CN110272625B - Conductive polymer composite material with multilayer hole structure and preparation method and application thereof - Google Patents
Conductive polymer composite material with multilayer hole structure and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of composite materials, and provides a multilayer porous structure conductive polymer composite material, a preparation method and application thereof, aiming at solving the problems of weaker mechanical property, poor structural stability, complex preparation process and high closed porosity of the traditional porous material, wherein the multilayer porous structure conductive polymer composite material comprises the following components in percentage by mass based on the total mass of the multilayer porous structure conductive polymer composite material: 2-50% of conductive filler and 50-98% of organic silicon elastomer. The conductive polymer composite material with the multilayer hole structure prepared by the invention has the characteristics of good compression resilience, excellent sensitivity, stability and recycling property when being used as a sensor material and the like, so that the conductive polymer composite material can be used as a conductive polymer material, an elastic strain sensor and a gas sensor material.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a conductive polymer composite material with a multilayer hole structure, and a preparation method and application thereof.
Background
When the conductive filler/polymer composite materials (CPCs) are subjected to external stimuli (such as strain, temperature, organic gas and the like), the resistance changes regularly, so that the conductive filler/polymer composite materials have wide application prospects in the field of sensors. Such as: the gas-sensitive material as an organic gas sensitive material has wide application prospects in the aspects of environmental monitoring, monitoring of harmful reagents and gas leakage in chemical production, electronic nose and the like; while strain sensing (pressure and tension) materials with elastic macromolecules as the matrix are the most popular researches in the fields of intelligent robots, health monitoring, human-computer interaction and the like.
At present, the traditional material used as a strain sensor has the defects of unstable output resistance signals, low responsivity, small strain range and the like, and practical application of the traditional material is limited. With the progress of research, it has been found that porous conductive filler/polymer composite materials having a pore structure (particularly a through-pore structure) have many advantages as sensor materials: if the strain sensor has a larger strain deformation range, a wider test domain can be provided for the strain sensor, and the strain sensor has excellent deformability and is suitable for exploring the micro-stress effect; in addition, when the material is used as a gas sensor material, the existence of the holes increases the contact surface of gas and the sensitive material, and simultaneously, a plurality of channels are provided for the invasion of harmful gas, so that the sensitivity of the material can be effectively improved.
Classified by preparation methods, such porous materials are mainly classified into two types: one uses foam as a template, and conductive particles are directly self-assembled on the surface of the foam by using the foam as the template, so that the conductive particle-based porous material is prepared; in another type, the bubbles are generated during the formation of the conductive filler/polymer composite by various chemical and physical foaming methods. However, the former of the two materials has weak mechanical property and poor structural stability, and the latter has complex process and basically closed cells.
Therefore, the porous CPCs material with larger compressive strain and higher structural stability is prepared by regulating and controlling the microstructure of the porous material, so that the material has excellent sensitivity, good sensitivity stability and repeatability and has great research significance.
The invention discloses a conductive polymer composite material with a continuous isolation structure and a preparation method thereof in Chinese patent literature, wherein the publication number is CN105647017A, the invention provides the conductive polymer composite material with the continuous isolation structure, the raw materials of the conductive polymer composite material comprise a polymer 1 and a conductive filler, and the continuous isolation structure is as follows: the conductive filler is regularly distributed in the polymer 1 in the form of a three-dimensional network of layers of particles, and the polymer 1 is separated by the layers of conductive filler particles, while the polymer 1 still maintains a continuous structure. However, the material of the invention has high preparation cost, is not beneficial to gas diffusion, and has certain limitation in the application of the sensing field.
Disclosure of Invention
The invention provides a conductive polymer composite material with a multilayer pore structure, which has good compression resilience, gas sensitivity, stability and excellent recycling property, and aims to solve the problems of weak mechanical property, poor structural stability, complex preparation process and high closed pore rate of the traditional porous material.
The invention also provides a preparation method of the conductive polymer composite material with the multilayer hole structure.
The invention also provides application of the conductive polymer composite material with the multilayer hole structure in the fields of conductive polymers, elastic strain sensing and gas-sensitive sensing.
