CN102718983A - Preparation method of polymer-based conductive microporous foam composite material - Google Patents
Preparation method of polymer-based conductive microporous foam composite material Download PDFInfo
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- CN102718983A CN102718983A CN201210218191XA CN201210218191A CN102718983A CN 102718983 A CN102718983 A CN 102718983A CN 201210218191X A CN201210218191X A CN 201210218191XA CN 201210218191 A CN201210218191 A CN 201210218191A CN 102718983 A CN102718983 A CN 102718983A
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Abstract
The invention discloses a preparation method of a polymer-based conductive microporous foam composite material. The method comprises the following steps of: filling conductive fillers into a polymer to prepare a polymer-based composite material through blending methods of solution blending, melt blending or in-situ polymerizing and the like; preparing a composite material blank with a certain thickness from the polymer-based composite material by die pressing under vacuum; placing the composite material blank into a foaming high-pressure reactor, and dissolving supercutical fluid serving as foaming agent in the composite material blank; and foaming the composite material blank through a quick pressure releasing method or quick heating method when the supercutical fluid in the composite material blank is saturated, and then cooling to shaping the foamed composite material blank. According to the preparation method, the nontoxic pollution-free supercutical fluid is taken as the foaming agent, thus, the preparation method has the advantages of environmental protection, safety, stability, etc. The preparation method serves as a conductive foam material preparation technology with good application prospect.
Description
Technical field
The present invention relates to the polymer foams technical field, particularly relate to a kind of preparation method of polymer-matrix electric conduction fine-celled foam matrix material.
Background technology
Polymer materials is compared with metallic substance, inorganic materials as one of three big materials, has light weight, is prone to processing, corrosion-resistant, low cost and other advantages, is widely used in fields such as packing, medical treatment, national defence.Macromolecular material has very big volume specific resistance usually, about 10
10~ 10
20Ω cm can be used as good electric insulating quality material.Yet higher volume specific resistance has limited the application of macromolecular material at aspects such as electron device packing, electromagnetic shieldings.
The conductive polymer foams material is widely used in aspects such as electron device, antistatic packaging, electromagnetic shielding, and with compared with metal, conductive polymer foams density is little, conductivity range is wide.The preparation of conductive polymer foams material at present mainly contains two kinds of methods: a kind of is to adopt traditional foam process; Utilize pneumatogens such as freonll-11, alkane or azo-bis-isobutyl cyanide chemical foaming agents such as (AIBN) to produce polymer foams; Then at foam materials surface-coated one deck conductive coating paint layer; The conductive polymer foams surface conductivity that this method makes is better, but volume conductance do not improve, and the conductive coating paint layer is prone to come off from the foam of polymers matrix simultaneously; Conductivity is unstable, the conductive polymer foams material that adopts this method the to produce market of fading out gradually; Another kind method is in polymeric matrix, to carry out the tradition foaming behind the conductive doped filler, and traditional foam process adopts pneumatogen or azo-bis-isobutyl cyanide chemical foaming agents such as (AIBN) such as freonll-11, alkane.The conductive polymer foams material of above-mentioned two kinds of methods preparation causes environmental issue and the production safety problem except all existing easily, and the foam material abscess of two kinds of method preparations is bigger; Like Li Jixin (Li Jixin, Ph D dissertation, Jilin University; Changchun; 2007) adopting Cellmic C 121 (AC) is whipping agent, has prepared high density polyethylene(HDPE) (HDPE)/carbon black (CB) conductive foam, the about 150 μ m of its abscess mean pore size.Bigger cell diameter makes the mechanical property of foam materials and conductivity relatively poor, big limitations conductive foaming material range of application.Affiliated technical field is badly in need of the conductive polymer foams preparation methods that exploitation makes new advances, and all is better conductive polymer foams material to prepare mechanical property and conductivity.
Summary of the invention
The deficiency that exists to the conductive polymer foams material preparation method of prior art; The object of the invention aims to provide a kind of novel method for preparing the polymer-matrix electric conduction foamed composite; Problems such as the cell diameter that exists with the polymer-matrix electric conduction foam materials that solves prior art for preparing is big, and the mechanical property of foam materials and conductivity are relatively poor.
