CN106497064A - A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material and preparation method and application - Google Patents
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material and preparation method and application Download PDFInfo
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- CN106497064A CN106497064A CN201610937317.7A CN201610937317A CN106497064A CN 106497064 A CN106497064 A CN 106497064A CN 201610937317 A CN201610937317 A CN 201610937317A CN 106497064 A CN106497064 A CN 106497064A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G5/00—Capacitors in which the capacitance is varied by mechanical means, e.g. by turning a shaft; Processes of their manufacture
- H01G5/01—Details
- H01G5/013—Dielectrics
- H01G5/0134—Solid dielectrics
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2439/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
- C08J2439/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
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Abstract
The invention discloses a kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：36 parts of 25 35 parts of dimethyl silicone polymer, 1 10 parts of inorganic filler, 1 10 parts of modifying agent and curing agent.Its preparation method is comprised the following steps：（1）Inorganic filler is mixed with modifying agent and organic solvent, dispersion liquid I is obtained；（2）Dimethyl silicone polymer is added in dispersion liquid I, is mixed, is made dispersion liquid II；（3）Curing agent is added and is stirred evenly in dispersion liquid II, made dispersion liquid III, wet film is made into by filming technology then, then 1 2h, 1 3h of last 120 150 DEG C of heat preservation solidifications is dried in 70 80 DEG C, obtain high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material.The preparation method is simple, and low cost, the product flexibility for preparing are good, and dielectric constant is big.
Description
Technical field
The invention belongs to inorganic/organic composite material technical field, and in particular to a kind of high-dielectric constant inorganic/poly- two
Methylsiloxane composite and flexible material and preparation method and application.
Background technology
" electronic skin " passes through for pressure, temperature, humidity etc. to be converted into electric signal so as to realizing artificial haptic system function.
The flexibility of sensor is the basic demand of " electronic skin " to sensor used.Dimethyl silicone polymer has excellent physiology
Inertia, heat-resisting cold resistance, flexibility and electrical insulating property.Have been developed over based on poly dimethyl silicon in laboratory level in the world at present
The presser sensor capacitor of oxygen alkane flexible material, the sensing principle based on the presser sensor flexible capacitor of dimethyl silicone polymer
It is：External pressure causes dimethyl silicone polymer dielectric layer between two plate electrodes to deform upon so as to causing capacitance variation.But
Be dimethyl silicone polymer Typical dielectric constant relatively low, only 2.8, cause the presser sensor capacitor based on the material system
Sensitvity constraint.
Being reported for the purpose of improving dielectric constant has：Add high dielectric in Pioloform, polyvinyl acetal organic dielectric resin normal
Number filler；Chinese invention patent CN102643543A by high dielectric inorganic filler and bismaleimide compound, cyanate,
The organic composites such as epoxy resin are achieved with high dielectric constant copper clad laminate material；In addition, Chinese invention patent
CN102653622A, CN101955667A, CN101921479A disclose respectively CaCu 3 Ti 4 O respectively with PVDF, polyimides with
And the composite film material of cyanate ester resin, effectively raise the dielectric constant of organic media.But above complex organisms
Finite elastic, is not suitable as presser sensor condenser dielectric.
Therefore, prepare a kind of dielectric constant high, compound material flexible is good, and be applicable to the poly- of presser sensor capacitor
Dimethyl siloxane composite and flexible material is urgent problem.
Content of the invention
For above-mentioned deficiency of the prior art, the invention provides a kind of high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material and preparation method and application, can dimethyl silicone polymer composite dielectric in effectively solving prior art
Constant is low, response sensitivity is low, flexible poor the problems such as.
For achieving the above object, the technical solution adopted for the present invention to solve the technical problems is：
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
Dimethyl siloxane 25-35 parts, inorganic filler 1-10 parts, modifying agent 1-10 parts and curing agent 3-6 parts；
Wherein, inorganic filler is BaTiO3(BTO)、SrTiO3(STO)、BaSrTiO3(BST)、CaCu3Ti4O12(CCTO)、
One or more in PbTiO3 (PTO)；
Modifying agent is one or more in silane coupler, polyvinylpyrrolidone, polystyrene and polypyrrole alkanone；
Silane coupler is preferably KH550, KH560, KH570 or KH590；
Curing agent is dimethyl methyl hydrogen siloxane, trimethyl silanol, alkoxy silane or silicol.
