CN103554910B - A kind of artificial dielectric material and preparation method thereof - Google Patents
A kind of artificial dielectric material and preparation method thereof Download PDFInfo
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- CN103554910B CN103554910B CN201310517207.1A CN201310517207A CN103554910B CN 103554910 B CN103554910 B CN 103554910B CN 201310517207 A CN201310517207 A CN 201310517207A CN 103554910 B CN103554910 B CN 103554910B
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- 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
- C08K9/10—Encapsulated ingredients
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- 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
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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- 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
- C08K2201/003—Additives being defined by their diameter
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Abstract
The present invention relates to a kind of artificial dielectric material and preparation method thereof.This material includes thermosetting resin, and titanium dioxide/hollow glass micropearl compounded mix, and wherein compounded mix and thermosetting resin mass ratio are 1:2~1:9.The method is: preparation TiO2Colloidal sol, immerses TiO by hollow glass micropearl2In colloidal sol and be sufficiently mixed, after filtering out unnecessary colloidal sol, obtain the hollow glass micropearl after dipping cladding;Then the hollow glass micropearl after described dipping cladding is dried and calcination process, obtains TiO2The hollow glass micropearl of cladding;Again by described TiO2The hollow glass micropearl of cladding is mixed homogeneously with thermosetting resin, obtains artificial dielectric material after curing molding.Titanium dioxide is plated in hollow glass micropearl surface and prepares density and the uniform artificial dielectric material of dielectric properties by the present invention, solves density and dielectric properties skewness problem that traditional artificial dielectric material brings.
Description
Technical field
The invention belongs to wave-penetrating composite material technical field, be specifically related to a kind of radome artificial dielectric material and preparation thereof
Method.
Background technology
Artificial dielectric material is the sandwich material of a kind of key in radome, and it has, and dielectric constant is adjustable, dielectric loss
The feature such as low, density is little, mechanical property is excellent, technology stability is good.Artificial dielectric material preparation method is usually at resin matrix
The titanium dioxide of middle interpolation high-k, low-density hollow glass micropearl, then stirring mixes.Resin density be 1.1~
1.2g/cm3, titanium dioxide density is 4.2~4.3g/cm3, and hollow glass micropearl density is 0.2~0.6g/cm3, due to titanium dioxide
Titanium density is relatively big, easily sinks, and hollow glass micropearl density is less, easily floats in resin matrix in resin matrix,
Cause artificial dielectric material density and the dielectric properties skewness of preparation, thus have a strong impact on the wave of radome
Energy.
Summary of the invention
It is an object of the invention to provide a kind of new artificial dielectric material and preparation method thereof, solve traditional artificial dielectric material
Density that preparation method is brought and dielectric properties skewness problem.
The principle of the present invention is, by sol-gel process, titanium dioxide is plated in hollow glass micropearl surface, controls hollow glass micro-
Bead surface content of titanium dioxide, can prepare density with the close titanium dioxide/hollow glass micropearl complex function filler of resin density,
Due to this packing density identical with resin density (or close), do not have after being added in resin matrix because density difference is made
The floating become and sinkage, thus prepare density and the uniform artificial dielectric material of dielectric properties.
The technical solution used in the present invention is as follows:
A kind of artificial dielectric material, this material includes thermosetting resin, and titanium dioxide/hollow glass micropearl compounded mix, its
Middle compounded mix and thermosetting resin mass ratio are 1:2~1:9.
Further, the one during described thermosetting resin can be cyanate ester resin, bimaleimide resin, epoxy resin.
Further, the particle diameter of described hollow glass micropearl is preferably 30 μm~100 μm, and wall thickness is preferably 1 μm~3 μm.
The preparation method of a kind of artificial dielectric material, method specifically comprises the following steps that
1) TiO is prepared2Colloidal sol, immerses TiO by hollow glass micropearl2In colloidal sol and be sufficiently mixed, after filtering out unnecessary colloidal sol
Obtain the hollow glass micropearl after dipping cladding;
2) hollow glass micropearl after described dipping cladding is dried and calcination process, obtains TiO2The hollow glass of cladding
Microballon;
3) by described TiO2The hollow glass micropearl of cladding is mixed homogeneously with thermosetting resin, obtains artificial dielectric after curing molding
Material.
Further, TiO described in step 1)2The preparation method of colloidal sol is: weigh a certain amount of butyl titanate ([Ti (OBu)4])
And prepare dehydrated alcohol (EtOH) deionized water solution of certain volume, butyl titanate is dissolved in the anhydrous second of 60%~70%
In alcohol deionized water solution, it is subsequently adding inhibitor acyl acetone (AcAc), under the conditions of strong agitation, is slowly added dropwise nitric acid
(HNO3) and remaining 30%~40% dehydrated alcohol deionized water solution, thus reduce reaction severe degree, obtain stable
TiO2Colloidal sol.
