音波を用いて、触媒を粉砕し、電極用ペースト中での分散性を促進させる等の方法が提案されている。
しかしながら、上記方法では、元々の粒子の小さい触媒凝集体をさらに細かく粉砕するにはエネルギー的に不足しがちであり、触媒凝集体を充分に粉砕し、電極用ペースト中での良好な分散性を確保することは困難であった。
本件発明に関連する技術を開示する文献として特許文献１を参照されたい。
In order to solve such problems, a method has been proposed in which catalyst agglomerates are mixed into an electrolyte solution or the like, and then the catalyst is pulverized using ultrasonic waves to promote dispersibility in the electrode paste. Yes.
However, in the above method, it tends to be insufficient in terms of energy to further pulverize the original catalyst aggregate with small particles, and the catalyst aggregate is sufficiently pulverized to provide good dispersibility in the electrode paste. It was difficult to secure.
Reference should be made to Patent Document 1 as a document disclosing a technique related to the present invention.
本発明は、上記従来の実情に鑑みてなされたものであり、電極用ペースト中における触媒担持カーボンの良好な分散性を確保することが可能な触媒担持カーボンの処理方法を提供することを解決すべき課題としている。 The present invention has been made in view of the above-described conventional situation, and solves the problem of providing a method for treating catalyst-carrying carbon capable of ensuring good dispersibility of catalyst-carrying carbon in an electrode paste. It should be a challenge.
この発明は上記課題を解決すべくなされたものであり、その第１の局面は次のように規定される。即ち、
カーボン粉末に触媒機能を有する金属微粒子が担持された触媒担持カーボンの処理方法であって、
前記触媒担持カーボンと液体とを含む混合物を湿式粉砕し、次いで、減圧下で凍結乾燥する、
ことを特徴とする触媒担持カーボンの処理方法である。
このように規定される第１の局面の触媒担持カーボンの処理方法によれば、粉砕方法として湿式粉砕を採用するため、高エネルギーで粉砕することができ、触媒担持カーボンを微粉砕することが可能となる。また、次いで行う乾燥工程として、減圧下での凍結乾燥を採用するため、当該微粉砕された触媒担持カーボンを再凝集させることなく乾燥できる。上記処理を施された触媒担持カーボンであれば、電極用ペースト中において良好な分散性を確保できる。
また、特に再凝集しやすい、元々の粒子の小さい触媒においても、第１の局面の処理方法によれば、効果的に分散させられる。
The present invention has been made to solve the above problems, and the first aspect thereof is defined as follows. That is,
A method for treating catalyst-carrying carbon in which metal fine particles having a catalytic function are carried on carbon powder,
Wet-pulverizing the mixture comprising the catalyst-supporting carbon and the liquid, and then freeze-drying under reduced pressure;
This is a method for treating catalyst-supported carbon.
According to the method for treating catalyst-carrying carbon of the first aspect defined as described above, wet crushing is adopted as a crushing method, so that it can be pulverized with high energy and the catalyst-carrying carbon can be finely pulverized. It becomes. Further, since freeze drying under reduced pressure is employed as the subsequent drying step, the finely pulverized catalyst-supported carbon can be dried without being re-agglomerated. If the catalyst-supported carbon is subjected to the above treatment, good dispersibility can be secured in the electrode paste.
In addition, even a catalyst having a small original particle size that is particularly easily re-aggregated can be effectively dispersed according to the treatment method of the first aspect.
この発明の第２の局面は次のように規定される。即ち、
第１の局面に規定の触媒担持カーボンの処理方法において、前記液体が水であり、ボールミル法又はビーズミル法により前記湿式粉砕を行う、ことを特徴とする触媒担持カーボンの処理方法である。
湿式粉砕に用いる液体として採用される水は、安価であるため好適に用いられる。また、湿式粉砕の方法として、ボールミル法又はビーズミル法を採用すれば、ボールやビーズ等のメディアによる粉砕効果も発揮されるため、より微粉砕された触媒担持カーボンを得ることが可能となる。
The second aspect of the present invention is defined as follows. That is,
In the method for treating catalyst-supporting carbon defined in the first aspect, the liquid is water, and the wet grinding is performed by a ball mill method or a bead mill method.
