CN107488277A - A kind of inorganic filler for loading heterogeneous granular and preparation method thereof - Google Patents
A kind of inorganic filler for loading heterogeneous granular and preparation method thereof Download PDFInfo
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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Abstract
The invention discloses a kind of inorganic filler for loading heterogeneous granular and preparation method thereof, to be prepared including inorganic material and metal salts of organic acids as raw material, the mass ratio of the inorganic material and metal salts of organic acids is 1~10 for the inorganic filler:1.Metal salts of organic acids is dissolved in solvent and forms solution, and inorganic material is added and mixed, evaporation solvent, is then heated so that inorganic filler of the metal salts of organic acids in inorganic material surface thermal cracking, i.e. formation load heterogeneous granular.The advantages of inorganic filler combination ceramic packing of the load heterogeneous granular of the present invention and conductive phase filling, compared to traditional ceramic packing and conductive phase filling, the inorganic filler of the structure can greatly improve the dielectric constant of polymer composites, while can guarantee that than relatively low dielectric loss.
Description
Technical field
The invention belongs to technical field of inorganic material, more particularly it relates to which a kind of load the inorganic of heterogeneous granular
Filler and preparation method thereof.
Background technology
Dielectric capacitor with high charge-discharge speed and high power density is in power system, impulse power electrical source etc.
Play key player.It is in recent years the generation information technology and industry of representative to electricity using Intelligent internet of things and wearable technology
The high integration of subsystem, miniaturization, the demand of lightweight and densification drive traditional ceramics dielectric substance to be thinned rapidly,
Leakage current sharply increases.Therefore find new high energy storage density dielectric substance and have become information functional material and microelectronics neck
The perspective study problem in domain.High energy storage density polymer composite dielectric material is because technique is simple, cost is cheap, Yi Yurou
Property matrix is compatible and turned into academic and industrial circle concern focus the advantages that the production of suitable large area.
In order to obtain the polymer composites of high energy storage density, method general at present includes：Firstth, according to effectively Jie
Matter is theoretical, and all kinds of high dielectric ceramic fillers are filled in polymeric matrix and construct the high dielectric polymer composite of 0-3 types.But
It is this that raising of the method for the dielectric property of composite for composite dielectric constant is regulated and controled by ceramic addition
Still limited (general dielectric constant ＜ 50), while the introducing of mass filler necessarily causes a large amount of defects, so as to reduce material
Compressive resistance.Secondth, conductive phase filling is added in polymeric matrix, it is normal to obtain higher dielectric using seep effect
Number, but dielectric loss skyrockets also with the increase of filler loading, therefore typically do not have practical value yet.
The content of the invention
Based on this, the defects of in order to overcome above-mentioned prior art, the inorganic of heterogeneous granular is loaded the invention provides a kind of
Filler and preparation method thereof.
In order to realize foregoing invention purpose, this invention takes following technical scheme：
A kind of inorganic filler for loading heterogeneous granular, the inorganic filler is by including inorganic material and organic acid metal
Salt is prepared for raw material, and the mass ratio of the inorganic material and metal salts of organic acids is 1~10:1.
In wherein some embodiments, the mass ratio of the inorganic material and metal salts of organic acids is 2.5~5:1.
In wherein some embodiments, the inorganic material is shaped as nanofiber, nano wire or particle.
In wherein some embodiments, the size of the nanofiber or nano wire is：20~1000 nanometers of diameter, length
100 nanometers~100 microns.
In wherein some embodiments, the size of the particle is：100 nanometers~10 microns of particle diameter.
In wherein some embodiments, the metal salts of organic acids is the acylate of conducting metal, such as：Copper, iron, nickel,
Magnesium, zinc, the gluconate of silver, the one or more of citrate and oxalates.
In wherein some embodiments, the inorganic material is barium titanate nano fiber, barium titanate nano line, rare earth doped
The BaTiO of element3Nanofiber and nano wire, CaCu 3 Ti 4 O nanofiber, CaCu 3 Ti 4 O nano wire, strontium titanates nanofiber,
Strontium titanates nano wire, barium strontium titanate nanofiber, barium strontium titanate nano wire, calcium titanate nanofiber, calcium titanate nano wire, metatitanic acid
Calcium barium nano wire, barium calcium titanate nanofiber, potassium-sodium niobate nano wire, zinc oxide nanowire, alumina nano fiber, aluminum oxide
Nano wire, boron nitride nano-tube, boron nitride nanometer line, beta-silicon nitride nanowire, nanometer silica line, aluminum nitride nanowire, two
TiOx nano fiber, titanium dioxide nano thread, silicon carbide nanometer line, nano cuprous oxide wire, cupric oxide nano line, titanium dioxide
Manganese nano wire, nickel oxide nanowires, zinc oxide nanowire, tin oxide nano-wire, tungsten oxide nano, zirconium oxide nano wire, oxygen
Change the one or more in Fe nanowire, ferrous oxide nano wire, metal nanometer line.