In order to achieve the purpose, the invention adopts the following technical scheme:
the multilayer hole structure conductive polymer composite material takes the total mass of the multilayer hole structure conductive polymer composite material as a reference, and comprises the following components in percentage by mass: 2-50% of conductive filler and 50-98% of organic silicon elastomer.
Preferably, the resistivity of the conductive polymer composite material with the multilayer hole structure is 102 ~ 108Omega cm; the conductive polymer composite material with the multilayer hole structure is provided with a three-dimensional conductive network structure and a multilayer hole structure.
Preferably, the conductive filler is selected from one or more of graphene, graphene derivatives, carbon black, carbon fibers, carbon nanofibers, graphite and carbon nanotubes.
Preferably, the graphene derivative is a graphene nanosheet or a graphene nanoribbon.
Preferably, the main raw material of the silicone elastomer is liquid silicone oil or solid silicone rubber.
Preferably, the silicone elastomer is self-crosslinking in an addition or condensation type.
Preferably, the main raw material of the silicone elastomer is addition type vinyl silicone oil.
A preparation method of a conductive polymer composite material with a multilayer hole structure comprises the following steps:
(1) adding a conductive filler into an organic solvent, and performing ultrasonic dispersion for 10-40 min to obtain a conductive filler suspension dispersion liquid; the concentration of the conductive filler suspension dispersion liquid is 0.01-0.2 g/ml;
(2) adding the organic silicon elastomer raw material into an organic solvent for full dissolution to obtain organic silicon elastomer raw material liquid; the raw materials of the organic silicon elastomer comprise a crosslinking curing auxiliary agent, an inhibitor and the like; the adding amount of the organic silicon elastomer raw material is that 1g of organic silicon elastomer raw material is added into every 1-5 ml of organic solvent;
(3) blending the conductive filler suspension dispersion liquid and the organic silicon elastomer raw material liquid, and uniformly stirring and mixing at a high speed to obtain a conductive filler/organic silicon elastomer mixed solution;
(4) soaking the foam metal into the conductive filler/organic silicon elastomer mixed solution prepared in the step (3), and enabling the conductive filler/organic silicon elastomer mixed solution to wrap the foam metal framework through vacuum bubble removal and oscillation;
(5) and (3) rotating the foam metal after full dip coating at a low speed, removing the conductive filler/organic silicon elastomer mixed solution at the hole blocking part, drying, discharging the organic solvent, curing the organic silicon elastomer, and finally etching the foam metal to obtain the conductive polymer composite material with the multilayer hole structure.
The invention comprehensively solves the defects of unstable output resistance signals, low responsiveness and small strain range of the traditional solid conductive filler/polymer composite material sensor, and the defects of insufficient structural firmness of the porous material, complex and harsh process and the like. The conductive polymer composite material with the multilayer hole structure prepared by the invention has the characteristics of good compression resilience, excellent sensitivity, stability and recycling property when being used as a sensor material and the like, so that the conductive polymer composite material can be used as a conductive polymer material, an elastic strain sensor and a gas sensor material.
Preferably, the foam metal is selected from one of nickel foam, copper foam and aluminum foam.
Preferably, in the step (5), 3-6 mol/l hydrochloric acid solution is adopted to etch the foamed nickel; etching the foam copper by adopting 1mol/l ferric trichloride/hydrochloric acid solution; etching by using 1-2 mol/l sodium hydroxide, then treating and etching the foamed aluminum by using 4-6 mol/l nitric acid, and dissolving the foamed aluminum by using 1mol/l sodium hydroxide solution/0.1 mol/l ferric trichloride mixed solution.
Preferably, in the step (3), the process conditions of high-speed stirring are as follows: firstly stirring at 500 rpm for 5-15 min, and then stirring at 2000-3000 rpm for 20-80 min; the concentration of the conductive filler/organic silicon elastomer mixed solution is 0.05-0.5 g/ml.
Preferably, in the steps (1), (2) and (5), the organic solvent is one or more selected from hexane, petroleum ether, n-heptane, toluene, xylene and tetrahydrofuran; the hexane is n-hexane or cyclohexane.