Water employed as a liquid used for wet pulverization is preferably used because it is inexpensive. In addition, if a ball mill method or a bead mill method is employed as a wet pulverization method, a pulverization effect by a medium such as a ball or a bead is also exhibited, so that more finely pulverized catalyst-supported carbon can be obtained.
また、この発明の処理方法により処理された触媒担持カーボンを燃料電池の触媒層の成分として用いることができる。 Further, the catalyst-supported carbon treated by the treatment method of the present invention can be used as a component of the catalyst layer of the fuel cell.
以下、本発明の具体化した実施形態を詳細に説明する。
＜触媒担持カーボンの処理＞
（湿式粉砕工程）
この発明において、触媒担持カーボンは湿式粉砕により微粉砕される。乾式粉砕では、粉砕時の触媒担持カーボンの再凝集が起こり易く、微粉砕することが困難だからである。
湿式粉砕は、触媒担持カーボンに液体を加え、スラリー状にして粉砕を行う。液体中で粉砕を行うことにより、触媒担持カーボンを高エネルギーで微粉砕することが可能である。また、湿式粉砕では、液体中で触媒担持カーボンを粉砕し、分散させるため、粉砕された触媒担持カーボンの再凝集を防ぐことができる。このように湿式粉砕により処理すれば、触媒担持カーボンを微細な状態まで粉砕することができ、また、粒度分布幅の狭い触媒担持カーボンを得ることが可能となる。
湿式粉砕によれば、さらに、触媒担持カーボンを洗浄する効果も得られる。触媒担持カーボン凝集体が微粉砕されることにより、凝集体内部に存在する油分等の不純物成分を取り除くことが可能となる。
湿式粉砕に用いられる液体は、上記湿式粉砕の機能に応じて適宜選択される。水やアルコール、エーテル等の有機溶媒を用いることができる。
Embodiments of the present invention will be described in detail below.
<Treatment of catalyst-supported carbon>
(Wet grinding process)
In this invention, the catalyst-supporting carbon is finely pulverized by wet pulverization. This is because in dry pulverization, re-aggregation of the catalyst-supporting carbon during pulverization easily occurs and it is difficult to pulverize.
In the wet pulverization, a liquid is added to the catalyst-supporting carbon to form a slurry and pulverize. By performing pulverization in a liquid, it is possible to finely pulverize the catalyst-supported carbon with high energy. Further, in the wet pulverization, the catalyst-carrying carbon is pulverized and dispersed in the liquid, so that re-aggregation of the pulverized catalyst-carrying carbon can be prevented. If the treatment is performed by wet pulverization in this way, the catalyst-supported carbon can be pulverized to a fine state, and catalyst-supported carbon having a narrow particle size distribution width can be obtained.
According to the wet pulverization, the effect of washing the catalyst-supporting carbon is further obtained. By finely pulverizing the catalyst-carrying carbon aggregate, it is possible to remove impurity components such as oil components present in the aggregate.
The liquid used for the wet pulverization is appropriately selected according to the function of the wet pulverization. Organic solvents such as water, alcohol and ether can be used.
上記湿式粉砕の方法としては特に限定されず、触媒担持カーボンが微粉砕される方法であればよい。例えば、ボールミル法、ビーズミル法、プロペラ式ミキサー法、コロイドミル法、ホモジナイザー法、超音波ホモジナイザー法、高圧ホモジナイザー法等が挙げられる。
また、湿式粉砕法として、超音波を用いる方法を採用することも可能である。超音波等のエネルギーは、水等の液体に印加することによりキャビテーションを発生させる。このキャビテーションに起因する衝撃を利用すれば、ボールミル法、ビーズミル法による粉砕効果と同等の効果を得ることができるからである。
上記湿式粉砕法のうち、特に好ましい方法として、ボールミル法又はビーズミル法が挙げられる。ボールやビーズ等のメディアの衝突エネルギーにより、さらに高エネルギーで粉砕されるため、触媒担持カーボンを非常に微細な状態まで粉砕可能であるからである。
The wet pulverization method is not particularly limited as long as the catalyst-carrying carbon is pulverized. Examples thereof include a ball mill method, a bead mill method, a propeller mixer method, a colloid mill method, a homogenizer method, an ultrasonic homogenizer method, and a high-pressure homogenizer method.
In addition, as a wet pulverization method, a method using ultrasonic waves can be employed. When energy such as ultrasonic waves is applied to a liquid such as water, cavitation is generated. This is because if the impact caused by the cavitation is used, an effect equivalent to the grinding effect by the ball mill method or the bead mill method can be obtained.
