CN110803940B - Preparation method of composite ceramic filler - Google Patents
Preparation method of composite ceramic filler Download PDFInfo
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- CN110803940B CN110803940B CN201911214213.3A CN201911214213A CN110803940B CN 110803940 B CN110803940 B CN 110803940B CN 201911214213 A CN201911214213 A CN 201911214213A CN 110803940 B CN110803940 B CN 110803940B
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Abstract
The invention belongs to the technical field of ceramic fillers, and particularly relates to a preparation method of a composite ceramic filler. The preparation method of the composite ceramic filler comprises the following steps: s1) putting the treated ceramic filler into mixing equipment, stirring for 3-7 min, then injecting the coupling agent into the mixing equipment in a spraying mode, stirring for 10-15 min, heating to 150 ℃, and stirring for 10-15 min to obtain a blend A; s2) mixing and stirring the blend A, the fluorine-containing resin emulsion and the water in the step S1 for 10-30 min to obtain a blend B; s3) pouring the blend B obtained in the step S2 into a tray, baking for 5-60 min at 80-120 ℃, heating to 250-300 ℃, and baking for 5-60 min to obtain powder; s4) sieving the powder obtained in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 5-10 min to obtain the composite ceramic filler. The composite ceramic filler prepared by the invention has a three-layer structure, greatly improves the miscibility with polytetrafluoroethylene, and has better interface binding property.
Description
Technical Field
The invention belongs to the technical field of ceramic fillers, and particularly relates to a preparation method of a composite ceramic filler.
Background
The fluororesin is a thermoplastic resin containing fluorine atoms in a molecular structure, has extremely low surface activity, is difficult to blend with other materials, and greatly limits the application of the fluororesin.
At present, the comprehensive performance of the fluororesin is improved by blending inorganic particles and the fluororesin, so that the strength, the hardness, the wear resistance, the thermal conductivity and the like of the fluororesin are improved. Therefore, how to disperse the inorganic particles in the fluororesin organic phase with high uniformity is the key to blending. The prior art includes a dry dispersion method and a wet dispersion method, wherein the dry dispersion method mainly comprises mechanical high-speed stirring, and the wet dispersion method mainly comprises adding inorganic particles into PTFE concentrated dispersion liquid and carrying out mechanical stirring or ultrasonic treatment. The above two methods are used for blending inorganic particles with a fluororesin, but these blends have poor bonding interfaces because the proportion of the inorganic particles in the blend is generally less than 30%, and when the amount of the inorganic particles is continuously increased, there is a defect that the inorganic particles are difficult to be uniformly dispersed or the porosity in the article is increased, which in turn decreases the properties of the blend.
Chinese patent CN106671517A discloses a fluorine-containing resin and compound ceramic filler composition and a high-frequency copper-clad plate manufactured by the same, and specifically discloses a composition comprising: mixing fluorine-containing resin; secondly, premixing a plurality of ceramic fillers with different proportions, particle sizes and morphologies by using a solvent; (III) mixing the fluorine-containing resin with the ceramic filler; fourthly, the glass cloth dipped with the composition of the fluorine-containing resin and the ceramic filler is dried, baked and sintered to prepare dipped cloth; preparing copper foil coated and sintered by fluororesin and compound ceramic filler; and (VI) laminating the high-frequency copper clad laminate. However, the mixing of the fluorine-containing resin and the ceramic filler in the patent is still similar to that of a wet dispersion method, the addition amount of the ceramic filler is limited, and the interface bonding of the blend cannot be improved well.
Disclosure of Invention
The invention aims to provide a preparation method of a composite ceramic filler, the composite ceramic filler prepared by the invention has a three-layer structure, the miscibility with polytetrafluoroethylene is greatly improved, and the composite ceramic filler has better interface bonding property; the sheet obtained by blending the composite ceramic filler and the polytetrafluoroethylene has the advantages of uniform size, low water absorption, high bending strength and good stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a composite ceramic filler comprises the following steps:
s1) putting the treated ceramic filler into mixing equipment, stirring for 3-7 min, then injecting the coupling agent into the mixing equipment in a spraying mode, stirring for 10-15 min, heating to 150 ℃, and stirring for 10-15 min to obtain a blend A;
s2) mixing and stirring the blend A, the fluorine-containing resin emulsion and the water in the step S1 for 10-30 min to obtain a blend B;
s3) pouring the blend B obtained in the step S2 into a tray, baking for 5-60 min at 80-120 ℃, heating to 250-300 ℃, and baking for 5-60 min to obtain powder;
s4) sieving the powder obtained in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 5-10 min to obtain the composite ceramic filler.
