CN104530616A - High dielectric property and low loss sheet-shaped barium titanate base/ polymer composite material and preparation method thereof - Google Patents
High dielectric property and low loss sheet-shaped barium titanate base/ polymer composite material and preparation method thereof Download PDFInfo
- Publication number
- CN104530616A CN104530616A CN201510001868.8A CN201510001868A CN104530616A CN 104530616 A CN104530616 A CN 104530616A CN 201510001868 A CN201510001868 A CN 201510001868A CN 104530616 A CN104530616 A CN 104530616A
- Authority
- CN
- China
- Prior art keywords
- sheet
- barium titanate
- batio
- dielectric property
- high dielectric
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 229920000642 polymer Polymers 0.000 title claims abstract description 15
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000011159 matrix material Substances 0.000 claims abstract description 27
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000004642 Polyimide Substances 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 229920001721 polyimide Polymers 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 229960004756 ethanol Drugs 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000007731 hot pressing Methods 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- -1 polyethylene Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- 230000010287 polarization Effects 0.000 abstract description 3
- 230000002269 spontaneous effect Effects 0.000 abstract description 3
- 239000002861 polymer material Substances 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Insulating Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a high dielectric property and low loss sheet-shaped barium titanate base/ polymer composite material and a preparation method thereof, and belongs to the field of multifunctional composite material preparation. A BaTio3 base ferroelectric material of a sheet-shaped structure is used for conducting strong spontaneous polarization in the a-b face, a polymer matrix is filled with the BaTio3 base ferroelectric material, a uniform and orderly distributed ferroelectric/polymer material composite structure is formed, the excellent performance of the ferroelectric material can be fully performed, and the dielectric property of the composite material is obviously improved.
Description
Technical field
The present invention relates to multifunctional composite preparation field, particularly relate to a kind of high dielectric property low-loss sheet-like barium titanate base/polymer composites.
Background technology
In IC passive device, because electrical condenser occupies printed circuit board (PCB) (Printed Circuit Board, PCB) volume and weight of the overwhelming majority, the energy storage density improving it just seems particularly important, and corresponding energy-accumulating medium material is also to Gao Jie, high frequency, reduce power consumption, low cost future development therewith.
In recent years, the dielectric substance preparing high energy storage density becomes the focus of people's concern, and how to prepare there is high-k (ε r=25-170) simultaneously, low-loss (tg δ <0.05), flexible, a focus of this research field is in recent years become with the organic substrate novel electron material that the over-all properties such as compatible is superior mutually, the electrical condenser that the dielectric utilizing it superior and mechanical property are designed and developed, microdrive, artificial-muscle and organ, the device such as intelligent material and microelectron-mechanical, the field such as aerospace and microelectronics can be widely used in.
With BaTiO
3the nano particle of base is compared with fiber, has the BaTiO of sheet structure
3base ferroelectric material, is positioned at a-b face and has stronger spontaneous polarization, and very little along the spontaneous polarization of c direction is even 0, and dielectric properties are more superior.If the ferroelectric material of sheet structure is filled in polymeric matrix, formed uniform sequential distribution ferroelectric/polymer composite structures, the high-performance of ferroelectric material will be given full play to, to new change be there will be to the dielectric properties of matrix material, thus the shortcoming caused by spherical particle can be made up to a great extent.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of high-k, compared with high-flexibility, low-loss sheet-like barium titanate base/polymer composites.
For reaching above-mentioned purpose, a kind of high dielectric property low-loss of the present invention sheet-like barium titanate base/polymer composites, it comprises polymeric matrix and the dispersion ceramic ferroelectric materials with sheet structure in the polymer matrix, and described sheet ferroelectric material and described polymeric matrix are made up of following mass percent:
Described polymeric matrix: 30.0wt.% ~ 95.0wt.%
The ceramic ferroelectric materials of described sheet: 5.0wt.% ~ 70.0wt.%
Wherein said length 100nm ~ 15 μm with the ceramic ferroelectric materials of sheet structure, width 100nm ~ 15 μm, thickness 10nm ~ 5 μm.
The ceramic ferroelectric materials of wherein said sheet structure has any one or bi-material to form: BaTiO
3, Ba
xsr
1-xtiO
3, wherein 0<x<1; Described polymeric matrix has following any one or bi-material to form: polyvinylidene difluoride (PVDF), polyimide, polyvinylidene fluoride copolymer, epoxy resin and polyethylene.
