CN112266617A - High-filling type modified ceramic composite material and preparation method thereof - Google Patents
High-filling type modified ceramic composite material and preparation method thereof Download PDFInfo
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- CN112266617A CN112266617A CN202010993728.4A CN202010993728A CN112266617A CN 112266617 A CN112266617 A CN 112266617A CN 202010993728 A CN202010993728 A CN 202010993728A CN 112266617 A CN112266617 A CN 112266617A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a high-filling modified ceramic composite material which comprises the following components in parts by weight: liquid resin, 1000 portions of modified heat-conducting filler powder and 2500 portions of modified heat-conducting filler powder, 0.01 portion to 10 portions of ceramic powder treating agent, wherein the modified heat-conducting filler powder is prepared by adopting the following method: adding ceramic filler powder into a high-speed dispersion machine, dispersing a ceramic powder treating agent on the ceramic filler powder in an atomizing and spraying mode, fully mixing, and then treating at the temperature of 100-130 ℃ for 20min to prepare modified heat-conducting filler powder, wherein the prepared modified heat-conducting filler powder needs to be mixed with liquid resin within 5 h. The invention adopts a secondary coating modification mode, namely, the modified powder is subjected to secondary wet coating modification by using the treating agent on the basis of the traditional dry-method modified ceramic powder, so that the powder is completely coated, and the compatibility with liquid resin is improved, thereby preparing the high-filling modified ceramic liquid composite material.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a high-filling type modified ceramic composite material and a preparation method thereof.
Background
With the rapid development of modern electronic communication industry, especially after the 5G era, the requirement of the electronic industry for heat dissipation is higher and higher, which means that more and more heat-conducting powder materials need to be added into resin, the processability, mechanical property, and flow property of the product are poorer and poorer as the powder content is increased. Therefore, there is a need to develop a composite material and a method for preparing the same to overcome the above-mentioned problems.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a high-filling type modified ceramic composite filler and a preparation method thereof.
The invention is realized by the following technical scheme:
the high-filling modified ceramic composite material is characterized by comprising the following components: liquid resin, 1000 portions of modified heat-conducting filler powder and 2500 portions of modified heat-conducting filler powder, and 0.01 portion to 10 portions of ceramic powder treating agent, wherein the total amount of the liquid resin and the ceramic powder treating agent is 100 portions,
the modified heat-conducting filler powder is prepared by the following method: adding ceramic filler powder into a high-speed dispersion machine, dispersing at the dispersion speed of 1500-plus-4000 rmp, dispersing a ceramic powder treating agent on the ceramic filler powder in an atomization spraying mode under high shear, fully mixing and treating for 5-10min, and then treating at the temperature of 100-plus-130 ℃ for 20min to prepare modified heat-conducting filler powder, wherein the prepared modified heat-conducting filler powder needs to be mixed with liquid resin within 5 h.
The high-filling modified ceramic composite material is characterized in that in the preparation method of the modified heat-conducting filler powder, the weight ratio of the ceramic filler powder to the ceramic powder treating agent is 1000: 0.01-10.
The high-filling modified ceramic composite material is characterized in that the ceramic filler powder comprises any two or three of spherical heat-conducting powder with the particle size of 0.2-2 microns, spherical heat-conducting powder with the particle size of 5-20 microns and spherical heat-conducting powder with the particle size of 40-120 microns.
The high-filling type modified ceramic composite material is characterized in that the ceramic filler powder is one or a mixture of any more of alumina powder, aluminum nitride powder, silicon nitride powder, boron nitride powder and silicon carbide powder.
The high-filling modified ceramic composite material is characterized in that the ceramic filler powder is alumina powder.
The high-filling modified ceramic composite material is characterized in that the ceramic powder treating agent is one or a mixture of any more of alkoxy silane monomers, alkoxy silane oligomers, monoalkoxy titanate, aluminate and zirconate.
The high-filling modified ceramic composite material is characterized in that the liquid resin is silicone resin, epoxy resin, polyurethane or acrylic resin.
The high-filling modified ceramic composite material is characterized in that the viscosity of the liquid resin is in a range of 10-1000 mPa.S, and preferably 30-500 mPa.S.
