CN104558606A - Method for preparing graphene composite polyimide conductive film - Google Patents
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- CN104558606A CN104558606A CN201410763000.7A CN201410763000A CN104558606A CN 104558606 A CN104558606 A CN 104558606A CN 201410763000 A CN201410763000 A CN 201410763000A CN 104558606 A CN104558606 A CN 104558606A
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Abstract
The invention belongs to the technical field of conductive films and relates to a method for preparing a graphene composite polyimide conductive film. Graphene oxide is compounded with the precursor of polyimide, namely polyamide acid, and since the graphene oxide contains rich functional groups of oxygen in the interlayer, the dispersibility of graphene oxide in polyamide acid is effectively improved; then cyclodehydration is carried out on the graphene oxide composite polyamide acid film to obtain the graphene composite polyimide conductive film. The graphene composite polyimide conductive film prepared in the invention has the advantages of more uniform thickness, good conductivity, high mechanical strength and the like.
Description
Technical field
The present invention relates to a kind of preparation method of graphene oxide compound polyimide conductive film, the invention belongs to conductive film preparation field.
Background technology
Existing conductive film is generally ink printing heating film, tetrafluoroethylene heating film etc., but the maximum feature of these materials is that temperature resistant range is narrow, and physical strength is low.And polyimide can use within the scope of the wide temperature of-269-400 DEG C, heat decomposition temperature reaches about 500 DEG C, also has desirable physical, mechanical property, is the ideal material preparing conductive film.
Adding conductive filler material is the typical modification method improving macromolecular material electroconductibility.Conventional conductive filler material can be divided into the large class of charcoal system and metal system two.Wherein Graphene is a kind of individual layer sheetlike material be made up of carbon atom, and resistivity only has an appointment 10
-8Ω m, than copper or silver lower, be the material that at present resistivity is minimum in the world.But the electronic structure of the large π key conjugation that Graphene is special causes its interlayer to there is very large Van der Waals force, its lamella occurs to reunite and pile up very easily again, and then is difficult to disperse to form stable solution many common are in machine solvent; And reactive behavior is not high, also more difficult with the compound of all kinds of polymer materials.In addition, prior art polyimide composite film many employings casting method is produced, obtained product exist in uneven thickness, color aberration large, the shortcomings such as production efficiency is low.
Chinese patent literature CN201210059833.6 discloses a kind of method utilizing graphene reinforced polyimide resin carbonization to prepare carbonized film, this invention adopts polyamic acid and Graphene situ aggregation method to obtain carbonized film, in the carbonized film process that the method is obtained, there is Graphene in polyimide, disperse uneven shortcoming; Chinese patent literature CN201310108138.9 discloses the preparation method of polyimide and graphene oxide, although this invention solves the dispersion of Graphene in polyimide matrix and compatible problem, this invention exists functional group due to graphene oxide.
Summary of the invention
Therefore, technical problem to be solved by this invention is to overcome the problem of Graphene and polyimide Complex Function in prior art, thus propose a kind of with functional diamine monomer and dianhydride monomer for primitive combined oxidation Graphene, prepared the method for conductive film by reduction.
For this reason, the invention provides a kind of method of Graphene compound polyimide conductive film, comprise the following steps:
(1) preparation of graphene oxide suspension: graphite oxide is scattered in polar solvent, ultrasonic stripping graphite oxide, obtains graphene oxide suspension;
(2) preparation of graphene oxide compound polyimide solution: under protection of inert gas and preset temp condition, successively add sulfur oxychloride and diamines in graphene oxide suspension, add dianhydride after sulfoxide to be chlorinated and diamines fully dissolve; The last solid content adding polar solvent diluting soln again, and stir into homogeneous phase, for subsequent use;
(3) preparation of Graphene compound polyimide conductive film: substrate is immersed in graphene oxide compound polyimide solution, lift plated film; Insert in tube furnace by the substrate being loaded with graphene oxide compound polyimide film, dehydration obtains Graphene compound polyimide film.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described polar solvent is N, one or more arbitrary proportions mixing in N-dimethyl formamide, N, N-N,N-DIMETHYLACETAMIDE, N-methyl-2-pyrrolidone, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF).