The preparation method of polymer-matrix electric conduction foamed composite provided by the invention mainly comprises following process step:
(1) adopt blend method that conductive filler material is filled into and obtain polymer matrix composite in the polymkeric substance, the consumption of conductive filler material satisfies the electric conductivity of design for the foamed composite that can make preparation;
(2) the resulting polymer matrix composite vacuum mold of step (1) is pressed into the base substrate of design shape;
(3) the resulting polymer matrix composite base substrate of step (2) is placed the foaming autoclave; Feed supercutical fluid; Pressure-controlling in the reaction kettle is being higher than the emergent pressure of supercutical fluid; Temperature is controlled at the critical temperature that is higher than supercutical fluid, supercutical fluid is added in the polymer matrix composite base substrate, when supercutical fluid reaches capacity state in composite body after; Make the composite body foaming through quick voltage drop method or the method for being rapidly heated, promptly prepare polymer-based carbon fine-celled foam matrix material behind the cooling and shaping with electroconductibility.
In the aforesaid method, be thermoplastic polymer as the polymkeric substance of conductive foam matrices of composite material, but amorphous thermoplastic polymers, or the crystalline thermoplastic polymkeric substance.
In the aforesaid method, conductive filler material can be selected from metal-powder, graphite, carbon black, carbon nanotube, thomel and Graphene etc., can select wherein one or more for use.Wherein carbon nanotube, Graphene have good electrical conductivity, and specific surface area is bigger, in polymkeric substance, more be prone to form conductive network, so addition are less, can keep the mechanical property of polymkeric substance better, should preferentially select for use.
In the aforesaid method, blend method can be selected a kind of in solution blending, melt blending, the in-situ polymerization blend according to the characteristic of conductive filler material and polymkeric substance, and purpose is to let conductive filler material be evenly dispersed in the polymeric matrix.
In the aforesaid method, supercritical gas is selected from carbonic acid gas, nitrogen, air and argon gas etc.
In the aforesaid method, the rate of pressure reduction (mean rate) of step-down foaming is 1MPa/s ~ 50MPa/s fast.
The preparation method of polymer-matrix electric conduction foamed composite provided by the invention is the CO with supercritical state
2, N
2Deng being whipping agent, rise sharply through pressure drop or temperature and foam, adopt pneumatogen such as freonll-11, alkane or azo-bis-isobutyl cyanide chemical foaming agents such as (AIBN) to compare the CO under the supercritical state with traditional foam process
2, N
2Significantly improve Deng solubleness in polymkeric substance and velocity of diffusion, and after supercutical fluid is dissolved in polymkeric substance, make it to get into hypersaturated state (or thermodynamic instability attitude) through pressure drop (or temperature rises sharply); And then cause a large amount of gas nucleus formation; The abscess nucleation rate reaches the high value order of magnitude of traditional foam process (be doubly) in this process, and is much higher than the speed (being the abscess growth velocity) that whipping agent diffuses into abscess, therefore under this condition; Before beginning to grow up, abscess can produce a large amount of abscesses; The conductive foam that makes, its cell density is big, and cell diameter is little and even.
The preparation method of polymer-matrix electric conduction foamed composite provided by the invention, the preparation method of polymer-matrix electric conduction foamed composite compared to prior art, summarize and get up to have the outstanding advantage of following ten minutes:
(1) the present invention prepares the polymer-matrix electric conduction foamed composite with supercritical gas, compares with the polymer foams that traditional method makes, and cell diameter is little, and cell density is high, and the mechanical property of foam materials is good.
(2) the polymer-matrix electric conduction foamed composite that makes of the present invention can be through its cell morphologies of foaming conditions control such as control saturation pressure, temperature of saturation, blowing temperature, rate of pressure reductions, thereby regulate its volume specific resistance, to satisfy different needs.
(3) the method for the invention adopt conventional rare gas element supercritical state as whipping agent, with low cost, help environment protection.
(4) the polymer-matrix electric conduction foamed composite that makes of the present invention can be widely used in fields such as biomedical engineering, antistatic packaging, electron device and electromagnetic shielding.
(5) the method for the invention technology is simple, and equipment is conventional equipment, is easy to realize industriallization.
Description of drawings
Accompanying drawing 1 is the Electronic Speculum figure of the polymer-matrix electric conduction foamed composite of the embodiment of the invention 1 preparation with electron microscope scanning.
