CN104985896B - Ceramics polymer composite material of high-k and preparation method thereof - Google Patents
Ceramics polymer composite material of high-k and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
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Abstract
The invention discloses ceramics polymer composite material of high-k and preparation method thereof, the preparation method includes：Step 1, silane coupler is dissolved in the first solvent, is prepared into the first solution；Step 2, ceramic powders are mixed with the first solution after, be prepared into suspension；Step 3, polymeric material is dissolved in the second solvent, is prepared into the second solution；Step 4, suspension is mixed with the second solution after, be prepared into ceramics polymer composite material slurry；Step 5, ceramics polymer composite material slurry is prepared into after solid film, makes solid film modified using heat treatment method；Step 6, face pressure larger for density polymer in two solid films is combined after, make multilayer materials.The ceramics polymer composite material that the present invention is obtained, microstructure are more uniform, and its dielectric constant is greatly improved, and dielectric absorption reduces, and dielectric properties are more excellent, can be widely applied in field of composite material preparation.
Description
Technical field
The present invention relates to field of compound material, more particularly to a kind of Ceramic-polymer Composite of high-k
And preparation method thereof.
Background technology
In prior art, the method that makes ceramic-polymer be usually using coupling agent and ceramic powder directly in conjunction with after again
The mode of polymeric material is added, but by coupling agent with ceramic powder directly in conjunction with open defect, when coupling agent consumption mistake
When big, the dielectric loss for being easily caused material increases；When coupling agent consumption is very few, if directly mixing with ceramic powder, easily only with
A small amount of ceramic powder conglomeration, is less useful for ceramic powders dispersion.In addition, the ceramic-polymer that method is made at present, its microstructure
And uneven, cause dielectric constant relatively low, dielectric properties are poor.
Content of the invention
In order to solve above-mentioned technical problem, it is an object of the invention to provide a kind of ceramic-polymer of high-k
The preparation method of composite, it is a further object of the present invention to provide a kind of Ceramic-polymer Composite of high-k.
The technical solution adopted for the present invention to solve the technical problems is：
The preparation method of the Ceramic-polymer Composite of high-k, including：
Step 1, silane coupler is dissolved in the first solvent, is prepared into the first solution；
Step 2, ceramic powders are mixed with the first solution after, be prepared into suspension；
Step 3, polymeric material is dissolved in the second solvent, is prepared into the second solution；
Step 4, suspension is mixed with the second solution after, be prepared into Ceramic-polymer Composite slurry；
Step 5, Ceramic-polymer Composite slurry is prepared into after solid film, solid-state is made using heat treatment method
Modified film；
Step 6, face pressure larger for density polymer in two solid films is combined after, make multilayer materials.
Further, the silane coupler selected from vinyl silanes, amino silane, epoxy radicals silicone hydride, hydrosulphonyl silane and
At least one in methacryloxypropyl silane coupling agent, first solvent selected from methanol, ethanol, isopropanol, toluene with
And at least one in acetone.
Further, the ceramic powders are selected from barium titanate, strontium titanates, barium strontium titanate, CaCu 3 Ti 4 O and La, Ce, Nd, Eu
With at least one in many barium titanate dopings of Fe.
Further, the polymeric material is selected from polyethylene, polypropylene, polyvinyl chloride, Kynoar, poly- trifluoro chloroethene
Alkene, polyethylene-tetrafluoroethene, Kynoar-trifluoro-ethylene, Kynoar-CTFE and Kynoar-three
At least one in PVF-difluoro vinyl chloride, second solvent selected from N,N-Dimethylformamide, ethyl acetate, acetone,
At least one in toluene, tetrahydrofuran and chloroform.
Further, in the suspension, silane coupler accounts for the 1% ~ 10% of ceramic powders gross mass or to account for ceramic powders total
The 5% ~ 30% of volume.
Further, in the Ceramic-polymer Composite slurry, volume ratio X of ceramic powders and polymeric material
Span is：0<X≤50%.
Further, the step 1, which is specially：
Silane coupler is added makes its hydrolysis obtain after hydrating solution in the first solvent, hydrating solution is sufficiently stirred for,
It is prepared into the first solution.
Further, the step 4, which is specially：
Ultrasonic disperse is carried out after suspension and the second solution are sufficiently mixed, be prepared into Ceramic-polymer Composite slurry
Body.
Further, the step 5, which is specially：
By Ceramic-polymer Composite slurry after solution casting method is prepared into solid film on quartz plate, adopt
Make solid film modified with heat treatment method.
