CN104610544A - Preparation method of thermal-control polyimide material and method for preparing devices from material - Google Patents
Preparation method of thermal-control polyimide material and method for preparing devices from material Download PDFInfo
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- CN104610544A CN104610544A CN201510084778.XA CN201510084778A CN104610544A CN 104610544 A CN104610544 A CN 104610544A CN 201510084778 A CN201510084778 A CN 201510084778A CN 104610544 A CN104610544 A CN 104610544A
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Abstract
The invention provides a preparation method of a thermal-control polyimide material and a method for preparing devices from the material, relating to the field of photoelectric material preparation and device assembly thereof. The invention aims to solve the technical problem that the polyimide material prepared in the prior art has very high glass transition temperature and melting point, can not be easily dissolved in the production process and can not be easily processed. The method comprises the following steps: firstly, depositing microspheres on a template; secondly, preparing triphenylamine-containing polyimide by chemical polymerization; thirdly, coating the polyimide on the template with deposited microspheres; and finally, removing the template with an etching agent, and assembling into a device. After the film structure is adjusted, the polyimide is soluble in the organic solvent, thereby facilitating production and processing. Since polyimide has favorable electrochromic effect, the thermal-control polyimide material is applicable to the field of photoelectricity.
Description
Technical field
The present invention relates to photoelectric material preparation and device assembling field thereof.
Background technology
At present, the extensive concern that electrochromic material attracts society can be there is, certain ambient conditions can be utilized their color to be carried out changing and the material reduced under another condition.It can thus be appreciated that electrochromic material has intelligent characteristic, change its color by regulation and control voltage, because different colours is different to the absorption intensity of ir radiation, make material both sides produce the temperature difference, reach the object of regulating and controlling temperature.
Polyimide is as a kind of high heat resistance, possess the photoconductivity of high chemical stability, high-mechanical property and excellent dielectric properties and compound, these make polyimide have widespread use space at photoelectric functional material and device, novel high-density information transmission and the field such as storage and space flight and aviation.
Along with the development of science and technology, the performance of material is had higher requirement.Intelligence thermal control polyimide is seldom studied by people, polyimide material second-order transition temperature prepared by prior art and fusing point very high, make in process of production its be difficult to dissolve, not easily processed shaping, make its range of application limited, be difficult to the growth requirement meeting society.
Summary of the invention
The present invention to solve polyimide material second-order transition temperature prepared by prior art and fusing point very high, it is made to be difficult to dissolve in process of production, not easily processed shaping technical problem, and a kind of preparation method of thermal control polyimide material is provided and utilizes the method for this material fabricate devices.
A preparation method for thermal control polyimide material, specifically carries out according to following steps:
One, polystyrene colloid microballoon is distributed in deionized water, ultrasonic vibration 10 ~ 30min, puts into ITO electrically-conductive backing plate, then put into 40 ~ 80 DEG C of constant incubators cultivations 3 ~ 7 days, obtain the electrically-conductive backing plate of polystyrene moulding;
Two, the diamines containing trianilino group and dicarboxylic anhydride are added in N-Methyl pyrrolidone solvent, room temperature reaction 10 ~ 30h; In reaction soln, add catalyzer again, pass into N
2, control temperature is 70 DEG C ~ 120 DEG C reactions 1 ~ 3 day, obtains polyimide;
Three, the polyimide that step 2 obtains is evenly coated on the electrically-conductive backing plate of the polystyrene moulding that step one obtains, and put into vacuum drying oven, under the condition of 90 DEG C ~ 200 DEG C, dry film 10 ~ 20h, the polyimide electrically-conductive backing plate of counter opal structure must be contained;
Four, step 3 polyimide electrically-conductive backing plate is put into toluene, soak 3 ~ 10h, obtain the Kapton with counter opal structure, i.e. thermal control polyimide material.
Utilize the method for above-mentioned thermal control polyimide material fabricate devices, specifically carry out according to following steps:
A, take 2 ~ 5g polymethylmethacrylate, 5 ~ 10g lithium perchlorate and 30 ~ 100mL carbonic allyl ester solution, the polymethylmethacrylate taken, lithium perchlorate and carbonic allyl ester solution are mixed, is mixed with gel electrolyte solution;
B, gel electrolyte solution steps A prepared are evenly coated between described thermal control polyimide material and ion storage layer, and adopt epoxy resin by two-layer electrode edge sealing, obtain thermal control polyimide device.
Put into toluene in step 4 and soak object for removing polystyrene colloid.
Step B adopts epoxy resin by two-layer electrode edge sealing to prevent gel electrolyte from volatilizing or to flow out impact test effect.
The invention has the beneficial effects as follows: polyimide material prepared by the present invention can make up common polyimide can not variable color, not soluble and be difficult to the shortcomings such as processing, realizes the object of polyimide intelligence thermal control.Invention introduces colloid template technology, the specific surface area of polymeric film can be improved, thus effectively shorten the distance of ion diffuse, improve the electrochromic property of film.