In the invention, the treated ceramic filler is coated with the coupling agent, the coupling agent can be promoted to be completely coated on the surface of the ceramic filler by controlling the temperature to be 150 ℃, when the temperature is lower than 150 ℃, the condensation dehydration reaction of the coupling agent is slow, and when the temperature is higher than 150 ℃, the coupling agent can be evaporated or undergoes a self-condensation reaction. The blend a obtained by coating the ceramic filler with the coupling agent was coated with a fluorine-containing resin emulsion, thereby obtaining a composite ceramic filler having a three-layer structure (ceramic filler + coupling agent layer + fluorine resin layer).
Further, the mass ratio of the ceramic filler treated in the step S1 to the coupling agent is 1000: (5-15).
Further, the treatment method of the treated ceramic filler comprises the following steps: taking the ceramic filler, the seaweed glycolipid fatty acid monoester and the ethanol for ultrasonic dispersion for 2-5 hours, and then drying for 8-10 hours under vacuum. The volume percentage of the ethanol is 25-50%, including 25%, 30%, 35%, 40%, 45% and 50%.
In the invention, the specific mechanism of the method is still analyzed, namely the dispersibility of the ceramic filler is possibly improved, the ceramic filler is more coated by the coupling agent, the ceramic filler is possibly activated, the ceramic filler is more coated by the coupling agent, and the dispersibility and uniformity of the coated composite ceramic filler and polytetrafluoroethylene are possibly improved.
Further, the mass ratio of the ceramic filler to the seaweed glycolipid fatty acid monoester to the ethanol is 1 (0.025-0.05): 25.
further, the ceramic filler comprises at least one of silicon dioxide, titanium dioxide, barium titanate, glass fiber yarn, graphite, aluminum oxide and silicon micropowder.
Further, the coupling agent comprises at least one of silane coupling agent, titanate coupling agent and zirconate coupling agent, and comprises tridecafluorooctane, namely triethoxysilane (F8261), phenyltrimethoxysilane (Z6124) and 3-aminopropyltriethoxysilane (KH 550).
Further, in the step S2, the mass ratio of the blend a, the fluorine-containing resin emulsion, and the water is (75 to 55): (5-25): (20-40).
Further, the fluorine-containing resin emulsion comprises at least one of polytetrafluoroethylene emulsion, polyperfluoroethylene propylene emulsion and polyperfluoroalkyl ether emulsion.
The invention provides a sheet material made of composite ceramic filler, which is prepared from any one of the composite ceramic filler and polytetrafluoroethylene according to the mass ratio of 1: 1, preparing the composition.
The invention also provides a preparation method of the sheet, which comprises the following steps: mixing the composite ceramic filler and polytetrafluoroethylene, molding into a sheet with the thickness of 1.0mm, and sintering at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler.
In the invention, the composite ceramic filler and the polytetrafluoroethylene are mixed by sectional treatment, so that the phenomenon that the performance of the sheet is changed sharply due to overlarge temperature difference is prevented.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the invention carries out surface coating treatment on the fluororesin, so that the surface of the ceramic filler is coated with a complete fluororesin layer, and the composite ceramic filler with a three-layer structure is obtained, thereby greatly improving the blending performance of the composite ceramic filler and the polytetrafluoroethylene, ensuring that the interface bonding of the composite ceramic filler and the polytetrafluoroethylene is good, and increasing the filling amount of the composite ceramic filler.
(2) The sheet obtained by blending the composite ceramic filler and the polytetrafluoroethylene has uniform size, lower water absorption and higher bending strength, and the comprehensive performance of the sheet is integrally improved.
(3) The sheet material obtained by blending the composite ceramic filler and the polytetrafluoroethylene has better dimensional stability and thermal stability.
Drawings
FIG. 1 is a schematic structural view of the composite ceramic packing of the present invention.
Wherein, 1-ceramic filler, 2-coupling agent layer and 3-fluorine resin layer.
Detailed Description
The present invention will be described in further detail with reference to the following examples. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Example 1 composite ceramic Filler
The method comprises the following steps:
s1) putting 1000g of the treated ceramic filler into a mixing device, stirring for 5min, then injecting 10g of coupling agent (coupling agent KH550) into the mixing device in a spray mode, stirring for 10min, heating to 150 ℃, and stirring for 10min to obtain a blend A;
s2) mixing and stirring 100g of the blend A obtained in the step S1, 10g of polytetrafluoroethylene emulsion (purchased from Dajin company D210, 60%) and 50g of water for 25min to obtain a blend B;
s3) pouring the blend B obtained in the step S2 into a tray, baking the blend B for 30min at 80 ℃, heating the blend B to 250 ℃, and baking the blend B for 15min to obtain powder;
s4), sieving the powder in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 5min to obtain the composite ceramic filler.
