CN101412852A - Preparation of precise resistance/strain sensitive conductive silicon rubber - Google Patents
Preparation of precise resistance/strain sensitive conductive silicon rubber Download PDFInfo
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- CN101412852A CN101412852A CNA2008102361920A CN200810236192A CN101412852A CN 101412852 A CN101412852 A CN 101412852A CN A2008102361920 A CNA2008102361920 A CN A2008102361920A CN 200810236192 A CN200810236192 A CN 200810236192A CN 101412852 A CN101412852 A CN 101412852A
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Abstract
The invention discloses a method for preparing a strain sensitivity-conductivity silicone rubber for a precise resistor and relates to a conductivity-strain sensitivity rubber material with low modulus and high repeatability. The preparation method comprises the following steps: the surface of a high-conductivity nanometer ruthenium oxide powder body is subjected to hydrophilization treatment; the surface of the nanometer ruthenium oxide powder body is modified through a silane coupling agent of which a terminal group is an ethylene group to form the conductive ruthenium oxide powder body containing the ethylene group on the surface; the conductive ruthenium oxide powder body is mixed with silicone rubber; the volume percentage of the ruthenium oxide powder body accounts for 17 to 30 percent of the total volume of the mixture; the mixture is added with a vulcanizing agent and a strengthening agent, is mixed, is kept stand for 30 minutes, is put to a mould, is pressurized to a pressure of between 10 and 15 Mpa, is kept at a temperature of between 172 and 178 DEG C for 15 to 30 minutes to obtain the vulcanized silicone rubber composite material; and the conductivity of the vulcanized silicone rubber composite material has the characteristic of repeated change along strain.
Description
Technical field
The present invention relates to a kind of low modulus, high duplication elastomeric material of electroconductibility strain sensitive, belong to field of functional polymer composites, is a kind of sophisticated sensor material.
Background technology
The various contact stress sensing elements that use are mostly by measuring certain material change in physical under the strained condition that stress produces at present, obtain the stress of analyte under the identical stress condition, as resistance-strain type, optical fiber type etc., because the springform quantitative limitation of sensing material itself, when measuring the strain of low-modulus material, the strain of sensing material is lower than the strain of analyte, not only can not obtain the strain of measured material, also cause to the interference of transmitter contact area strain field.Based on low modulus strain sensing material strain transmitter, can be used for contact process measures various with the approaching material strain of sensing elasticity modulus of materials, as plastics, rubber etc., can overcome the difficulty of the inapplicable occasion of a large amount of non-contact type strain measurements, the error in the time of also can solving based on the strain of high-modulus strain sensing Materials Measurement low-modulus material.
Conductive particle is compound with macromolecular material, when the conductive particle volume fraction surpasses the seepage flow threshold value, mixture becomes conductor, and the body resistance of discovering matrix material changes with material strain, research is also found, the resistance-strain characteristic of mixture is influenced by the kind of conductive phase and constitutional features, both at home and abroad at present carbon blacks that adopt more, graphite, particles such as metal are as conductive phase, in suitable conductive phase volume fraction scope, when material is subjected to strain, lead with strain at the electricity of the material of should changing direction and to change, utilize this electricity to lead, can lead and obtain material strain by measuring electricity with the strained relation.Because body material is a macromolecular material, the Young's modulus of matrix material is far below metal, and the strain-gauging scope can reach from 10
-2To 10
2, much larger than metal strain transmitter (10
-7To 10
-3).
