JP2585226B2 - Electrolyte matrix for molten carbonate fuel cells - Google Patents
Electrolyte matrix for molten carbonate fuel cellsInfo
- Publication number
- JP2585226B2 JP2585226B2 JP61159137A JP15913786A JP2585226B2 JP 2585226 B2 JP2585226 B2 JP 2585226B2 JP 61159137 A JP61159137 A JP 61159137A JP 15913786 A JP15913786 A JP 15913786A JP 2585226 B2 JP2585226 B2 JP 2585226B2
- Authority
- JP
- Japan
- Prior art keywords
- electrolyte
- molten carbonate
- zro
- holding material
- carbonate fuel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- H01M8/02—Details
- H01M8/0289—Means for holding the electrolyte
- H01M8/0295—Matrices for immobilising electrolyte melts
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fuel Cell (AREA)
Description
【発明の詳細な説明】 ［発明の目的］ （産業上の利用分野） 本発明は溶融炭酸塩燃料電池用電解質マトリックスの
改良に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial application field) The present invention relates to an improvement of an electrolyte matrix for a molten carbonate fuel cell.
（従来の技術） 近年開発が進められている溶融炭酸塩燃料電池は、ア
ルカリ炭酸塩からなる電解質を高温下で溶融状態にし、
電極反応を起こさせるもので、リン酸型、固体電解質型
等の他の燃料電池に比べ、電極反応が起こりやすく、発
電熱効率が高いという利点を有する。(Prior art) Molten carbonate fuel cells, which are being developed in recent years, make an electrolyte composed of an alkali carbonate into a molten state at a high temperature,
It has an advantage that the electrode reaction easily occurs and the heat generation efficiency is high as compared with other fuel cells such as a phosphoric acid type and a solid electrolyte type.
こうした溶融炭酸塩燃料電池の主要部は、通常、電解
質となるアルカリ炭酸塩とセラミックス系保持材とを混
合し平板状に成形した電解質マトリックスの両面にニッ
ケル合金等のガス拡散極を密接して単位電池を構成し、
この単位電池の複数個を相互間に双極性隔離板を介在さ
せて積層した構造を有している。The main part of such a molten carbonate fuel cell is usually formed by mixing a gas diffusion electrode such as a nickel alloy on both sides of an electrolyte matrix formed by mixing an alkali carbonate serving as an electrolyte and a ceramic holding material and forming a flat plate. Make up the battery,
It has a structure in which a plurality of unit batteries are stacked with a bipolar separator interposed therebetween.
従来、保持材としては、例えば粒径0.1〜0.5μｍ、比
表面積10〜25m2/gのγ相を主な構成相とするLiAlO2が用
いられている。このγ‐LiAlO2は溶融炭酸塩中では比較
的安定な化合物であるが、LiAlO2はγ相以外にもβ相、
α相の多形を有し、長時間溶融炭酸塩と反応すると、構
成相の変化が生じる場合がある。特に、α相への転移が
生じると、比表面積が著しく低下するため、電解質保持
性が劣化する。Conventionally, as a holding material, for example, LiAlO 2 having a γ phase having a particle size of 0.1 to 0.5 μm and a specific surface area of 10 to 25 m 2 / g as a main constituent phase has been used. This γ-LiAlO 2 is a relatively stable compound in the molten carbonate, but LiAlO 2 has a β phase,
It has an α-phase polymorph, and when it reacts with molten carbonate for a long time, a change in the constituent phase may occur. In particular, when the transition to the α phase occurs, the specific surface area is significantly reduced, and the electrolyte retention is deteriorated.
保持材の電解質保持特性が劣化すると、電解質の漏
洩、揮散が生じ、内部抵抗を増加させるだけでなく、電
解質の局部的な散逸に伴うクロスオーバーの原因ともな
り、発電特性を著しく低下させるという問題がある。Deterioration of the electrolyte retention characteristics of the holding material causes leakage and volatilization of the electrolyte, which not only increases the internal resistance, but also causes crossover due to the local dissipation of the electrolyte, which significantly reduces the power generation characteristics. There is.