The present invention solves another technical scheme that its technical problem adopted：
The Ceramic-polymer Composite of high-k, the composite are the potteries using described high-k
The preparation method of porcelain-polymer composites is made.
The invention has the beneficial effects as follows：The preparation method of the Ceramic-polymer Composite of the high-k of the present invention,
Including：Step 1, silane coupler is dissolved in the first solvent, is prepared into the first solution；Step 2, ceramic powders are molten with first
After liquid mixing, suspension is prepared into；Step 3, polymeric material is dissolved in the second solvent, is prepared into the second solution；Step 4,
After suspension is mixed with the second solution, Ceramic-polymer Composite slurry is prepared into；Step 5, will be multiple for ceramic-polymer
After condensation material slurry is prepared into solid film, make solid film modified using heat treatment method；Step 6, by two solid films
After the larger face pressure of density polymer is combined, multilayer materials are made.The ceramic-polymer composite wood that this method is made
Material, polymeric material is preferable with the conjugation of ceramic powders, it is to avoid clustering phenomena, and microstructure is more uniform, and which is situated between
Electric constant is greatly improved, and dielectric absorption reduces, and dielectric properties are more excellent.
Another beneficial effect of the present invention is：The Ceramic-polymer Composite of the high-k of the present invention, is to adopt
The preparation method of the Ceramic-polymer Composite of described high-k is made.This Ceramic-polymer Composite,
Polymeric material is preferable with the conjugation of ceramic powders, it is to avoid clustering phenomena, and microstructure is more uniform, and its dielectric is normal
Number is greatly improved, and dielectric absorption reduces, and dielectric properties are more excellent.
Description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Obtain in the step of Fig. 1 is the preparation method of the Ceramic-polymer Composite of the high-k of the present invention 5
The internal structure schematic diagram of solid film；
Fig. 2 is schematic diagram solid film pressed using conventional method；
Fig. 3 is the preparation method of the Ceramic-polymer Composite of the high-k using the present invention to solid film
The schematic diagram for being pressed；
Fig. 4 is obtained composite and Jie using composite obtained in prior art in embodiments of the invention two
Electric constant experimental data comparison diagram；
Fig. 5 is that obtained composite is multiple with obtained in the pressing mode using prior art in embodiments of the invention two
The dielectric constant experimental data comparison diagram of condensation material；
Fig. 6 is that obtained composite is multiple with obtained in the pressing mode using prior art in embodiments of the invention two
The dielectric absorption experimental data comparison diagram of condensation material.
Specific embodiment
The invention provides a kind of preparation method of the Ceramic-polymer Composite of high-k, including：
Step 1, silane coupler is dissolved in the first solvent, is prepared into the first solution；
Step 2, ceramic powders are mixed with the first solution after, be prepared into suspension；
Step 3, polymeric material is dissolved in the second solvent, is prepared into the second solution；
Step 4, suspension is mixed with the second solution after, be prepared into Ceramic-polymer Composite slurry；
Step 5, Ceramic-polymer Composite slurry is prepared into after solid film, solid-state is made using heat treatment method
Modified film；
Step 6, face pressure larger for density polymer in two solid films is combined after, make multilayer materials.
Silane coupler is dissolved in the first solvent in step 3 and is prepared into after the first solution, after mixing with ceramic powders, energy
Improve compatibility and the interface cohesion of ceramic powders and polymer, contribute to ceramic powder dispersion in the polymer.And by silicon
Alkane coupling agent is dissolved in after being prepared into the first solution in the first solvent, then is mixed with ceramic powders, and silane coupler can be avoided direct
The clustering phenomena occurred when mixing with ceramic powder.
With reference to Fig. 1, the solid film that makes using the method for step 5, ceramic powders skewness phenomenon will be presented, its
The ceramic powders density of middle one side is larger, is defined as C face, and the ceramic powders density of another side is less, and polymeric material is close
Degree is larger, is defined as P face.P face contact larger for the polymeric material density of two solid films is pressed together on one by step 6
Rise, i.e., pressed using P-P mode, multilayer materials are made, as shown in Figure 3.Pressing mode can be the modes such as hot pressing.Compare
Conventional method shown in Fig. 2 is directly by C face larger for ceramic powders density and the side of the larger P face hot pressing of polymeric material density
Method（C-P mode）, this method using P-P face pressure conjunction by the way of, residue in the air in composite material film when prepared by pour mask
It is easier to be removed, and polymeric matrix is more easy to spread in cavernous structure, so that the microstructure of composite material film
More uniform, its dielectric constant is greatly improved, and dielectric absorption reduces, and dielectric properties are more excellent.Polymeric material is the application system
Composite matrix, therefore the application be also referred to as polymeric matrix.
