JPH0832770B2 - Electrolytic organic polymer membrane - Google Patents
Electrolytic organic polymer membraneInfo
- Publication number
- JPH0832770B2 JPH0832770B2 JP61023219A JP2321986A JPH0832770B2 JP H0832770 B2 JPH0832770 B2 JP H0832770B2 JP 61023219 A JP61023219 A JP 61023219A JP 2321986 A JP2321986 A JP 2321986A JP H0832770 B2 JPH0832770 B2 JP H0832770B2
- Authority
- JP
- Japan
- Prior art keywords
- organic polymer
- electrolytic
- particles
- metal
- fine powder
- 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
- 229920000620 organic polymer Polymers 0.000 title claims description 18
- 239000012528 membrane Substances 0.000 title claims 2
- 239000000843 powder Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000000919 ceramic Substances 0.000 claims 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims 1
- 229910001507 metal halide Inorganic materials 0.000 claims 1
- 150000005309 metal halides Chemical class 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- 229910052976 metal sulfide Inorganic materials 0.000 claims 1
- 150000004767 nitrides Chemical class 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 description 29
- 239000008151 electrolyte solution Substances 0.000 description 12
- 229920000642 polymer Polymers 0.000 description 10
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 229920006254 polymer film Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910013063 LiBF 4 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- -1 demethylformamide Chemical compound 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- DZKDPOPGYFUOGI-UHFFFAOYSA-N tungsten(iv) oxide Chemical compound O=[W]=O DZKDPOPGYFUOGI-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 本発明は電解酸化重合によって得られる有機高分子膜
に関するもので、特に、微粉末を含有した有機高分子膜
に関するものである。TECHNICAL FIELD The present invention relates to an organic polymer film obtained by electrolytic oxidation polymerization, and more particularly to an organic polymer film containing fine powder.
従来の技術 電解酸化重合によって得られる高分子は、その合成の
コントロールが電圧、通電電気量によって行なう事が出
来るため、又最近では、合成した高分子のもつ物性にお
いて、電子伝導性あるいは半導体特性を附与させうるこ
とから活発に検討されている。例えば、有機高分子とし
て、ポリピロールを例にとると、その電解重合は次の如
く行なわれる。即ち、電解液として、有機溶媒（例え
ば、アセトニトリル，デメチルホルムアミド，プロピレ
ンカーボネート等）に、ホウフッ化リチウム（LiB
F4），過塩素酸リチウム（LiClO4）等の電解質を溶解し
た溶液中に重合したい有機モノマー（この場合、ピロー
ル）を溶解させた電解液を用い、該電解液中に試料電極
と対向電極、更に必要に応じて、試料電極に印加する電
位を規制するための参照電極を挿入し、試料電極に正電
圧を印加しながら、ピロールを電解酸化することによ
り、ピロールポリマーを試料電極表面に重合析出させて
いる。このようにして得られた有機高分子は、高分子内
への陰イオン、例えばBF4 -のドーピング又は脱ドーピン
グにより、電子伝導性の程度あるいは半導体特性を変化
させうる性質を有している。したがって、これらの特性
を利用して、電池、FETトランジスター、電磁波シール
ド材への応用が検討されている。しかし、電池とした場
合、そのエネルギー密度が比較的小さい事、FETトラン
ジスターとした場合、有分子が緻密で、かつ平滑な状態
で析出させる事が困難なため、P,N接合面の接合状態が
悪く、従来のFETと比較して、優れた特性が少ないな
ど、のことから、その応用展開を活発に進めるための魅
力に欠けていた。2. Description of the Related Art Polymers obtained by electrolytic oxidative polymerization can be controlled by the voltage and the amount of electricity applied, and recently, in the physical properties of the synthesized polymers, electronic conductivity or semiconductor characteristics have been improved. It is being actively studied because it can be attached. For example, taking polypyrrole as the organic polymer, the electrolytic polymerization is carried out as follows. That is, as an electrolytic solution, an organic solvent (for example, acetonitrile, demethylformamide, propylene carbonate, etc.) and lithium borofluoride (LiB
F 4 ), lithium perchlorate (LiClO 4 ), etc., in which an organic monomer to be polymerized (in this case, pyrrole) is dissolved in a solution in which an electrolyte is dissolved. If necessary, a reference electrode for regulating the potential applied to the sample electrode is inserted, and the pyrrole polymer is polymerized on the sample electrode surface by electrolytically oxidizing pyrrole while applying a positive voltage to the sample electrode. Have been deposited. The organic polymer thus obtained has a property that the degree of electronic conductivity or semiconductor characteristics can be changed by doping or dedoping anion, for example, BF 4 − into the polymer. Therefore, using these characteristics, application to batteries, FET transistors, and electromagnetic wave shielding materials is being studied. However, in the case of a battery, the energy density is relatively small, and in the case of a FET transistor, it is difficult to deposit the molecules with a dense and smooth state, so the bonding state of the P and N bonding surfaces is Poorly, it lacked the superior characteristics compared to conventional FETs, so it lacked the attractiveness for actively promoting its application development.