The present invention obtains intelligent thermal control polyimide material and dissolves in organic solvent; by the method suitability for industrialized production of big area film, the infrared conduction function materials'use of temperature-sensitive on military project, aerospace, industrial detection and monitoring, health care, nuclear reactor protection, petrochemical complex, intelligent robot and miniature aerospacecraft.
Accompanying drawing explanation
Fig. 1 is thermal control polyimide device schematic diagram described in embodiment one, and wherein 1 represent gel electrolyte, 2 represent thermal control polyimide material, and 3 represent ITO, and 4 represent glass, and 5 represent epoxy resin;
Fig. 2 is the cyclic voltammetry curve of thermal control polyimide material film described in embodiment one.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of a kind of thermal control polyimide material of present embodiment, specifically carry out according to following steps:
One, polystyrene colloid microballoon is distributed in deionized water, ultrasonic vibration 10 ~ 30min, puts into ITO electrically-conductive backing plate, then put into 40 ~ 80 DEG C of constant incubators cultivations 3 ~ 7 days, obtain the electrically-conductive backing plate of polystyrene moulding;
Two, the diamines containing trianilino group and dicarboxylic anhydride are added in N-Methyl pyrrolidone solvent, room temperature reaction 10 ~ 30h; In reaction soln, add catalyzer again, pass into N
2, control temperature is 70 DEG C ~ 120 DEG C reactions 1 ~ 3 day, obtains polyimide;
Three, the polyimide that step 2 obtains is evenly coated on the electrically-conductive backing plate of the polystyrene moulding that step one obtains, and put into vacuum drying oven, under the condition of 90 DEG C ~ 200 DEG C, dry film 10 ~ 20h, the polyimide electrically-conductive backing plate of counter opal structure must be contained;
Four, step 3 polyimide electrically-conductive backing plate is put into toluene, soak 3 ~ 10h, obtain the Kapton with counter opal structure, i.e. thermal control polyimide material.
Embodiment two: present embodiment and embodiment one unlike: put into 55 DEG C of constant incubators in step one and cultivate 4 days.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one unlike: be (0.8 ~ 1.1) containing the diamines of trianilino group and the mol ratio of dicarboxylic anhydride in step 2: 1.Other is identical with embodiment one.
Embodiment four: present embodiment and embodiment one unlike: be 1:1 containing the diamines of trianilino group and the mol ratio of dicarboxylic anhydride in step 2.Other is identical with embodiment one.
Embodiment five: present embodiment and embodiment one unlike: in step 2, catalyzer is mixing of diacetyl oxide and pyridine.Other is identical with embodiment one.
Embodiment six: present embodiment and embodiment one unlike: in step 2, control temperature is 75 DEG C.Other is identical with embodiment one.
Embodiment seven: present embodiment and embodiment one unlike: soak 4h in step 4.Other is identical with embodiment one.
Embodiment eight: the method utilizing the thermal control polyimide material fabricate devices described in embodiment one, specifically carry out according to following steps:
A, take 2 ~ 5g polymethylmethacrylate, 5 ~ 10g lithium perchlorate and 30 ~ 100mL carbonic allyl ester solution, the polymethylmethacrylate taken, lithium perchlorate and carbonic allyl ester solution are mixed, is mixed with gel electrolyte solution;
B, gel electrolyte solution steps A prepared are evenly coated between thermal control polyimide material according to claim 1 and ion storage layer, and adopt epoxy resin by two-layer electrode edge sealing, obtain thermal control polyimide device.
Following examples and contrast experiment is adopted to verify beneficial effect of the present invention:
Embodiment one:
The preparation method of a kind of thermal control polyimide material of the present embodiment, specifically carries out according to following steps:
One, polystyrene colloid microballoon is distributed in deionized water, ultrasonic vibration 30min, puts into ITO electrically-conductive backing plate, then put into 55 DEG C of constant incubators cultivations 4 days, obtain the electrically-conductive backing plate of polystyrene moulding;
Two, the diamines containing trianilino group and dicarboxylic anhydride are added in N-Methyl pyrrolidone solvent, room temperature reaction 10h; In reaction soln, add catalyst acetic acid acid anhydride and pyridine again, pass into N
2, control temperature is 75 DEG C of reactions 1 day, obtains polyimide;
Be wherein 1:1 containing the diamines of trianilino group and the mol ratio of dicarboxylic anhydride;
Three, the polyimide that step 2 obtains is evenly coated on the electrically-conductive backing plate of the polystyrene moulding that step one obtains, and puts into vacuum drying oven, under the condition of 90 DEG C, dry film 10h, the polyimide electrically-conductive backing plate of counter opal structure must be contained;
Four, step 3 polyimide electrically-conductive backing plate is put into toluene, soak 4h, obtain the Kapton with counter opal structure, i.e. thermal control polyimide material.
Utilize the method for above-mentioned thermal control polyimide material fabricate devices, specifically carry out according to following steps:
A, take 5g polymethylmethacrylate, 10g lithium perchlorate and 100mL carbonic allyl ester solution, the polymethylmethacrylate taken, lithium perchlorate and carbonic allyl ester solution are mixed, is mixed with gel electrolyte solution;
B, gel electrolyte solution steps A prepared are evenly coated between described thermal control polyimide material and ion storage layer, and adopt epoxy resin by two-layer electrode edge sealing, obtain thermal control polyimide device.