The preparation method of Graphene compound polyimide conductive film provided by the invention, described ultrasonic stripping graphite oxide, ultrasonic frequency is 20-100KHz, and ultrasonic time is 4-6h; The temperature of ultrasonic stripping graphite oxide is 15-35 DEG C.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described diamines is any one in 2TFMPPD, BBH, FPPD, BDAF, FBA.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described dianhydride is any one in pyromellitic dianhydride, BPDA, PMDA, PHDA, DNDA, CBDA, CHDAn, BCHDABPDA, BTDA, NDO, PDO, Br-PDO, TDO.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described sulfur oxychloride can be replaced PCl3 or PCl5.
The preparation method of Graphene compound polyimide conductive film provided by the invention, the ratio control of described graphene oxide and diamines is at 0.1-1.4:1; The mass ratio of described graphene oxide diamine monomer and dianhydride controls at 0.8-1.2:1.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described preset temp is 80-110 DEG C; The solid content of described solution is 5%-30%.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described in be loaded with graphene oxide compound polyimide film substrate insert in tube furnace, adopt staged to heat up, temperature controls at 200-480
oc.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described ladder-elevating temperature speed is 2-5
oc/min, is warming up to 80-120
oafter C constant temperature 30-90min, then be warming up to 180-220 DEG C of constant temperature 30-90min; Finally be warming up to 280-480
oc constant temperature 20-160min.
The preparation method of Graphene compound polyimide conductive film provided by the invention, described substrate can select sheet glass, silicon chip, aluminium sheet or steel plate; The pull rate of lift film is 5-100mm/min, substrate and liquid level preferred right angle in 90 ° during lift.
The preparation method of Graphene compound polyimide conductive film provided by the invention, graphene oxide compound polyimide conductive film prepared by described method is applied to TFT soft drive circuit.
Oxidation graphene oxide compound polyimide conductive film prepared by the inventive method has the following advantages:
1, the invention provides the preparation method of Graphene compound polyimide conductive film, by the presoma polyamic acid compound by graphene oxide and polyimide, graphene oxide, due to the rich oxygen containing functional groups of its interlayer, effectively improves the dispersiveness of Graphene in polyamic acid; Again graphene oxide composite polyamide acid film is carried out cyclodehydration, obtain Graphene compound polyimide conductive film.
2, the invention provides the preparation method of Graphene compound polyimide conductive film, crystal pulling method is utilized to prepare graphene oxide compound polyimide conductive film, compared with the film prepared with casting method, graphene oxide compound polyimide conductive film thickness prepared by the present invention evenly, good conductivity, physical strength advantages of higher.
Accompanying drawing explanation
Fig. 1 is diamines and the dianhydride monomer structure iron of graphene oxide compound polyimide prepared by embodiment 1.
Fig. 2 is the graphene oxide compound polyimide reaction formula of preparation in embodiment 1.
Fig. 3 is the graphene oxide compound trifluoromethoxy polyimide material reaction formula of preparation in embodiment 2.
Fig. 4 is that the graphene oxide acid anhydrides compound diamines repolymerization dianhydride of preparation in embodiment 3 prepares graphene oxide 3 methyl fluoride polyimide.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.
embodiment 1
(1) preparation of graphite oxide: the 120ml vitriol oil (98%) is poured in the beaker of 2g Graphite Powder 99, then by under beaker dislocation 0 DEG C of ice bath, and 100r/min magnetic agitation 30 minutes, then add 35g potassium permanganate in batches, and stirring velocity is increased to 200r/min stirring 30min, afterwards beaker is displaced to after being incubated 2-3h in 35 DEG C of water-baths and takes out beaker cool to room temperature, in 100r/min whipping process slowly and add 400ml deionized water continuously, control the temperature of mixed solution in this process at 90 DEG C, and be incubated 2h, after sample temperature cool to room temperature, slowly add 100ml, the hydrogen peroxide of 30%, 400ml warm water (40 DEG C) is added after complete reaction, then suction filtration, and wash repeatedly with the dilute hydrochloric acid of 10%, use deionized water water washing more repeatedly, finally dry 12h in 60 DEG C of vacuum drying ovens, obtain graphite oxide.
