CN109251335A - Regulate and control the method for its surface topography based on polypyrrole polymerization reaction time is changed - Google Patents
Regulate and control the method for its surface topography based on polypyrrole polymerization reaction time is changed Download PDFInfo
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- CN109251335A CN109251335A CN201810741543.7A CN201810741543A CN109251335A CN 109251335 A CN109251335 A CN 109251335A CN 201810741543 A CN201810741543 A CN 201810741543A CN 109251335 A CN109251335 A CN 109251335A
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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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
- C08J2379/00—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 C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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Abstract
Regulate and control the method for its surface topography based on polypyrrole polymerization reaction time is changed the invention discloses a kind of, its preparation process includes: to prepare flexible PDMS first as substrate, then certain thickness polypyrrole (PPy) film is deposited on its surface, the PPy film of patterned surface can be obtained finally by washing and drying, wherein, by the polymerization time of PPy, the PPy thin-film material with different surface morphology can be obtained.The present invention is in the way of shirtsleeve operation, the conducting polymer thin film with certain surface terrain is obtained, it is successfully realized regulation PPy film surface appearance, 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 a kind of preparation method of thin polymer film more particularly to a kind of regulation polymeric film surface patterns
Method.
Background technique
The extensive concern of people has been caused with patterned surface film of poly pyrrole material, and has also been widely used
In people's lives, such as super hydrophobic material and flexible electronic device.Tradition preparation has the method master of patterned surface PPy
It is complicated for operation due to higher cost if patterning methods such as photoetching, seriously limit its application prospect.In recent years, pass through
Original position makes film of poly pyrrole surface generate surface topography from wrinkling on a flexible substrate, because its is easy to operate and has centainly
Controllability and more and more paid attention to.
Summary of the invention
For the above-mentioned prior art, a kind of side regulating and controlling its film surface appearance based on polypyrrole polymerization reaction time
Method.It is substrate that the present invention, which selects elastic material PDMS, then deposits certain thickness polypyrrole (PPy) film on its surface, most
The PPy film of patterned surface can be obtained by washing and drying afterwards.By the polymerization time of PPy, can obtain with different surfaces
The PPy thin-film material of pattern.The present invention is successfully realized regulation PPy film surface appearance using simple and efficient mode of operation
Method, so as to avoid complicated cumbersome operating procedure, the damage of longer preparation time and high equipment and experiment consumptive material
Consumption.
In order to solve the above technical problems, one kind proposed by the present invention regulates and controls it based on polypyrrole polymerization reaction time is changed
The method of surface topography, 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 to form uniform mixture；
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: the mixture of the performed polymer and crosslinking agent that pour into container is subjected to Fruit storage 30min-
60min, after be put into baking oven, be heating and curing 4h at 70 DEG C；
Step 4: pyrrole monomer is dissolved in hydrochloric acid for 6.5~7.0mg/ml according to mass volume ratio, ultrasound mixes
To solution A, iron chloride is dissolved in hydrochloric acid for 30~35mg/ml according to mass volume ratio, ultrasound is uniformly mixed so as to obtain solution B；
Step 5: solution A made from step 4 is transferred in the culture dish for being contained with PDMS substrate, step is then added
Solution B made from four, wherein the volume ratio of solution A and solution B is 1:1, is put into the refrigerator that temperature is 2~5 DEG C after evenly mixing
Interior reaction 1h-9h；
Step 6: taking out culture dish from refrigerator after reaction, removes residual liquid, and clean with distilled water flushing,
It is dry, it can finally obtain the film of poly pyrrole with certain surface terrain.
In the present invention, by changing the reaction time in step 5, to obtain having the polypyrrole of different surface morphology thin
Film, the reaction time is longer, and the period of obtained film of poly pyrrole pattern is bigger.
