CN102675883A - Surface modified graphene polymer-based piezoresistive composite material and preparation method thereof - Google Patents
Surface modified graphene polymer-based piezoresistive composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a surface modified graphene polymer-based piezoresistive composite material and a preparation method thereof. According to the polymer-based piezoresistive composite material, room-temperature vulcanized silicon rubber is used as a matrix, and surface modified graphene grafted and modified by octadecylamine is used as a conductive filler; in the reaction of grafting the octadecylamine to graphene, the mass ratio of the octadecylamine to graphene oxide is 1:1; and the graphene volume fractions of the surface modified graphene/ silicon rubber composite material are respectively 0.96 percent, 1.19 percent and 1.43 percent. The surface modified graphene/ silicon rubber piezoresistive composite material prepared by a solution blending method has the advantages of graphene dispersion uniformity, low percolation threshold value, high piezoresistive sensitivity, high piezoresistive repeatability, low preparation cost and the like.
Description
Technical field
The invention belongs to polymer-based carbon pressure drag field of compound material, being specifically related to a kind of is the pressure drag matrix material and preparation method thereof of conductive filler material with surface modified graphite alkene.
Background technology
Polymer-based carbon pressure drag matrix material has that snappiness is good, the piezoresistance sensitivity degree is big, and is big thereby low cost and other advantages overcomes the fragility of traditional metal and silicon semiconductor, not flexible, shortcomings such as cost height.Along with electron device develops to the flexibility direction, have flexible sensor material and obtained paying close attention to the equivalent material that the complete organic pressure drag matrix material of polymer-based carbon is a kind of ideal stress strain gauge widely.
For conventional polymer base pressure drag matrix material, subject matter is with the carbon black to be that the pressure drag matrix material of filler has low sensitivity, high filler loading capacity, the problem that repeatability is not good.And be though that the pressure drag matrix material of filler has higher piezoresistance sensitivity degree and lower loading level with the carbon nanotube, the pressure drag characteristic of this excellence is difficult in and obtains ideal in the loop test and repeat.And be mainly the interface combination degree between filler and the matrix for the textural factor that influences the pressure drag matrix material.When filling surface and polymeric matrix can produce stronger interface bonded, the extraneous stress that is applied to polymeric matrix can be delivered on the filler timely, thereby causes effective displacement of conductive filler material, and then causes the reconstruct of conductive network in the system.Therefore we carry out alkylation modification with the Graphene surface, thus expect its with Zylox between form and combine combination more closely, and then help the performance of matrix material pressure drag performance.
Graphene had caused physics as a novel two-dimensional nano material in recent years, chemistry, the many-sided research interest of biological field.Along with the graphite oxide legal system is equipped with the maturation of Graphene technology, be that the graphite oxide of raw material is able to the magnanimity preparation with cheap graphite.If in advance alkylation modification is carried out on the graphene oxide surface it can be dispersed in the non-polar solvent YLENE; Taking solution blended process that Zylox is carried out blend with it then, just be expected to prepare cheap conductive graphene/polymkeric substance pressure drag matrix material with low seepage flow threshold value.
Summary of the invention
The object of the present invention is to provide a kind of preparation simple to operate to possess the surface modified graphite alkene/Zylox pressure drag matrix material of excellent pressure drag repeatability.
Technical scheme of the present invention is: the polymer-based carbon pressure drag matrix material that a kind of surface modified graphite alkene is conductive filler material, this matrix material comprise that accounting for TV percentage mark is 0.96-1.43% conductive filler material, and all the other are polymeric matrix; Wherein, used polymeric matrix is the room temperature vulcanized silicone rubber of terminal hydroxy group;
The surface modified graphite alkene of said conductive filler material stearylamine graft modification.