Further, step 1) prepares described TiO2The ratio of the amount of the material of each material of colloidal sol is:
[Ti(OBu)4]:EtOH:H20:HN03: AcAc=1:(18~23): (3~5): (0.1~0.2): (0.5~0.7).
Further, step 2) hollow glass micropearl is immersed TiO2Time in colloidal sol, TiO2Butyl titanate in colloidal sol is with hollow
The mass ratio of glass microsphere is 2~4:1.
Further, step 3) use baking oven carry out described dried, temperature is 100 DEG C~130 DEG C, the time be 30min~
50min。
Further, step 3) use Muffle furnace carry out described calcination process, temperature is 600 DEG C~650 DEG C, the time be 30min~
50min。
Further, TiO in step 3)2The hollow glass micropearl of cladding and thermosetting resin mass ratio are 1:2~1:9.
Titanium dioxide is plated in hollow glass micropearl surface by sol-gel process by the present invention, by controlling hollow glass micropearl surface
Content of titanium dioxide, can prepare density and the uniform artificial dielectric material of dielectric properties, solve traditional artificial dielectric material
The problem of the antenna house wave transparent poor performance that material exists due to density and dielectric properties skewness.
Accompanying drawing explanation
Fig. 1 is the flow chart of steps of the preparation method of the artificial dielectric material of the present invention.
Fig. 2 is scanning electron microscope (SEM) photo of the preparation method of the artificial dielectric material that embodiment prepares.
Detailed description of the invention
Below by specific embodiments and the drawings, the present invention is described in detail.
Fig. 1 is the flow chart of steps of the preparation method of the artificial dielectric material of the present invention, first prepares TiO2Colloidal sol, by hollow glass
Glass microballon immerses TiO2In colloidal sol and be sufficiently mixed, after filtering out unnecessary colloidal sol, obtain the hollow glass micropearl after dipping cladding;
Then the hollow glass micropearl after described dipping cladding is dried and calcination process, obtains TiO2The hollow glass micropearl of cladding;
Again by described TiO2The hollow glass micropearl of cladding is mixed homogeneously with thermosetting resin, obtains artificial dielectric material after curing molding.
Embodiment 1:
The artificial dielectric material of the present embodiment is made up of cyanate ester resin and titanium dioxide/hollow glass micropearl.Its preparation method is:
The first step: preparation TiO2Colloidal sol
270ml dehydrated alcohol (EtOH) and 2ml deionized water mixing and stirring are made into mixed solution, accurately weigh 39ml
Butyl titanate [Ti (OBu)4] join in the above-mentioned mixed solution of 181ml, it is subsequently added 13ml inhibitor acyl acetone
(AcAc), under the conditions of strong agitation, it is slowly added dropwise the nitric acid (HNO of 0.7g3) and the dehydrated alcohol of remaining 91ml go from
Sub-water mixed solution, obtains stable TiO2Colloidal sol.
Second step: by hollow glass micropearl and TiO2Colloidal sol mixes, and is dried and calcination process
Weigh 8g hollow glass micropearl, glass microsphere particle diameter 100 μm, wall thickness 3 μm, the glass microsphere weighed is immersed TiO2
In colloidal sol, stirring makes microballon and colloidal sol be sufficiently mixed, and is then filtered off unnecessary colloidal sol.Micro-for the hollow glass after dipping cladding
Pearl is put into and is dried 30min in the baking oven of temperature 100 DEG C.Microballon after drying is again at the Muffle kiln roasting 30min of 600 DEG C, clearly
Wash dry, obtain TiO2The hollow glass micropearl of cladding, the TiO of cladding2Thickness 1.5 μm.
3rd step: with mixed with resin curing molding
The TiO that the first step is obtained2The hollow glass micropearl of cladding is mixed homogeneously with 92g cyanate ester resin resin agitating, 170 DEG C
Heating 2h, then obtains artificial dielectric material after 200 DEG C of heating 2h curing moldings.
Fig. 2 is scanning electron microscope (SEM) photo of the artificial dielectric material that the present embodiment prepares, wherein sub-circular portion
It is divided into TiO2The hollow glass micropearl of cladding, compares and is evenly distributed in resin.
The density of the artificial dielectric material that the present embodiment obtains is 1.14g/cm3~1.17g/cm3, and dielectric constant is 2.42~2.47,
Dielectric loss is 0.007.