一方、溶融炭酸塩に対して比較的安定な物質としてZr
O2が知られており、特にY2O3、CaO等の添加により安定
化又は部分安定化されたものは溶融炭酸塩に対する長期
にわたる安定性が立証されている。しかし、ZrO2や部分
安定化ZrO2は溶融炭酸塩に対するぬれ性に乏しいため、
やはり電解質保持特性が悪く、保持材として用いること
はできない。On the other hand, Zr is a relatively stable substance to molten carbonate.
O 2 is known, and particularly those stabilized or partially stabilized by the addition of Y 2 O 3 , CaO, etc., have demonstrated long-term stability to molten carbonate. However, since ZrO 2 and partially stabilized ZrO 2 have poor wettability to molten carbonate,
Again, the electrolyte retention properties are poor and cannot be used as a retention material.
（発明が解決しようとする問題点） 本発明は上記問題点を解決するためになされたもので
あり、電解質保持特性が劣化しない保持材を用い、長時
間にわたって良好な発電特性を得ることができる溶融炭
酸塩燃料電池用電解質マトリックスを提供することを目
的とする。(Problems to be Solved by the Invention) The present invention has been made in order to solve the above problems, and a good power generation characteristic can be obtained for a long time by using a holding material that does not deteriorate the electrolyte holding characteristics. An object of the present invention is to provide an electrolyte matrix for a molten carbonate fuel cell.
［発明の構成］ （問題点を解決するための手段と作用） 本発明の溶融炭酸塩燃料電池用電解質マトリックス
は、アルカリ炭酸塩粉末からなる電解質と、0.5〜５モ
ル％のイットリアを添加した部分安定化ジルコニアをリ
チウム化することにより合成されたLi2（YxZr1-x）O3で
表される化合物の粉末からなる保持材とを含有すること
を特徴とするものである。[Structure of the Invention] (Means and Action for Solving the Problems) The electrolyte matrix for a molten carbonate fuel cell of the present invention comprises an electrolyte composed of an alkali carbonate powder and a portion to which 0.5 to 5 mol% of yttria is added. it is characterized in that it contains a holding material made of powder of Li 2 synthesized (YxZr 1- x) O 3 in the compound represented by by lithiation stabilized zirconia.
保持材としてのLiAlO2やZrO2の問題点から明らかなよ
うに、保持材に要求される特性としては、溶融炭酸塩
に対して長時間化学的に安定であること、溶融炭酸塩
に対するぬれ性に優れていること、という２点が挙げら
れる。本発明者らは、上記２つの特性を満足する材料に
ついて種々検討した。As is evident from the problems of LiAlO 2 and ZrO 2 as the holding material, the properties required of the holding material are that it is chemically stable for a long time in molten carbonate, wettability to molten carbonate And that it is excellent. The present inventors have studied various materials that satisfy the above two characteristics.
その結果、まずZrO2や部分安定化ZrO2をLiOHやLi2CO3
と反応させることによりリチウム化したものは、溶融炭
酸塩に対するぬれ性が改善されることが確認された。As a result, first, ZrO 2 or partially stabilized ZrO 2 was converted to LiOH or Li 2 CO 3
It was confirmed that the lithiated one was allowed to react with the compound to improve the wettability to molten carbonate.
ところが、ZrO2（単斜晶）を出発原料としてこれをリ
チウム化することにより生成されるLi2ZrO3は、溶融炭
酸塩との反応により部分的に原料であるZrO2（単斜晶）
を相転移することが判明した。ZrO2（単斜晶）は、上述
したように溶融炭酸塩に対するぬれ性が悪いので、Li2Z
rO3は保持材として適当な材料ではない。However, Li 2 ZrO 3 produced by lithiating ZrO 2 (monoclinic) as a starting material is partially converted into ZrO 2 (monoclinic) by reaction with molten carbonate.
Was found to undergo a phase transition. Since ZrO 2 (monoclinic) has poor wettability to molten carbonate as described above, Li 2 Z
rO 3 is not a suitable material as a holding material.