Polymer-based carbon pressure drag matrix material that it is conductive filler material that another object of the present invention provides above-mentioned surface modified graphite alkene and preparation method thereof may further comprise the steps:
1) Graphene surface-treated:
Be dispersed in the water 1.1 take by weighing a certain amount of graphite oxide, and pH value be adjusted to 8, obtain the graphene oxide dispersion liquid that concentration is 2.5 mg/mL through supersound process with ammoniacal liquor, subsequent use;
1.2 the ethanolic soln that with concentration is the stearylamine of 5.0 mg/mL is mixing of 1:2 with the graphene oxide dispersion liquid according to volume ratio; And at 90 ℃ of following heating reflux reaction 20h; Then Hydrazine Hydrate 80 is added in the mixed solution, and continue to obtain surperficial alkylation modification Graphene at 90 ℃ of following reacting by heating 4h; Wherein, said Hydrazine Hydrate 80 add-on and graphite oxide ratio are 1mL:1g;
2) Composite Preparation: surperficial alkylation modification Graphene that step 1 is prepared and xylene solution are according to the mixed of 1mg:1ml; Carried out supersound process 2 hours; Obtaining concentration is the Graphene stable dispersions of 1 mg/mL; Again 2 g Zylox being dissolved in 10 mL xylene solvents, to be prepared into concentration be that 0.2 g/mL Zylox dispersion liquid joins said Graphene stable dispersions, mixes the back solvent flashing, obtains the exsiccant mixture;
3) self-vulcanizing moulding: 7 parts of tetraethoxys are added in the dried mixture that steps 1 obtain stir; Put it into mould then and at room temperature with 15 MPa pressure-cure 12 hours, being prepared into diameter after the moulding is that 11.2 mm thickness are 1.15 mm disk shapes surface alkylation modification graphene/silicon rubber composite sample.
With resulting disk shape surface alkylation modification graphene/silicon rubber composite sample, be under the 100V condition sample body pressure drag to be tested in TV through Keithley 6517B megger.Pressure drag loop test system is the laboratory self-control, and it mainly comprises the coupling of Tianjin, island drawing machine and Keithley 6517B, and with the data sync input computer of LabVIEW program with the two.
The present invention has following excellent effect:
1) surface modified graphite alkene technology is one kettle way, and its technological process is easy to operate, but the mass preparation modified graphene.Because the modification of surface grafting stearylamine can effectively reduce the Graphene surface energy; The modified graphene that obtains can be dispersed in the non-polar organic solvent YLENE by higher concentration on the one hand; Also improved the consistency of itself and Zylox on the other hand; Further help the homodisperse of Graphene in the Zylox matrix; Successfully solved traditional technology and can not Graphene be dispersed in the problem among the silastic polymer matrix, it is excellent to have prepared conductivity, pressure drag matrix material that the pressure drag characteristic is good.
2) have benefited from good fillers dispersed surface modified graphite alkene/silicon rubber composite material seepage flow threshold value and be merely 0.63 vol.%, be lower than same seepage flow threshold value 1.00 vol.% through the surface-modified carbon nanotubes matrix material.Lower seepage flow threshold value not only helps keeping the flexibility and the elasticity of Zylox, more helps setting up the conductive network of unstable overlap joint, thereby improves matrix material piezoresistance sensitivity degree.Simultaneously, also owing to the minimizing of required filler addition, the Composite Preparation cost also reduces greatly.
3) have benefited from advantage to two-dimentional Graphene surface-treated and Graphene self bigger serface, volume(tric)fraction is that the matrix material of 1.19 % has shown excellent pressure drag repeatability.In preceding four times working cycle, can observe some unsettled resistance change.But in 6 working cyclees subsequently, sample has shown very excellent pressure drag repeat property.Do not catch up with the variation of external force fully at same test condition lower surface modified carbon nano-tube/inner conductive network of silicon rubber composite material, excellent piezoresistance sensitivity characteristic is difficult to keep.
4) under the uniaxial compression, present exponential relationship between the resistance change of surface modified graphite alkene/silicon rubber composite material and the pressure.Homogenization resistance increases and the index increase with pressure.Matrix material homogenization resistance is if become good linear to concern in that logarithmic coordinate are next with pressure.