Wherein said barium titanate/polymer composites is obtained by solution blending-pressure sintering or solution blending-spin-coating method.
As the preferred preparation method of one, concrete steps are as follows:
1) according to mass ratio 23:100, TiO is taken
2and Bi
2o
3raw material, wherein Bi
2o
3excessive 5% ~ 15wt%, adds TiO simultaneously
2and Bi
2o
3naCl or KCl of both quality sums is placed in nylon ball grinder ball mill mixing (300r/min), and add zirconia ball and dehydrated alcohol or deionized water ball milling 20 ~ 24 hours, wherein the mass ratio of zirconia ball and ball milling material is 1.2 ~ 1.5; The mass ratio of dehydrated alcohol or deionized water and ball milling material is 1.5 ~ 3.0, and discharging is dried and obtained mixed powder; Deionized water is added after sintering, after softening, by washed with de-ionized water 3-5 time, the Bi of final acquisition sheet structure
4ti
3o
12;
2) by 1) the middle sheet Bi obtained
4ti
3o
12with BaCO
3take raw material according to mass ratio 91:100, add Bi simultaneously
4ti
3o
12with BaCO
3naCl or KCl of both quality sums is placed in nylon ball grinder batch mixing (100r/min); Sintering, obtains sheet BaTiO after washing
3powder;
3) by described sheet BaTiO
3put into hydrogen peroxide, at 80 ~ 120 DEG C, stir 3h, centrifugal, washing, obtains the hydroxylated sheet BaTiO in interface
3;
4) by hydroxylated for interface sheet BaTiO
3powder puts into ethanol solution, adopts ultrasonic oscillation and magnetic agitation to be disperseed to form stable suspension;
5) to 4) in suspension in add in described polymeric matrix, ultrasonic and magnetic agitation makes its Homogeneous phase mixing;
6) by 5) in obtain mixed solution dry in loft drier after, putting into hot pressing die, is 150 ~ 180 DEG C in temperature, pressure 5 ~ 10MPa, and 20 minutes time is hot-forming, obtains described matrix material.
The invention difference from existing technology is that the present invention achieves following technique effect:
The ferroelectric material of sheet structure of the present invention has certain length-to-diameter ratio, compared to granular ferroelectric powder, effectively can improve the specific inductivity of matrix material, thus can have higher snappiness under lower content.
Below in conjunction with accompanying drawing, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is sheet structure BaTiO of the present invention
3the XRD figure spectrum of structure;
Fig. 2 is sheet structure BaTiO of the present invention
3the SEM collection of illustrative plates of structure;
Fig. 3 is sheet structure BaTiO of the present invention
3the specific inductivity of/polyvinylidene fluoride composite material is with the change curve of component;
Fig. 4 is sheet structure BaTiO of the present invention
3the dielectric loss of/polyvinylidene fluoride composite material is with the change curve of component;
Fig. 5, sheet BaTiO
3the specific inductivity of/composite polyimide material and dielectric loss are with the change curve of component.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
Embodiment 1
Prepare pure PVDF material
First the alcohol taking 20ml is placed in clean beaker, then adds 2g polyvinylidene difluoride (PVDF) (PVDF), after ultrasonic 1h, utilizes magnetic agitation 24h, insert in loft drier by the mixing solutions of acquisition, and temperature is 100 DEG C, obtains pure PVDF powder after drying;
Secondly, take above-mentioned obtained pure PVDF powder 0.03g, put into hot pressing grinding tool, at temperature 170 DEG C, be incubated 20 minutes, apply pressure 5MPa, after naturally cooling, obtain the pure PVDF material that thickness is 120 μm.
As shown in Figure 3,4, its specific inductivity is about 16 for the specific inductivity of pure PVDF and dielectric loss, dielectric loss >5%.