Test: the voltage being applied 0 ~ 2V by cyclic voltammetric method in electrochemical workstation, ion embeds, deviates from from polyimide, and film color is changed to black-and-blue by reddish-brown, then to become reddish-brown reversible change from black-and-blue.
Described in the present embodiment, thermal control polyimide device schematic diagram as shown in Figure 1, wherein 1 represents gel electrolyte, and 2 represent thermal control polyimide material, and 3 represent ITO, and 4 represent glass, and 5 represent epoxy resin.
The cyclic voltammetry curve of thermal control polyimide material film described in the present embodiment as shown in Figure 2, is found out the oxidizing potential of polyimide by figure, reduction potential is respectively 1 ~ 1.5V (black-and-blue) and 0.5 ~ 0.95V (reddish-brown).
The present invention makes its difference of perviousness to light, infrared radiation absorption intensity different thus temperature control by the difference of polyimide electrochromism color.Its principle is that under the different voltage of trianilino group in polyimide structures, valence state is different.Reaction principle is as follows:
Being reddish-brown during reduction-state, is black-and-blue during oxidation state, and it is all black-and-blue that oxidation state has several resonance form to exist.
Claims (8)
1. a preparation method for thermal control polyimide material, is characterized in that what the method was specifically carried out according to following steps:
One, polystyrene colloid microballoon is distributed in deionized water, ultrasonic vibration 10 ~ 30min, puts into ITO electrically-conductive backing plate, then put into 40 ~ 80 DEG C of constant incubators cultivations 3 ~ 7 days, obtain the electrically-conductive backing plate of polystyrene moulding;
Two, the diamines containing trianilino group and dicarboxylic anhydride are added in N-Methyl pyrrolidone solvent, room temperature reaction 10 ~ 30h; In reaction soln, add catalyzer again, pass into N
2, control temperature is 70 DEG C ~ 120 DEG C reactions 1 ~ 3 day, obtains polyimide;
Three, the polyimide that step 2 obtains is evenly coated on the electrically-conductive backing plate of the polystyrene moulding that step one obtains, and put into vacuum drying oven, under the condition of 90 DEG C ~ 200 DEG C, dry film 10 ~ 20h, the polyimide electrically-conductive backing plate of counter opal structure must be contained;
Four, step 3 polyimide electrically-conductive backing plate is put into toluene, soak 3 ~ 10h, obtain the Kapton with counter opal structure, i.e. thermal control polyimide material.
2. the preparation method of a kind of thermal control polyimide material according to claim 1, is characterized in that putting into 55 DEG C of constant incubators in step one cultivates 4 days.
3. the preparation method of a kind of thermal control polyimide material according to claim 1, is characterized in that the mol ratio of the diamines and dicarboxylic anhydride containing trianilino group in step 2 is (0.8 ~ 1.1): 1.
4. the preparation method of a kind of thermal control polyimide material according to claim 1, to is characterized in that in step 2 containing the diamines of trianilino group and the mol ratio of dicarboxylic anhydride being 1:1.
5. the preparation method of a kind of thermal control polyimide material according to claim 1, is characterized in that in step 2, catalyzer is the mixing of diacetyl oxide and pyridine.
6. the preparation method of a kind of thermal control polyimide material according to claim 1, is characterized in that in step 2, control temperature is 75 DEG C.
7. the preparation method of a kind of thermal control polyimide material according to claim 1, is characterized in that soaking 4h in step 4.
8. utilize the method for the thermal control polyimide material fabricate devices described in claim 1, it is characterized in that specifically carrying out according to following steps:
A, take 2 ~ 5g polymethylmethacrylate, 5 ~ 10g lithium perchlorate and 30 ~ 100mL carbonic allyl ester solution, the polymethylmethacrylate taken, lithium perchlorate and carbonic allyl ester solution are mixed, is mixed with gel electrolyte solution;
B, gel electrolyte solution steps A prepared are evenly coated between thermal control polyimide material according to claim 1 and ion storage layer, and adopt epoxy resin by two-layer electrode edge sealing, obtain thermal control polyimide device.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104861162A (en) * | 2015-05-20 | 2015-08-26 | 上海交通大学 | Soluble polyimide with tert-butyl and triphenylamine structure and preparation method of soluble polyimide |
| CN105778045A (en) * | 2016-04-25 | 2016-07-20 | 哈尔滨工业大学 | Polyurethane material with electrochromic property as well as preparation method and application of polyurethane material |
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Cited By (2)
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| CN104861162A (en) * | 2015-05-20 | 2015-08-26 | 上海交通大学 | Soluble polyimide with tert-butyl and triphenylamine structure and preparation method of soluble polyimide |
| CN105778045A (en) * | 2016-04-25 | 2016-07-20 | 哈尔滨工业大学 | Polyurethane material with electrochromic property as well as preparation method and application of polyurethane material |
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Application publication date: 20150513 |