Further, a kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including following weight portion
Raw material：3 parts of 30 parts of dimethyl silicone polymer, 9 parts of inorganic filler, 9.9 parts of modifying agent and curing agent.
Further, inorganic filler is CaCu3Ti4O12.
Further, modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:The mixture of 10 mixing.
Further, curing agent is dimethyl methyl hydrogen siloxane.
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) fine powder is worn in inorganic filler, mixes with modifying agent and organic solvent, magnetic agitation 0.5-1h, then in 90-
Ultrasonic disperse 15-60min under the conditions of 200W, is obtained uniform dispersion I；
(2) dimethyl silicone polymer is added in step (1) gained dispersion liquid I, magnetic agitation 1-3h, then in 200W bars
Ultrasonic disperse 20-60min under part, makes dispersion liquid II；
(3) by curing agent add dispersion liquid II in, stir, make dispersion liquid III, then by filming technology by its
Make wet film, by wet film be placed in 70-80 DEG C baking 1-2h, last 120-150 DEG C of heat preservation solidification 1-3h, obtain high-dielectric constant inorganic/
Dimethyl silicone polymer composite and flexible material.
Further, in step (1), inorganic filler particle diameter is 10-500nm.
Further, in step (1), organic solvent is ethanol, chloroform, dichloromethane or toluene.
Further, in step (3), high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material thickness is
500nm-1mm.
The present invention provide high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material and preparation method and should
With having the advantages that：
(1) preparation method is simple, and process costs are low, is suitable for large-scale production；
(2) high-dielectric constant inorganic for preparing/dimethyl silicone polymer composite and flexible material flexibility is good, dielectric constant
Greatly, and can according to application need easily to adjust the scope of dielectric constant.
Description of the drawings
Preparation flow figures of the Fig. 1 for high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material；
Fig. 2 is the complex media membrane capacitance pressure-electric capacity response curve of different BTO dopings.
Fig. 3 is the complex media membrane capacitance pressure-electric capacity response curve of different STO dopings.
Fig. 4 is the complex media membrane capacitance pressure-electric capacity response curve of different CCTO dopings.
Specific embodiment
Embodiment 1
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3.3 parts of 33 parts of dimethyl siloxane, 1 part of inorganic filler, 1.1 parts of modifying agent and curing agent；
Wherein, inorganic filler is BaTiO3(BTO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
BaTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(BTO) doping ratio
For 3% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by BaTiO3The powder that particle diameter is 120nm is worn into, 1g powders and 0.1g KH570,1g polyvinylpyrrolidines is taken
Ketone mixes, and is dissolved in 30mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, ultrasound point under the conditions of 200W
Scattered 15min, forms uniform dispersion I；
(2) 33g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min, then
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3.3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, pass through
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then shifted wet film by silk-screen printing technique
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 120 DEG C forms high-dielectric constant inorganic/poly dimethyl silicon
Oxygen alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 115%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 14, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 2.
Embodiment 2
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 3 parts of inorganic filler, 3.3 parts of modifying agent and curing agent；
Wherein, inorganic filler is BaTiO3(BTO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane.
BaTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(BTO) doping ratio
For 10% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by BaTiO3The powder that particle diameter is 120nm is worn into, 3g powders and 0.3g KH570,3g polyvinylpyrrolidines is taken
Ketone mixes, and is dissolved in 30mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasound point under the conditions of 90W
Scattered 15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by silk
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by net typography
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 120 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 110%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 32, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 2.
Embodiment 3
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 6 parts of inorganic filler, 6.6 parts of modifying agent and curing agent；
Wherein, inorganic filler is BaTiO3(BTO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
BaTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(BTO) doping ratio
For 20% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by BaTiO3The powder that particle diameter is 120nm is worn into, 6g powders and 0.6g KH570,6g polyvinylpyrrolidines is taken
Ketone mixes, and is dissolved in 30mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasound point under the conditions of 90W
Scattered 15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by silk
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by net typography
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 135 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 107%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 60, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 2.