(2) preparation of graphene oxide compound polyimide solution: take the dried graphite oxide of 0.1g, be dissolved in 50g N, N-N,N-DIMETHYLACETAMIDE (DMAc), ultrasonic 4h, ultrasonic frequency 50KHz.Again above-mentioned solution is placed in flask with three necks,round bottom; under passing into nitrogen protection; add 8mL sulfur oxychloride; and add 10.01g Ursol D PPD; stirring makes it abundant dissolving, then adds 10.91g PMDA and 28.98g DMAc solution in batches, stirs under ice bath; reaction 6h, obtains the graphene oxide composite polyamide acid composite solution of solid content 20%.Wherein used diamine monomer and dianhydride monomer are as shown in Figure 1.The process of its reaction as shown in Figure 2.
(3) preparation of Graphene compound polyimide conductive film: being immersed by sheet glass in graphene oxide composite polyamide acid composite solution, is that 20mm/min lifts plated film with speed, obtained graphene oxide composite polyamide acid film;
The substrate being loaded with graphene oxide composite polyamide acid film is put into vacuum drying oven (under nitrogen environment), ladder-elevating temperature, and cyclodehydration obtains Graphene compound polyimide laminated film; Controlling temperature rise rate in wherein said ladder-elevating temperature process is 2 DEG C/min; First be warmed up to 100 DEG C of constant temperature 60min; Be warmed up to 200 DEG C of constant temperature 60min again; Finally be warmed up to 300 DEG C of constant temperature 60min, obtain Graphene compound polyimide laminated film.Thickness through measurement Graphene compound polyimide laminated film is 20 μm, surface resistivity 4.60 × 10
-8Ω m.
Embodiment 2
(1) graphene oxide step is prepared with step 1 in embodiment 1.
(2) preparation of graphene oxide compound polyimide solution: take the dried graphite oxide of 0.8g, be dissolved in 50g N, N-N,N-DIMETHYLACETAMIDE (DMAc), ultrasonic 6h, ultrasonic frequency 50KHz.Again above-mentioned solution is placed in flask with three necks,round bottom; under passing into nitrogen protection; add 12mL sulfur oxychloride, and add 8.46g N, N '-3 methyl fluoride Ursol D base ether; stirring makes it abundant dissolving; then add 10.91g BPDA and 36.947g DMAc solution in batches, stir under ice bath, reaction 5.4h; obtain the graphene oxide composite polyamide acid composite solution of solid content 10%, reaction as shown in Figure 3.
(3) preparation of Graphene compound polyimide conductive film: sheet glass is immersed in graphene oxide composite polyamide acid composite solution, lift plated film, pull rate is that 10mm/min obtains graphene oxide composite polyamide acid laminated film; The substrate being loaded with graphene oxide composite polyamide acid laminated film is put into vacuum drying oven (under nitrogen environment), ladder-elevating temperature, and cyclodehydration obtains Graphene compound polyimide laminated film; Controlling temperature rise rate in wherein said ladder-elevating temperature process is 5 DEG C/min; First be warmed up to 120 DEG C of constant temperature 60min; Be warmed up to 220 DEG C of constant temperature 40min again; Finally be warmed up to 380 DEG C of constant temperature 30min, obtain Graphene compound polyimide laminated film.Thickness through measurement Graphene compound polyimide laminated film is 30 μm, surface resistivity 1.40 × 10-8 Ω m.
Embodiment 3
(1) graphene oxide step is prepared with step 1 in embodiment 1.
(2) preparation of graphene oxide composite polyamide acid composite solution: take the dried graphite oxide of 1.2g, be dissolved in 50g N, N-N,N-DIMETHYLACETAMIDE (DMAc), ultrasonic 12h, ultrasonic frequency 40KHz.Again above-mentioned solution is placed in flask with three necks,round bottom, under passing into nitrogen protection, temperature is risen to 110 DEG C, form graphene oxide acid anhydrides, rear reduction temperature is to room temperature.Then 1.28g N, N is added '-Ursol D base ether, stirs and makes it abundant dissolving, then add 1.24g PHDA and 16.85g DMAc solution in batches, stir under ice bath, reaction 5.4h, obtain the graphene oxide composite polyamide acid composite solution of solid content 8%, its reaction process as shown in Figure 4.