5) preparation method provided by the present invention, technology is simple, need not large-scale processing equipment, helps the graphene/silicon rubber pressure drag matrix material of low-cost mass preparation excellent performance.
Description of drawings
Fig. 1, surface modified graphite alkene transmission electron microscope photo.
The profile scanning electromicroscopic photograph of Fig. 2, surface modified graphite alkene/silicon rubber composite material.
Fig. 3, surface modified graphite alkene/silicon rubber composite material volume specific resistance are with the change curve of Graphene content.
The homogenization resistance changing trend diagram under pressure of the surface modified graphite alkene/silicon rubber composite material of Fig. 4, embodiment 1 and 2 preparations.
The changing trend diagram of homogenization resistance under the circulating pressure effect of the surface modified graphite alkene/silicon rubber composite material of Fig. 5, embodiment 2 preparations.
The changing trend diagram of homogenization resistance under the circulating pressure effect of the surface modified graphite alkene/silicon rubber composite material of Fig. 6, embodiment 3 preparations.
Embodiment
Below the present invention will be described in more detail through specific embodiment.Embodiment only is to a kind of explanation of the present invention, and is not construed as limiting the invention.Embodiment is the practical application example, is easy to grasp and checking for those skilled in the art.If on basis of the present invention, make certain change, its essence does not exceed scope of the present invention so.
Embodiment 1
1) all test raw material is before experiment all in 80 ℃ of vacuum drying ovens dry 24 hours, to remove moisture content wherein.The graphite oxide that will make through the Hummers method is dispersed in it in water with the concentration of 2.5 mg/mL, and with ammoniacal liquor pH value is adjusted to 8, and we can obtain finely dispersed brown graphene oxide dispersion liquid through supersound process.Next step is that the ethanolic soln of 5.0 mg/mL stearylamines adds in the dispersion liquid of 40 mL graphene oxides with previously prepd 20 mL concentration, and at 90 ℃ of following heating reflux reaction 20 h.Then 0.1 mL Hydrazine Hydrate 80 (Hydrazine Hydrate 80 add-on and graphite oxide ratio are 1 mL:1 g) is added in the mixed solution, and continue at 90 ℃ of following reacting by heating 4h.Reaction is cleaned with 60 ℃ of hot ethanols product through the moving phase strainer after finishing repeatedly.After the cleaning product that obtains is put into 70 ℃ vacuum drying oven and preserve and to obtain surperficial alkylation modification Graphene after 24 hours, its transmission electron microscope photo is as shown in Figure 1;
2) the surperficial alkylation modification Graphene that the first step the is obtained 40mg that weighs adds among the 40mL xylene solvent subsequently and carried out supersound process 2 hours, and can obtain stable Graphene concentration is the dispersion liquid of 1mg/mL.Next step with 2g Zylox be dissolved in 10 mL xylene solvents to prepare concentration be 0.2 g/mL Zylox dispersion liquid with at room temperature stir after surperficial alkylation modification Graphene dispersion liquid mixes 30 minutes with at room temperature stirred 30 minutes after surperficial alkylation modification Graphene dispersion liquid mixes; Subsequently mixed solution is transferred on the hot platform and carried out the magnetic agitation solvent flashing, and products therefrom is further carried out drying putting into 80 ℃ of vacuum drying ovens with 80 ℃.
3) in step 2) to obtain the Graphene volume(tric)fraction be to add 7 parts of tetraethoxys in the 0.96 % matrix material and stir, and puts it into mould then and at room temperature with 15 MPa pressure-cure 12 hours.Being prepared into diameter after the moulding is that 11.2 mm thickness are 1.15 mm disk shape samples, with to be tested.The section surface sweeping electromicroscopic photograph of matrix material is as shown in Figure 2;
4) with step 2) obtain the Graphene volume(tric)fraction be 0.96 % composite sample to add diameter be 70 mm, be cured in the thickness 1 mm circular die.The big circular slice sample of preparing is put into 8009 anchor clamps boxes, in Keithely 6517B megger, is under the 100 V conditions sample volume resistivity to be tested with TV.Direct current volume specific resistance under its room temperature is as shown in Figure 3.