About the technology of preparing and the performance of conductive elastomer strain sensing material, some Europe, the U.S., Japanese Patent technology and paper report are arranged at present, as EP1901311-A1, US2008067477-A1, JP2008069313-A; WO2004102144-A2, EP1623198-A2, US2006147700-A1, JP2006528366-W; JP49116595-A, JP78026676-B, these methods adopt carbon black or graphite as conductive phase, because its very big surface adsorption power and good unreactiveness, carbon black or graphite form conductive path in rubber under very low volume fraction, this low volume fraction conductive phase and rubber matrix are compound, has the bigger advantage of resistance-strain coefficient, but because conductive phase position rheology in matrix with strain, low volume fraction makes conductive channel few, body resistance is to the microstructure sensitivity, therefore most of electricity lead the elastomeric electricity of strain lead/the strain variation relation presents deviation with the increase of strain cycle index, this deviation has largely influenced material in applications that precision is had certain requirements.U.S. Nanosonic company utilizes electrostatic adhesion (United States Patent (USP) 6,447,887), metal nanoparticle is deposited on the polyelectrolyte membrane surface by the layer assembly method, form laminated film, obtain having the strain sensing elastomerics of certain resistance/strain repeatability, because the Young's modulus higher (10MPa) of polyelectrolyte still needs to design low modulus strain sensitive elastomerics.Domestic also have a multinomial relevant patent, conductive phase has carbon black (or graphite), conductive polymers and metal nickel powder, substantially can not reach repeatedly strain circulation down electricity lead/repeatability of strain stress relation, the present invention will provide a kind of new method for preparing the responsive elastomer material of conductive strain, lead/strain stress relation to reach the following certain repeated electricity of repeatedly strain circulation.
Summary of the invention
Technical problem: the preparation method who the purpose of this invention is to provide a kind of precise resistance/strain sensitive conductive silicon rubber, conductive rubber with this method preparation has the good mechanical performance, and its resistance reduces with compressive strain, increase with tension strain, resistance/strain stress relation has repetition stability, for low-modulus material strain-gauging, biomechanics detection, touch sensor etc. provide the high-performance sensing material.
Technical scheme: the preparation method of precise resistance/strain sensitive conductive silicon rubber of the present invention is:
Earlier high electrical-conductive nanometer ruthenium oxide powder surface is carried out hydrophilicity-imparting treatment, the silane coupling agent that is vinyl with nano oxidized ruthenium powder surface end group is modified again, forms the electric conductive oxidation ruthenium nano-powder that the surface contains vinyl, mixes with silicon rubber then; The volume percent of ruthenium oxide powder accounts for 17%～30% of this mixture cumulative volume, in this mixture, add vulcanizing agent, strengthening agent again, left standstill after the mixing 30 minutes, insert mould, pressurization 10～15Mpa, between 172～178 ℃, be incubated 15～30 minutes, obtain having electroconductibility has the repetition variation characteristic with strain sulphurated siliastic matrix material.
Described silicon rubber is the polydimethyl vinylsiloxane, and its contents of ethylene is between 0.3%～1%; The particle size of described ruthenium oxide powder is less than 20 nanometers.
Forming the surperficial method that contains the electric conductive oxidation ruthenium nano-powder of vinyl is:
Concentration by 1 grams per liter is dissolved in the hydration ruthenium chloride in the propylene glycol, be heated to 60 ℃, after the dissolving fully, being heated to 150 ℃ kept 30 minutes, left standstill 48 hours, precipitate and separate propylene glycol supernatant solution, precipitate with washing with alcohol, obtain the individual particle mean sizes in 2 nanometers, the coacervate mean sizes is at the metal Ru powder of 200 nanometers, above-mentioned powder is heated to 600 ℃ in air, be incubated 0.5 hour, obtain the rutile phase oxidation ruthenium powder of abundant oxidation, powder is rolled dispersion, obtaining single ruthenium oxide particle mean size is 20 nanometers, the coacervate mean sizes is the ruthenium oxide of 80 nanometers, this ruthenium oxide powder with the ammoniacal liquor of 1:5 dilution ultra-sonic dispersion at room temperature, was left standstill centrifugation 20 minutes, repeat to use methanol extraction then, clean, dried above-mentioned powder with 1:1 ethanol ultrapure water solution ultra-sonic dispersion, is added the silane coupling agent that 5% end group is a vinyl, precipitate after 3 hours, remove supernatant liquor, use the washing with alcohol several times, drying obtains the electric conductive oxidation ruthenium nano-powder that the surface contains vinyl.