Accompanying drawing 3 is the polymer-matrix electric conduction foamed composite of the embodiment of the invention 3 preparations Electronic Speculum figure with electron microscope scanning.
Embodiment
Below in conjunction with embodiment the present invention is described further, but it is important to point out, can not embodiment be interpreted as protection domain of the present invention.
In following each embodiment, involved material component percentage composition is mass content per-cent except that specifying.
Embodiment 1
Present embodiment is a raw material with POLYACTIC ACID (PLA) and hydroxylation multi-walled carbon nano-tubes (MWNTs), and POLYACTIC ACID is produced by U.S. NatureWorks company, and model 2002D is semi-crystalline polymer, and dextrorotation POLYACTIC ACID mass content is 4.25%, and density is 1.24 g/cm
3, the hydroxylation multi-walled carbon nano-tubes is produced by Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences, model: TNMH5, and purity is greater than 95%, and-OH mass content is 1.76%, external diameter: 20-30 nm, the about 30 μ m of length.
Processing condition and step are following:
(1) 5 g POLYACTIC ACIDs is dissolved in the dichloromethane solvent of 50 ml; Simultaneously 208 mg carbon nanotube sonic oscillations are dispersed in the 20 ml methylene dichloride; Carry out sonic oscillation after pouring into the carbon nanotube dispersion liquid in the POLYACTIC ACID solution then; After treating that carbon nanotube is uniformly dispersed, dispersion liquid poured in the cover glass petridish made solvent evaporates, after methylene dichloride is evaporated completely basically; Transfer in the vacuum drying oven drying and remove residual solvent, obtain the carbon nanotube massfraction and be 4% PLA/ MWCNTs matrix material;
(2) matrix material that step (1) is made shreds and carries out vacuum compression molding; Molding temperature is 190 ℃; Pressure is 10 MPa, and the dwell time is 5 minutes, adopts the quick cooling and shaping of frozen water then; Obtaining thickness is the matrix material sheet base substrate of 0.5 mm, with the vacuum-drying 4 hours at ambient temperature of matrix material sheet base substrate;
(3) the matrix material sheet base substrate with step (2) gained places the foaming autoclave, feeds supercritical CO
2, the pressure-controlling in the reaction kettle is controlled at 115 ℃ in 20 MPa, temperature, makes supercritical CO
2Be added in the matrix material sheet base substrate, work as supercritical CO
2In matrix material sheet base substrate, reach capacity behind the state, with the release speed of about 20 MPa/s the pressure in the reaction kettle is unloaded and be depressed into normal pressure, promptly obtain having the polymer-based carbon fine-celled foam matrix material of electroconductibility through cooling and shaping.
The volume specific resistance test of the polymer-matrix electric conduction foamed composite of gained: for reducing contact resistance; After conduction cellular material two ends are coated with elargol; Employing is carried out resistance test with favour TH2684 high precision Insulation Resistance Tester, and the volume specific resistance that obtains conductive foams is 1.4 * 10
4Ω cm.
For observing the microscopic pattern of conductive foams, with foam materials brittle failure in liquid nitrogen, (SEM) observes its cross-section morphology with sem, and its fracture morphology is as shown in Figure 1.Adopt Image-pro plus 6.0 statistics abscess mean diameters to be about 10 μ m.
The present embodiment raw material is identical with embodiment 1
Processing condition and step are following:
(1) identical with embodiment 1 step (1);
(2) identical with embodiment 1 step (2);
(3) base substrate with step (2) gained places the foaming autoclave, feeds supercritical CO
2, the pressure-controlling in the reaction kettle is controlled at 115 ℃ in 24 MPa, temperature, makes supercritical CO
2Be added in the matrix material sheet base substrate, work as supercritical CO
2In matrix material sheet base substrate, reach capacity behind the state, with the release speed of about 30 MPa/s the pressure in the reaction kettle is unloaded and be depressed into normal pressure, promptly obtain having the polymer-based carbon fine-celled foam matrix material of electroconductibility behind the cooling and shaping.
Volume specific resistance: for reducing contact resistance, after conduction abscess two ends are coated with elargol, adopt and carry out resistance test, obtain the conductive foam volume specific resistance: 4.0 * 10 with favour TH2684 high precision Insulation Resistance Tester
3Ω cm.