(3) preparation of Graphene compound polyimide laminated film: sheet glass is immersed in graphene oxide composite polyamide acid composite solution, lift plated film, pull rate is that 5mm/min obtains graphene oxide composite polyamide acid laminated film; The substrate being loaded with graphene oxide composite polyamide acid laminated film is put into vacuum drying oven (under nitrogen environment), ladder-elevating temperature, and cyclodehydration obtains Graphene compound polyimide laminated film; Controlling temperature rise rate in wherein said ladder-elevating temperature process is 5 DEG C/min; First be warmed up to 140 DEG C of constant temperature 40min; Be warmed up to 160 DEG C of constant temperature 20min again; Finally be warmed up to 420 DEG C of constant temperature 30min, obtain Graphene compound polyimide laminated film.Thickness through measurement Graphene compound polyimide laminated film is 18 μm, surface resistivity 8.12 × 10-7 Ω m.
Embodiment 4
(1) graphene oxide step is prepared with step 1 in embodiment 1.
(2) preparation of graphene oxide composite polyamide acid composite solution: take the dried graphite oxide of 1.2g, be dissolved in 50g N, N-N,N-DIMETHYLACETAMIDE (DMAc), ultrasonic 6h, ultrasonic frequency 40KHz.Again above-mentioned solution is placed in flask with three necks,round bottom, under passing into nitrogen protection, temperature is risen to 110 DEG C, form graphene oxide acid anhydrides, rear reduction temperature is to room temperature.Then 1.28g N, N is added '-Ursol D base ether, stirs and makes it abundant dissolving, then add 1.24g PHDA and 16.85g DMAc solution in batches, stir under ice bath, reaction 5.4h, obtain the graphene oxide composite polyamide acid composite solution of solid content 8%.
(3) preparation of Graphene compound polyimide laminated film: sheet glass is kept flat in graphene oxide composite polyamide acid composite solution, lift plated film, pull rate is that 5mm/min obtains the film prepared of graphene oxide composite polyamide acid laminated film; The substrate being loaded with graphene oxide composite polyamide acid laminated film is put into vacuum drying oven (under nitrogen environment), ladder-elevating temperature, and cyclodehydration obtains Graphene compound polyimide laminated film; Controlling temperature rise rate in wherein said ladder-elevating temperature process is 5 DEG C/min; First be warmed up to 140 DEG C of constant temperature 40min; Be warmed up to 160 DEG C of constant temperature 20min again; Finally be warmed up to 380 DEG C of constant temperature 30min, obtain Graphene compound polyimide laminated film.Thickness through measurement Graphene compound polyimide laminated film is 28 μm, surface resistivity 6.45 × 10-7 Ω m.Prepared functional polyalkylene imide membrane is prepared TFT soft drive circuit.
Claims (10)
1. a preparation method for Graphene compound polyimide conductive film, comprises the steps:
(1) preparation of graphene oxide suspension: graphite oxide is scattered in polar solvent, ultrasonic stripping graphite oxide, obtains graphene oxide suspension;
(2) preparation of graphene oxide compound polyimide solution: under protection of inert gas and preset temp condition, successively add sulfur oxychloride and diamines in graphene oxide suspension, add dianhydride after sulfoxide to be chlorinated and diamines fully dissolve; The last solid content adding polar solvent diluting soln again, and stir into homogeneous phase, for subsequent use;
(3) preparation of Graphene compound polyimide conductive film: substrate is immersed in graphene oxide compound polyimide solution, lift plated film; Insert in tube furnace by the substrate being loaded with graphene oxide compound polyimide film, dehydration obtains Graphene compound polyimide conductive film.
2. the preparation method of Graphene compound polyimide conductive film according to claim 1, is characterized in that: described ultrasonic stripping graphite oxide, and ultrasonic frequency is 20-100KHz, and ultrasonic time is 4-6h; The temperature of ultrasonic stripping graphite oxide is 15-35 DEG C.
3. the preparation method of Graphene compound polyimide conductive film according to claim 1, it is characterized in that: described polar solvent is N, one or more arbitrary proportions mixing in N-dimethyl formamide, N, N-N,N-DIMETHYLACETAMIDE, N-methyl-2-pyrrolidone, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF); Described diamines is any one in 2TFMPPD, BBH, FPPD, BDAF, FBA.