Preparation sheet BaTiO
3
First, the TiO of 3.6099g is taken
2, the Bi of 15.6601g
2o
3with the NaCl of 19.27g, put in ball grinder, add 150ml dehydrated alcohol and 70g zirconium ball, put into ball mill ball mill mixing 24h, rotating speed is 300r/min, and ball milling puts into corundum crucible after drying, heating curve is as follows: room temperature is incubated 1h after rising to 805 DEG C, temperature rise rate 3 DEG C/min, is incubated 2h after then rising to 1000 DEG C by 805 DEG C, temperature rise rate 2 DEG C/min; Appropriate deionized water is added after sintering, after softening, by washed with de-ionized water 3-5 time, the Bi of final acquisition sheet structure
4ti
3o
12;
Secondly, 9.0125g sheet Bi is taken
4ti
3o
12, the BaCO of 9.8873g
3with the NaCl of 18.8998g, with ball mill batch mixing 8 ~ 12h, rotational speed of ball-mill 100r/min; Ball milling puts into corundum crucible after drying, and heating curve is as follows: room temperature is incubated 1h after rising to 805 DEG C, temperature rise rate 3 DEG C/min, is incubated 2h after then rising to 970 DEG C by 805 DEG C, temperature rise rate 2 DEG C/min; After sintering, sample adds appropriate deionized water, and after softening, interpolation concentrated hydrochloric acid or concentrated nitric acid wash Bi off
2o
3, then with deionized water rinsing number time, to washing lotion, instill AgNO
3generate without precipitation, obtain sheet BaTiO
3structured material; By described sheet BaTiO
3put into 200ml hydrogen peroxide, at 80 ~ 120 DEG C, stir 3h, centrifugal, washing, obtains the hydroxylated sheet BaTiO in interface
3;
Preparation PVDF based composites
Take the hydroxylation sheet BaTiO of PVDF and 0.2g of 1.8g
3, joined in the ethanol solution of 20ml, ultrasonic disperse 1h, after magnetic agitation 24h, gained suspension be placed in loft drier, at temperature 100 DEG C, ethanol is volatilized completely, obtain mixed powder;
The mixed powder taking above-mentioned 0.03g is hot-forming on thermocompressor, temperature 170 DEG C, and pressure 5Mpa, obtains sheet BaTiO after naturally cooling at 20 minutes time
3massfraction is the PVDF based composites of 10wt%, and wherein the thickness of matrix material is about 120 μm.The dielectric characteristics of sample as shown in Figure 3,4.
The specific inductivity of this matrix material is about 20, dielectric loss <0.03, specific inductivity and loss more stable within the scope of institute's measured frequency.
Embodiment 2
Pure PVDF material and sheet BaTiO is obtained by embodiment 1 method
3
Preparation PVDF based composites
Take the sheet BaTiO of PVDF and 1g of 1g
3, joined in the ethanol solution of 20ml, ultrasonic disperse 1h, after magnetic agitation 24h, gained suspension be placed in loft drier, at temperature 100 DEG C, ethanol is volatilized completely, obtain mixed powder;
The mixed powder taking above-mentioned 0.03g is hot-forming on thermocompressor, temperature 170 DEG C, and pressure 5Mpa, obtains sheet BaTiO after naturally cooling at 20 minutes time
3massfraction is the PVDF based composites of 50wt%, and wherein the thickness of matrix material is about 120 μm, and the dielectric characteristics of sample as shown in Figure 3,4.
The specific inductivity of this matrix material is about 63, dielectric loss <0.02, specific inductivity and loss more stable within the scope of institute's measured frequency.
Same mode is taked to prepare sheet BaTiO
3massfraction is respectively from the PVDF based composites of 5%-60%, and as shown in Figure 3,4, the specific inductivity of the matrix material obtained is all higher, and dielectric loss is lower for the PVDF based composites dielectric characteristics obtained.
Embodiment 3 prepares polyimide-based composite material
Sheet BaTiO is obtained by embodiment 1 method
3
Take the sheet BaTiO of 1.3031g
3, put in the DMAc solution of 50ml, ultrasonic disperse, after 30 minutes, adds 0.3400g ODA, utilizes magnetic agitation by dispersed for its mixing liquid; In the process stirred, add 0.3570g PMDA subsequently, stir 24 hours, obtain BT-PAA mixing solutions; By BT-PAA solution on the glass sheet, carry out hot-imide, heat-up rate curve is as follows:
80 DEG C/30min → 150 DEG C/30min → 200 DEG C/30min → 250 DEG C/60min → 300 DEG C/60min, then furnace cooling.Finally obtain BT volume fraction 30vol%/PI matrix material, wherein the thickness of matrix material is about 60 μm.The dielectric characteristics of sample as shown in Figure 5.
The specific inductivity of this matrix material is about 26, dielectric loss <0.05, specific inductivity and loss more stable within the scope of institute's measured frequency.