Embodiment 4
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 9 parts of inorganic filler, 9.9 parts of modifying agent and curing agent；
Wherein, inorganic filler is BaTiO3(BTO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane.
BaTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(BTO) doping ratio
For 30% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by BaTiO3The powder that particle diameter is 120nm is worn into, 9g powders and 0.9g KH570,9g polyvinylpyrrolidines is taken
Ketone mixes, and is dissolved in 60mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasound point under the conditions of 90W
Scattered 15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by silk
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by net typography
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 150 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 103%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 88, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 2.
As shown in Figure 2, compared with pure dimethyl silicone polymer, adulterate BaTiO3Dielectric composite film, dielectric constant obtains
To significantly improving, with the increase of doping ratio, dielectric constant also increases, while its elongation at break is still maintained at 103%
More than, embody preferable elasticity.
With with pure dimethyl silicone polymer as compared with dielectric capacitor, doped with BaTiO3Dielectric composite film for electricity
The capacitor of medium, its rate of change of capacitance still keep the preferable linearity, BaTiO to the response of pressure3Doping cause electricity
The pressure of container-electric capacity response curve is integrally raised, and rate of change of capacitance is improved to the response sensitivity of pressure；BaTiO3Doping
Amount is bigger, and pressure-electric capacity response curve elevation amplitude is bigger.Such as in 400KPa, with pure dimethyl silicone polymer as electricity Jie
The condenser capacitance rate of change of matter is 10%, and under equal pressure, embodiment 1-4 condenser capacitance rate of change respectively 12%,
16%th, the pressure in 25%, 33%, but embodiment 4-electric capacity response curve line property degree after more than 600KPa is deteriorated, and electric capacity becomes
There is saturation trend with the increase of pressure in rate, and therefore, the doping ratio of BTO fine powders is no more than 30%.
Embodiment 5
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3.3 parts of 33 parts of dimethyl siloxane, 1 part of inorganic filler, 1.1 parts of modifying agent and curing agent；
Wherein, inorganic filler is SrTiO3(STO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
SrTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(STO) doping ratio
For 3% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by SrTiO3The powder that particle diameter is 80nm is worn into, 1g powders and 0.1g KH570,1g polyvinylpyrrolidones is taken
Mixing, is dissolved in 10mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 33g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3.3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, pass through
Automatically dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then shifted wet film by levelling technique
1h is dried in 80 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 140 DEG C forms high-dielectric constant inorganic/poly dimethyl silicon
Oxygen alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 119%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 25, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 3.
Embodiment 6
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 3 parts of inorganic filler, 3.3 parts of modifying agent and curing agent；
Wherein, inorganic filler is SrTiO3(STO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
SrTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(STO) doping ratio
For 10% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by SrTiO3The powder that particle diameter is 80nm is worn into, 3g powders and 0.3g KH570,3g polyvinylpyrrolidones is taken
Mixing, is dissolved in 30mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by certainly
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by dynamic levelling technique
1h is dried in 80 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 140 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 116%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 85, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 3.
Embodiment 7
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 6 parts of inorganic filler, 6.6 parts of modifying agent and curing agent；
Wherein, inorganic filler is SrTiO3(STO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane.
SrTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(STO) doping ratio
For 20% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by SrTiO3The powder that particle diameter is 80nm is worn into, 6g powders and 0.6g KH570,6g polyvinylpyrrolidones is taken
Mixing, is dissolved in 60mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by certainly
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by dynamic levelling technique
1h is dried in 80 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 140 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 113%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 125, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 3.
Embodiment 8
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 9 parts of inorganic filler, 9.9 parts of modifying agent and curing agent；
Wherein, inorganic filler is SrTiO3(STO)；Modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:
The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
SrTiO in above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material3(STO) doping ratio
For 30% the weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) by SrTiO3The powder that particle diameter is 80nm is worn into, 9g powders and 0.9g KH570,9g polyvinylpyrrolidones is taken
Mixing, is dissolved in 60mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by certainly
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by dynamic levelling technique
1h is dried in 80 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 140 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 110%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 200, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 3.