一方、部分安定化ZrO2、例えばY2O3部分安定化ZrO
2は、ZrO2（単斜晶）とY0.15 Zr0.85 O1.93（以下YZと
記す）とを構成相とし、ZrO2添加量の増加に伴ってYZの
比率が増加する。この部分安定化ZrO2をリチウム化する
ことにより得られる化合物は、Li2（YxZr1-x）O3（以
下、LZ（Ｙ）と記す）で示される。そして、このLZ
（Ｙ）は、溶融炭酸塩との反応により若干のYZを生成す
ることはあるが、ZrO2（単斜晶）の生成は著しく低減化
され、全体的には低温相（ZrO2（単斜晶）及びYZ）の生
成は抑制される。また、低温相は、ほとんど溶融炭酸塩
との反応の初期段階で生じ、その後は構成比がほとんど
変化せずLZ（Ｙ）が安定に存在する。このことは、Y2O3
以外のCaO等で部分安定化したZrO2を用いた場合でも同
様である。On the other hand, partially stabilized ZrO 2 , for example, Y 2 O 3 partially stabilized ZrO 2
2, and ZrO 2 and (monoclinic) and Y 0. 15 Zr 0. 85 O 1. 93 ( hereinafter referred to as YZ) and the configuration phase, the ratio of the YZ increases with increasing ZrO 2 amount . A compound obtained by lithiating the partially stabilized ZrO 2 is represented by Li 2 (YxZr 1 -x) O 3 (hereinafter, referred to as LZ (Y)). And this LZ
(Y) may form a small amount of YZ due to the reaction with the molten carbonate, but the formation of ZrO 2 (monoclinic) is significantly reduced, and the low-temperature phase (ZrO 2 (monoclinic) ) And YZ) are suppressed. Further, the low-temperature phase occurs almost at the initial stage of the reaction with the molten carbonate, and thereafter, the composition ratio hardly changes and LZ (Y) is stably present. This means that Y 2 O 3
The same applies to the case where ZrO 2 partially stabilized with CaO or the like other than that described above is used.
以上のような部分安定化ZrO2をリチウム化した粉末を
保持材として用いれば、長期間にわたって電解質保持特
性が維持され、発電特性の劣化の少ない溶融炭酸塩燃料
電池用電解質マトリックスを提供することができる。By using the above-mentioned powder obtained by lithiating partially stabilized ZrO 2 as a holding material, it is possible to provide an electrolyte matrix for a molten carbonate fuel cell in which the electrolyte holding characteristics are maintained for a long time and the power generation characteristics are less deteriorated. it can.
なお、本発明に係る電解質マトリックスは、アルカリ
炭酸塩粉末、部分安定化ZrO2をリチウム化した粉末のほ
かに、補強材を含んでいてもよい。補強材としては、例
えば部分安定化ZrO2をリチウム化した繊維が挙げられ
る。また、部分安定化ZrO2をリチウム化した粉末や繊維
が化学的に安定であるという要求を満たすためには、Zr
O2を部分安定化するための酸化物の添加量が適当である
ことが必要であり、例えばY2O3の添加量は0.5〜５モル
％であることが望ましい。The electrolyte matrix according to the present invention may contain a reinforcing material in addition to the alkali carbonate powder and the powder obtained by lithiating partially stabilized ZrO 2 . As the reinforcing material, for example, a fiber obtained by lithiating partially stabilized ZrO 2 may be mentioned. In order to satisfy the requirement that powder or fiber obtained by lithiating partially stabilized ZrO 2 be chemically stable, ZrO 2
It is necessary that the addition amount of the oxide for partially stabilizing O 2 be appropriate, for example, the addition amount of Y 2 O 3 is 0.5 to 5 mol%.
（実施例） 以下、本発明の実施例を説明する。(Example) Hereinafter, an example of the present invention will be described.
まず、下記表に示すようにY2O3添加量が異なり、構成
相の比率が異なる５種類の部分安定化ZrO2（以下、PSZ
と記す）粉末を出発原料とし、これらとLiOH・H2Oとを
モル比でそれぞれ1:2の割合で混合した。次に、これら
の混合粉をそれぞれ高純度アルミナ容器に充填し、大気
中、1100℃において10時間熱処理してリチウム化を行な
い、保持材を合成した。合成された保持材の構成相の比
率を下記表に示す。First, as shown in the table below, five types of partially stabilized ZrO 2 (hereinafter, PSZ) having different amounts of added Y 2 O 3 and different ratios of the constituent phases.