Same mode is taked to prepare sheet BaTiO
3massfraction is respectively from polyimide (PI) based composites of 10%-30%, and as shown in Figure 5, the specific inductivity of the matrix material obtained is all higher, and dielectric loss is lower for the PI based composites dielectric characteristics obtained.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (5)
1. high dielectric property low-loss sheet-like barium titanate base/polymer composites, it is characterized in that it comprises polymeric matrix and the dispersion ceramic ferroelectric materials with sheet structure in the polymer matrix, and described sheet ferroelectric material and described polymeric matrix are made up of following mass percent:
Described polymeric matrix: 30.0wt.% ~ 95.0wt.%
The ceramic ferroelectric materials of described sheet: 5.0wt.% ~ 70.0wt.%
2. high dielectric property low-loss sheet-like barium titanate base/polymer composites according to claim 1, it is characterized in that: described length 100nm ~ 15 μm with the ceramic ferroelectric materials of sheet structure, width 100nm ~ 15 μm, thickness 10nm ~ 5 μm.
3. high dielectric property low-loss sheet-like barium titanate base/polymer composites according to claim 1, is characterized in that: the ceramic ferroelectric materials of described sheet structure has any one or bi-material to form: BaTiO
3, Ba
xsr
1-xtiO
3, wherein 0<x<1; Described polymeric matrix has following any one or bi-material to form: polyvinylidene difluoride (PVDF), polyimide, polyvinylidene fluoride copolymer, epoxy resin and polyethylene.
4. prepare a method for the high dielectric property low-loss sheet-like barium titanate base/polymer composites according to any one of claim 1-3, it is characterized in that: described barium titanate/polymer composites is obtained by solution blending-pressure sintering or solution blending-spin-coating method.
5. the preparation method of high dielectric property low-loss sheet-like barium titanate base/polymer composites according to claim 4, is characterized in that:
1) according to mass ratio 23:100, TiO is taken
2and Bi
2o
3raw material, wherein Bi
2o
3excessive 5% ~ 15wt%, adds TiO simultaneously
2and Bi
2o
3naCl or KCl of both quality sums is placed in nylon ball grinder ball mill mixing (300r/min), and add zirconia ball and dehydrated alcohol or deionized water ball milling 20 ~ 24 hours, wherein the mass ratio of zirconia ball and ball milling material is 1.2 ~ 1.5; The mass ratio of dehydrated alcohol or deionized water and ball milling material is 1.5 ~ 3.0, and discharging is dried and obtained mixed powder; Deionized water is added after sintering, after softening, by washed with de-ionized water 3-5 time, the Bi of final acquisition sheet structure
4ti
3o
12;
2) by 1) the middle sheet Bi obtained
4ti
3o
12with BaCO
3take raw material according to mass ratio 91:100, add Bi simultaneously
4ti
3o
12with BaCO
3naCl or KCl of both quality sums is placed in nylon ball grinder batch mixing (100r/min); Sintering, obtains sheet BaTiO after washing
3powder;
3) by described sheet BaTiO
3put into hydrogen peroxide, at 80 ~ 120 DEG C, stir 3h, centrifugal, washing, obtains the hydroxylated sheet BaTiO in interface
3;
4) by hydroxylated for interface sheet BaTiO
3powder puts into ethanol solution, adopts ultrasonic oscillation and magnetic agitation to be disperseed to form stable suspension;
5) to 4) in suspension in add in described polymeric matrix, ultrasonic and magnetic agitation makes its Homogeneous phase mixing;
6) by 5) in obtain mixed solution dry in loft drier after, putting into hot pressing die, is 150 ~ 180 DEG C in temperature, pressure 5 ~ 10MPa, and 20 minutes time is hot-forming, obtains described matrix material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510001868.8A CN104530616B (en) | 2015-01-05 | 2015-01-05 | A kind of high dielectric property low-loss sheet-like barium titanate base/polymer composites and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510001868.8A CN104530616B (en) | 2015-01-05 | 2015-01-05 | A kind of high dielectric property low-loss sheet-like barium titanate base/polymer composites and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104530616A true CN104530616A (en) | 2015-04-22 |
| CN104530616B CN104530616B (en) | 2017-06-09 |
Family
ID=52846264