In wherein some embodiments, the metal nanometer line is in silver, copper, iron, aluminium, silicon, nickel, titanium, tungsten, stannum nanowire
One or more.
In wherein some embodiments, the rare earth element is in La, Ce, Pr, Nd, Sm, Eu, Ga, Dy, Er and Lu
It is one or more of.
Present invention also offers the preparation method of the inorganic filler of above-mentioned load heterogeneous granular, comprise the following steps：
The first step：Metal salts of organic acids is dissolved in solvent and forms solution, and inorganic material is added and mixes and fully stirs
Mix；
Second step：It is heated to 60~200 DEG C the solvent in mixture volatilizees, then continuous heating to metal salts of organic acids
Inorganic material surface thermal cracking, so as to formed load heterogeneous granular inorganic filler.
In wherein some embodiments, heating-up temperature described in step (2) is 60~180 DEG C.
The inorganic filler of the present invention comprises at least two kinds of different materials, and one of which is inorganic material, and one kind is metal
Or metal oxide nanoparticles, wherein metal or metal oxide nanoparticles is the side by thermal cracking metal salts of organic acids
Method is supported on the surface of inorganic material.Compared with prior art, the invention has the advantages that：
The advantages of inorganic filler combination ceramic packing of the load heterogeneous granular of the present invention and conductive phase filling, compared to tradition
Ceramic packing and conductive phase filling, the inorganic filler of the structure can greatly improve the dielectric constant of polymer composites, together
When can guarantee that than relatively low dielectric loss.
Brief description of the drawings
Fig. 1 is the cross-section structure of the bariumtitanatefiber inorganic filler of the obtained load nano-nickel oxide of the embodiment of the present invention 4
Figure.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below in conjunction with the accompanying drawings to the present invention
Embodiment be described in detail.Many details are elaborated in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.Below
Reagent or raw material used in embodiment, unless otherwise specified, derive from commercially available.
Embodiment 1
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：1 part of copper gluconate (metal salts of organic acids) is dissolved in 10 parts of water, forms solution, and by 20 parts
A diameter of 200 nanometers of barium titanate spheric granules (inorganic material), which adds, to be mixed and is sufficiently stirred；
Second step：After mixture filtering (not having to rinse), solid is directly placed into baking oven, being warming up to 180 DEG C will
Solvent volatilization in mixture, 6 hours are then incubated to copper gluconate in barium titanate spheric granules surface thermal cracking, so as to shape
Into the barium titanate nano filler of load Nanometer Copper (20 nanometers).
Embodiment 2
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：1 part of copper gluconate (metal salts of organic acids) is dissolved in 10 parts of water, forms solution, and by 20 parts
A diameter of 200 nanometers of barium titanate spheric granules (inorganic material), which adds, to be mixed and is sufficiently stirred；
Second step：After mixture filtering (not having to rinse), solid is directly placed into baking oven, being warming up to 180 DEG C will
In mixture solvent volatilization, then be incubated 12 hours to copper gluconate barium titanate spheric granules surface thermal cracking, so as to
Form the barium titanate nano filler of load Nanometer Copper (about 40 nanometers).
Embodiment 3
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：1 part of zinc gluconate (metal salts of organic acids) is dissolved in 10 parts of boiling water, forms solution, and by 20
The barium titanate spheric granules (inorganic material) of a diameter of 200 nanometers of part, which adds, to be mixed and is sufficiently stirred；
Second step：After mixture filtering (not having to rinse), solid is directly placed into baking oven, being warming up to 120 DEG C will
Solvent volatilization in mixture, 6 hours are then incubated to zinc gluconate in barium titanate spheric granules surface thermal cracking, so as to shape
Into the barium titanate nano filler of supported nano zinc oxide (about 20 nanometers).
Embodiment 4
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：5 parts of nickel oxalate dihydrates (metal salts of organic acids) are dissolved in 10 parts of certain density ammonia spirits, formed
Solution, and 20 parts of a diameter of 200 nanometers of bariumtitanatefibers (inorganic material) are added and mixes and is sufficiently stirred；
Second step：The mixture is directly placed into Muffle furnace, 200 DEG C is warming up to and the solvent in mixture volatilizees, and
Insulation 6 hours is to nickel oxalate dihydrate in barium titanate spheric granules surface thermal cracking (320~450 DEG C), so as to forming load nanometer
The barium titanate nano fiberfill of nickel oxide (about 20 nanometers) (shown in Fig. 1).