From the figure 3, it may be seen that compared with pure dimethyl silicone polymer, adulterate SrTiO3(STO) dielectric composite film, dielectric are normal
Number is improved significantly, and with the increase of doping ratio, dielectric constant also increases, while its elongation at break is still maintained at
More than 110%, embody preferable elasticity.
With with pure dimethyl silicone polymer as compared with dielectric capacitor, doped with SrTiO3(STO) dielectric is combined
Film is dielectric capacitor, and its rate of change of capacitance still keeps the doping of the preferable linearity, STO to cause the response of pressure
The pressure of capacitor-electric capacity response curve is integrally raised, and rate of change of capacitance is improved to the response sensitivity of pressure；The doping of STO
Amount is bigger, and pressure-electric capacity response curve elevation amplitude is bigger.Such as in 400KPa, with pure dimethyl silicone polymer as electricity Jie
The condenser capacitance rate of change of matter is 10%, and under equal pressure, embodiment 5-8 condenser capacitance rate of change is respectively
13.5%th, when more than 550KPa, the linearity is obvious for the pressure in 18%, 27%, 40%, but embodiment 8-electric capacity response curve
It is deteriorated, and rate of change of capacitance saturation trend occurs with the increase of pressure, therefore, the doping ratio of BTO fine powders is no more than
30%.
Embodiment 9
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3.3 parts of 33 parts of dimethyl siloxane, 1 part of inorganic filler, 1.1 parts of modifying agent and curing agent；
Wherein, inorganic filler is CaCu3Ti4O12(CCTO)；Modifying agent be KH570 and polyvinylpyrrolidone by weight
For 1:The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
In above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, the doping ratio of CCTO is 3% (nothing
The weight ratio of machine filler and dimethyl silicone polymer).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) CCTO is worn into the powder that particle diameter is 50nm, takes 1g powders and mix with 0.1g KH570,1g polyvinylpyrrolidone
Close, be dissolved in 10mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 33g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3.3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, pass through
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then shifted wet film by silk-screen printing technique
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 150 DEG C forms high-dielectric constant inorganic/poly dimethyl silicon
Oxygen alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 122%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 66, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 4.
Embodiment 10
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 3 parts of inorganic filler, 3.3 parts of modifying agent and curing agent；
Wherein, inorganic filler is CaCu3Ti4O12(CCTO)；Modifying agent be KH570 and polyvinylpyrrolidone by weight
For 1:The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
In above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, the doping ratio of CCTO is 10%
The weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) CCTO is worn into the powder that particle diameter is 50nm, takes 3g powders and mix with 0.3g KH570,3g polyvinylpyrrolidone
Close, be dissolved in 30mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by silk
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by net typography
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 150 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 120%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 160, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 4.
Embodiment 11
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
30 parts of dimethyl siloxane, 6 parts of inorganic filler, 6.6 parts of modifying agent, 3 parts of curing agent, catalyst；
Wherein, inorganic filler is CaCu3Ti4O12(CCTO)；Modifying agent is KH570 and polyvinylpyrrolidone；Curing agent
For dimethyl methyl hydrogen siloxane；
In above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, the doping ratio of CCTO is 20%
The weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) CCTO is worn into the powder that particle diameter is 50nm, takes 6g powders and mix with 0.6g KH570,6g polyvinylpyrrolidone
Close, be dissolved in 60mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by silk
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by net typography
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 150 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 118%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil alkane of × 15mm adheres to medium composite film surface as Top electrode, by two surface soldered of FTO conductive layers and aluminium foil
Go out lead, then make the presser sensor capacitor that upper and lower electrode is respectively with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 290, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 4.
Embodiment 12
A kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, including the raw material of following weight portion：Poly-
3 parts of 30 parts of dimethyl siloxane, 9 parts of inorganic filler, 9.9 parts of modifying agent and curing agent；
Wherein, inorganic filler is CaCu3Ti4O12(CCTO)；Modifying agent be KH570 and polyvinylpyrrolidone by weight
For 1:The mixture of 10 mixing；Curing agent is dimethyl methyl hydrogen siloxane；
In above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, the doping ratio of CCTO is 30%
The weight ratio of dimethyl silicone polymer (inorganic filler with).
