CN100336174C - Method of preparating pattern conducting polyphenyl amine film - Google Patents
Method of preparating pattern conducting polyphenyl amine film Download PDFInfo
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- CN100336174C CN100336174C CNB2003101193291A CN200310119329A CN100336174C CN 100336174 C CN100336174 C CN 100336174C CN B2003101193291 A CNB2003101193291 A CN B2003101193291A CN 200310119329 A CN200310119329 A CN 200310119329A CN 100336174 C CN100336174 C CN 100336174C
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Abstract
The present invention discloses a method for preparing a silicon surface patterned conductive polyaniline film, which adopts organosilane and aniline which are easily adsorbed on the surface of a single crystal silicon chip as raw materials. The preparation method comprises two preparation steps of patterning a self-assembled film and a conductive polyaniline film. The method is characterized in that the preparation method is simple, and the product compositions are easy to control. The obtained patterns have smooth surface and clear boundary.
Description
Technical field
The present invention relates to a kind of preparation method of silicon pattern conducting pan film.
Background technology
Polyaniline has the total character of other aromatic ring conducting polymer, and with its higher conductivity and charge storage capacity, environmental stability, raw material are easy to get and prepare advantages such as simple preferably, and be considered to have the conducting high polymers thing of wishing to obtain practical application at present most.From Diza (Electroanal.Chem. in 1980,1980,111 (1): 111) successfully utilize electrochemical oxidation to prepare since the electroactive polyaniline film, electrochemical behavior about the electrochemical polymerization polyaniline, people have done number of research projects, and the research of aspects such as synthetic, the structure of relevant polyaniline and performance also has the lot of documents report.Even it is but rare about the electrochemical preparation method of patterning polyaniline film.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of silicon pattern conducting pan film.
A kind of preparation method of pattern conducting pan film is characterized in that this method in turn includes the following steps:
A. the preparation of patterning self-assembled film
The seal of cleaning is immersed in the n-hexane or anhydrous toluene solution of octadecyl trichlorosilane (OTS) monomer that concentration is 1mM-10mM, keep 1-5s; After treating the n-hexane or dry toluene volatilization fully on the seal, contact 10s-30s, use acetone supersound washing monocrystalline silicon piece then, obtain the monocrystalline silicon piece of patterning, promptly form the self-assembled film of patterning at monocrystalline silicon surface with the monocrystalline silicon sheet surface of cleaning;
B. the preparation of pattern conducting pan film
Monocrystalline silicon piece with described patterning is a work electrode, platinum is auxiliary electrode, the Ag/AgCl electrode is a reference electrode, KCl or NaCl are supporting electrolyte, in the acid solution of 0.05M-0.5M aniline monomer, carry out electrochemical polymerization, the PH of control solution is between 0-2, and silicon chip carried out ultrasonic cleaning with secondary water after polymerization was finished.
The used seal of the present invention press literature method preparation (Annu.Rev.Matter.Sci., 1998,28:153).At first, the silicon chip sample after surface treatment, is carried out etching with photoetching process on the surface, make the micrometre-grade pattern of its surperficial formation rule.Be mould with this template again, Sylgard184 (Dow Corning company) is cast in the surface of its patterning, at 65 ℃--150 ℃ of following curing moldings form the elastomeric stamp with little pattern.
The used monocrystalline silicon piece of the present invention is n (100), p (100) or p (111) type monocrystalline silicon.
Used acid solution is selected from hydrochloric acid solution or sulfuric acid solution in the B step of the present invention.
Said electrochemical method refers to cyclic voltammetry, potentiostatic method or galvanostatic method in the B step of the present invention.
Utilization of the present invention has the semiconductor monocrystal silicon base and different electrochemical polymerization conditions of pattern, and the speed of growth of control polyaniline film is for the preparation of pattern conductive polyaniline film provides a new approach.The preparation method is simple for this method, and the product composition is easy to control, and the patterned surfaces that is obtained is smooth, sharpness of border.