Described silicon rubber is a kind of nano-scale gas-phase silica that adds the different volumes ratio, the mixing silicon rubber of white carbon black, the highest 30% of the ruthenium oxide volume fraction that is no more than of the volume fraction of white carbon black, white carbon black wherein, the white carbon black surface adopts silane coupling agent to modify.
The method that described white carbon black surface adopts silane coupling agent to modify is: the ammoniacal liquor ultra-sonic dispersion of white carbon black being inserted the 1:5 dilution, 80 ℃ keep 30 minutes after, left standstill 20 minutes in room temperature, remove supernatant liquor then, repeat three times, with dried above-mentioned powder 1:1 ethanol ultrapure water solution ultra-sonic dispersion, add the silane coupling agent that 5% end group is a vinyl, precipitate after 3 hours, remove supernatant liquor, use the washing with alcohol several times, drying obtains the white carbon black that the surface contains vinyl.
Described silane coupling agent is any of vinyltriethoxysilane, vinyltrimethoxy silane or vinyl three tert.-butoxy silane.
Beneficial effect: the invention provides the method for preparing the precise resistance/strain sensitive elastomer material; the rubber matrix conductive elastomer that obtains in this way; has good electrical conductivity and ductility; electroconductibility can be adjusted within the specific limits; repeatedly repeat under the deformation resistance-strain relation and have good reproducibility, prepare simple, with low cost, suitable scale preparation.In the certain size scope, have scale invariance, be fit to the integrated strain sensing of small size, also can prepare complex construction according to the application scenario.
Conductive rubber of the present invention has good environment compatibility, because electrical conductor is an oxide conductor, all keeps stable electroconductibility and resistance-strain repeatability at high humidity, weak acid, weak base environment mesocomplex.The present invention uses the nano-oxide conducting body, and most of particle size is lower than 20 nanometers, and cluster of grains aggressiveness size is less than 200 nanometers, and most of nano particle is uniformly dispersed in rubber matrix.
Nano-oxide is obvious to the rubber matrix reinforcing effect, a small amount of other isolator nanometer strengthening agents of interpolation do not influence the electroconductibility and the resistance-strain repeatability of complex body, the Young's modulus of complex body and viscoelasticity property can be regulated by regulating strengthening agent content and degree of crosslinking, oxide surface and silane coupling agent form covalent attachment, active group covalent attachment on silane coupling agent end group and the rubber raw rubber molecular chain is stable under the complicated chemical environment when carrying out various modification on basis of the present invention.
Utilize precise resistance/strain sensitive rubber to make strain transducer, can overcome the difficulty that is not suitable for non-cpntact measurement under a large amount of on-line monitoring conditions, also can overcome little, the big Young's modulus of rigidity strain transducer (metal, optical fiber etc.) useful range difficulties such as analyte strained constraints; Utilize this material simultaneously, can prepare plane or arbitrary surface piezoresistance sensitivity array, for fields such as ergonomics, robot provide biomechanics transmitter, touch sensor.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the nano oxidized ruthenium of finishing.
Fig. 2 is an x-ray diffraction pattern.
Fig. 3 is for modifying nano oxidized ruthenium (a) behind the silane coupling agent, the infrared absorption spectrum of silicon rubber after not adding the nanometer ruthenium oxide and adding the sulfuration of nano oxidized ruthenium.
Fig. 4 leads-pressure curve for 12 repetition electricity of typical composition compounded rubber.
Embodiment
The preparation method of precise resistance/strain sensitive conductive silicon rubber of the present invention is:
Use nano-scale rutile phase oxidation ruthenium as conductive phase, nano oxidized ruthenium prepares with solvent-thermal method, earlier the concentration of hydration ruthenium chloride with 1 grams per liter is dissolved in the propylene glycol solvent under 60 ℃, being heated to 150 ℃ kept 30 minutes, the hydration ruthenium chloride decomposes, obtain metal Ru, precipitate and separate propylene glycol supernatant solution precipitates with washing with alcohol, after the repeated washing drying, obtain the individual particle mean sizes in 2 nanometers, the coacervate mean sizes heats metal Ru at the metal Ru powder of 200 nanometers again in air, obtain the rutile structure ruthenium oxide, control Heating temperature and time, the metal Ru complete oxidation, particle still keeps nano-scale simultaneously.