The preparation method of above-mentioned high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, comprises the following steps：
(1) CCTO is worn into the powder that particle diameter is 50nm, takes 9g powders and mix with 0.9g KH570,9g polyvinylpyrrolidone
Close, be dissolved in 60mL absolute ethyl alcohols, magnetic agitation 30min under the conditions of 200r/min, then ultrasonic disperse under the conditions of 90W
15min, forms uniform dispersion I；
(2) 30g dimethyl silicone polymers are added in dispersion liquid I, magnetic agitation 1h under the conditions of 200r/min then exists
Ultrasonic disperse 60min under the conditions of 200W, makes dispersion liquid II；
(3) 3g dimethyl methyl hydrogen siloxane is added in dispersion liquid II, stirs, make dispersion liquid III, by silk
Dispersion liquid III in the FTO Conducting Glass of 20mm × 20mm is made wet film, is then transferred to wet film by net typography
1h is dried in 70 DEG C of baking ovens, and heat preservation solidification 2h under the conditions of being finally placed in 150 DEG C forms high-dielectric constant inorganic/polydimethylsiloxanes
Alkane composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 115%.
It is used for making presser sensor capacitor by medium composite membrane obtained in said method, its preparation process is：By 15mm
The aluminium foil of × 15mm adheres to medium composite film surface as Top electrode, by going out in FTO conductive layers and two surface soldered of aluminium foil
Lead, then make the presser sensor capacitor for being respectively upper and lower electrode with FTO conductive layers and aluminium foil layer.
Pressure-loaded test is carried out to above-mentioned capacitor, its dielectric constant is 400, the pass of capacitor surface pressure and electric capacity
It is that curve map is shown in Fig. 4.
Embodiment 13
In 12 step of embodiment (4), dispersion liquid III is made wet film on the quartz glass substrate of 20mm × 20mm, then
Wet film is transferred in 70 DEG C of baking ovens and dries 1h, heat preservation solidification 2h under the conditions of being finally placed in 150 DEG C, formation high-dielectric constant inorganic/
Dimethyl silicone polymer composite and flexible material is medium composite membrane, and measurement thickness is 25 μm, and elongation at break is 115%；
The mask of 15mm × 15mm is covered directly over gained medium composite membrane, then by 0.1mL concentration for 10g/L silver
Nano wire conductive ink is evenly applied to deielectric-coating surface in mask, and then uniform levelling is dried 30min at 100 DEG C, formed soft
Property conductive layer；Deielectric-coating of the front with nano silver wire conductive layer is carefully taken off from quartz glass substrate, then using same
Technique prepare nano silver wire conductive layer in another surface relevant position, respectively in four angles coating about 1mm of upper and lower conductive layers2
Low temperature silver paste, then solidify to form silver electrode in 135 DEG C of insulation 30min, welding lead in silver electrode respectively is formed flexible
Voltage-sensitive capacitor.
Capacitor obtained above is carried out pressure-loaded test, its dielectric constant be 400, capacitor surface pressure with electricity
The graph of relation (30%CCTO is flexible) of appearance is shown in Fig. 4.
As shown in Figure 4, compared with pure dimethyl silicone polymer, the dielectric composite film of the CCTO that adulterates, dielectric constant are obtained
Significantly improve, with the increase of doping ratio, dielectric constant also increases, at the same its elongation at break be still maintained at 110% with
On, embody preferable elasticity.
With with pure dimethyl silicone polymer as compared with dielectric capacitor, doped with CCTO dielectric composite film for electricity Jie
The capacitor of matter, its rate of change of capacitance still keep the doping of the preferable linearity, CCTO to cause capacitor the response of pressure
Pressure-electric capacity response curve integrally raise, rate of change of capacitance is improved to the response sensitivity of pressure；The doping of CCTO is got over
Greatly, pressure-electric capacity response curve elevation amplitude is bigger.Such as in 400KPa, with pure dimethyl silicone polymer as dielectric
Condenser capacitance rate of change is 10%, and under equal pressure, embodiment 9-12 condenser capacitance rate of change respectively 15%,
25%th, the pressure in 30%, 40%, but embodiment 12-electric capacity response curve line property degree after more than 400KPa becomes and is gradually deteriorated,
There is saturation trend with the increase of pressure in rate of change of capacitance.In comparison, two sides is with silver nanoparticle tunica fibrosa as electrode, and 30%
The composite dielectric film flexible capacitor of the doping doping of CCTO, its pressure-electric capacity response curve linearity preferably, are entirely being pressed
Higher sensitivity is shown in power test scope.
