CN109293963A - A method of preparing polythiophene and the compound wrinkle pattern of polypyrrole - Google Patents
A method of preparing polythiophene and the compound wrinkle pattern of polypyrrole Download PDFInfo
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- CN109293963A CN109293963A CN201810913087.XA CN201810913087A CN109293963A CN 109293963 A CN109293963 A CN 109293963A CN 201810913087 A CN201810913087 A CN 201810913087A CN 109293963 A CN109293963 A CN 109293963A
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- polypyrrole
- polythiophene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/123—Treatment by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2465/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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Abstract
The invention discloses a kind of methods for preparing polythiophene and the compound wrinkle pattern of polypyrrole.Its preparation process includes: that PDMS substrate oxygen plasma treatment 30s a certain amount of poly- 3- hexyl thiophene is added dropwise in PDMS substrate surface, and it is made to be swollen certain time first；Then, the PDMS substrate with poly- 3- hexyl thiophene is placed on spin coating instrument, with 3000r/min, spin coating 30s.Then, the PDMS substrate that spin coating has poly- 3- hexyl thiophene is put into a period of time in air, solvent is removed, to obtain the surface with poly- 3- hexyl thiophene wrinkle pattern.Then, the PDMS substrate with wrinkle pattern is placed in chromium solution, reacts the regular hour, finally washes away the polypyrrole of excess surface, obtain polythiophene and the compound wrinkle pattern of polypyrrole.The present invention is successfully prepared polythiophene and the compound wrinkle pattern of polypyrrole using simple and efficient mode of operation, so as to avoid complicated cumbersome operating procedure, the loss of longer preparation time and high equipment and experiment consumptive material.
Description
Technical field
The present invention relates to the preparation technical fields of free independent polymers surface topography.
Background technique
With the discovery of conducting polymer, conductive material be not confined to conventional metals field.Polypyrrole and polythiophene are made
For most typical conducting polymer, it is considered being most likely applied in actual production and life.Currently, polypyrrole and polythiophene
It has been widely used in organic photoelectric field.Such as Organic Thin Film Transistors and organic solar batteries.And polypyrrole and polythiophene
Surface topography it is most important to device performance, material can be significantly increased as a kind of simple method in surface wrinkling
Surface roughness increases specific surface area, and can directionally adjust surface topography.In recent years, by generating pattern from corrugation,
It forms controllable compound wrinkle pattern to attract attention, by more due to its is easy to operate and has certain controllability
Carry out more attention.But in existing research, this method is not also especially mature, so preparing polythiophene and polypyrrole is multiple
Closing wrinkle also becomes the trend and hot spot of future technical advances.
Summary of the invention
For the above-mentioned prior art, the present invention provides a kind of method for preparing polythiophene and the compound wrinkle pattern of polypyrrole.
It is substrate that elastic material PDMS is selected in the present invention, with oxygen plasma treatment 30s, in the certain thickness poly- thiophene of its surface spin coating
Pure P3HT wrinkle pattern is made in air completely to solvent volatilization in pheno film.PDMS is placed in plastic petri dishes,
Enter to be uniformly mixed ground chromium solution reaction 5h, to obtain polythiophene and the compound wrinkle of polypyrrole.By adjusting substrate thickness, gather
The swelling time of thiophene can obtain having the polythiophene of different surface morphology and the compound wrinkle of polypyrrole.The present invention utilizes simplicity
Efficiently mode of operation, which was successfully realized in the short time, prepares polythiophene and the compound wrinkle of polypyrrole, so as to avoid complicated cumbersome
Operating procedure, longer preparation time and high equipment and the loss for testing consumptive material.
In order to solve the above-mentioned technical problem, the present invention proposes a kind of side for preparing polythiophene and the compound wrinkle pattern of polypyrrole
Method, comprising the following steps:
Step 1: it after PDMS performed polymer is mixed with crosslinking agent according to mass ratio for 10:1, pours into centrifuge tube, after stirring
Form the mixture of uniform PDMS performed polymer and crosslinking agent；
Step 2: pouring into culture dish after the mixture of PDMS performed polymer and crosslinking agent is carried out Fruit storage 1h,
And it is allowed to be evenly distributed in culture dish；
Step 3: the mixture of the PDMS performed polymer and crosslinking agent that pour into culture dish is subjected to Fruit storage
30min, after be put into baking oven, be heating and curing 4h at 70 DEG C, obtains the PDMS substrate with a thickness of 300~700 microns；
PDMS substrate: being cut into fixed shape by step 4, with oxygen plasma treatment 30s；
Step 5: being 40 microlitres/CM according to bulk area ratio2Poly- 3- hexyl thiophene is added dropwise in PDMS substrate surface, it is molten
Then swollen 1~10s makes solvent volatilization complete in air with 3000r/s spin coating 30s；
Step 6: being that pyrrole monomer is dissolved in concentration is to obtain pyrrole in the hydrochloric acid of 1mol/L to 0.1mol/L according to concentration
Solution is coughed up, ultrasound mixes spare；It is that iron chloride is dissolved in concentration is to obtain in the hydrochloric acid of 1mol/L to 0.2mol/L according to concentration
Ferric chloride solution, ultrasound mix spare；
The chromium solution prepared: being first transferred in PDMS culture dish, be put into refrigerator by step 7, is then added and prepares
The volume ratio of good ferric chloride solution, chromium solution and ferric chloride solution is 1:1, is uniformly mixed, and 2h is reacted；
Step 8: taking out culture dish from refrigerator after reaction, removes supernatant liquid, and clean with distilled water flushing,
Polythiophene and the compound wrinkle pattern of polypyrrole are obtained after drying.