Embodiment 5
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：5 parts of aluminium citrates (metal salts of organic acids) are dissolved in 10 parts of certain density ammonia spirits, formed molten
Liquid, and 20 parts a diameter of 200 nanometers of CaCu 3 Ti 4 O fiber (inorganic material) is added and mixes and is sufficiently stirred；
Second step：The mixture is directly placed into Muffle furnace, 200 DEG C is warming up to and the solvent in mixture volatilizees, and
Insulation 6 hours is to nickel oxalate dihydrate in CaCu 3 Ti 4 O fiber surface thermal cracking (320~450 DEG C), so as to forming load nano oxygen
Change the CaCu 3 Ti 4 O nanofiber filler of aluminium (about 20 nanometers).
Embodiment 6
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：5 parts of nickel oxalate dihydrates (metal salts of organic acids) are dissolved in 10 parts of certain density ammonia spirits, formed
Solution, and 20 parts of a diameter of 200 nanometers of ball-aluminium oxides are added and mixes and is sufficiently stirred；
Second step：The mixture is directly placed into Muffle furnace, 150 DEG C is warming up to and the solvent in mixture volatilizees, and
Insulation (about 20 is received for 6 hours to nickel oxalate dihydrate in alumina powder surface thermal cracking, so as to form load nano-nickel oxide
Rice) alumina packing.
Embodiment 7
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：By basic nickel carbonate and citric acid (mol ratio 1:1.3) it is well mixed in aqueous, and in 60-
Stirred at 80 DEG C and be incubated 8 hours, form nickeliferous citrate sol
Second step：20 parts a diameter of 200 nanometers of barium strontium titanate nanofiber is taken to add in nickeliferous citrate sol
It is well mixed；
3rd step：The mixture is directly placed into Muffle furnace, 150 DEG C is warming up to and the solvent in mixture volatilizees, and
Insulation 6 hours is to nickeliferous citrate in barium strontium titanate nanofiber surface thermal cracking, so as to forming load nano-nickel oxide
The barium strontium titanate nanofiber filler of (about 20 nanometers).
Embodiment 8
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：By basic magnesium carbonate and citric acid (mol ratio 1:1.3) it is well mixed in aqueous, and in 60-
Stirred at 80 DEG C and be incubated 8 hours, form colloidal sol
Second step：Take 20 parts a diameter of 200 nanometers of barium strontium titanate nanofiber to add in 5 parts of colloidal sols to be well mixed；
3rd step：The mixture is directly placed into Muffle furnace, 150 DEG C is warming up to and the solvent in mixture volatilizees, and
Insulation is filled out for 6 hours to colloidal sol thermal cracking, so as to form the barium strontium titanate nanofiber of load nano magnesia (about 20 nanometers)
Material.
Embodiment 9
The preparation method of the inorganic filler of the load heterogeneous granular of the present embodiment, comprises the following steps：
The first step：1 part of copper gluconate (metal salts of organic acids) is dissolved in 10 parts of water, forms solution, and by 20 parts
A diameter of 200 nanometers of Titanium dioxide spherical particle (inorganic material), which adds, to be mixed and is sufficiently stirred；
Second step：After mixture filtering (not having to rinse), solid is directly placed into baking oven, being warming up to 180 DEG C will
In mixture solvent volatilization, then be incubated 6 hours to copper gluconate Titanium dioxide spherical particle surface thermal cracking, so as to
Form the nano titania filler of load Nanometer Copper (20 nanometers).
The inorganic filler that will be obtained in 10 grams of embodiment 1- embodiments 9, it is compound with 10 grams of epoxy resin respectively, formed compound
Material, tests its dielectric constant (dk) and dielectric loss tangent angle (df) result is as shown in table 1.
In order to compare, while also provide the ceramic packing filled polymer of different volumes percentage and conductive phase filling
The dielectric constant (dk) and dielectric loss tangent angle (df) result of the composite of filled polymer matrix, such as table 2 and the institute of table 3
Show.
The dielectric constant and dielectric loss of the Inorganic Fillers Filled polymeric matrix of the embodiment 1~9 of table 1
| Embodiment No. | 1 | 2 | 3 | 4 | 5 |
| DK(1KHz) | 132.3 | 154.6 | 127 | 291 | 349 |
| Df(1KHz) | 0.006 | 0.007 | 0.006 | 0.008 | 0.009 |
| 6 | 7 | 8 | 9 | ||
| DK(1KHz) | 512 | 364 | 151 | 124 | |
| Df(1KHz) | 0.012 | 0.01 | 0.007 | 0.005 |
The ceramic packing filled polymer matrix of table 2 composition composite dielectric constant and dielectric loss
The dielectric constant and dielectric loss of the composite of the conductive phase filling filled polymer matrix composition of table 3
Understood with reference to the result of table 1~3, for the epoxy composite material of pure ceramic filler, even in 70% (weight ratio)
Loading under, the dielectric constant of composite also is difficult to breakthrough 50.Although the polymer composites of conductive phase filling filling
Higher dielectric constant can be obtained in percolation threshold annex, but loss is very big, it is difficult to practical.And the present invention
The advantages of loading the inorganic filler combination ceramic packing of heterogeneous granular and conductive phase filling, compared to traditional ceramic packing and conduction
Phase filling, the inorganic filler of the structure can greatly improve the dielectric constant of polymer composites, while can guarantee that than relatively low
Dielectric loss.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of inorganic filler for loading heterogeneous granular, it is characterised in that the inorganic filler is with including inorganic material, Yi Jiyou
Machine acid metal salt is prepared for raw material, and the mass ratio of the inorganic material and metal salts of organic acids is 1~10:1.