The preparation method of the high-filling modified ceramic composite material is characterized by comprising the following steps:
adding liquid resin with the viscosity of 10-1000 mPa.S and a ceramic powder treating agent into a planetary machine, uniformly mixing, adding modified heat-conducting filler powder, uniformly mixing at room temperature, heating to the material temperature of 100-150 ℃, mixing for 10min-4h, and reducing the temperature for 10min-4h under the condition that the vacuum degree is more than 0.095 MPa.
The preparation method of the high-filling modified ceramic composite material is characterized in that the total usage amount of the liquid resin and the ceramic powder treating agent is 100 parts, the usage amount of the ceramic powder treating agent is 0.01-10 parts, and the usage amount of the modified heat-conducting filler powder is 1000-2500 parts.
The invention adopts a secondary coating modification mode, namely, the modified powder is subjected to secondary wet coating modification by using the treating agent on the basis of the traditional dry-method modified ceramic powder, so that the powder is completely coated, and the compatibility with liquid resin is improved, thereby preparing the high-filling modified ceramic liquid composite material. The powder processing technology endows the material with excellent physical properties, and can be used for preparing high-heat-conduction high-fluidity encapsulating materials, high-heat-conduction interface materials and the like.
Detailed Description
The present invention will be described in further detail with reference to specific examples below in order to better understand the present invention.
Example 1
Modification of heat-conducting filler powder: adding 3000 parts of spherical alumina powder with different particle size ratios into a high-speed dispersion machine, wherein the dispersion speed is 2000rmp, dispersing 5 parts of ceramic powder treating agent solution on the alumina powder in an atomization spraying mode under high shear, fully mixing for 10min, and then treating at 110 ℃ for 20min to obtain the modified ceramic filler powder. The composite preparation phase is immediately entered.
Preparing a composite material: adding 98 parts of liquid resin with the viscosity of 50 mPa.S and 2 parts of ceramic powder treating agent into a planetary machine, uniformly mixing, adding 2000 parts of modified heat-conducting filler powder, uniformly mixing the composite material at room temperature, heating to the material temperature of 140 ℃, mixing for 1 hour, and reducing the temperature for 1 hour under the condition that the vacuum degree is more than 0.095 MPa.
Example 2
Modification of heat-conducting filler powder: adding 3000 parts of spherical alumina powder with different particle size ratios into a high-speed dispersion machine, wherein the dispersion speed is 2000rmp, dispersing 5 parts of ceramic powder treating agent solution on the alumina powder in an atomization spraying mode under high shear, fully mixing for 10min, and then treating at 110 ℃ for 20min to obtain the modified ceramic filler powder. Placing for 2h and entering a composite material preparation stage.
Preparing a composite material: adding 98 parts of liquid resin with the viscosity of 50 mPa.S and 2 parts of ceramic powder treating agent into a planetary machine, uniformly mixing, adding 2000 parts of modified heat-conducting filler powder, uniformly mixing the composite material at room temperature, heating to the material temperature of 140 ℃, mixing for 1 hour, and reducing the temperature for 1 hour under the condition that the vacuum degree is more than 0.095 MPa.
Example 3
Modifying ceramic filler powder: adding 3000 parts of spherical alumina powder with different particle size ratios into a high-speed dispersion machine, wherein the dispersion speed is 2000rmp, dispersing 5 parts of ceramic powder treating agent solution on the alumina powder in an atomization spraying mode under high shear, fully mixing for 10min, and then treating at 110 ℃ for 20min to obtain the modified ceramic filler powder. Placing for 5h and entering a composite material preparation stage.
Preparing a composite material: adding 98 parts of liquid resin with the viscosity of 50 mPa.S and 2 parts of ceramic powder treating agent into a planetary machine, uniformly mixing, adding 2000 parts of modified heat-conducting filler powder, uniformly mixing the composite material at room temperature, heating to the material temperature of 140 ℃, mixing for 1 hour, and reducing the temperature for 1 hour under the condition that the vacuum degree is more than 0.095 MPa.
Comparative example 1
Adding 98 parts of liquid resin with the viscosity of 50 mPa.S and 2 parts of ceramic powder treating agent into a planetary machine, uniformly mixing, adding 2000 parts of ceramic filler powder, uniformly mixing the composite material at room temperature, heating to the material temperature of 140 ℃, mixing for 1 hour, and reducing the vacuum degree for 1 hour under the condition that the vacuum degree is more than 0.095 Mpa.