5) the small dia wafer sample surface that step 3) is obtained is carried out metal spraying and is handled; Under the test speed of the sample that obtains with 0.3 mm/min; In between 0.1 MPa-0.9 MPa pressure zone it is carried out the test of single pressure drag, TV is 100 V, and test curve is as shown in Figure 4.
Embodiment 2
1) surperficial alkylation modification Graphene technology is with instance 1;
2) the surperficial alkylation modification Graphene that the first step is obtained 50 mg that weigh add among the 50 mL xylene solvents subsequently and carried out supersound process 2 hours, and can obtain stable Graphene concentration is the dispersion liquid of 1 mg/mL.Next step is dissolved in 2g Zylox 10 mL xylene solvents to prepare concentration is 0.2 g/mL Zylox dispersion liquid and at room temperature stirred 30 minutes after surperficial alkylation modification Graphene dispersion liquid mixes; Subsequently mixed solution is transferred on the hot platform and carried out the magnetic agitation solvent flashing, and products therefrom is further carried out drying putting into 80 ℃ of vacuum drying ovens with 80 ℃.
3) in step 2) to obtain the Graphene volume(tric)fraction be to add the solidifying agent tetraethoxy in the 1.19 % matrix materials and stir, and puts it into mould then and at room temperature with 15 MPa pressure-cure 12 hours.Being prepared into diameter after the moulding is that 11.2 mm thickness are 1.15 mm disk shape samples, with to be tested.
4) with step 2) obtain the Graphene volume(tric)fraction be 1.19 % matrix materials to add diameter be 70 mm, be cured in the thickness 1 mm circular die.The big circular slice sample of preparing is put into 8009 anchor clamps boxes, in Keithely 6517B megger, is under the 100 V conditions sample volume resistivity to be tested with TV.Direct current volume specific resistance under its room temperature is as shown in Figure 3.
5) the small dia wafer sample surface that step 3) is obtained is carried out metal spraying and is handled; Under the test speed of the sample that obtains with 0.3 mm/min; In between 0.1 MPa-0.9 MPa pressure zone it is carried out the test of single pressure drag, TV is 100 V, and test curve is as shown in Figure 4.
6) the small dia wafer sample surface that step 3) is obtained is carried out metal spraying and is handled; Under the test speed of the sample that obtains with 0.3 mm/min; Between 0.1 MPa-1 MPa pressure zone, carry out the pressure drag loop test in 10 cycles, TV is 100 V, and test curve is as shown in Figure 5.
Embodiment 3
1) surperficial alkylation modification Graphene technology is with instance 1;
2) the surperficial alkylation modification Graphene that the first step is obtained 60 mg that weigh add among the 60 mL xylene solvents subsequently and carried out supersound process 2 hours, and can obtain stable Graphene concentration is the dispersion liquid of 1 mg/mL.Next step is dissolved in 2g Zylox 10 mL xylene solvents to prepare concentration is 0.2 g/mL Zylox dispersion liquid and at room temperature stirred 30 minutes after surperficial alkylation modification Graphene dispersion liquid mixes; Subsequently mixed solution is transferred on the hot platform and carried out the magnetic agitation solvent flashing, and products therefrom is further carried out drying putting into 80 ℃ of vacuum drying ovens with 80 ℃.
3) in step 2) the Graphene volume(tric)fraction is to add 7 parts of tetraethoxys in the 1.43 % matrix materials and stir, and puts it into mould then and at room temperature with 15 MPa pressure-cure 12 hours.Being prepared into diameter after the moulding is that 11.2 mm thickness are 1.15 mm disk shape samples, with to be tested.The section surface sweeping electromicroscopic photograph of matrix material is as shown in Figure 2;
4) with step 2) obtain the Graphene volume(tric)fraction be 1.43 % matrix materials to add diameter be 70 mm, be cured in the thickness 1 mm circular die.The big circular slice sample of preparing is put into 8009 anchor clamps boxes, in Keithely 6517B megger, is under the 100 V conditions sample volume resistivity to be tested with TV.Direct current volume specific resistance under its room temperature is as shown in Figure 3.