Among the wet pulverization methods, a ball mill method or a bead mill method is particularly preferable. This is because the catalyst-carrying carbon can be pulverized to a very fine state because it is pulverized with higher energy by the collision energy of media such as balls and beads.
上記ボールミル法、ビーズミル法で用いられる粉砕容器及びメディアの材質は、特に限定されず、ガラス、ジルコン、ジルコニア、アルミナ等が挙げられる。カーボン材料より硬く、かつ、触媒上に付着しても反応等に悪影響を与えないことから、ジルコニア等のセラミックス材料が好ましく用いられる。
上記ボールミル法、ビーズミル法において、触媒担持カーボンを微粉砕するためのエネルギーは、粉砕回転数、粉砕時間、メディアの径及び数、触媒担持カーボンと液体とメディアの比率等を幅広く変化させることにより制御することができる。
The material of the pulverization container and media used in the above ball mill method and bead mill method is not particularly limited, and examples thereof include glass, zircon, zirconia, and alumina. A ceramic material such as zirconia is preferably used because it is harder than the carbon material and does not adversely affect the reaction even if it adheres to the catalyst.
In the above ball mill method and bead mill method, the energy for finely pulverizing the catalyst-supported carbon is controlled by widely changing the pulverization speed, the pulverization time, the diameter and number of media, the ratio of catalyst-supported carbon, liquid, and media. can do.
（減圧下凍結乾燥工程）
上記湿式粉砕工程で作製した試料（微粉砕された触媒担持カーボンと液体との混合物）を、まず低温下で凍結し、その後減圧下で凍結乾燥する。通常の乾燥では、乾燥時に試料中を液体が移動する際、あるいは、試料から液体が蒸発する際に、毛管収縮現象等により微粉砕した触媒担持カーボンが強い結合力で再凝集するため、微粉砕された触媒担持カーボンを得ることが困難であるからである。なお上記湿式粉砕工程で使用する液体と、減圧下凍結乾燥工程で使用する液体は必ずしも同じものである必要はなく、各々の用途に適した最適なものを選ぶことができる。
適当な減圧下で凍結乾燥すれば、試料中の余分な液体は固体の状態から昇華により気体となって除去され、微粉砕された触媒担持カーボンを再凝集させることなく乾燥させることが可能である。
上記減圧下で凍結乾燥する際の圧力は、使用する液体の種類、温度等によって異なるが、使用する液体が凍結し、固体から気体に昇華できるような圧力、すなわち使用する液体の昇華曲線より低い圧力であることが必要である。
また、試料と真空ポンプの間に、液体窒素トラップ等のコールドトラップを設置してもよい。コールドトラップの設置により、より真空度を上げることが可能であるため、乾燥速度を向上することができるからである。乾燥速度を向上させるための手段として、試料の入った容器をヒーター等により加熱することにより、試料温度を適度に上昇させることとしても良い。これらの乾燥速度を向上させるための手段は、いずれか一つを採用しても良いし、併用しても良い。
上記凍結乾燥後の触媒担持カーボンは、後述する電極用ペーストを作製する際に、水等の液体との混合割合を厳密に制御することが望まれるため、確実に乾燥させることが必要である。
(Freeze drying process under reduced pressure)
The sample (mixture of finely pulverized catalyst-supporting carbon and liquid) prepared in the wet pulverization step is first frozen at a low temperature and then lyophilized under reduced pressure. In normal drying, when the liquid moves through the sample during drying, or when the liquid evaporates from the sample, the finely pulverized catalyst-carrying carbon re-aggregates with a strong binding force due to capillary contraction, etc. This is because it is difficult to obtain a catalyst-supported carbon. The liquid used in the wet pulverization step and the liquid used in the freeze-drying step under reduced pressure are not necessarily the same, and an optimal one suitable for each application can be selected.
If lyophilized under an appropriate reduced pressure, excess liquid in the sample is removed from the solid state as a gas by sublimation, and the finely pulverized catalyst-supported carbon can be dried without re-aggregation. .
The pressure at the time of lyophilization under reduced pressure varies depending on the type of liquid used, temperature, etc., but is lower than the pressure at which the liquid used can be frozen and sublimated from solid to gas, that is, lower than the sublimation curve of the liquid used. It needs to be pressure.