Comparative example 2
Adding 100 parts of liquid resin with the viscosity of 50 mPa.S into a planetary machine, adding 2000 parts of ceramic filler powder, uniformly mixing the composite material at room temperature, heating to the material temperature of 140 ℃, mixing for 1 hour, and reducing for 1 hour under the vacuum degree of more than 0.095 Mpa.
For the products prepared in the above examples and comparative examples, the viscosity of the composites was measured according to ASTM D2196-2015, and the results are shown in Table 1.
TABLE 1
| Item | Example 1 | Examples2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Viscosity, cps | 16.3 ten thousand | 17.3 ten thousand | 20.7 ten thousand | 50.1 ten thousand | Packaged material |
| Fluidity of the resin | Good taste | Good taste | Good taste | Very poor | No fluidity |
The above description is only a preferred embodiment of the present invention, and any construction, modification and principle equivalent changes, equivalents and improvements made within the scope of the present invention are included in the protection scope of the present invention.
Claims (10)
1. The high-filling modified ceramic composite material is characterized by comprising the following components: liquid resin, 1000 portions of modified heat-conducting filler powder and 2500 portions of modified heat-conducting filler powder, and 0.01 portion to 10 portions of ceramic powder treating agent, wherein the total amount of the liquid resin and the ceramic powder treating agent is 100 portions,
the modified heat-conducting filler powder is prepared by the following method: adding ceramic filler powder into a high-speed dispersion machine, dispersing at the dispersion speed of 1500-plus-4000 rmp, dispersing a ceramic powder treating agent on the ceramic filler powder in an atomization spraying mode under high shear, fully mixing and treating for 5-10min, and then treating at the temperature of 100-plus-130 ℃ for 20min to prepare modified heat-conducting filler powder, wherein the prepared modified heat-conducting filler powder needs to be mixed with liquid resin within 5 h.
2. The highly filled modified ceramic composite material according to claim 1, wherein the modified heat conductive filler powder is prepared by using the ceramic filler powder and the ceramic powder treating agent in a weight ratio of 1000: 0.01-10.
3. The high-filling type modified ceramic composite material as claimed in claim 1, wherein the ceramic filler powder comprises any two or three of spherical heat-conducting powder with a particle size of 0.2-2 μm, spherical heat-conducting powder with a particle size of 5-20 μm, and spherical heat-conducting powder with a particle size of 40-120 μm.
4. The high-filling type modified ceramic composite material according to claim 3, wherein the ceramic filler powder is one or a mixture of any more of alumina powder, aluminum nitride powder, silicon nitride powder, boron nitride powder and silicon carbide powder.
5. The highly filled modified ceramic composite material according to claim 4, wherein the ceramic filler powder is alumina powder.
6. The high-filling type modified ceramic composite material as claimed in claim 1, wherein the ceramic powder treating agent is one or a mixture of any more of alkoxysilane monomer, alkoxysilane oligomer, monoalkoxytitanate, aluminate and zirconate.
7. The highly filled modified ceramic composite material according to claim 1, wherein the liquid resin is selected from silicone resins, epoxy resins, polyurethanes, or acrylic resins.
8. High-filled modified ceramic composite according to claim 1, characterized in that the liquid resin viscosity ranges between 10 and 1000 mpa.s, preferably between 30 and 500 mpa.s.
9. The preparation method of the high-filling modified ceramic composite material as claimed in claim 1 is characterized by comprising the following steps:
adding liquid resin with the viscosity of 10-1000 mPa.S and a ceramic powder treating agent into a planetary machine, uniformly mixing, adding modified heat-conducting filler powder, uniformly mixing at room temperature, heating to the material temperature of 100-150 ℃, mixing for 10min-4h, and reducing the temperature for 10min-4h under the condition that the vacuum degree is more than 0.095 MPa.
10. The method of claim 9, wherein the total amount of the liquid resin and the ceramic powder treating agent is 100 parts, the amount of the ceramic powder treating agent is 0.01-10 parts, and the amount of the modified heat-conducting filler powder is 1000-2500 parts.
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