With this ruthenium oxide powder with the ammoniacal liquor of 1:5 dilution ultra-sonic dispersion at room temperature, left standstill 20 minutes, centrifugation repeats to use methanol extraction then, cleans, with dried above-mentioned powder 1:1 ethanol ultrapure water solution ultra-sonic dispersion, add the silane coupling agent that 5% end group is a vinyl, precipitate after 3 hours, remove supernatant liquor, use the washing with alcohol several times, drying obtains the electric conductive oxidation ruthenium nano-powder that the surface contains vinyl.Silane coupling agent is any of vinyltriethoxysilane, vinyltrimethoxy silane or vinyl three tert.-butoxy silane.
The ruthenium oxide powder that annealing obtained in 30 minutes in air, particle size are less than 20 nanometers, and after the silane coupling agent processing, the coacervate size is less than 80 nanometers.The body resistance of composite silicone rubber reduces with the volume fraction increase of the ruthenium oxide that adds, in suitable scope, resistance presents monotone variation with the strained increase, and repeatedly strain circulation, resistance repeats to change, the volume ratio of ruthenium oxide is adjusted between 17% to 25%, can in silicon rubber, add the Nano carbon white reinforcement according to the mechanical property needs, the average particle size particle size of white carbon black is less than 20 nanometers, the volume ratio maximum of white carbon black can be 30% of ruthenium oxide, white carbon black adopts with the similar method of ruthenium oxide and modifies silane coupling agent, be about to white carbon black and behind the ultra-sonic dispersion, kept 30 minutes down at 80 ℃ in the ammoniacal liquor of 1:5 dilution, post precipitation washs 3 times with ultrapure water, insert 1:1 ethanol ultrapure water solution ultra-sonic dispersion again, add the silane coupling agent that 5% end group is a vinyl, precipitate after 3 hours, remove supernatant liquor, use the washing with alcohol several times, drying obtains the white carbon black that the surface contains vinyl.Used silane coupling agent is identical with above-mentioned modified oxidized ruthenium nano-particle.
Raw-silastic continuously is the polydimethyl vinylsiloxane, the ruthenium oxide powder of finishing is mixed with raw-silastic continuously, after rolling repeatedly, add solidifying agent, solidifying agent adopts 2,5-dimethyl-2, the 5-di-t-butyl hexane peroxide, between 172 to 178 ℃, pressure solidified between 10 to 15Mpa 15 to 30 minutes, obtained having the elastomer material that certain strain/electricity is led repeatability.Used dimethyl vinyl polysiloxane, molecular weight ranges is 500 to 750kDa, and it contains vinyl between 0.3% to 1% mol ratio, regulates the contents of ethylene of base rubber by the green stock that mixes differing ethylene base mol ratio.
Embodiment 1:
3 gram hydration ruthenium chlorides are dissolved in 3 liters of analytical pure 1, in the 2-propylene glycol, be heated to 60 ℃, after the high degree of agitation dissolving fully, slowly be heated to 150 ℃, kept 30 minutes, solution changes black into by reddish-brown, cools to room temperature naturally, leaves standstill 24 hours, the nano particle major part that forms in the solution is deposited to container bottom, remove most of propylene glycol solution, add and the isopyknic analytical pure ethanol of residue propylene glycol, leave standstill 3 hours behind the ultra-sonic dispersion after, remove supernatant solution, add 100 milliliters of ethanol again, repeated washing three times, drying, obtain the individual particle mean sizes in 2 nanometers, the coacervate mean sizes is at the metal Ru powder of 200 nanometers.Above-mentioned powder is heated to 600 ℃ in air, is incubated 0.5 hour, obtain the rutile phase oxidation ruthenium powder of abundant oxidation, powder is rolled dispersion, obtaining single ruthenium oxide particle mean size is 20 nanometers, and the coacervate mean sizes is the ruthenium oxide of 80 nanometers.