It is further used as preferred embodiment, the silane coupler is selected from vinyl silanes, amino silane, epoxy radicals
At least one in silane, hydrosulphonyl silane and methacryloxypropyl silane coupling agent, first solvent selected from methanol, second
At least one in alcohol, isopropanol, toluene and acetone.
It is further used as preferred embodiment, the ceramic powders are selected from barium titanate, strontium titanates, barium strontium titanate, metatitanic acid
At least one in copper calcium and many barium titanate dopings of La, Ce, Nd, Eu and Fe.
It is further used as preferred embodiment, the polymeric material is selected from polyethylene, polypropylene, polyvinyl chloride, gathers
Vinylidene, polytrifluorochloroethylene, polyethylene-tetrafluoroethene, Kynoar-trifluoro-ethylene, Kynoar-trifluoro chloroethene
At least one in alkene and Kynoar-trifluoro-ethylene-difluoro vinyl chloride, second solvent are selected from nitrogen nitrogen dimethyl methyl
At least one in acid amides, ethyl acetate, acetone, toluene, tetrahydrofuran and chloroform.
Be further used as preferred embodiment, in the suspension, silane coupler account for ceramic powders gross mass 1% ~
10% accounts for the 5% ~ 30% of ceramic powders cumulative volume.In such span, silane coupler has preferable coupling effect,
Can be wrapped up according to the granular size of ceramic powders and shape, while this ratio is less, become will not silane coupler
For the third phase beyond polymeric matrix and ceramic powder filled thing.
Be further used as preferred embodiment, in the Ceramic-polymer Composite slurry, ceramic powders be polymerized
The span of volume ratio X of thing material is：0<X≤50%.When ceramic powders are more than 50%, as inorganic powder is excessive, it is combined
The pliability of material and the high pressure resistant ability for puncturing can be decreased obviously, therefore in the present invention, ceramic powders and polymeric material
The scope of volume ratio be more than 0, less than 50%.
It is further used as preferred embodiment, the step 1, which is specially：
Silane coupler is added makes its hydrolysis obtain after hydrating solution in the first solvent, hydrating solution is sufficiently stirred for,
It is prepared into the first solution.
It is further used as preferred embodiment, the step 4, which is specially：
Ultrasonic disperse is carried out after suspension and the second solution are sufficiently mixed, be prepared into Ceramic-polymer Composite slurry
Body.
It is further used as preferred embodiment, the step 5, which is specially：
By Ceramic-polymer Composite slurry after solution casting method is prepared into solid film on quartz plate, adopt
Make solid film modified with heat treatment method.
Present invention also offers a kind of Ceramic-polymer Composite of high-k, the composite is to adopt institute
The preparation method of the Ceramic-polymer Composite of the high-k that states is made.
Embodiment one
A kind of preparation method of the Ceramic-polymer Composite of high-k, including：
Step 1, by molten for silane coupler in ethanol, be prepared into the first solution, specially：Silane coupler is added the
After making its hydrolysis obtain hydrating solution in one solvent, hydrating solution is sufficiently stirred for, is prepared into the first solution.
In the present embodiment, the first solvent using 95% ethanol and the alcohol solvent that constitutes of 5% water, by silane coupler plus
Enter in alcohol solvent, and wait 5 minutes so as to after hydrolyzing to form silanol, stir 12 hours, be prepared into the first solution.
Step 2, by barium strontium titanate（BaSrTiO3, BST）After ceramic powders are mixed with the first solution, strontium titanates is prepared into
Barium silica alkane coupling agent suspension.
Step 3, polymeric material Kynoar-CTFE P (VDF-CTFE) is dissolved in the second solvent, prepares
Become the second solution, the wherein mixed proportion of VDF/ CTFE is 88/12 mol%；
BST is 0 with the span of volume ratio X of polymeric matrix<X≤50%.
Step 4, barium strontium titanate-silane coupler suspension is mixed with the second solution after, ultrasonic disperse 1 hour, prepare
Become Ceramic-polymer Composite slurry.
Step 5, Ceramic-polymer Composite slurry is prepared into solid film by solution casting method on quartz plate
Afterwards, make solid film modified using methods such as heat treatments.
Step 6, reference Fig. 3, by face larger for density polymer in two solid films（That is P face）Using the mode pressure such as hot pressing
After being combined, multilayer materials are made.
The copolymer conduct of Kynoar -88/12 mol% of CTFE P (VDF-CTFE) is adopted in the present embodiment
The matrix of Ceramic-polymer Composite, the copolymer have very weak piezo-electric effect and high dielectric constant at room temperature,
Dielectric constant can reach 10 or so.