The powders were used as starting materials, and these and LiOH.H 2 O were mixed at a molar ratio of 1: 2. Next, each of these mixed powders was filled in a high-purity alumina container, and heat-treated at 1100 ° C. in the air for 10 hours to perform lithiation to synthesize a holding material. The ratio of the constituent phases of the synthesized holding material is shown in the following table.
つづいて、各保持材をボールミルを用いて粉砕し、粒
径0.5μｍ以下の微粉末とした。更に、各保持材粉末と
アルカリ炭酸塩粉末とを、保持材:Li2CO3:K2CO3＝40:2
8:32の重量比で混合した。これら混合粉40gをそれぞれ1
0cm角の金型に充填し、460℃において300kg/cm2の圧力
を加え、１時間保持してホットプレス成形した。これに
よって、厚み約1.5mm、見掛け密度2.6g/cm3の電解質マ
トリックスが得られた。Subsequently, each holding material was pulverized using a ball mill to obtain a fine powder having a particle size of 0.5 μm or less. Further, each of the holding material powder and the alkali carbonate powder was mixed with the holding material: Li 2 CO 3 : K 2 CO 3 = 40: 2
They were mixed at a weight ratio of 8:32. 40 g of these mixed powders each 1
The mold was filled into a 0 cm square mold, and a pressure of 300 kg / cm 2 was applied at 460 ° C., and held for 1 hour to perform hot press molding. As a result, an electrolyte matrix having a thickness of about 1.5 mm and an apparent density of 2.6 g / cm 3 was obtained.
次いで、得られた各電解質マトリックスを4cm角に切
断し、その両面を多孔質Ni電極で挟んで溶融炭酸塩燃料
電池の単位電池を構成した。各単位電池について、アノ
ード側にH2ガス及びCOガスを、カソード側に空気及びCO
2ガスをそれぞれ供給して300時間の発電試験を行なっ
た。試験後、それぞれの単位電池から電解質マトリック
スを取出し、保持材の構成相及び電解質の保持率を調べ
た。その結果を下記表に示す。Next, each of the obtained electrolyte matrices was cut into 4 cm squares, and both sides thereof were sandwiched between porous Ni electrodes to form a unit cell of a molten carbonate fuel cell. For each unit cell, the H 2 gas and CO gas to the anode side, air and CO on the cathode side
A power generation test was performed for 300 hours by supplying each of the two gases. After the test, the electrolyte matrix was taken out of each unit cell, and the constituent phases of the holding material and the holding ratio of the electrolyte were examined. The results are shown in the table below.
なお、下記表には比較例として、保持材にLiAlO2を用
い、上記と全く同様な試験を行なった場合の結果も併記
する。The following table also shows, as a comparative example, the results obtained when the same test was performed using LiAlO 2 as the holding material.
上記表から明らかなように、部分安定化ZrO2（PSZ）
はNo.1〜No.5の順に、Y2O3添加量が増加するにしたがっ
て、その構成相はYZの比率が増加している。これらPSZ
をリチウム化して合成された保持材では、No.1〜No.5の
順にLZ（Ｙ）の比率が減少している。そして、発電試験
後の保持材のLZ（Ｙ）の比率と電解質の保持率とはほぼ
対応しており、LZ（Ｙ）の比率が高いほど電解質の保持
率が高くなっている。ただし、PSZ中のY2O3の添加量が
少ない場合（No.1）には、発電試験後にZrO2（単斜晶）
が多く生成し、ぬれ性が悪くなるため電解質の保持率が
低下している。 As is clear from the above table, partially stabilized ZrO 2 (PSZ)
In the No. 1 to No. 5, in the order of addition of Y 2 O 3 , the ratio of YZ increases in the constituent phases as the addition amount increases. These PSZ
In the holding material synthesized by lithiation of, the ratio of LZ (Y) decreases in the order of No. 1 to No. 5. The LZ (Y) ratio of the holding material after the power generation test substantially corresponds to the electrolyte retention, and the higher the LZ (Y) ratio, the higher the electrolyte retention. However, when the addition amount of Y 2 O 3 in PSZ is small (No. 1), ZrO 2 (monoclinic) after the power generation test
Are generated and the wettability deteriorates, so that the retention of the electrolyte is lowered.