Description of drawings
What Fig. 1 represented is silicon pattern conducting pan film preparation method process chart.
What Fig. 2 represented is pattern conducting pan film.
Embodiment
For a better understanding of the present invention, describe by example
Embodiment 1:
The preparation of patterning polyaniline film on n (100) the type monocrystal silicon substrate:
1. the preparation of patterning elastomeric stamp
The monocrystal silicon substrate that will have little pattern is put into homemade mould, and makes pattern upwards.Sylgard184 (Dow Corning company) left standstill inject mould after 2 hours, solidified 15 minutes, form elastomeric stamp with little pattern at 150 ℃.
2. the preparation of patterning self-assembled film
(1) doing substrate with monocrystalline silicon piece, is that 70%: 30% the concentrated sulfuric acid and the mixed solution of hydrogen peroxide (Piranha solution) were handled 30 minutes with volume ratio down at 100 ℃.
(2) preparation 1 * 10
-3The anhydrous toluene solution of M OTS;
The seal that (3) will clean immerses in the OTS weak solution for preparing and keeps 2s, and nitrogen dries up;
(4) seal that will adsorb OTS is stamped in clean monocrystalline silicon surface, takes seal behind the 20s off, can obtain to have the OTS self-assembled monolayer of certain ordered patterning.
3. the preparation of pattern conducting pan film
(1) aqueous solution of preparation 0.05M aniline, 1MHCl, 1MKCl;
(2) monocrystalline silicon piece with patterning is a work electrode, and platinum is auxiliary electrode, and the Ag/AgCl electrode is a reference electrode, utilizes cyclic voltammetry polymerization aniline film in above-mentioned solution.Sweep speed 100mv/s; Circulation 20 circles; Sweep limits 0-2.0V.Be pattern conducting pan film as shown in Figure 2.
Embodiment 2:
The preparation of patterning polyaniline film on p (111) the type monocrystal silicon substrate:
1. the preparation of patterning elastomeric stamp
Method is the same, solidifies 90 minutes at 65 ℃.
2. the preparation of patterning self-assembled film
(1) doing substrate with monocrystalline silicon piece, is that 70%: 30% the concentrated sulfuric acid and the mixed solution of hydrogen peroxide (Piranha solution) were handled 2 hours with volume ratio down at 85 ℃;
(2) preparation 10 * 10
-3The hexane solution of M OTS;
The seal that (3) will clean immerses in the OTS weak solution for preparing and keeps 10s, and nitrogen dries up;
(4) seal that will adsorb OTS is stamped in clean monocrystalline silicon surface, takes seal behind the 15s off, can obtain to have the OTS self-assembled monolayer of certain ordered patterning.
3. the preparation of pattern conducting pan film
(1) aqueous solution of preparation 0.1M aniline, 1MHCl, 1MKCl;
(2) monocrystalline silicon piece with patterning is a work electrode, and platinum is auxiliary electrode, and the Ag/AgCl electrode is a reference electrode, utilizes potentiostatic method polymerization aniline film in above-mentioned solution.Polymerization 240s.
Claims (4)
1, a kind of preparation method of pattern conducting pan film is characterized in that this method in turn includes the following steps:
A. the preparation of patterning self-assembled film
The seal of cleaning is immersed in the n-hexane or anhydrous toluene solution of octadecyl trichlorosilane (OTS) monomer that concentration is 1mM-10mM, keep 1-5s; After treating the n-hexane or dry toluene volatilization fully on the seal, contact 10s-30s, use acetone supersound washing monocrystalline silicon piece then, obtain the monocrystalline silicon piece of patterning with the monocrystalline silicon sheet surface of cleaning;
B. the preparation of pattern conducting pan film
Monocrystalline silicon piece with described patterning is a work electrode, platinum is auxiliary electrode, the Ag/AgCl electrode is a reference electrode, KCl or NaCl are supporting electrolyte, in the acid solution of 0.05M-0.5M aniline monomer, carry out electrochemical polymerization, the PH of control solution is between 0-2, and silicon chip carried out ultrasonic cleaning with secondary water after polymerization was finished.