In the present invention, by adjusting by adjusting swelling time in substrate thickness or step 5, to obtain in step 3
The compound wrinkle pattern of polythiophene and polypyrrole with different surface morphology.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides the methods that one kind can prepare polythiophene and the compound wrinkle of polypyrrole in a short time, pass through letter
Single control swelling time and substrate thickness, can prepare polythiophene and the compound wrinkle of polypyrrole with different surface morphology,
Has the characteristics that the disadvantages of simple, quick, reproducible, to avoid complicated preparation process, equipment valuableness, low efficiency, on surface
There is potential application prospect in the equal fields of constructing of hydrophobic material, microcircuit.
Detailed description of the invention
Fig. 1 is the optical microscope picture of the P3HT film of swelling 1s obtained in the embodiment of the present invention 1；
Fig. 2 is the optical microscope picture that the embodiment of the present invention 1 is swollen the polythiophene of 1s and the compound wrinkle of polypyrrole；
Fig. 3 is the optical microscope picture that the embodiment of the present invention 2 is swollen the polythiophene of 5s and the compound wrinkle of polypyrrole；
Fig. 4 is the optical microscope picture that the embodiment of the present invention 3 is swollen the polythiophene of 10s and the compound wrinkle of polypyrrole；
Fig. 5 be the embodiment of the present invention 4 swelling be 5s, the compound wrinkle of the polythiophene that substrate thickness is 700 microns and polypyrrole
The optical microscope picture of line；
Specific embodiment
Technical solution of the present invention is described in further detail in the following with reference to the drawings and specific embodiments, it is described specific
Embodiment is only explained the present invention, is not intended to limit the invention.
Embodiment 1: a method of preparing polythiophene and the compound wrinkle pattern of polypyrrole, comprising the following steps:
Step 1: it after PDMS performed polymer is mixed with crosslinking agent according to mass ratio for 10:1, pours into centrifuge tube, uses glass
Stick stirs the mixture to form uniform PDMS performed polymer and crosslinking agent；
Step 2: rectangular culture dish is poured into after the mixture of PDMS performed polymer and crosslinking agent is carried out Fruit storage 1h
In, and be allowed to be evenly distributed in culture dish；
Step 3: carrying out Fruit storage 30min for the mixture of the performed polymer and crosslinking agent that pour into culture dish, after
It is put into baking oven, be heating and curing 4h at 70 DEG C, obtains PDMS substrate, which is 300 microns.
Step 4: PDMS substrate is cut into 1CM2Shape, with oxygen plasma (OP) handle 30s；
Step 5: 40 microlitres of poly- 3- hexyl thiophenes (P3HT) being added dropwise in the PDMS substrate surface, the time of 1s is swollen, with
3000r/s spin coating 30s is used afterwards, puts 30s in air, makes solvent volatilization completely, as shown in Figure 1.
Step 6: the pyrrole monomer of 0.1342g is dissolved in the hydrochloric acid of 20ml, obtains pyrroles's hydrochloric acid solution, and ultrasound is mixed
It is even；The iron chloride of 0.6488g is dissolved in the hydrochloric acid of 20ml, iron chloride salt acid solution is obtained, ultrasound mixes；
Step 7: first the above-mentioned pyrroles's dissolved salt acid solution prepared is transferred in PDMS culture dish, is put into 2~5 DEG C of ice
In case, above-mentioned prepared iron chloride salt acid solution is then added, uniformly mixes, reacts 2h；
Step 8: taking out culture dish from refrigerator after reaction, removes supernatant liquid, and clean with distilled water flushing,
It is dried up afterwards with ear washing bulb, obtains polythiophene and the compound wrinkle pattern of polypyrrole, as shown in Figure 2.