Preferably, in the step (5), the rotation speed of the low-speed rotation is controlled to be 300-800 rpm.
Therefore, the invention has the following beneficial effects:
(1) multilayer hole structure: the structure has a large foam pore structure with the size of mum-mm, the foam pore framework is a hollow structure, and an irregular small pore structure can be constructed on the wall of the hollow framework;
(2) the material can generate large deformation under the action of micro force, and the deformation detection range of the material as a sensor is large and the sensitivity is good; as a gas sensor, the material has large surface area and a through hole structure is easy to diffuse gas.
Drawings
FIG. 1 is an SEM image of a multi-layer porous conductive polymer composite prepared in example 1.
FIG. 2 is an SEM image of a multi-layer porous conductive polymer composite prepared in example 2.
FIG. 3 is an SEM image of a multi-layer porous conductive polymer composite prepared in example 3.
FIG. 4 is a response curve of the conductive polymer composite with multi-layer porous structure prepared in example 1 in hexane vapor, whereinRelative resistance (instantaneous resistance R/initial resistance R)0) The gas sensitivity responsivity of the material is characterized.
FIG. 5 is a pressure-sensitive cycle curve of the multi-layer porous structure conductive polymer composite prepared in example 3 at 40% deformation, wherein the relative resistance ((difference between the instantaneous resistance R and the initial resistance)/the initial resistance R0) The pressure sensitive responsivity of the material is characterized.
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the accompanying drawings.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
(1) Adding the carbon nanofibers into n-hexane, and performing ultrasonic dispersion for 20 min to obtain a carbon nanofiber/n-hexane dispersion liquid with the concentration of 0.05 g/ml;
(2) adding the addition type liquid silicone oil and the crosslinking curing auxiliary agent, the inhibitor and the like thereof into n-hexane for full dissolution, wherein the adding amount of the organic silicon elastomer raw material is that 1g of the organic silicon elastomer raw material is added into every 2ml of organic solvent;
(3) blending the two solutions, and mechanically stirring at a high speed: stirring at 500 rpm for 10 min, then stirring at 3000 rpm for 30 min, and removing part of solvent to obtain n-hexane dispersion liquid of conductive filler/organic silicon elastomer with concentration of 0.5 g/ml;
(4) soaking foamed nickel into the prepared mixed solution, and uniformly coating the foamed nickel by a vacuum bubble removal and 500 rpm rotary centrifugation method without blocking holes;
(5) curing for 2h at the temperature of 80 ℃, and finally etching off the foamed nickel in the material by using 4 mol/l hydrochloric acid solution to obtain the conductive polymer composite material with the multilayer hole structure.
As shown in FIG. 1, SEM (scanning electron microscope) of the conductive polymer composite material with the multilayer hole structure prepared by the embodiment shows that the material has a cell structure of 500-800 mu m, and a framework is hollowStructurally, the skeleton has small holes distributed in the wall. Wherein the mass percent of the carbon nanofibers is 16 percent, the mass percent of the organic silicon elastomer is 84 percent, and the resistivity of the conductive polymer composite material 1 with the multilayer porous structure is about 2 multiplied by 104 Ω.cm。
The response curve of the conductive polymer composite material with a multilayer porous structure prepared in this example in hexane solvent vapor is shown in fig. 4, where the relative resistance (instantaneous resistance R/initial resistance R) is shown in fig. 40) Characterizing the gas-sensitive responsivity of the material; as can be seen from fig. 4, the material has excellent gas sensitive response behavior: the relative resistance change rate is as high as 105The above, the repetitive stability is good.