Embodiment 2:
The artificial dielectric material of the present embodiment is made up of bimaleimide resin and titanium dioxide/hollow glass micropearl.Its preparation side
Method is:
The first step: preparation TiO2Colloidal sol
300ml dehydrated alcohol (EtOH) and 3ml deionized water mixing and stirring are made into mixed solution, accurately weigh 39ml
Butyl titanate [Ti (OBu)4] join in the above-mentioned mixed solution of 202ml, it is subsequently added 16ml inhibitor acyl acetone
(AcAc), under the conditions of strong agitation, it is slowly added dropwise the nitric acid (HNO of 1.05g3) and the dehydrated alcohol of remaining 101ml go
Ionized water mixed solution, obtains stable TiO2Colloidal sol.
Second step: by hollow glass micropearl and TiO2Colloidal sol mixes, and is dried and calcination process
Weigh 6g hollow glass micropearl, glass microsphere particle diameter 65 μm, wall thickness 2 μm, the glass microsphere weighed is immersed TiO2
In colloidal sol, stirring makes microballon and colloidal sol be sufficiently mixed, and is then filtered off unnecessary colloidal sol.Micro-for the hollow glass after dipping cladding
Pearl is put into and is dried 40min in the baking oven of temperature 120 DEG C.Microballon after drying is again at the Muffle kiln roasting 40min of 625 DEG C, clearly
Wash dry, obtain TiO2The hollow glass micropearl of cladding, the TiO of cladding2Thickness 1.0 μm.
3rd step: the TiO that the first step is obtained2The hollow glass micropearl of cladding mixes with the stirring of 108g bimaleimide resin
Uniformly, 180 DEG C of heating 2h, then obtain artificial dielectric material after 200 DEG C of heating 2h curing moldings.
The density of the artificial dielectric material that the present embodiment obtains is 1.18g/cm3~1.22g/cm3, and dielectric constant is 2.73~2.76,
Dielectric loss is 0.013.
Embodiment 3:
The artificial dielectric material of the present embodiment is made up of epoxy resin and titanium dioxide/hollow glass micropearl.Its preparation method is:
The first step: preparation TiO2Colloidal sol
345ml dehydrated alcohol (EtOH) and 3.3ml deionized water mixing and stirring are made into mixed solution, accurately weigh 39ml
Butyl titanate [Ti (OBu)4] join in the above-mentioned mixed solution of 232.3ml, it is subsequently added 18.2ml inhibitor acyl acetone
(AcAc), under the conditions of strong agitation, it is slowly added dropwise the nitric acid (HNO of 1.4g3) and the dehydrated alcohol of remaining 116ml go
Ionized water mixed solution, obtains stable TiO2Colloidal sol.
Second step: by hollow glass micropearl and TiO2Colloidal sol mixes, and is dried and calcination process
4g hollow glass micropearl is immersed TiO2In colloidal sol, glass microsphere particle diameter 30 μm, wall thickness 1 μm, stirring makes microballon and molten
Glue is sufficiently mixed, and is then filtered off unnecessary colloidal sol.Hollow glass micropearl after dipping cladding is put into the baking oven of temperature 130 DEG C
In be dried 50min.Microballon after drying at the Muffle kiln roasting 50min of 650 DEG C, cleaning-drying, obtains TiO again2Cladding
Hollow glass micropearl, the TiO of cladding2Thickness 0.5 μm.
3rd step: the TiO that the first step is obtained2The hollow glass micropearl of cladding and 76g epoxy resin, 7.6g butyl glycidyl
Ether, 9.8g triethylene tetramine are uniformly mixed, and obtain artificial dielectric material after cold curing molding.
The density of the artificial dielectric material that the present embodiment obtains is 1.24g/cm3~1.28g/cm3, dielectric constant is 2.82~2.85,
Dielectric loss is 0.018.
Although disclosing the specific embodiments and the drawings of the present invention for the purpose of illustration, its object is to help and understanding present disclosure
And implement according to this, but it will be appreciated by those skilled in the art that: without departing from the present invention and appended claim spirit and
In the range of, various replacements, to change and modifications be all possible.The present invention should not be limited to this specification most preferred embodiment and accompanying drawing
Disclosure of that, the scope of protection of present invention defines in the range of standard with claims.