2. the inorganic filler of load heterogeneous granular according to claim 1, it is characterised in that the inorganic material and organic
The mass ratio of acid metal salt is 2.5~5:1.
3. the inorganic filler of load heterogeneous granular according to claim 1 or 2, it is characterised in that the inorganic material
It is shaped as nanofiber, nano wire or particle.
4. the inorganic filler of load heterogeneous granular according to claim 3, it is characterised in that the nanofiber or nanometer
The size of line is：20~1000 nanometers of diameter, 100 nanometers~100 microns of length, the size of the particle are：100 nanometers of particle diameter
~10 microns.
5. the inorganic filler of load heterogeneous granular according to claim 1, it is characterised in that the metal salts of organic acids is
Copper, iron, nickel, magnesium, zinc, the gluconate of silver, the one or more of citrate and oxalates.
6. the inorganic filler of load heterogeneous granular according to claim 1, it is characterised in that the inorganic material is metatitanic acid
Barium nanofiber, barium titanate nano line, the BaTiO of rare earth doped element3Nanofiber and nano wire, CaCu 3 Ti 4 O Nanowire
Dimension, CaCu 3 Ti 4 O nano wire, strontium titanates nanofiber, strontium titanates nano wire, barium strontium titanate nanofiber, barium strontium titanate nanometer
Line, calcium titanate nanofiber, calcium titanate nano wire, barium calcium titanate nano wire, barium calcium titanate nanofiber, potassium-sodium niobate nanometer
Line, zinc oxide nanowire, alumina nano fiber, alumina nanowires, boron nitride nano-tube, boron nitride nanometer line, silicon nitride
Nano wire, nanometer silica line, aluminum nitride nanowire, titanium dioxide nanofiber, titanium dioxide nano thread, nanometer silicon carbide
Line, nano cuprous oxide wire, cupric oxide nano line, manganese dioxide nanowire, nickel oxide nanowires, zinc oxide nanowire, oxidation
In stannum nanowire, tungsten oxide nano, zirconium oxide nano wire, iron oxide nano-wire, ferrous oxide nano wire, metal nanometer line
It is one or more of.
7. the inorganic filler of load heterogeneous granular according to claim 6, it is characterised in that the metal nanometer line is
One or more in silver, copper, iron, aluminium, silicon, nickel, titanium, tungsten, stannum nanowire.
8. it is according to claim 6 load heterogeneous granular inorganic filler, it is characterised in that the rare earth element be La,
One or more in Ce, Pr, Nd, Sm, Eu, Ga, Dy, Er and Lu.
9. the preparation method of the inorganic filler of the load heterogeneous granular described in any one of claim 1~8, it is characterised in that bag
Include following steps：
The first step：Metal salts of organic acids is dissolved in solvent and forms solution, and inorganic material is added and mixes and is sufficiently stirred；
Second step：It is heated to 60~200 DEG C the solvent in mixture volatilizees, then continuous heating to metal salts of organic acids is in nothing
Machine material surface thermal cracking, so as to formed load heterogeneous granular inorganic filler.
10. the preparation method of the inorganic filler of load heterogeneous granular according to claim 9, it is characterised in that step (2)
Described in heating-up temperature be 60~180 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114429865A (en) * | 2022-01-10 | 2022-05-03 | 重庆文理学院 | Preparation method of nickel wire/ferric oxide/manganese dioxide composite fiber |
| CN115028932A (en) * | 2022-06-24 | 2022-09-09 | 郑荣妹 | Preparation method of organic polymer composite ceramic material |
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| CN114429865A (en) * | 2022-01-10 | 2022-05-03 | 重庆文理学院 | Preparation method of nickel wire/ferric oxide/manganese dioxide composite fiber |
| CN114429865B (en) * | 2022-01-10 | 2023-10-13 | 重庆文理学院 | Preparation method of nickel wire/ferric oxide/manganese dioxide composite fiber |
| CN115028932A (en) * | 2022-06-24 | 2022-09-09 | 郑荣妹 | Preparation method of organic polymer composite ceramic material |
| CN115028932B (en) * | 2022-06-24 | 2024-03-22 | 郑荣妹 | Preparation method of organic polymer composite ceramic material |
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