Example 2
(1) Adding graphene nanosheets into n-hexane, and carrying out ultrasonic treatment for 15min to obtain graphene nanosheet/n-hexane dispersion liquid with the concentration of 0.01 g/ml;
(2) adding the addition type liquid silicone oil and the crosslinking curing auxiliary agent, the inhibitor and the like thereof into n-hexane for full dissolution, wherein the adding amount of the organic silicon elastomer raw material is that 1g of the organic silicon elastomer raw material is added into every 5ml of organic solvent;
(3) blending the two solutions, and mechanically stirring at a high speed: stirring at 500 rpm for 10 min, then stirring at 3000 rpm for 50 min, and removing part of solvent to obtain n-hexane dispersion liquid of conductive particles/organic silicon elastomer with concentration of 0.2 g/ml;
(4) soaking the foamy copper into the prepared mixed solution, and uniformly coating the foamy copper without blocking holes by a vacuum bubble removal and 700 rpm rotary centrifugation method;
(5) and (3) discharging the solvent for 4 hours at the temperature of 50 ℃, curing for 2.5 hours at the temperature of 80 ℃, and finally etching the foamy copper in the material by using 1mol/l ferric trichloride/hydrochloric acid solution to obtain the multilayer porous structure conductive polymer composite material.
As shown in FIG. 2, an SEM image of the conductive polymer composite material with the multilayer hole structure prepared by the embodiment shows that the material has a through hole structure, the size of a large pore is 300 mu m, the framework is of a hollow structure, and a small amount of irregular holes are distributed on the wall. Wherein the graphene nano-sheet accounts for 6 percent by mass, andthe weight percentage of the organic silicon elastomer is 94 percent, and the resistivity of the conductive polymer composite material 2 with the multilayer porous structure is about 1.5 multiplied by 104 Ω.cm。
Example 3
(1) Adding the carbon nano tube into dimethylbenzene, and carrying out ultrasonic treatment for 15min to obtain a carbon nano tube/dimethylbenzene dispersion liquid with the concentration of 0.08 g/ml;
(2) adding the addition type liquid silicone oil, the crosslinking curing auxiliary agent, the inhibitor and the like into dimethylbenzene for full dissolution, wherein the adding amount of the organic silicon elastomer raw material is that 1g of the organic silicon elastomer raw material is added into each 3ml of organic solvent;
(3) blending the two solutions, and mechanically stirring at a high speed: stirring at 500 rpm for 10 min, then stirring at 3000 rpm for 50 min, and removing part of solvent to obtain xylene dispersion of conductive particles/organic silicon elastomer with concentration of 0.2 g/ml;
(4) soaking foamed nickel into the prepared mixed solution, and uniformly coating the foamed nickel by a vacuum bubble removal and 400 rpm rotary centrifugation method without blocking holes;
(5) and (3) curing for 5 hours at the temperature of 80 ℃, finishing solvent removal and curing, and finally etching off the foamed nickel in the material by using 5 mol/l of dilute hydrochloric acid to obtain the multilayer hole structure conductive polymer composite material.
As shown in fig. 3, the SEM image of the conductive polymer composite material with a multilayer porous structure prepared in this embodiment shows that the material is a through-hole structure, has large pores, and the skeleton of the pores is a hollow structure, and a large number of irregular pores are also present on the skeleton wall, and some irregular small pores are also present on the hollow skeleton wall of the material. Wherein, the mass percent of the carbon nano tube is 4 percent, the mass percent of the organic silicon elastomer is 96 percent, and the resistivity of the conductive polymer composite material with the multilayer hole structure is about 3 multiplied by 104 Ω.cm。
The pressure-sensitive behavior response curve of the conductive polymer composite material with the multi-layer porous structure prepared in this example at 40% deformation is shown in fig. 5, where the relative resistance (instantaneous resistance R/initial resistance R)0) The pressure sensitive responsivity of the material is characterized. As can be seen from FIG. 5, the stress required to produce 40% deformation of the material is only thatAbout 0.4 kPa, the relative resistance change rate of the pressure-sensitive response behavior reaches 35 percent, and the repeated stability is good.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. The conductive polymer composite material with the multilayer hole structure is characterized by comprising the following components in percentage by mass based on the total mass of the conductive polymer composite material with the multilayer hole structure: 2-50% of conductive filler and 50-98% of organic silicon elastomer;
the preparation method of the conductive polymer composite material with the multilayer hole structure comprises the following steps:
(1) adding a conductive filler into an organic solvent, and performing ultrasonic dispersion to obtain a conductive filler suspension dispersion liquid;
(2) adding the organic silicon elastomer raw material into an organic solvent for full dissolution to obtain organic silicon elastomer raw material liquid;
(3) blending the conductive filler suspension dispersion liquid and the organic silicon elastomer raw material liquid, and uniformly stirring and mixing at a high speed to obtain a conductive filler/organic silicon elastomer mixed solution;
(4) soaking the foam metal into the conductive filler/organic silicon elastomer mixed solution prepared in the step (3), and enabling the conductive filler/organic silicon elastomer mixed solution to wrap the foam metal framework through vacuum bubble removal and oscillation;
(5) and rotating the fully dip-coated foam metal at a low speed, removing the conductive filler/organic silicon elastomer mixed solution at the hole blocking part, drying, discharging the organic solvent, curing the organic silicon elastomer, and etching the foam metal to obtain the conductive polymer composite material with the multilayer hole structure.