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510001868.8A Expired - Fee Related CN104530616B (en) | 2015-01-05 | 2015-01-05 | A kind of high dielectric property low-loss sheet-like barium titanate base/polymer composites and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104530616B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910583A (en) * | 2015-05-04 | 2015-09-16 | 芜湖市宝艺游乐科技设备有限公司 | High-dielectric graphene oxide melamine resin and preparation method thereof |
| CN105419328A (en) * | 2016-01-11 | 2016-03-23 | 苏州大学 | Modified barium titanate foamed ceramic/thermosetting resin composite material and preparation method thereof |
| CN106065132A (en) * | 2016-06-13 | 2016-11-02 | 吴江佳亿电子科技有限公司 | A kind of composite polystyrene capacitor material and preparation method thereof |
| CN107434897A (en) * | 2016-05-27 | 2017-12-05 | 北京化工大学 | Barium titanate particles, barium titanate/fluoropolymer composite and preparation method thereof |
| CN108484980A (en) * | 2018-06-26 | 2018-09-04 | 兰州理工大学 | A kind of new type structure of hud composite material and preparation method thereof |
| CN110964294A (en) * | 2019-12-02 | 2020-04-07 | 江苏科技大学 | Epoxy resin-based high-dielectric composite material, preparation method and application |
| CN111635543A (en) * | 2020-05-15 | 2020-09-08 | 内蒙古科技大学 | Friction layer for improving electrical property of nano generator by using composite interlayer and preparation method thereof |
| CN114874582A (en) * | 2022-03-24 | 2022-08-09 | 华北电力大学 | Electroluminescent material and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0787046B2 (en) * | 1990-03-02 | 1995-09-20 | 株式会社大真空 | Polymer composite dielectric |
| CN1432598A (en) * | 2003-02-28 | 2003-07-30 | 清华大学 | High-dielectric composite material containing carbon nanotube and its prepn process |
| CN102199356A (en) * | 2010-03-22 | 2011-09-28 | 北京化工大学 | Triphase-body nanometer composite material with high dielectric constant and high elasticity and preparation method thereof |
| CN102558718A (en) * | 2010-12-07 | 2012-07-11 | 北京有色金属研究总院 | Barium titanate/polyvinylidene fluoride composite dielectric film and preparation method thereof |
| CN102775705A (en) * | 2012-06-05 | 2012-11-14 | 西安交通大学 | Polymer-matrix composite material and preparation method thereof |
| CN103382240A (en) * | 2013-07-15 | 2013-11-06 | 上海交通大学 | Barium titanate/polymer composite material with high dielectric constant and its preparation method |
| CN103408775A (en) * | 2013-07-20 | 2013-11-27 | 北京化工大学 | Preparation method of flexible composite dielectric material with high dielectric constant and low dielectric loss |
-
2015
- 2015-01-05 CN CN201510001868.8A patent/CN104530616B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0787046B2 (en) * | 1990-03-02 | 1995-09-20 | 株式会社大真空 | Polymer composite dielectric |
| CN1432598A (en) * | 2003-02-28 | 2003-07-30 | 清华大学 | High-dielectric composite material containing carbon nanotube and its prepn process |
| CN102199356A (en) * | 2010-03-22 | 2011-09-28 | 北京化工大学 | Triphase-body nanometer composite material with high dielectric constant and high elasticity and preparation method thereof |
| CN102558718A (en) * | 2010-12-07 | 2012-07-11 | 北京有色金属研究总院 | Barium titanate/polyvinylidene fluoride composite dielectric film and preparation method thereof |
| CN102775705A (en) * | 2012-06-05 | 2012-11-14 | 西安交通大学 | Polymer-matrix composite material and preparation method thereof |
| CN103382240A (en) * | 2013-07-15 | 2013-11-06 | 上海交通大学 | Barium titanate/polymer composite material with high dielectric constant and its preparation method |
| CN103408775A (en) * | 2013-07-20 | 2013-11-27 | 北京化工大学 | Preparation method of flexible composite dielectric material with high dielectric constant and low dielectric loss |
Non-Patent Citations (2)
| Title |
|---|
| 丁西亚等: "双重熔盐法制备片状BaTiO3粉体", 《硅酸盐学报》 * |
| 荆丽娜: "片状钛酸钡的制备及其电磁性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910583A (en) * | 2015-05-04 | 2015-09-16 | 芜湖市宝艺游乐科技设备有限公司 | High-dielectric graphene oxide melamine resin and preparation method thereof |
| CN105419328A (en) * | 2016-01-11 | 2016-03-23 | 苏州大学 | Modified barium titanate foamed ceramic/thermosetting resin composite material and preparation method thereof |
| WO2017121204A1 (en) * | 2016-01-11 | 2017-07-20 | 苏州大学张家港工业技术研究院 | Modified barium titanate foam ceramic/thermosetting resin composite material and preparation method therefor |