Compared with prior art, the beneficial effects of the present invention are:
By simply changing polymerization reaction time in the present invention, the surface topography of the film finally obtained is adjusted
Control, can prepare the film of poly pyrrole with different surface morphology, have the characteristics that simple, quick, reproducible, avoid system
The disadvantages of standby process is complicated, equipment is expensive, low efficiency, in surface hydrophobicity material, the equal fields of constructing of microcircuit have and potentially answer
Use prospect.
Detailed description of the invention
Fig. 1 is the optical microscope picture for the film of poly pyrrole that the embodiment of the present invention 1 obtains；
Fig. 2 is the optical microscope picture for the film of poly pyrrole that the embodiment of the present invention 2 obtains；
Fig. 3 is the optical microscope picture for the film of poly pyrrole that the embodiment of the present invention 3 obtains.
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.
A kind of method regulating and controlling its surface topography based on change polypyrrole polymerization reaction time proposed by the present invention, first
Flexibility PDMS is prepared as substrate, then deposits certain thickness polypyrrole (PPy) film on its surface, it is dry finally by washing
The dry PPy film that patterned surface can be obtained, wherein by the polymerization time of PPy, can obtain that there is different surface morphology
PPy thin-film material.The present invention has obtained the conducting polymer thin film with certain surface terrain in the way of shirtsleeve operation,
The method for being successfully realized regulation PPy film surface appearance, so as to avoid complicated cumbersome operating procedure, when longer preparation
Between with high equipment and test the loss of consumptive material.
Embodiment 1: regulate and control the method for its surface topography, including following step based on polypyrrole polymerization reaction time is changed
It is rapid:
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 to form uniform mixture；
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；
Step 4: pyrrole monomer is dissolved in hydrochloric acid for 6.5mg/ml according to mass volume ratio, ultrasound is uniformly mixed so as to obtain molten
Iron chloride is dissolved in hydrochloric acid according to mass volume ratio for 30mg/ml by liquid A, and ultrasound is uniformly mixed so as to obtain solution B；
Step 5: solution A made from step 4 is transferred in the culture dish for being contained with PDMS substrate, step is then added
Solution B made from four, wherein the volume ratio of solution A and solution B is 1:1, is put into the refrigerator that temperature is 4 DEG C after evenly mixing
React 1h；
Step 6: taking out culture dish from refrigerator after reaction, removes residual liquid, and clean with distilled water flushing,
Dry, the optical microscope picture of the film of poly pyrrole finally obtained is as shown in Figure 1.
Embodiment 2: regulating and controlling the method for its surface topography based on polypyrrole polymerization reaction time is changed, and in embodiment 2, removes
Step 4 and step 5 are different from the step in embodiment 1, other steps are all the same.Step 4, by pyrrole monomer in solution A
7.0mg/ml is changed to by 6.5mg/ml with the mass volume ratio of hydrochloric acid, by the mass volume ratio of iron chloride and hydrochloric acid in solution B
35mg/ml is changed to by 30mg/ml；In step 5, polymerization reaction time is adjusted to 5h.The finally obtained polypyrrole of embodiment 2
The optical microscope picture of film is as shown in Figure 2.
Embodiment 3: regulating and controlling the method for its surface topography based on polypyrrole polymerization reaction time is changed, and in embodiment 3, removes
Step 5 is different from the step in embodiment 1, other steps are all the same.In step 5, polymerization reaction time is adjusted into 9h,
The optical microscope picture of finally obtained film of poly pyrrole is as shown in Figure 3.