For observing the microscopic pattern of conductive foam, with porous plastics brittle failure in liquid nitrogen, (SEM) observes its cross-section morphology with sem, and its fracture morphology is as shown in Figure 2.Adopt Image-pro plus 6.0 statistics abscess mean diameters to be about 6 μ m.
Embodiment 3
The present embodiment raw material is identical with embodiment 1
Processing condition and step are following:
(1) 5 g POLYACTIC ACIDs is dissolved in the dichloromethane solvent of 50 ml; Simultaneously 102 mg carbon nanotube sonic oscillations are dispersed in the 20 ml methylene dichloride; Carry out sonic oscillation after pouring into the carbon nanotube dispersion liquid in the POLYACTIC ACID solution then; After treating that carbon nanotube is uniformly dispersed, dispersion liquid poured in the cover glass petridish made solvent evaporates, after methylene dichloride is evaporated completely basically; Transfer in the vacuum drying oven drying and remove residual solvent, obtain the carbon nanotube massfraction and be 2% PLA/ MWCNTs matrix material;
(2) identical with embodiment 1 step (2);
(3) identical with embodiment 1 step (3).
Volume specific resistance: for reducing contact resistance, after conduction abscess two ends are coated with elargol, adopt and carry out resistance test, obtain the conductive foam volume specific resistance: 1.4 * 10 with favour TH2684 high precision Insulation Resistance Tester
7Ω cm.
For observing the microscopic pattern of conductive foam, with porous plastics brittle failure in liquid nitrogen, (SEM) observes its cross-section morphology with sem, and its fracture morphology is as shown in Figure 3.Adopt Image-pro plus 6.0 statistics abscess mean diameters to be about 9 μ m.
Embodiment 4
Present embodiment is a raw material with PS (PS) and carbon black (CB).PS (PS) is produced by platform plastic cement ltd, model 5250 A230, and density is 1.04g/cm
3Carbon black (CB) is produced by U.S. Cabot Co.,Ltd, model VXC-605, and butylene phthalate (DBP) absorption value is 148 ± 15cm
3/ g, before using under 120 ℃ of conditions baking oven inner drying 10 hours to remove moisture.
Processing condition and step are following:
(1) press PS and carbon black mass than for 80:20 prepares burden, under normal pressure, 200 ℃ in torque rheometer mixing 10 minutes, carbon black is dispersed in the PS, obtain the carbon black mass mark and be 20% PS/CB matrix material.
(2) matrix material that step (1) is made carries out vacuum compression molding, and molding temperature is 200 ℃, and pressure is 10 MPa, and the dwell time is 5 minutes, and obtaining thickness is the matrix material sheet base substrate of 1 mm;
(3) base substrate with step (2) gained places the foaming autoclave, feeds overcritical N
2, the pressure-controlling in the reaction kettle is controlled at 100 ℃ in 20 MPa, temperature, makes overcritical N
2Be added in the matrix material sheet base substrate, as overcritical N
2In matrix material sheet base substrate, reach capacity behind the state, with the release speed of about 50 MPa/s the pressure in the reaction kettle is unloaded and be depressed into normal pressure, promptly obtain having the polymer-based carbon fine-celled foam matrix material of electroconductibility behind the cooling and shaping.
Volume specific resistance: for reducing contact resistance, after conduction abscess two ends are coated with elargol, adopt and carry out resistance test, obtain the conductive foam volume specific resistance: 2.0 * 10 with favour TH2684 high precision Insulation Resistance Tester
3Ω cm.
Embodiment 5
The present embodiment raw material is identical with embodiment 4
Processing condition and step are following:
(1) press PS and carbon black mass than for 90:10 prepares burden, under normal pressure, 200 ℃ in torque rheometer mixing 10 minutes, carbon black is dispersed in the PS, obtain the carbon black mass mark and be 10% PS/CB matrix material;
(2) identical with embodiment 4 steps (2);
(3) base substrate with step (2) gained places the foaming autoclave, feeds overcritical N
2, the pressure-controlling in the reaction kettle is controlled at 80 ℃ in 20 MPa, temperature, makes overcritical N
2Be added in the matrix material sheet base substrate, as overcritical N
2In matrix material sheet base substrate, reach capacity behind the state, with the release speed of about 30 MPa/s the pressure in the reaction kettle is unloaded and be depressed into normal pressure, promptly obtain having the polymer-based carbon fine-celled foam matrix material of electroconductibility behind the cooling and shaping.