2,, it is characterized in that monocrystalline silicon piece is n (100), p (100) or p (111) type monocrystalline silicon as the said method of claim 1.
3,, it is characterized in that acid solution is selected from hydrochloric acid solution or sulfuric acid solution as the said method of claim 1.
4,, it is characterized in that electrochemical method refers to cyclic voltammetry, potentiostatic method or galvanostatic method as the said method of claim 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101193291A CN100336174C (en) | 2003-12-04 | 2003-12-04 | Method of preparating pattern conducting polyphenyl amine film |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2003101193291A CN100336174C (en) | 2003-12-04 | 2003-12-04 | Method of preparating pattern conducting polyphenyl amine film |
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| CN1624872A CN1624872A (en) | 2005-06-08 |
| CN100336174C true CN100336174C (en) | 2007-09-05 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358937C (en) * | 2006-03-02 | 2008-01-02 | 扬州大学 | Electrochemical synthesis method for producing homogeneous and odered aniline nanometer particles |
| KR100829385B1 (en) * | 2006-11-27 | 2008-05-13 | 동부일렉트로닉스 주식회사 | Semiconductor device and method of manufacturing the same |
| CN102731141B (en) * | 2011-04-07 | 2015-02-18 | 北京化工大学 | Polyaniline/n-type monocrystalline silicon combined electrode material and preparation method thereof |
| CN103966549A (en) * | 2014-05-07 | 2014-08-06 | 哈尔滨工业大学 | Method for preparing patterned electrochromatic polyaniline film |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108573A (en) * | 1990-06-05 | 1992-04-28 | The United States Of America As Represented By The United States Department Of Energy | Morphology in electrochemically grown conducting polymer films |
| WO1996029629A2 (en) * | 1995-03-01 | 1996-09-26 | President And Fellows Of Harvard College | Microcontact printing on surfaces and derivative articles |
| US5686548A (en) * | 1993-03-25 | 1997-11-11 | Research Corporation Technologies, Inc. | Polymers useful in forming self-assembled bonded anisotropic ultrathin layers and their use |
| CN1244265A (en) * | 1996-12-18 | 2000-02-09 | 金伯利-克拉克环球有限公司 | Method of contact printing on gold coated films |
| CN1254728A (en) * | 1998-11-23 | 2000-05-31 | 电子科技大学 | Adoping, induction and deposition process for preparing self-assembly superfilm of polyphenylamine |
| CN1401685A (en) * | 2002-09-15 | 2003-03-12 | 中国科学院兰州化学物理研究所 | Method for mfg. patterned conductive polymer film |
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2003
- 2003-12-04 CN CNB2003101193291A patent/CN100336174C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108573A (en) * | 1990-06-05 | 1992-04-28 | The United States Of America As Represented By The United States Department Of Energy | Morphology in electrochemically grown conducting polymer films |
| US5686548A (en) * | 1993-03-25 | 1997-11-11 | Research Corporation Technologies, Inc. | Polymers useful in forming self-assembled bonded anisotropic ultrathin layers and their use |
| WO1996029629A2 (en) * | 1995-03-01 | 1996-09-26 | President And Fellows Of Harvard College | Microcontact printing on surfaces and derivative articles |
| CN1244265A (en) * | 1996-12-18 | 2000-02-09 | 金伯利-克拉克环球有限公司 | Method of contact printing on gold coated films |
| CN1254728A (en) * | 1998-11-23 | 2000-05-31 | 电子科技大学 | Adoping, induction and deposition process for preparing self-assembly superfilm of polyphenylamine |
| CN1401685A (en) * | 2002-09-15 | 2003-03-12 | 中国科学院兰州化学物理研究所 | Method for mfg. patterned conductive polymer film |
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