4. the preparation method of Graphene compound polyimide conductive film according to claim 1, is characterized in that: described dianhydride is any one in pyromellitic dianhydride, BPDA, PMDA, PHDA, DNDA, CBDA, CHDAn, BCHDABPDA, BTDA, NDO, PDO, Br-PDO, TDO.
5. the preparation method of Graphene compound polyimide conductive film according to claim 1, it is characterized in that: described polar solvent is N, one or more arbitrary proportions mixing in N-dimethyl formamide, N, N-N,N-DIMETHYLACETAMIDE, N-methyl-2-pyrrolidone, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF).
6. the preparation method of Graphene compound polyimide conductive film according to claim 1-6 any one, is characterized in that: the mass ratio of described graphene oxide and diamines controls at 0.1-1.4:1; The mass ratio of described graphene oxide grafting diamine monomer and dianhydride controls at 0.8-1.2:1.
7. the preparation method of Graphene compound polyimide conductive film according to claim 1-6 any one, is characterized in that: described preset temp is 80-110 DEG C; The solid content of described solution is 5%-30%.
8. the preparation method of Graphene compound polyimide conductive film according to claim 1-6 any one, it is characterized in that: described in be loaded with graphene oxide compound polyimide film substrate insert in tube furnace, employing staged heats up, and temperature controls at 200-480
oc.
9. the preparation method of Graphene compound polyimide conductive film according to claim 9, is characterized in that: described ladder-elevating temperature speed is 2-5
oc/min, is warming up to 80-120
oafter C constant temperature 30-90min, then be warming up to 180-220 DEG C of constant temperature 30-90min; Finally be warming up to 280-480
oc constant temperature 20-160min.
10. the preparation method of Graphene compound polyimide conductive film according to claim 1-6 any one, is characterized in that: the graphene oxide compound polyimide conductive film of preparation is applied to TFT soft drive circuit.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110550956A (en) * | 2019-09-25 | 2019-12-10 | 深圳烯创先进材料研究院有限公司 | preparation method of graphene-polyimide-based composite sponge precursor heat-conducting film |
| CN111349255A (en) * | 2020-04-14 | 2020-06-30 | 安徽宇航派蒙健康科技股份有限公司 | Graphene-polyimide conductive film and preparation method thereof |
| CN113088124A (en) * | 2021-04-02 | 2021-07-09 | 宁波龙圣新材料科技有限公司 | Preparation process and method of graphene heating film |
| CN113831734A (en) * | 2021-09-30 | 2021-12-24 | 浙江中科玖源新材料有限公司 | Antistatic polyimide/graphene composite film and preparation method thereof |
| CN116375472A (en) * | 2023-02-28 | 2023-07-04 | 安徽国风新材料股份有限公司 | Super-thick polyimide-based graphite film and preparation method thereof |
-
2014
- 2014-12-15 CN CN201410763000.7A patent/CN104558606A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110550956A (en) * | 2019-09-25 | 2019-12-10 | 深圳烯创先进材料研究院有限公司 | preparation method of graphene-polyimide-based composite sponge precursor heat-conducting film |
| CN110550956B (en) * | 2019-09-25 | 2022-01-11 | 深圳烯创先进材料研究院有限公司 | Preparation method of graphene-polyimide-based composite sponge precursor heat-conducting film |
| CN111349255A (en) * | 2020-04-14 | 2020-06-30 | 安徽宇航派蒙健康科技股份有限公司 | Graphene-polyimide conductive film and preparation method thereof |
| CN113088124A (en) * | 2021-04-02 | 2021-07-09 | 宁波龙圣新材料科技有限公司 | Preparation process and method of graphene heating film |
| CN113831734A (en) * | 2021-09-30 | 2021-12-24 | 浙江中科玖源新材料有限公司 | Antistatic polyimide/graphene composite film and preparation method thereof |
| CN116375472A (en) * | 2023-02-28 | 2023-07-04 | 安徽国风新材料股份有限公司 | Super-thick polyimide-based graphite film and preparation method thereof |
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Application publication date: 20150429 |