Volume specific resistance: for reducing contact resistance, after conduction abscess two ends are coated with elargol, adopt and carry out resistance test, obtain the conductive foam volume specific resistance: 4.8 * 10 with favour TH2684 high precision Insulation Resistance Tester
8Ω cm.
Claims (10)
1. the preparation method of a polymer-matrix electric conduction fine-celled foam matrix material is characterized in that may further comprise the steps:
(1) adopt blend method that conductive filler material is filled into and obtain polymer matrix composite in the polymkeric substance, the consumption of conductive filler material satisfies the electric conductivity of design for the foamed composite that can make preparation;
(2) the resulting polymer matrix composite vacuum mold of step (1) is pressed into the base substrate of design shape;
(3) the resulting polymer matrix composite base substrate of step (2) is placed the foaming autoclave; Feed supercutical fluid; Pressure-controlling in the reaction kettle is being higher than the emergent pressure of supercutical fluid; Temperature is controlled at the critical temperature that is higher than supercutical fluid, supercutical fluid is added in the polymer matrix composite base substrate, when supercutical fluid reaches capacity state in composite body after; Make composite body foaming, the polymer-based carbon fine-celled foam matrix material that promptly obtains having electroconductibility behind the cooling and shaping through quick voltage drop method or the method for being rapidly heated.
2. the preparation method of polymer-matrix electric conduction fine-celled foam matrix material according to claim 1 is characterized in that said conductive filler material is selected from metal-powder, carbon black, graphite, carbon nanotube, thomel and Graphene.
3. the preparation method of polymer-matrix electric conduction fine-celled foam matrix material according to claim 2 is characterized in that said conductive filler material is selected from carbon nanotube and Graphene.
4. the preparation method of polymer-matrix electric conduction fine-celled foam matrix material according to claim 1 is characterized in that said polymkeric substance is a thermoplastic polymer.
5. the preparation method of polymer-matrix electric conduction fine-celled foam matrix material according to claim 1 is characterized in that described supercutical fluid is selected from carbonic acid gas, nitrogen, air and argon gas.
6. according to the preparation method of the described polymer-matrix electric conduction fine-celled foam of one of claim 1 to 5 matrix material, it is characterized in that the conductive filler material mass content is 0.1 ~ 20% of a polymer matrix composite.
7. according to the preparation method of the described polymer-matrix electric conduction fine-celled foam of one of claim 1 to 5 matrix material, it is characterized in that said blend method is a kind of in solution blending, melt blending or the in-situ polymerization blend.
8. the preparation method of polymer-matrix electric conduction fine-celled foam matrix material according to claim 6 is characterized in that said blend method is a kind of in solution blending, melt blending or the in-situ polymerization blend.
9. according to the preparation method of the described polymer-matrix electric conduction fine-celled foam of one of claim 1 to 5 matrix material, it is characterized in that the polymer matrix composite base substrate adopts quick voltage drop method foaming, the rate of pressure reduction of said quick step-down is 1 MPa/s ~ 50 MPa/s.
10. the preparation method of polymer-matrix electric conduction fine-celled foam matrix material according to claim 8 is characterized in that the polymer matrix composite base substrate adopts quick voltage drop method foaming, and the rate of pressure reduction of said quick voltage drop method is 1 MPa/s ~ 50 MPa/s.
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| CN104842568A (en) * | 2015-04-20 | 2015-08-19 | 中国科学院长春应用化学研究所 | Preparation method of conductive polymeric material |
| CN107629443A (en) * | 2017-08-04 | 2018-01-26 | 浙江新恒泰新材料有限公司 | Microporous foam conductive thermoplastic elastomer material and its production method with pressure-sensitive character |
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| CN114295775B (en) * | 2020-10-08 | 2023-08-08 | 中国石油大学(华东) | Experimental method for representing rheological property of foam fluid in pipe flow state |
| CN114864892A (en) * | 2022-04-25 | 2022-08-05 | 昆明理工大学 | Preparation method and application of microporous conversion alloying material |
| CN114864892B (en) * | 2022-04-25 | 2023-11-14 | 昆明理工大学 | Preparation method and application of microporous transformation alloying material |
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