Embodiment two
A kind of preparation method of the Ceramic-polymer Composite of high-k, including：
Step 1, by molten for silane coupler in ethanol, be prepared into the first solution, specially：Silane coupler is added the
After making its hydrolysis obtain hydrating solution in one solvent, hydrating solution is sufficiently stirred for, is prepared into the first solution.
Step 2, by barium strontium titanate（BaSrTiO3, BST）After ceramic powders are mixed with the first solution, strontium titanates is prepared into
Barium silica alkane coupling agent suspension.
Step 3, polymeric material Kynoar-CTFE P (VDF-CTFE) is dissolved in the second solvent, prepares
Become the second solution, the wherein mixed proportion of VDF/ CTFE is 88/12 mol%；
BST is 40% with the volume ratio of polymeric matrix.
Step 4, barium strontium titanate-silane coupler suspension is mixed with the second solution after, ultrasonic disperse 1 hour, prepare
Become Ceramic-polymer Composite slurry.
Step 5, Ceramic-polymer Composite slurry is prepared into solid film by solution casting method on quartz plate
Afterwards, make solid film modified using methods such as heat treatments.
Step 6, reference Fig. 3, by face larger for density polymer in two solid films（That is P face）Using the mode pressure such as hot pressing
After being combined, multilayer materials are made.
The composite that makes using the preparation method of the present embodiment is illustrated in Fig. 4（In figure composite 1 represents）,
With silane coupler is not carried out processing, does not carry out the composite obtained by P-P mode hot pressing using in prior art（In figure
Represented with composite 2）Between dielectric constant experimental data contrast, from figure, the composite wood that this method is prepared
Material, dielectric properties have obtained significantly being lifted.
For the superiority of further verification step 6, illustrate in Fig. 5 multiple obtained in the preparation method using the present embodiment
Condensation material（In figure is represented with PP hot pressing）, with combined in conventional art using step 1 to 5 direct will be larger for ceramic powders density
C face and the larger P face hot pressing of polymeric material density method obtained in composite（In figure is represented with PC hot pressing）Between
Dielectric constant experimental data contrast, as shown in Figure 5, using step 6 the hot pressing of P-P mode obtain composite, its dielectric
Constant is greatly improved.Composite obtained in the preparation method using the present embodiment is illustrated in Fig. 6（In figure PP heat
Pressure represents）, direct by C face larger for ceramic powders density and polymeric material in conventional art with being combined to 5 using step 1
Composite obtained in the method for the larger P face hot pressing of density（In figure is represented with PC hot pressing）Between dielectric absorption experimental data
Contrast, in Fig. 6, ordinate dielectric loss is dielectric absorption, it will be appreciated from fig. 6 that using answering that the P-P mode hot pressing of step 6 is obtained
Condensation material, generally dielectric absorption are reduced, and dielectric properties are more excellent.Generally speaking, using the pressing mode of step 6, system
The dielectric constant of the composite for becoming is greatly improved, and dielectric absorption reduces, and dielectric properties are more excellent.
Embodiment three
The Ceramic-polymer Composite of the high-k prepared using the preparation method of embodiment one or two.
It is more than that the preferable enforcement to the present invention is illustrated, but the invention is not limited to the enforcement
Example, those of ordinary skill in the art can also made a variety of equivalent variations without prejudice to present invention spirit on the premise of or replace
Change, the modification of these equivalents or replacement are all contained in the application claim limited range.
Claims (8)
1. the preparation method of the Ceramic-polymer Composite of high-k, it is characterised in that include：
Step 1, silane coupler is dissolved in the first solvent, is prepared into the first solution；
Step 2, ceramic powders are mixed with the first solution after, be prepared into suspension；
Step 3, polymeric material is dissolved in the second solvent, is prepared into the second solution；
Step 4, suspension is mixed with the second solution after, be prepared into Ceramic-polymer Composite slurry；
Step 5, Ceramic-polymer Composite slurry is prepared into after solid film, solid film is made using heat treatment method
Modified；
Step 6, face pressure larger for density polymer in two solid films is combined after, make multilayer materials；
At least one in first solvent selected from methanol, ethanol, isopropanol, toluene and acetone, the ceramic powders choosing
At least one from barium titanate, strontium titanates, barium strontium titanate, CaCu 3 Ti 4 O and many barium titanate dopings of La, Ce, Nd, Eu and Fe,
The polymeric material is selected from polyethylene, polypropylene, polyvinyl chloride, Kynoar, polytrifluorochloroethylene, polyethylene-tetrafluoro
Ethene, Kynoar-trifluoro-ethylene, Kynoar-CTFE and Kynoar-trifluoro-ethylene-difluoro chlorine
At least one in ethene, second solvent are selected from N,N-Dimethylformamide, ethyl acetate, acetone, toluene, tetrahydrofuran
And at least one in chloroform.