| US10807916B2 (en) | 2016-01-11 | 2020-10-20 | Soochow University | Modified barium titanate foam ceramic/thermosetting resin composites and preparation method thereof |
| CN107434897A (en) * | 2016-05-27 | 2017-12-05 | 北京化工大学 | Barium titanate particles, barium titanate/fluoropolymer composite and preparation method thereof |
| CN106065132A (en) * | 2016-06-13 | 2016-11-02 | 吴江佳亿电子科技有限公司 | A kind of composite polystyrene capacitor material and preparation method thereof |
| CN108484980A (en) * | 2018-06-26 | 2018-09-04 | 兰州理工大学 | A kind of new type structure of hud composite material and preparation method thereof |
| CN110964294A (en) * | 2019-12-02 | 2020-04-07 | 江苏科技大学 | Epoxy resin-based high-dielectric composite material, preparation method and application |
| CN111635543A (en) * | 2020-05-15 | 2020-09-08 | 内蒙古科技大学 | Friction layer for improving electrical property of nano generator by using composite interlayer and preparation method thereof |
| CN114874582A (en) * | 2022-03-24 | 2022-08-09 | 华北电力大学 | Electroluminescent material and preparation method thereof |
| CN114874582B (en) * | 2022-03-24 | 2023-02-28 | 华北电力大学 | Electroluminescent material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104530616B (en) | 2017-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104530616A (en) | High dielectric property and low loss sheet-shaped barium titanate base/ polymer composite material and preparation method thereof | |
| CN107474312B (en) | The preparation method of ceramic filled polytetrafluoroethylglass microwave composite medium substrate | |
| Lin et al. | Synthetic multifunctional graphene composites with reshaping and self‐healing features via a facile biomineralization‐inspired process | |
| CN101712784B (en) | Core-shell structured packing/polymer-based composite material and preparation method thereof | |
| CN105541389A (en) | Barium titanate foam ceramic/thermosetting resin composite material and preparation method thereof | |
| CN104211962A (en) | High dielectric polyimide composite material and preparation method thereof | |
| CN108501488A (en) | A kind of high-frequency high-speed copper-clad plate and preparation method thereof | |
| CN107434897B (en) | Barium titanate particles, barium titanate/fluoropolymer composite material and preparation method thereof | |
| Yin et al. | Cellulose/BaTiO3 nanofiber dielectric films with enhanced energy density by interface modification with poly (dopamine) | |
| CN109762278A (en) | A kind of two-dimensional nano piece-polymer flexibility laminated film and preparation method thereof | |
| CN103388197B (en) | A kind of preparation method of graphene fiber | |
| CN103396548B (en) | A kind of preparation method of high dielectric polyimide/CaCu 3 Ti 4 O nanowire composite | |
| CN103570959A (en) | Preparation method of polyvinylidene fluoride/one-dimensional columnar structural lead titanate monocrystal nanofiber composite film | |
| CN104650509A (en) | Preparation method of high-energy-storage-density polyvinylidene fluoride composite film | |
| CN102936351B (en) | Method for preparing polyvinylidene fluoride (PVDF)/barium titanate (BT) composite membrane materials | |
| CN102627817A (en) | High-energy-storage density dielectric material and preparation method thereof | |
| CN103724622A (en) | Preparation method for potassium-sodium niobate/polyimide high dielectric thin film | |
| CN108003520B (en) | Preparation method of polyvinylidene fluoride titanium carbide nanosheet composite material with high dielectric property | |
| CN106699177B (en) | Lead-free piezoelectric energy collecting material with high power generation characteristic and preparation method thereof | |
| Wang et al. | The size-matching effect in 0.1 Na1/3Ca1/3Bi1/3Cu3Ti4O12-xBa (Fe0. 5Nb0. 5) O3-(0.9-x) PVDF composites | |
| CN104072128A (en) | Nanoscale square-phase barium titanate powder and preparation method thereof | |
| CN109777009A (en) | A kind of GR-TiO being used to prepare high density capacitors2- PVDF nanocomposite and preparation method thereof | |
| CN103570347B (en) | Method for tetragonal phase conversion of nano barium titanate | |
| CN107586060B (en) | A kind of High-energy-storage density dielectric material and preparation method thereof | |
| CN105778362B (en) | A kind of copper titanate bismuth sodium/polymer matrix three-phase composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170609 |