発明が解決しようとする問題点 本発明は、従来高分子膜が有している機能以外に、種
々の機能を有した高分子膜とすることにより、多用途
へ、高分子の応用を展開をひろげようとするものであ
る。DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention The present invention expands the application of polymers to various uses by providing a polymer film having various functions in addition to the functions that conventional polymer films have. It is an attempt to expand.
問題点を解決するための手段 各種機能に応じた微粉末を電解有機高分子膜中に含有
させる。Means for Solving the Problems Fine powders corresponding to various functions are contained in the electrolytic organic polymer film.
作用 微粉末を含有させることにより出来た膜は、有機高分
子単独の特性のみならず、微粉末のもつ特性を兼ねそな
えた膜とすることが出来る。Action The film formed by containing the fine powder can have not only the characteristics of the organic polymer alone but also the characteristics of the fine powder.
実施例 本発明の電解有機高分子膜は、微粉末を電解液中に含
有させ、有機モノマーを電解酸化重合させることによ
り、容易に作成できる。Example The electrolytic organic polymer film of the present invention can be easily prepared by containing fine powder in an electrolytic solution and electrolytically oxidizing and polymerizing an organic monomer.
粒子を導体内に共析させることは、電気鍍金技術分野
において広く使われている。即ち、電気メッキ浴中に粒
子を分散させ、浴中の金属イオンを還元することによ
り、析出金属内に粒子を共析するものである。即ち、浴
中でに帯電している粒子が、金属イオンを還元する際
負極に引き寄せられ、金属と共に析出するとされてい
る。本発明は、前記現象が反応の全く異なる系である電
解酸化重合に適用出来ることを見出したことによる。そ
の原因は明確でないが、単に機械的に微粉末が電極表面
に接触すると同時に析出する有機高分子にトラップされ
るものと考える。以下、実施例をもとに本発明を説明す
る。Co-depositing particles within a conductor is widely used in the electroplating art. That is, the particles are dispersed in an electroplating bath and the metal ions in the bath are reduced to eutect the particles in the deposited metal. That is, it is said that the particles charged in the bath are attracted to the negative electrode when the metal ions are reduced and deposited together with the metal. The present invention is based on the finding that the above phenomenon can be applied to electrolytic oxidative polymerization, which is a system having completely different reactions. The reason for this is not clear, but it is considered that the fine powder is mechanically trapped by the organic polymer that comes into contact with the electrode surface and is deposited at the same time. Hereinafter, the present invention will be described based on examples.
実施例１ 第１図は本発明による電解重合装置を示したものであ
る。図中１はアノード室、カソード室を分離するガラス
よりなるセパレーター２を中間に介在させたガラス製の
電解槽である。３は有機高分子を得るためのステンレス
スティール（１cm2）製の試料電極であり、４は試料電
極に印加する電位を規制するために使用した参照電極
で、こゝでは銀を用いた。５は白金電極よりなる対向電
極、６は電解液で、１％ピロールを含む1M−LiBF4／ア
セトニトリルを用いた。７は微粉末で、こゝでは粒径50
μ以下の粒子状酸化タングステン（WO3）粉末を用い
た。８は電解液を撹はんするための撹はん棒で、9,10は
各々撹はん棒を支えるための軸受と回転を伝えるための
プーリーである。該電解液を撹はんしながら、ポテシオ
スタット11とファンクションゼネレーター12を用い電解
電位を規制しながら電解した。電解条件は20℃，＋0.7V
（VvsAg）で１時間電解した。Example 1 FIG. 1 shows an electrolytic polymerization apparatus according to the present invention. In the figure, 1 is a glass electrolytic cell with a separator 2 made of glass for separating the anode chamber and the cathode chamber interposed in between. 3 is a sample electrode made of stainless steel (1 cm 2 ) for obtaining an organic polymer, 4 is a reference electrode used to regulate the potential applied to the sample electrode, and silver is used here. 5 is a counter electrode composed of a platinum electrode, 6 is an electrolytic solution, and 1 M-LiBF 4 / acetonitrile containing 1% pyrrole was used. 7 is a fine powder, and the particle size is 50 here.