A cold trap such as a liquid nitrogen trap may be installed between the sample and the vacuum pump. This is because the vacuum rate can be further increased by installing a cold trap, so that the drying rate can be improved. As a means for improving the drying rate, the sample temperature may be appropriately increased by heating the container containing the sample with a heater or the like. Any one of these means for improving the drying speed may be employed or may be used in combination.
Since the catalyst-supported carbon after lyophilization is desired to strictly control the mixing ratio with a liquid such as water when preparing an electrode paste described later, it is necessary to dry it reliably.
以下、本発明の実施例について説明する。
（実施例）
Ｐｔ触媒担持カーボン（カーボン：Cabot社製、商品名Black Pearl 880、白金担持量：20wt%）３ｇを、純水２７ｇとともにボールミル粉砕用容器（材質：部分安定化ジルコニア、内容積８０ｃｃ）に投入し、そこにさらにジルコニアボール（直径５ｍｍ）を約４５０個を投入し、蓋で密閉した。
このＰｔ触媒担持カーボン、純水、ボールを含む粉砕用容器１個を遊星回転ボールミル粉砕装置（伊藤製作所製、商品名：遊星回転ポットミル、型番：ＬＰ−４）に設置し、回転数２４０ｒｐｍで、２０分間、自転・公転させることで、Ｐｔ触媒担持カーボンの湿式粉砕を実施した。
粉砕終了後、容器から試料を取り出し、目の粗いふるい等を通してボールを取り除いた。また、容器内及び縁、蓋等に付着した試料は純水で洗い流して回収した。
Examples of the present invention will be described below.
(Example)
3 g of Pt catalyst-supported carbon (carbon: Cabot, trade name: Black Pearl 880, platinum support: 20 wt%) was put into a ball mill grinding container (material: partially stabilized zirconia, internal volume 80 cc) together with 27 g of pure water. Further, about 450 zirconia balls (diameter 5 mm) were put there and sealed with a lid.
One container for pulverization containing this Pt catalyst-supporting carbon, pure water, and balls was installed in a planetary rotating ball mill pulverizer (product name: planetary rotating pot mill, model number: LP-4), and rotated at 240 rpm. By rotating and revolving for 20 minutes, wet pulverization of Pt catalyst-supported carbon was performed.
After completion of the pulverization, the sample was taken out from the container, and the ball was removed through a coarse sieve or the like. Moreover, the sample adhering to the inside of the container, the edge, the lid, and the like was recovered by washing with pure water.
次に、上記粉砕工程で作製した試料を真空凍結乾燥法により乾燥させた。図１に、本実施例で行った真空凍結乾燥装置１の概略を示す。
上記粉砕工程で作製した試料、すなわち、微粉砕Ｐｔ触媒担持カーボンと純水とを含む混合物、をステンレス製容器に入れ、恒温・真空チャンバー２内に設置した。
まず、常圧の状態で、チャンバー２内を０℃以下の温度に設定し、試料を完全に凍結させた。続いて、チャンバー２と接続された真空ポンプ３を用いて、チャンバー２内を減圧し、氷の昇華による乾燥を実施した。なお、本実施例では、真空度を上げて乾燥速度を向上させるため、チャンバー２と真空ポンプ３の間にコールドトラップ４として液体窒素トラップを設置した。また、さらに乾燥速度を向上させるため、チャンバー２の下部に設置したヒーター５で加熱し、試料温度を適度に上昇させた。
この凍結乾燥法により、試料中の純水は全て昇華により除去され、粉砕工程で微粉砕されたＰｔ触媒担持カーボンを再凝集させることなく、回収することができた。
Next, the sample produced in the pulverization step was dried by a vacuum freeze-drying method. In FIG. 1, the outline of the vacuum freeze-drying apparatus 1 performed in the present Example is shown.
The sample prepared in the above pulverization step, that is, a mixture containing finely pulverized Pt catalyst-carrying carbon and pure water, was placed in a stainless steel container and placed in a constant temperature / vacuum chamber 2.