Embodiment 2:
With above-mentioned ruthenium oxide powder ultra-sonic dispersion in 1:5 volume ratio ultrapure water and ammoniacal liquor, kept 20 minutes, centrifugation under the 15000g, remove supernatant solution, sedimentary powder is disperseed precipitation, repeated washing three times with methyl alcohol, obtain hydrophilic surface after the drying and be rich in the nano oxidized ruthenium powder of hydroxyl, its infrared absorption spectrum as shown in Figure 3, Figure 4.
The above-mentioned powder of 0.3 gram is dispersed in 10 ml volumes than in the 1:1 ethanol ultrapure water solution, add 0.5 milliliter of triethoxy vinyl silanes again, ultrasonic 3 minutes, left standstill 3 hours, remove supernatant liquor, clean sedimentation with ethanol, wash three times, dry, obtain the ruthenium oxide powder of finishing vinyl, its infrared absorption spectrum as shown in Figure 2, the transmission electron microscope image of ruthenium oxide powder and x-ray diffraction pattern as shown in Figure 1, the body resistance that records surface finish nano ruthenium oxide briquetting with four probe method is 4.3 * 10
-4Ω cm.
Embodiment 3:
Getting 200 milligrams of vinyl mol ratios is 1%, molecular weight is the methylvinyl-polysiloxane green stock of 500kDa, add 472 milligrams of above-mentioned finishing ruthenium oxide powders, add 6 milligrams of finishing gas-phase silicas that particle size is 20 nanometers, add 3 ml n-hexanes, after treating the silica gel dissolving, grind, ultra-sonic dispersion, drying is 2 hours under 60 ℃, adds 13 milligram 2 again, 5-dimethyl-2, the 5-di-t-butyl hexane peroxide after the ground and mixed, left standstill 30 minutes repeatedly, insert mould, die pressure is not less than 10Mpa, is incubated 20 minutes down at 175 ℃, cooling, the demoulding, obtain the conductive phase volume ratio and be 25% conductive silicon rubber material, this material resistance-pressure under continuous 12 repeated compression deformation concerns as shown in Figure 4.
Claims (6)
1, a kind of preparation method of precise resistance/strain sensitive conductive silicon rubber, it is characterized in that this preparation method is: earlier high electrical-conductive nanometer ruthenium oxide powder surface is carried out hydrophilicity-imparting treatment, the silane coupling agent that is vinyl with nano oxidized ruthenium powder surface end group is modified again, form the electric conductive oxidation ruthenium nano-powder that the surface contains vinyl, mix with silicon rubber then; The volume percent of ruthenium oxide powder accounts for 17%～30% of this mixture cumulative volume, in this mixture, add vulcanizing agent, strengthening agent again, left standstill after the mixing 30 minutes, insert mould, pressurization 10～15Mpa, between 172～178 ℃, be incubated 15～30 minutes, obtain having electroconductibility has the repetition variation characteristic with strain sulphurated siliastic matrix material.
2, the preparation method of precise resistance/strain sensitive conductive silicon rubber according to claim 1 is characterized in that described silicon rubber is the polydimethyl vinylsiloxane, and its contents of ethylene is between 0.3%～1%; The particle size of described ruthenium oxide powder is less than 20 nanometers.
3, the preparation method of precise resistance/strain sensitive conductive silicon rubber as claimed in claim 1 is characterized in that forming the method that the surface contains the electric conductive oxidation ruthenium nano-powder of vinyl and is:
Concentration by 1 grams per liter is dissolved in the hydration ruthenium chloride in the propylene glycol, be heated to 60 ℃, after the dissolving fully, being heated to 150 ℃ kept 30 minutes, left standstill 48 hours, precipitate and separate propylene glycol supernatant solution, precipitate with washing with alcohol, obtain the individual particle mean sizes in 2 nanometers, the coacervate mean sizes is at the metal Ru powder of 200 nanometers, above-mentioned powder is heated to 600 ℃ in air, be incubated 0.5 hour, obtain the rutile phase oxidation ruthenium powder of abundant oxidation, powder is rolled dispersion, obtaining single ruthenium oxide particle mean size is 20 nanometers, the coacervate mean sizes is the ruthenium oxide of 80 nanometers, this ruthenium oxide powder with the ammoniacal liquor of 1:5 dilution ultra-sonic dispersion at room temperature, was left standstill centrifugation 20 minutes, repeat to use methanol extraction then, clean, dried above-mentioned powder with 1:1 ethanol ultrapure water solution ultra-sonic dispersion, is added the silane coupling agent that 5% end group is a vinyl, precipitate after 3 hours, remove supernatant liquor, use the washing with alcohol several times, drying obtains the electric conductive oxidation ruthenium nano-powder that the surface contains vinyl.