A particulate tungsten oxide (WO 3 ) powder having a particle size of μ or less was used. Reference numeral 8 is a stirring rod for stirring the electrolytic solution, and 9 and 10 are bearings for supporting the stirring rod and pulleys for transmitting rotation. While stirring the electrolytic solution, electrolysis was carried out while controlling the electrolytic potential using a potato stat 11 and a function generator 12. Electrolysis conditions are 20 ℃, + 0.7V
(VvsAg) was electrolyzed for 1 hour.
実施例２ 電解液中に含有させる微粉末粒子として、直径50μの
酸化タングステン（WO2）を用いた以外、実施例１と全
く同様にして、有機高分子を電解重合した。Example 2 An organic polymer was electrolytically polymerized in exactly the same manner as in Example 1 except that tungsten oxide (WO 2 ) having a diameter of 50 μm was used as the fine powder particles contained in the electrolytic solution.
実施例３ 電解液中に含有させる微粉末粒子として、直径50μ以
下の金属タングステン粒子Ｗを用いた以外は実施例１と
全く同様にして、有機高分子を電解重合した。Example 3 An organic polymer was electrolytically polymerized in exactly the same manner as in Example 1 except that metal tungsten particles W having a diameter of 50 μm or less were used as the fine powder particles to be contained in the electrolytic solution.
以上、実施例１〜３によって得た有機高分子は直視的
にも、各微粉末粒子が入っていることが確認することが
出来るが、各々の膜に含まれる粒子をＸ線光電子分光装
置により確認した結果、各々の粒子について第２図の如
きチャートを得、有機高分子内に粒子の存在を確認し
た。As described above, the organic polymers obtained in Examples 1 to 3 can be confirmed, even directly, that each fine powder particle is contained. The particles contained in each film can be analyzed by an X-ray photoelectron spectrometer. As a result of the confirmation, a chart as shown in FIG. 2 was obtained for each particle, and the presence of the particle in the organic polymer was confirmed.
実施例４ 電解液中に含有させる粒子として、直径30μ以下の酸
化モリブデンを用い、実施例１の装置を用い電解重合し
た。この際、電解重合の為に電極に印加した電圧は＋0.
7、４秒、−0.6V、１秒の周期的に一定時間逆電圧が加
わる反転パルス電圧波形を与えた。表１は電気量（酸化
電流の積分値）を同一（1.0/cm2）にし、電解酸化重合
によって得られる有機高分子の重量変化を粒子を入れな
いで得た高分子の重量を100とした場合、粒子を入れ、
直流のみで得た高分子、粒子を入れ、反転パルス電圧を
与え電解し得た高分子について重量を示したものであ
る。表から明らかなように反転パルス電圧を与え電解し
得た高分子の重量が大きい事が分る。これは、電解液中
の粒子が陰分極した際に電極に引き寄せられると共に、
電極面で電荷ｅを受けとり、粒子内に電解液中のH+がト
ラップされ、粒子自身が絶縁体から導体へ変化し、次
に、この状態で陽分極が起こると電極面と粒子面で有機
モノマーの酸化が進行するため、実施例１〜３の方法以
上に効率よくルールが有機高分子の中に入ったためと考
えられる。Example 4 As the particles to be contained in the electrolytic solution, molybdenum oxide having a diameter of 30 μm or less was used, and electrolytic polymerization was performed using the apparatus of Example 1. At this time, the voltage applied to the electrode for electrolytic polymerization is +0.
An inverted pulse voltage waveform was applied to which a reverse voltage was periodically applied for 7, 4 seconds, -0.6 V, and 1 second for a fixed time. Table 1 shows that the amount of electricity (integrated value of oxidation current) was the same (1.0 / cm 2 ) and the weight change of the organic polymer obtained by electrolytic oxidation polymerization was 100 without weight. If you put particles,
The weight is shown for the polymer obtained by only applying a direct current and the polymer obtained by introducing particles and electrolyzing by applying an inversion pulse voltage. As is clear from the table, it is found that the weight of the polymer obtained by applying an inversion pulse voltage and electrolyzing is large. This is because when the particles in the electrolyte are negatively polarized, they are attracted to the electrode,
The charge e is received on the electrode surface, H + in the electrolytic solution is trapped inside the particle, the particle itself changes from an insulator to a conductor, and then when anodic polarization occurs in this state, the organic surface on the electrode surface and the particle surface. It is considered that the rule entered the organic polymer more efficiently than the method of Examples 1 to 3 because the oxidation of the monomer proceeded.