また、上記表から、従来のLiAlO2よりも優れた電解質
保持特性を得るためには、PSZ中のY2O3添加量は0.5〜５
モル％が適当であることがわかる。From the above table, in order to obtain an electrolyte retention characteristic superior to conventional LiAlO 2, the amount of Y 2 O 3 added in PSZ is 0.5 to 5
It turns out that mol% is appropriate.
なお、上記実施例ではアルカリ炭酸塩粉末と部分安定
化ZrO2をリチウム化した粉末とで電解質マトリックスを
構成したが、これらのほかに補強材として部分安定化Zr
O2をリチウム化した繊維を混合してもよい。In the above embodiment, the electrolyte matrix was composed of an alkali carbonate powder and a powder obtained by lithiating partially stabilized ZrO 2 , but in addition to these, partially stabilized ZrO 2 was used as a reinforcing material.
The O 2 can be mixed lithiated fibers.
［発明の効果］ 以上詳述したように本発明によれば、電解質保持特性
が劣化しない保持材を用い、長時間にわたって良好な発
電特性を得ることができる溶融炭酸塩燃料電池用電解質
マトリックスを提供できるものである。[Effects of the Invention] As described in detail above, according to the present invention, there is provided an electrolyte matrix for a molten carbonate fuel cell that can obtain good power generation characteristics over a long period of time using a holding material that does not deteriorate the electrolyte retention characteristics. You can do it.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 柘植 章彦 神奈川県川崎市幸区小向東芝町１番地 株式会社東芝総合研究所内 (56)参考文献 特開 昭60−151976（ＪＰ，Ａ) 特開 昭56−82583（ＪＰ，Ａ) 特開 昭60−35468（ＪＰ，Ａ) ──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Akihiko Tsuge 1 Kogamu Toshiba-cho, Saiwai-ku, Kawasaki-shi, Kanagawa Prefecture Toshiba Research Institute, Inc. (56) References JP-A-60-151976 (JP, A) JP-A-56-82583 (JP, A) JP-A-60-35468 (JP, A)
Claims (1)
5〜５モル％のイットリアを添加した部分安定化ジルコ
ニアをリチウム化することにより合成されたLi2（YxZr
1-x）O3で表される化合物の粉末からなる保持材とを含
有することを特徴とする溶融炭酸塩燃料電池用電解質マ
トリックス。1. An electrolyte comprising an alkali carbonate powder,
Li 2 (YxZr) synthesized by lithiating partially stabilized zirconia to which 5 to 5 mol% yttria has been added.
1- x) An electrolyte matrix for a molten carbonate fuel cell, comprising: a holding material comprising a powder of a compound represented by O 3 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61159137A JP2585226B2 (en) | 1986-07-07 | 1986-07-07 | Electrolyte matrix for molten carbonate fuel cells |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61159137A JP2585226B2 (en) | 1986-07-07 | 1986-07-07 | Electrolyte matrix for molten carbonate fuel cells |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6316567A JPS6316567A (en) | 1988-01-23 |
| JP2585226B2 true JP2585226B2 (en) | 1997-02-26 |
Family
ID=15687057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61159137A Expired - Fee Related JP2585226B2 (en) | 1986-07-07 | 1986-07-07 | Electrolyte matrix for molten carbonate fuel cells |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2585226B2 (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5682583A (en) * | 1979-12-10 | 1981-07-06 | Hitachi Ltd | Fuel cell |
| JPS6035468A (en) * | 1983-08-03 | 1985-02-23 | Agency Of Ind Science & Technol | Electrolyte matrix for fuel cell |
| JPS60151976A (en) * | 1984-01-20 | 1985-08-10 | Fuji Electric Corp Res & Dev Ltd | Manufacturing of electrolyte holding plate |
-
1986
- 1986-07-07 JP JP61159137A patent/JP2585226B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6316567A (en) | 1988-01-23 |
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