Embodiment 2: a method of polythiophene and the compound wrinkle pattern of polypyrrole are prepared, in embodiment 2, in addition to step 5
Different from the step in embodiment 1, other steps are all the same.In step 5, swelling time is adjusted to 5s by 1s, it is final to obtain
The compound wrinkle pattern of the polythiophene and polypyrrole arrived is as shown in Figure 3.
Embodiment 3: a method of polythiophene and the compound wrinkle pattern of polypyrrole are prepared, in embodiment 3, in addition to step 5
Different from the step in embodiment 1, other steps are all the same.In step 5, swelling time is adjusted to 10s by 1s, finally
The compound wrinkle pattern of obtained polythiophene and polypyrrole is as shown in Figure 4.
Embodiment 4: a method of polythiophene and the compound wrinkle pattern of polypyrrole are prepared, in embodiment 4, in addition to step 3
Different from the step in embodiment 2, other steps are all the same.In step 3, PDMS substrate thickness is adjusted to by 300 microns
700 microns, finally obtained polythiophene and the compound wrinkle pattern of polypyrrole are as shown in Figure 5.
To sum up, if present invention spin coating polythiophene in PDMS substrate, it is thin that polypyrrole is then deposited by chemical oxidization method
Film.The polythiophene and the compound wrinkle of polypyrrole of different surface morphology can be obtained by adjusting different swelling time and substrate thickness
Line, with the increase of swelling time, the pattern of P3HT is more clear；And with the increase of substrate thickness, the period of wrinkle is gradually
Reduce, but changes unobvious.The shortcomings that it is complicated that the present invention overcomes preparation process before, poor process control.
Although above in conjunction with attached drawing, invention has been described, and the invention is not limited to above-mentioned specific implementations
Mode, the above mentioned embodiment is only schematical, rather than restrictive, and those skilled in the art are at this
Under the enlightenment of invention, without deviating from the spirit of the invention, many variations can also be made, these belong to of the invention
Within protection.
Claims (2)
1. a kind of method for preparing polythiophene and the compound wrinkle pattern of polypyrrole, which comprises the following steps:
Step 1: it after PDMS performed polymer is mixed with crosslinking agent according to mass ratio for 10:1, pours into centrifuge tube, is formed after stirring
The mixture of uniform PDMS performed polymer and crosslinking agent；
Step 2: it pours into culture dish, and makes after the mixture of PDMS performed polymer and crosslinking agent is carried out Fruit storage 1h
Be evenly distributed in culture dish；
Step 3: carrying out Fruit storage 30min for the mixture of the PDMS performed polymer and crosslinking agent that pour into culture dish, after
It is put into baking oven, be heating and curing 4h at 70 DEG C, obtains the PDMS substrate with a thickness of 300~700 microns
PDMS substrate: being cut into fixed shape by step 4, with oxygen plasma treatment 30s；
Step 5: being 40 microlitres/CM according to bulk area ratio2Poly- 3- hexyl thiophene is added dropwise in PDMS substrate surface, swelling 1~
Then 10s makes solvent volatilization complete in air with 3000r/s spin coating 30s；
Step 6: being that pyrrole monomer is dissolved in concentration is that it is molten to obtain pyrroles in the hydrochloric acid of 1mol/L to 0.1mol/L according to concentration
Liquid, ultrasound mix spare；It is that iron chloride is dissolved in concentration is to obtain chlorination in the hydrochloric acid of 1mol/L to 0.2mol/L according to concentration
Ferrous solution, ultrasound mix spare；
The chromium solution prepared: being first transferred in PDMS culture dish, be put into refrigerator by step 7, is then added prepared
The volume ratio of ferric chloride solution, chromium solution and ferric chloride solution is 1:1, is uniformly mixed, and 2h is reacted；
Step 8: taking out culture dish from refrigerator after reaction, removes supernatant liquid, and clean with distilled water flushing, dry
After obtain polythiophene and the compound wrinkle pattern of polypyrrole.
2. the method for preparing polythiophene and the compound wrinkle pattern of polypyrrole according to claim 1, wherein pass through in step 3
It adjusts by adjusting swelling time in substrate thickness or step 5, to obtain the polythiophene with different surface morphology and gather
The compound wrinkle pattern of pyrroles.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114524956A (en) * | 2020-10-30 | 2022-05-24 | 北京化工大学 | Method for producing oriented and stretchable organic semiconductor thin film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114524956A (en) * | 2020-10-30 | 2022-05-24 | 北京化工大学 | Method for producing oriented and stretchable organic semiconductor thin film |
| CN114524956B (en) * | 2020-10-30 | 2023-11-24 | 北京化工大学 | Method for producing oriented and stretchable organic semiconductor film |
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Application publication date: 20190201 |