Claims (6)
1. an artificial dielectric material, it is characterised in that include thermosetting resin, and titanium dioxide/hollow glass micropearl compounded mix, wherein compounded mix and thermosetting resin mass ratio are 1:2~1:9, and the particle diameter of hollow glass micropearl is 30 μm~100 μm, and wall thickness is 1 μm~3 μm;Described artificial dielectric material is adopted and is prepared from the following method:
1) TiO is prepared2Colloidal sol, immerses TiO by hollow glass micropearl2In colloidal sol and be sufficiently mixed, after filtering out unnecessary colloidal sol, obtain the hollow glass micropearl after dipping cladding;Described TiO2The method of colloidal sol is: weigh the dehydrated alcohol deionized water solution of a certain amount of butyl titanate and certain volume, butyl titanate is dissolved in the dehydrated alcohol deionized water solution of 60%~70%, it is subsequently adding inhibitor acetylacetone,2,4-pentanedione, under the conditions of strong agitation, it is slowly added dropwise nitric acid and remaining 30%~40% dehydrated alcohol deionized water solution, obtains stable TiO2Colloidal sol;Prepare described TiO2The ratio of the amount of the material of each material of colloidal sol is: [Ti (OBu)4]:EtOH:H20:HN03: AcAc=1:(18~23): (3~5): (0.1~0.2): (0.5~0.7);
2) hollow glass micropearl after described dipping cladding is dried and calcination process, obtains TiO2The hollow glass micropearl of cladding;Using baking oven to carry out described dried, temperature is 100 DEG C~130 DEG C, and the time is 30min~50min;Using Muffle furnace to carry out described calcination process, temperature is 600 DEG C~650 DEG C, and the time is 30min~50min;
3) by described TiO2The hollow glass micropearl of cladding is mixed homogeneously with thermosetting resin, obtains artificial dielectric material after curing molding.
2. artificial dielectric material as claimed in claim 1, it is characterised in that: described thermosetting resin is the one in cyanate ester resin, bimaleimide resin, epoxy resin.
3. a preparation method for artificial dielectric material described in claim 1, its step includes:
1) TiO is prepared2Colloidal sol, immerses TiO by hollow glass micropearl2In colloidal sol and be sufficiently mixed, after filtering out unnecessary colloidal sol, obtain the hollow glass micropearl after dipping cladding;Described TiO2The method of colloidal sol is: weigh the dehydrated alcohol deionized water solution of a certain amount of butyl titanate and certain volume, butyl titanate is dissolved in the dehydrated alcohol deionized water solution of 60%~70%, it is subsequently adding inhibitor acetylacetone,2,4-pentanedione, under the conditions of strong agitation, it is slowly added dropwise nitric acid and remaining 30%~40% dehydrated alcohol deionized water solution, obtains stable TiO2Colloidal sol;Prepare described TiO2The ratio of the amount of the material of each material of colloidal sol is: [Ti (OBu)4]:EtOH:H20:HN03: AcAc=1:(18~23): (3~5): (0.1~0.2): (0.5~0.7);
2) hollow glass micropearl after described dipping cladding is dried and calcination process, obtains TiO2The hollow glass micropearl of cladding;Using baking oven to carry out described dried, temperature is 100 DEG C~130 DEG C, and the time is 30min~50min;Using Muffle furnace to carry out described calcination process, temperature is 600 DEG C~650 DEG C, and the time is 30min~50min;
3) by described TiO2The hollow glass micropearl of cladding is mixed homogeneously with thermosetting resin, obtains artificial dielectric material after curing molding.
4. method as claimed in claim 3, it is characterised in that: step 1) hollow glass micropearl is immersed TiO2Time in colloidal sol, TiO2Butyl titanate in colloidal sol is 2~4:1 with the mass ratio of hollow glass micro-ball.
5. method as claimed in claim 3, it is characterised in that: step 3) in TiO2The hollow glass micropearl of cladding and thermosetting resin mass ratio are 1:2~1:9.
6. method as claimed in claim 5, it is characterised in that: described thermosetting resin is the one in cyanate ester resin, bimaleimide resin, epoxy resin;The particle diameter of described hollow glass micropearl is 30 μm~100 μm, and wall thickness is 1 μm~3 μm.
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CN105820602B (en) * | 2016-03-24 | 2018-05-04 | 青岛科技大学 | A kind of preparation method of nano-titanium dioxide modified hollow glass micropearl |
CN106380977A (en) * | 2016-08-31 | 2017-02-08 | 广东慧信环保有限公司 | Hydrophobic heat-insulation coating and preparation method therof |
CN106433225A (en) * | 2016-09-22 | 2017-02-22 | 深圳大学 | Surface-coated modified hollow glass beads and preparation method thereof |
CN106497199A (en) * | 2016-10-25 | 2017-03-15 | 浙江大学 | A kind of reflective insulation nano modification quartz sand and preparation method thereof |
CN108614241A (en) * | 2018-05-03 | 2018-10-02 | 合肥光博量子科技有限公司 | A kind of fire-retardant dustproof rain cover for protecting radar |
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