以下、各種材料粒子について検討した実施例を表にし
て示す。 Examples of various material particles are shown below in a table.
尚、本発明では、粒子を電解液中に分散し、電解する
方法のみを示したが、電極表面に粒子を沈降せしめなが
ら、あるいは多量の粒子を電解液で湿潤せしめた中に試
料電極を挿入し電解合成することによって、多量の粒子
内に高分子を析出させた膜も、本発明の範囲に属するも
のである。又、実施例より明らかなごとく、電解液に対
して、不溶な材料は全く使用することが可能である。し
たがって、微細な軽いパルプ、有機繊維も使用すること
が出来る。 In the present invention, only the method of dispersing particles in an electrolytic solution and electrolyzing is shown, but while the particles are allowed to settle on the electrode surface, or a large amount of particles are wetted with the electrolytic solution, the sample electrode is inserted. A film obtained by precipitating a polymer in a large amount of particles by electrolytic synthesis also belongs to the scope of the present invention. Further, as is clear from the examples, it is possible to use a material that is insoluble in the electrolytic solution. Therefore, fine light pulp and organic fibers can also be used.
発明の効果 粒子を含有した高分子膜を得られることは、粒子とし
て種々の機能を有した材料を用いることにより、各種機
能を有したセンサー，ディスプレー素子，電池の容量の
向上等、その応用展開技術分野を拡大しうることに効果
が期待される。EFFECTS OF THE INVENTION It is possible to obtain a polymer film containing particles, by using materials having various functions as particles, it is possible to improve the capacity of sensors, display elements, batteries, etc. having various functions. The effect is expected to be able to expand the technical field.
【図面の簡単な説明】 第１図は、本発明の一実施例における高分子膜を得るた
めの電解装置の断面図、第２図は、高分子中の粒子のES
CAによる分析結果を示すグラフである。 １……電解槽、３……試料電極、４……参照電極、５…
…対向電極、６……電解液、７……微粉末粒子。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a cross-sectional view of an electrolyzer for obtaining a polymer film in one embodiment of the present invention, and FIG. 2 is an ES of particles in a polymer.
It is a graph which shows the analysis result by CA. 1 ... electrolytic cell, 3 ... sample electrode, 4 ... reference electrode, 5 ...
... Counter electrode, 6 ... electrolyte, 7 ... fine powder particles.
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｂ 1/12 Ｅ Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI technical display area H01B 1/12 E
Claims (2)
高分子膜。1. An electrolytic organic polymer film comprising a fine powder.
物，金属硫化物，金属ハロゲン化物，金属炭化物，カー
ボン，フッ化カーボン，ガラス，セラミック，有機金属
又は有機物からなる事を特徴とする特許請求範囲第１項
記載の電解有機高分子膜。2. A fine powder comprising a metal, a metal oxide, a metal nitride, a metal sulfide, a metal halide, a metal carbide, carbon, a fluorocarbon, glass, a ceramic, an organic metal or an organic substance. The electrolytic organic polymer membrane according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61023219A JPH0832770B2 (en) | 1986-02-05 | 1986-02-05 | Electrolytic organic polymer membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61023219A JPH0832770B2 (en) | 1986-02-05 | 1986-02-05 | Electrolytic organic polymer membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62181325A JPS62181325A (en) | 1987-08-08 |
| JPH0832770B2 true JPH0832770B2 (en) | 1996-03-29 |
Family
ID=12104542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61023219A Expired - Fee Related JPH0832770B2 (en) | 1986-02-05 | 1986-02-05 | Electrolytic organic polymer membrane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0832770B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0757699B2 (en) * | 1987-12-24 | 1995-06-21 | 株式会社リコー | Method for producing composite of conductive polymer material |
| JP2002198067A (en) * | 2000-12-25 | 2002-07-12 | Hitachi Ltd | High temperature operation type solid polymer composite electrolyte membrane, membrane / electrode assembly, and fuel cell |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5975943A (en) * | 1982-10-25 | 1984-04-28 | Showa Denko Kk | Production of electrically conductive polymer composition |
-
1986
- 1986-02-05 JP JP61023219A patent/JPH0832770B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62181325A (en) | 1987-08-08 |
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