First, the inside of the chamber 2 was set to a temperature of 0 ° C. or lower under normal pressure, and the sample was completely frozen. Subsequently, the inside of the chamber 2 was decompressed using a vacuum pump 3 connected to the chamber 2, and drying by sublimation of ice was performed. In this example, a liquid nitrogen trap was installed as a cold trap 4 between the chamber 2 and the vacuum pump 3 in order to increase the degree of vacuum and improve the drying rate. Further, in order to further improve the drying speed, the sample was heated appropriately by the heater 5 installed at the lower part of the chamber 2 to raise the sample temperature appropriately.
By this freeze-drying method, all pure water in the sample was removed by sublimation, and the Pt catalyst-supported carbon finely pulverized in the pulverization step could be recovered without reaggregation.
上記粉砕工程及び凍結乾燥工程を経て作製された微粉砕Ｐｔ触媒担持カーボンを用いて、本発明者らが通常用いている方法にて、電極用ペースト、燃料電池用電極を作製した。
＜電極用ペーストの製造＞
上記の方法により得られたＰｔ触媒担持カーボン１．３ｇと水３．６ｇとを混合した後、ナフィオン（登録商標、Ｎａｆｉｏｎ（Ｄｕｐｏｎ社製））をイソプロピルアルコールに溶かした５質量％溶液を５．４ｇ加え、公転式遠心攪拌機を用いてよく混合し、実施例の電極用ペーストを得た。
上記Ｐｔ触媒担持カーボンと水との混合の際、さらに超音波等のエネルギーを適度に加えれば、触媒担持カーボンが速やかに水中に分散し、より凝集のない高分散なペーストを製造することが可能である。
Using the finely pulverized Pt catalyst-supported carbon prepared through the pulverization step and the freeze-drying step, an electrode paste and a fuel cell electrode were prepared by a method usually used by the present inventors.
<Manufacture of electrode paste>
After mixing 1.3 g of Pt catalyst-carrying carbon obtained by the above method and 3.6 g of water, 5. 5% by mass solution of Nafion (registered trademark, Nafion (manufactured by Dupon)) dissolved in isopropyl alcohol is used. 4 g was added and mixed well using a revolving centrifugal stirrer to obtain the electrode paste of the example.
When mixing the Pt catalyst-carrying carbon and water, if energy such as ultrasonic waves is added appropriately, the catalyst-carrying carbon is quickly dispersed in water, making it possible to produce a highly dispersed paste with less aggregation. It is.
＜燃料電池単層セルの製造＞
上記電極用ペーストを用いて燃料電池単層セルを作製した。すなわち、上記電極用ペーストをガス拡散層（本実施例ではカーボンクロスを用いた）の表面にスクリーン印刷法により塗布し、乾燥させて、電極Ａを得た。この電極ＡにおけるＰｔ触媒担持量は０．１ｍｇ／ｃｍ２である。
得られた電極Ａをカソード電極とし、このカソード電極、電解質膜（Nafion NRE212CS）、アノード電極を接合して、燃料電池用電極（ＭＥＡ）を作製した。
<Manufacture of fuel cell single layer cells>
A fuel cell single-layer cell was produced using the electrode paste. That is, the electrode paste was applied to the surface of a gas diffusion layer (carbon cloth was used in this example) by screen printing and dried to obtain electrode A. The amount of Pt catalyst supported on this electrode A is 0.1 mg / cm 2 .
The obtained electrode A was used as a cathode electrode, and the cathode electrode, the electrolyte membrane (Nafion NRE212CS), and the anode electrode were joined to produce a fuel cell electrode (MEA).
（比較例）
比較例では、触媒担持カーボンとして、Ｐｔ触媒担持カーボン（カーボン：Cabot社製、商品名Black Pearl 880、白金担持量：20wt%）を何ら処理することなく、そのまま用いた点を除いて、実施例と同様の方法により、電極Ｂを得た。電極ＢにおけるＰｔ触媒担持量は０．１ｍｇ／ｃｍ２である。
得られた電極Ｂを用いて、上記実施例と同様の方法により、燃料電池用電極を作製した。
(Comparative example)
In the comparative example, the Pt catalyst supporting carbon (carbon: manufactured by Cabot, trade name: Black Pearl 880, platinum supporting amount: 20 wt%) was used as the catalyst supporting carbon without any treatment. Electrode B was obtained by the same method as described above. The amount of Pt catalyst supported on electrode B is 0.1 mg / cm 2 .
Using the obtained electrode B, a fuel cell electrode was produced in the same manner as in the above example.