2. The conductive polymer composite material with multi-layer porous structure as claimed in claim 1, wherein the conductive polymer composite material with multi-layer porous structure is prepared by mixing a polymer material with a solventThe resistivity of the conductive polymer composite material with the multi-layer hole structure is 102 ~ 108Omega cm; the conductive polymer composite material with the multilayer hole structure is provided with a three-dimensional conductive network structure and a multilayer hole structure.
3. The composite material of claim 1, wherein the conductive filler is one or more selected from graphene, graphene derivatives, carbon black, carbon fibers, graphite, and carbon nanotubes.
4. The composite material of claim 1, wherein the silicone elastomer is liquid silicone oil or solid silicone rubber.
5. The composite material of claim 1, wherein the silicone elastomer is self-crosslinked by an addition or condensation method.
6. The composite material as claimed in claim 1, wherein the silicone elastomer is an addition vinyl silicone oil.
7. The method for preparing the conductive polymer composite material with the multilayer porous structure according to claim 1, 2, 3, 4, 5 or 6, which comprises the following steps:
(1) adding a conductive filler into an organic solvent, and performing ultrasonic dispersion to obtain a conductive filler suspension dispersion liquid;
(2) adding the organic silicon elastomer raw material into an organic solvent for full dissolution to obtain organic silicon elastomer raw material liquid;
(3) blending the conductive filler suspension dispersion liquid and the organic silicon elastomer raw material liquid, and uniformly stirring and mixing at a high speed to obtain a conductive filler/organic silicon elastomer mixed solution;
(4) soaking the foam metal into the conductive filler/organic silicon elastomer mixed solution prepared in the step (3), and enabling the conductive filler/organic silicon elastomer mixed solution to wrap the foam metal framework through vacuum bubble removal and oscillation;
(5) and rotating the fully dip-coated foam metal at a low speed, removing the conductive filler/organic silicon elastomer mixed solution at the hole blocking part, drying, discharging the organic solvent, curing the organic silicon elastomer, and etching the foam metal to obtain the conductive polymer composite material with the multilayer hole structure.
8. The method for preparing the conductive polymer composite material with the multi-layer hole structure according to claim 7, wherein in the step (3), the process conditions of high-speed stirring are as follows: firstly stirring at 500 rpm for 5-15 min, and then stirring at 2000-3000 rpm for 20-80 min; the concentration of the conductive filler/organic silicon elastomer mixed solution is 0.05-0.5 g/mL.
9. The method for preparing the conductive polymer composite material with the multilayer porous structure according to claim 7, wherein in the steps (1), (2) and (5), the organic solvent is one or more selected from hexane, petroleum ether, n-heptane, toluene, xylene and tetrahydrofuran; in the step (5), the rotating speed of the low-speed rotation is controlled to be 300-800 rpm.
10. The use of the conductive polymer composite material with a multilayer pore structure as claimed in claim 1, 2, 3, 4, 5 or 6 in the fields of conductive polymers, elastic strain sensing and gas sensing.
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| CN103627139B (en) * | 2013-09-25 | 2015-10-28 | 杭州师范大学 | A kind of preparation method of functional graphene oxide/epoxy resin nano composites |
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