5) the small dia wafer sample surface that step 3) is obtained is carried out metal spraying and is handled; Under the test speed of the sample that obtains with 0.3 mm/min; Between 0.1 MPa-1 MPa pressure zone, carry out the pressure drag loop test in 10 cycles, TV is 100 V, and test curve is as shown in Figure 6.
Think that the surface modified graphite alkene that the present invention obtains/Zylox pressure drag matrix material has Graphene and is uniformly dispersed, hangs down advantages such as seepage flow threshold value, piezoresistance sensitivity degree height and pressure drag good reproducibility.
Claims (2)
1. a surface modified graphite alkene polymer base pressure drag matrix material is characterized in that, this matrix material comprises that accounting for TV percentage mark is 0.96-1.43% conductive filler material, and all the other are polymeric matrix; Wherein, used polymeric matrix is the room temperature vulcanized silicone rubber of terminal hydroxy group; The surface modified graphite alkene of said conductive filler material stearylamine graft modification.
2. the preparation method of a kind of surface modified graphite alkene polymer base pressure drag matrix material according to claim 1 is characterized in that, may further comprise the steps:
The Graphene surface-treated:
Be dispersed in the water 1.1 take by weighing a certain amount of graphite oxide, and pH value be adjusted to 8, obtain the graphene oxide dispersion liquid that concentration is 2.5 mg/mL through supersound process with ammoniacal liquor, subsequent use;
1.2 the ethanolic soln that with concentration is the stearylamine of 5.0 mg/mL is mixing of 1:2 with the graphene oxide dispersion liquid according to volume ratio; And at 90 ℃ of following heating reflux reaction 20h; Then Hydrazine Hydrate 80 is added in the mixed solution, and continue to obtain surperficial alkylation modification Graphene at 90 ℃ of following reacting by heating 4h; Wherein, said Hydrazine Hydrate 80 add-on and graphite oxide ratio are 1mL:1g;
2) Composite Preparation: surperficial alkylation modification Graphene that step 1 is prepared and xylene solution are according to the mixed of 1mg:1ml; Carried out supersound process 2 hours; Obtaining concentration is the Graphene stable dispersions of 1 mg/mL; Again 2 g Zylox being dissolved in 10 mL xylene solvents, to prepare concentration be that 0.2 g/mL Zylox dispersion liquid joins said Graphene stable dispersions, mixes the back solvent flashing, obtains mixture after the drying;
3) self-vulcanizing moulding: 7 parts of tetraethoxys are added in the dried mixture that steps 2 prepare stir; Put it into mould then and at room temperature with 15 MPa pressure-cure 12 hours, being prepared into diameter after the moulding is that 11.2 mm thickness are 1.15 mm disk shapes surface alkylation modification graphene/silicon rubber composite sample.