Claims (10)
1. a kind of high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material, it is characterised in that including following weight portion
Raw material：Dimethyl silicone polymer 25-35 parts, inorganic filler 1-10 parts, modifying agent 1-10 parts and curing agent 3-6 parts；
Wherein, inorganic filler is BaTiO3(BTO)、SrTiO3(STO)、BaSrTiO3(BST)、CaCu3Ti4O12(CCTO)、
One or more in PbTiO3 (PTO)；
Modifying agent is one or more in silane coupler, polyvinylpyrrolidone, polystyrene and polypyrrole alkanone；
Curing agent is dimethyl methyl hydrogen siloxane, trimethyl silanol, alkoxy silane or silicol.
2. high-dielectric constant inorganic according to claim 1/dimethyl silicone polymer composite and flexible material, its feature exist
In including the raw material of following weight portion：30 parts of dimethyl silicone polymer, 9 parts of inorganic filler, 9.9 parts of modifying agent and curing agent 3
Part.
3. high-dielectric constant inorganic according to claim 1 and 2/dimethyl silicone polymer composite and flexible material, its feature
It is, inorganic filler is CaCu3Ti4O12.
4. high-dielectric constant inorganic according to claim 1/dimethyl silicone polymer composite and flexible material, its feature exist
In silane coupler is KH550, KH560, KH570 or KH590.
5. high-dielectric constant inorganic according to claim 4/dimethyl silicone polymer composite and flexible material, its feature exist
In modifying agent is KH570 and polyvinylpyrrolidone is 1 by weight:The mixture of 10 mixing.
6. high-dielectric constant inorganic according to claim 1 and 2/dimethyl silicone polymer composite and flexible material, its feature
It is, curing agent is dimethyl methyl hydrogen siloxane.
7. the system of the high-dielectric constant inorganic as described in any one of claim 1-6/dimethyl silicone polymer composite and flexible material
Preparation Method, it is characterised in that comprise the following steps：
（1）Fine powder is worn in inorganic filler, is mixed with modifying agent and organic solvent, magnetic agitation 0.5-1h, then in 90-200W
Under the conditions of ultrasonic disperse 15-60min, be obtained uniform dispersion I；
（2）Dimethyl silicone polymer is added step（1）In gained dispersion liquid I, magnetic agitation 1-3h, then under the conditions of 200W
Ultrasonic disperse 20-60min, makes dispersion liquid II；
（3）Curing agent is added in dispersion liquid II, is stirred, is made dispersion liquid III, be then made into by filming technology
Wet film is placed in 70-80 DEG C of baking 1-2h by wet film, and last 120-150 DEG C of heat preservation solidification 1-3h obtains high-dielectric constant inorganic/poly- two
Methylsiloxane composite and flexible material.
8. the preparation method of high-dielectric constant inorganic according to claim 7/dimethyl silicone polymer composite and flexible material,
Characterized in that, step（1）Middle inorganic filler particle diameter is 10-500nm.
9. the preparation method of high-dielectric constant inorganic according to claim 7/dimethyl silicone polymer composite and flexible material,
Characterized in that, step（1）Middle organic solvent is ethanol, chloroform, dichloromethane or toluene.
10. the preparation side of high-dielectric constant inorganic according to claim 7/dimethyl silicone polymer composite and flexible material
Method, it is characterised in that step（3）Middle high-dielectric constant inorganic/dimethyl silicone polymer composite and flexible material thickness is 500nm-
1mm.
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| CN106928723A (en) * | 2017-03-21 | 2017-07-07 | 电子科技大学 | CaCu 3 Ti 4 O/dimethyl silicone polymer composite and flexible foam and its preparation method and application |
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| CN108929542A (en) * | 2018-08-09 | 2018-12-04 | 上海海事大学 | A kind of dimethyl silicone polymer with negative permittivity/graphene flexible composite film and preparation method thereof |
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