To sum up, the present invention is the deposition PPy film in PDMS substrate, utilizes the modulus difference of PDMS substrate and PPy film
Induction generates picture on surface.By changing PPy polymerization reaction time, and then change the modulus of PPy film, finally preparing has
The PPy film of different surfaces pattern, the reaction time is longer, and the period of obtained film of poly pyrrole pattern is bigger.Side of the present invention
The shortcomings that preparation process is complicated before method overcomes, 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 regulate and control the method for its surface topography based on polypyrrole polymerization reaction time is changed, which is characterized in that including with
Lower step:
Step 1: it after PDMS performed polymer is mixed with crosslinking agent according to mass ratio for 10:1, pours into centrifuge tube, is stirred with glass bar
It mixes to form uniform mixture；
Step 2: pouring into rectangular 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: carrying out Fruit storage 30min-60min for the mixture of the performed polymer and crosslinking agent that pour into container, after
It is put into baking oven, be heating and curing 4h at 70 DEG C；
Step 4: pyrrole monomer is dissolved in hydrochloric acid for 6.5~7.0mg/ml according to mass volume ratio, ultrasound is uniformly mixed so as to obtain molten
Iron chloride is dissolved in hydrochloric acid according to mass volume ratio for 30~35mg/ml by liquid A, and ultrasound is uniformly mixed so as to obtain solution B；
Step 5: solution A made from step 4 is transferred in the culture dish for being contained with PDMS substrate, and step 4 system is then added
The solution B obtained, wherein the volume ratio of solution A and solution B is 1:1, is put into after evenly mixing anti-in the refrigerator that temperature is 2~5 DEG C
Answer 1h-9h；
Step 6: taking out culture dish from refrigerator after reaction, removes residual liquid, and clean with distilled water flushing, dry,
The film of poly pyrrole with certain surface terrain can finally be obtained.
2. regulating and controlling the method for its surface topography based on polypyrrole polymerization reaction time is changed according to claim 1, wherein
By changing the reaction time in step 5, to obtain having the polypyrrole of different surface morphology thin, the reaction time is longer, gained
The period of the thin pattern of the polypyrrole arrived is bigger.
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| CN201810741543.7A CN109251335A (en) | 2018-07-09 | 2018-07-09 | Regulate and control the method for its surface topography based on polypyrrole polymerization reaction time is changed |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628074A (en) * | 2019-09-30 | 2019-12-31 | 天津大学 | Method for preparing internal structure based on porous PDMS |
| CN110885462A (en) * | 2019-11-05 | 2020-03-17 | 湖南师范大学 | Preparation method of patterned thin film |
| CN115969312A (en) * | 2023-03-22 | 2023-04-18 | 中国人民解放军总医院第一医学中心 | Intraocular pressure monitoring device connected with glaucoma drainage valve |
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|---|---|---|---|---|
| CN105061731A (en) * | 2015-07-31 | 2015-11-18 | 天津大学 | Method for constructing multistage morphology polypyrrole membrane based on in situ wrinkling and thermal expansion |
| CN105085908A (en) * | 2015-07-31 | 2015-11-25 | 天津大学 | Method for preparing patterned polypyrrole film based on in-situ wrinkling |
| CN106916325A (en) * | 2017-03-22 | 2017-07-04 | 天津大学 | A kind of method for preparing free patterned surface film of poly pyrrole |
-
2018
- 2018-07-09 CN CN201810741543.7A patent/CN109251335A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105061731A (en) * | 2015-07-31 | 2015-11-18 | 天津大学 | Method for constructing multistage morphology polypyrrole membrane based on in situ wrinkling and thermal expansion |
| CN105085908A (en) * | 2015-07-31 | 2015-11-25 | 天津大学 | Method for preparing patterned polypyrrole film based on in-situ wrinkling |
| CN106916325A (en) * | 2017-03-22 | 2017-07-04 | 天津大学 | A kind of method for preparing free patterned surface film of poly pyrrole |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628074A (en) * | 2019-09-30 | 2019-12-31 | 天津大学 | Method for preparing internal structure based on porous PDMS |
| CN110885462A (en) * | 2019-11-05 | 2020-03-17 | 湖南师范大学 | Preparation method of patterned thin film |
| CN115969312A (en) * | 2023-03-22 | 2023-04-18 | 中国人民解放军总医院第一医学中心 | Intraocular pressure monitoring device connected with glaucoma drainage valve |
| CN115969312B (en) * | 2023-03-22 | 2023-08-22 | 中国人民解放军总医院第一医学中心 | Intraocular pressure monitoring device connected with glaucoma drainage valve |
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