2. the preparation method of the Ceramic-polymer Composite of high-k according to claim 1, its feature exist
In the silane coupler is selected from vinyl silanes, amino silane, epoxy radicals silicone hydride, hydrosulphonyl silane and methacryloxypropyl
At least one in base silane coupling agent.
3. the preparation method of the Ceramic-polymer Composite of high-k according to claim 1, its feature exist
In, in the suspension, silane coupler accounts for the 1% ~ 10% of ceramic powders gross mass or accounts for the 5% ~ 30% of ceramic powders cumulative volume.
4. the preparation method of the Ceramic-polymer Composite of high-k according to claim 1, its feature exist
In, in the Ceramic-polymer Composite slurry, ceramic powders with the span of volume ratio X of polymeric material are：0<
X≤50%.
5. the preparation method of the Ceramic-polymer Composite of high-k according to claim 1, its feature exist
In, the step 1, which is specially：
Silane coupler is added makes its hydrolysis obtain after hydrating solution in the first solvent, hydrating solution is sufficiently stirred for, is prepared
Become the first solution.
6. the preparation method of the Ceramic-polymer Composite of high-k according to claim 1, its feature exist
In, the step 4, which is specially：
Ultrasonic disperse is carried out after suspension and the second solution are sufficiently mixed, be prepared into Ceramic-polymer Composite slurry.
7. the preparation method of the Ceramic-polymer Composite of high-k according to claim 1, its feature exist
In, the step 5, which is specially：
By Ceramic-polymer Composite slurry after solution casting method is prepared into solid film on quartz plate, using heat
Processing method makes solid film modified.
8. the Ceramic-polymer Composite of high-k, it is characterised in that the composite be using claim 1 to 7
Any one of the preparation method of Ceramic-polymer Composite of high-k make.
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| CN105347788B (en) * | 2015-11-13 | 2018-09-21 | 南京工业大学 | The microwave composite dielectric materials and preparation method of low-dielectric loss |
| CN105778361A (en) * | 2016-03-08 | 2016-07-20 | 西北工业大学 | High-dielectric tunability ceramic/high polymer functional composite and preparation method |
| CN106751241B (en) * | 2016-11-21 | 2019-01-04 | 中南大学 | A kind of barium titanate/polymer composites, preparation method and application |
| CN106751240B (en) * | 2016-11-21 | 2019-01-04 | 中南大学 | A kind of sodium titanate/polymer composites, preparation method and application |
| CN106751242B (en) * | 2016-11-21 | 2019-01-22 | 中南大学 | A kind of ceramic/polymer composite, preparation method and application |
| CN109957194A (en) * | 2017-12-14 | 2019-07-02 | 中国科学院深圳先进技术研究院 | A kind of laminated film and preparation method thereof |
| CN108314865A (en) * | 2018-01-22 | 2018-07-24 | 西安理工大学 | An a kind of core bivalve dielectric composite material and preparation method thereof for embedding nano silver |
| CN109503962A (en) * | 2018-10-25 | 2019-03-22 | 北京石油化工学院 | A kind of high electroluminescent deformation dielectric elastomer composite material and preparation method thereof |
| CN109608190A (en) * | 2018-12-25 | 2019-04-12 | 佛山科学技术学院 | A kind of high dielectric ceramic and preparation method thereof |
| CN110330676A (en) * | 2019-06-20 | 2019-10-15 | 杭州电子科技大学 | A kind of preparation method of the high dielectric constant compound film material based on ceramic packing |
| CN110233047A (en) * | 2019-07-03 | 2019-09-13 | 华中科技大学 | A kind of preparation method of high energy storage density dielectric substance |
| CN110615963A (en) * | 2019-09-24 | 2019-12-27 | 北京化工大学 | High-dielectric elastomer composite material with barium titanate as filler and preparation method thereof |
| CN113771471B (en) * | 2021-02-06 | 2023-05-26 | 四川建筑职业技术学院 | Mxenes polymer dielectric composite material and preparation process thereof |
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| CA2830269A1 (en) * | 2011-03-23 | 2012-10-26 | The Curators Of The University Of Missouri | High dielectric constant composite materials and methods of manufacture |
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