＜評価＞
（電極表面のＳＥＭ写真による比較）
実施例及び比較例の電極表面におけるＰｔ触媒担持カーボンの凝集度合いを比較した。図２（Ａ）に示すのが実施例の電極Ａ、図２（Ｂ）に示すのが比較例の電極Ｂの表面におけるＳＥＭ写真である。
比較例の電極Ｂ表面には、触媒の凝集と思われる“ダマ”が多数発生している。一方、実施例の電極Ａ表面には、電極Ｂで観察されたような“ダマ”はほとんど存在せず、より均質な構造の電極を作製することができていると考えられた。
また、電極Ｂ表面のＥＤＸ（エネルギー分散型Ｘ線分光法）分析の結果、このような“ダマ”の部分では、電極Ｂ全体の平均と比べ、担持したＰｔの比率が高くなるのに対し、一方で、電解質量が少なくなる傾向が見られた。このことから、“ダマ”の部分ではＰｔに電解質が行き届かず、利用できないＰｔの比率が増えるため、“ダマ”が多数存在する電極は、性能が低下すると予想された。
<Evaluation>
(Comparison by SEM photograph of electrode surface)
The degree of aggregation of Pt catalyst-supporting carbon on the electrode surfaces of the example and the comparative example was compared. 2A shows a SEM photograph on the surface of the electrode A of the example, and FIG. 2B shows a surface of the electrode B of the comparative example.
On the surface of the electrode B of the comparative example, a lot of “dama” which seems to be agglomeration of the catalyst is generated. On the other hand, almost no “dama” as observed with the electrode B was present on the surface of the electrode A of the example, and it was considered that an electrode having a more homogeneous structure could be produced.
In addition, as a result of EDX (energy dispersive X-ray spectroscopy) analysis on the surface of the electrode B, the ratio of supported Pt is higher in the “dama” portion than the average of the entire electrode B, whereas On the other hand, the tendency for electrolysis mass to decrease was seen. From this, the electrolyte does not reach Pt in the “dama” portion, and the ratio of unusable Pt increases, so that it was expected that the performance of an electrode having a large number of “dama” would be reduced.
（燃料電池電極性能の比較）
実施例及び比較例の各電極Ａ及びＢを、それぞれ空気極に用いて燃料電池用電極（ＭＥＡ）を作製し、性能の比較を行った。水素−空気フロー時の空気性能の比較を図３示す。
上記ＥＤＸ分析の結果から予想されたとおり、ほぼ全電流域において、比較例と比べ実施例の電極の方が高い性能を示す結果が得られた。本発明の方法で電極を作製することで、より高性能の燃料電池が得られることが確認できた。
(Comparison of fuel cell electrode performance)
A fuel cell electrode (MEA) was produced by using the electrodes A and B of Examples and Comparative Examples as an air electrode, and the performance was compared. FIG. 3 shows a comparison of air performance during hydrogen-air flow.
As expected from the results of the above EDX analysis, in the almost entire current range, the results of the electrode of the example were higher than those of the comparative example. It was confirmed that a fuel cell with higher performance can be obtained by producing an electrode by the method of the present invention.
この発明は、上記発明の実施の形態及び実施例の説明に何ら限定されるものではない。特許請求の範囲の記載を逸脱せず、当業者が容易に想到できる範囲で種々の変形態様もこの発明に含まれる。 The present invention is not limited to the description of the embodiments and examples of the invention described above. Various modifications may be included in the present invention as long as those skilled in the art can easily conceive without departing from the description of the scope of claims.
１ 真空凍結乾燥装置
２ 恒温・真空チャンバー
３ 真空ポンプ
４ コールドトラップ
５ ヒーター
1 Vacuum freeze-drying device 2 Constant temperature / vacuum chamber 3 Vacuum pump 4 Cold trap 5 Heater
Claims (3)
前記触媒担持カーボンと水及び有機溶媒から選択される液体とを含む混合物を湿式粉砕法によって微粉砕し、次いで、減圧下で凍結乾燥する、
ことを特徴とする触媒担持カーボンの処理方法。 A method for treating catalyst-carrying carbon in which metal fine particles having a catalytic function are carried on carbon powder,
A mixture containing the catalyst-supporting carbon and a liquid selected from water and an organic solvent is pulverized by a wet pulverization method , and then freeze-dried under reduced pressure.
A method for treating a catalyst-supporting carbon.
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