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Cited By (13)
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| CN103073930A (en) * | 2013-01-30 | 2013-05-01 | 同济大学 | Preparation method and application of alkylated functional graphene |
| CN103756324A (en) * | 2014-01-06 | 2014-04-30 | 金坛市德博密封技术有限公司 | Graphene conductive silicon rubber plate and preparation method thereof |
| CN104616826A (en) * | 2014-12-30 | 2015-05-13 | 浙江大学 | Graphene-PDMS (Polydimethylsiloxane) flexible electrode and preparation method and application thereof |
| CN106328256A (en) * | 2016-10-28 | 2017-01-11 | 济宁利特纳米技术有限责任公司 | Conductive slurry for lithium ion battery and preparation method of conductive slurry |
| CN106479166A (en) * | 2016-10-21 | 2017-03-08 | 安徽江淮汽车集团股份有限公司 | Low VOC polyamide 6 composite material of a kind of antistatic and preparation method thereof |
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| CN109593362A (en) * | 2018-10-12 | 2019-04-09 | 安徽理工大学 | A kind of layer graphene/organic silicon rubber composite material and preparation method less flexible |
| CN109990695A (en) * | 2019-04-28 | 2019-07-09 | 中南大学 | A kind of soft graphite alkenyl piezoresistance sensor and preparation method thereof |
| CN110207585A (en) * | 2019-05-08 | 2019-09-06 | 沈阳航空航天大学 | A kind of graphene flexible sensor and preparation method thereof |
| CN113121893A (en) * | 2021-04-20 | 2021-07-16 | 慕思健康睡眠股份有限公司 | Antistatic graphene latex slurry and process and application thereof |
| CN114220619A (en) * | 2021-12-06 | 2022-03-22 | 厦门大学 | Flexible piezoresistive composite material and preparation method thereof |
| CN114262520A (en) * | 2022-01-20 | 2022-04-01 | 青岛科技大学 | Preparation method of flexible stretchable silicone rubber-based strain sensor based on emulsion blending |
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| CN103073930A (en) * | 2013-01-30 | 2013-05-01 | 同济大学 | Preparation method and application of alkylated functional graphene |
| CN103756324A (en) * | 2014-01-06 | 2014-04-30 | 金坛市德博密封技术有限公司 | Graphene conductive silicon rubber plate and preparation method thereof |
| CN104616826A (en) * | 2014-12-30 | 2015-05-13 | 浙江大学 | Graphene-PDMS (Polydimethylsiloxane) flexible electrode and preparation method and application thereof |
| CN106479166B (en) * | 2016-10-21 | 2019-04-16 | 安徽江淮汽车集团股份有限公司 | Antistatic low VOC polyamide 6 composite material of one kind and preparation method thereof |
| CN106479166A (en) * | 2016-10-21 | 2017-03-08 | 安徽江淮汽车集团股份有限公司 | Low VOC polyamide 6 composite material of a kind of antistatic and preparation method thereof |
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| CN108624054B (en) * | 2018-04-02 | 2020-09-18 | 浙江大学 | Transparent conductive compound regulated and controlled by magnetic field and preparation method thereof |
| CN108624054A (en) * | 2018-04-02 | 2018-10-09 | 浙江大学 | A kind of electrically conducting transparent compound and preparation method thereof of magnetic field regulation and control |
| CN109593362A (en) * | 2018-10-12 | 2019-04-09 | 安徽理工大学 | A kind of layer graphene/organic silicon rubber composite material and preparation method less flexible |
| CN109354877A (en) * | 2018-10-29 | 2019-02-19 | 西南大学 | A kind of flexible strain-responsive material and preparation method thereof mismatching region with modulus |
| CN109990695A (en) * | 2019-04-28 | 2019-07-09 | 中南大学 | A kind of soft graphite alkenyl piezoresistance sensor and preparation method thereof |
| CN109990695B (en) * | 2019-04-28 | 2020-05-08 | 中南大学 | Flexible graphene-based piezoresistive sensor and preparation method thereof |
| CN110207585A (en) * | 2019-05-08 | 2019-09-06 | 沈阳航空航天大学 | A kind of graphene flexible sensor and preparation method thereof |
| CN113121893A (en) * | 2021-04-20 | 2021-07-16 | 慕思健康睡眠股份有限公司 | Antistatic graphene latex slurry and process and application thereof |
| CN114220619A (en) * | 2021-12-06 | 2022-03-22 | 厦门大学 | Flexible piezoresistive composite material and preparation method thereof |
| CN114220619B (en) * | 2021-12-06 | 2023-11-10 | 厦门大学 | Flexible piezoresistive composite material and preparation method thereof |
| CN114262520A (en) * | 2022-01-20 | 2022-04-01 | 青岛科技大学 | Preparation method of flexible stretchable silicone rubber-based strain sensor based on emulsion blending |
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Application publication date: 20120919 |