4, the preparation method of precise resistance/strain sensitive conductive silicon rubber as claimed in claim 1 or 2, it is characterized in that described silicon rubber is a kind of nano-scale gas-phase silica that adds the different volumes ratio, the mixing silicon rubber of white carbon black, the highest 30% of the ruthenium oxide volume fraction that is no more than of the volume fraction of white carbon black, white carbon black wherein, the white carbon black surface adopts silane coupling agent to modify.
5, the preparation method of precise resistance/strain sensitive conductive silicon rubber as claimed in claim 4, it is characterized in that the method that described white carbon black surface adopts silane coupling agent to modify is: white carbon black is inserted the ammoniacal liquor of 1:5 dilution at 80 ℃ of following ultra-sonic dispersion, keep after 30 minutes, at room temperature left standstill 30 minutes, remove supernatant liquor, clean with ultrapure water, staticly settle, repeat three times, dried above-mentioned powder with 1:1 ethanol ultrapure water solution ultra-sonic dispersion, is added the silane coupling agent that 5% end group is a vinyl, precipitate after 3 hours, remove supernatant liquor, use the washing with alcohol several times, drying obtains the white carbon black that the surface contains vinyl.
6,, it is characterized in that described silane coupling agent is any of vinyltriethoxysilane, vinyltrimethoxy silane or vinyl three tert.-butoxy silane as the preparation method of claim 3 or 5 described precise resistance/strain sensitive conductive silicon rubbers.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153987A (en) * | 2011-05-18 | 2011-08-17 | 杨福河 | High-performance single-component high-temperature vulcanized conductive glue and preparation method thereof |
| CN105086419A (en) * | 2015-08-11 | 2015-11-25 | 东华大学 | Fluorine-contained polyimide modified engineering plastic alloy capable of being electroplated and preparation method thereof |
| CN105585850A (en) * | 2015-12-22 | 2016-05-18 | 杭州师范大学 | Ag quantum dot composited anti-static organic silicon rubber as well as preparation method and application thereof |
| CN106848104A (en) * | 2017-04-14 | 2017-06-13 | 京东方科技集团股份有限公司 | Top emission type luminescent device |
-
2008
- 2008-11-26 CN CNA2008102361920A patent/CN101412852A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153987A (en) * | 2011-05-18 | 2011-08-17 | 杨福河 | High-performance single-component high-temperature vulcanized conductive glue and preparation method thereof |
| CN105086419A (en) * | 2015-08-11 | 2015-11-25 | 东华大学 | Fluorine-contained polyimide modified engineering plastic alloy capable of being electroplated and preparation method thereof |
| CN105086419B (en) * | 2015-08-11 | 2017-08-01 | 东华大学 | A kind of electrodepositable fluorinated polyimide modified engineered plastic alloy and preparation method thereof |
| CN105585850A (en) * | 2015-12-22 | 2016-05-18 | 杭州师范大学 | Ag quantum dot composited anti-static organic silicon rubber as well as preparation method and application thereof |
| CN105585850B (en) * | 2015-12-22 | 2019-03-05 | 杭州师范大学 | A kind of antistatic organic silicon rubber and the preparation method and application thereof that Ag quantum dot is compound |
| CN106848104A (en) * | 2017-04-14 | 2017-06-13 | 京东方科技集团股份有限公司 | Top emission type luminescent device |
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Open date: 20090422 |