The treatment method of the treated ceramic filler comprises the following steps: 1000g of fine silica powder (particle size range D of 10 μm), 25g of trehalose fatty acid monoester and 25kg of 30 wt% ethanol were ultrasonically dispersed for 3.5h, and then dried under vacuum for 10 h. (micropowder of silica: trehalose fatty acid monoester: ethanol ═ 1: 0.025: 25)
Example 2 composite ceramic Filler
The method comprises the following steps:
s1) putting 1000g of the treated ceramic filler into a mixing device, stirring for 5min, then injecting 15g of coupling agent (Z6124+ KH550) into the mixing device in a spray form, stirring for 10min, heating to 150 ℃, and stirring for 10min to obtain a blend A;
s2) mixing and stirring 100g of the blend A obtained in the step S1, 10g of polytetrafluoroethylene emulsion (purchased from Dajin company D210, 60%) and 50g of water for 25min to obtain a blend B;
s3) pouring the blend B obtained in the step S2 into a tray, baking for 30min at 100 ℃, heating to 270 ℃, and baking for 15min to obtain powder;
s4), sieving the powder in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 7min to obtain the composite ceramic filler.
The treatment method of the treated ceramic filler comprises the following steps: 1000g of glass fiber yarn (particle size range D of 10 μm), 30g of trehalose fatty acid monoester and 25kg of 30 wt% ethanol were taken for ultrasonic dispersion for 3.5h, and then dried under vacuum for 10 h. (micropowder of silica: trehalose fatty acid monoester: ethanol ═ 1: 0.03: 25)
Example 3A composite ceramic Filler
The method comprises the following steps:
s1) putting 1000g of the treated ceramic filler into a mixing device, stirring for 5min, then injecting 10g of coupling agent (coupling agent KH550) into the mixing device in a spray form, stirring for 15min, heating to 150 ℃, and stirring for 15min to obtain a blend A;
s2) mixing and stirring 100g of the blend A obtained in the step S1, 20g of polytetrafluoroethylene emulsion (purchased from Dajin company D210, 60%) and 60g of water for 25min to obtain a blend B;
s3) pouring the blend B obtained in the step S2 into a tray, baking for 30min at 120 ℃, heating to 300 ℃, and baking for 10min to obtain powder;
s4), sieving the powder in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 7.5min to obtain the composite ceramic filler.
The treatment method of the treated ceramic filler comprises the following steps: 1000g of fine silica powder (particle size range D of 10 μm), 25g of trehalose fatty acid monoester and 25kg of 25 wt% ethanol were ultrasonically dispersed for 3 hours, and then dried under vacuum for 10 hours. (micropowder of silica: trehalose fatty acid monoester: ethanol ═ 1: 0.025: 25)
Example 4A sheet made with a composite ceramic Filler
The method comprises the following steps:
the composite ceramic filler of example 1 and polytetrafluoroethylene (powder) were mixed in the following ratio 1: 1, die pressing into a sheet with the thickness of 1.0mm, and then sintering at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler.
Example 5A sheet made with a composite ceramic Filler
The method comprises the following steps:
the composite ceramic filler of example 2 and polytetrafluoroethylene (powder) were mixed in the following ratio 1: 1, die pressing into a sheet with the thickness of 1.0mm, and then sintering at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler.
Example 6A sheet made with a composite ceramic Filler
The method comprises the following steps:
the composite ceramic filler of example 3 and polytetrafluoroethylene (powder) were mixed in the following ratio 1: 1, die pressing into a sheet with the thickness of 1.0mm, and then sintering at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler.
Comparative example 1 sheet made with composite ceramic filler
100g of ceramic filler (silica powder (particle size range D is 10 μm)), 1g of coupling agent (coupling agent KH550), 20g of polytetrafluoroethylene emulsion and 121g of polytetrafluoroethylene (powder) are mixed, molded into a sheet of 1.0mm, and then sintered at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain a sheet made of the composite ceramic filler.
The difference compared to example 4 is that all the raw materials are mixed directly.
Comparative example 2 sheet made with composite ceramic Filler
The preparation method of the composite ceramic filler comprises the following steps:
s1) mixing and stirring 100g of the treated ceramic filler, 10g of polytetrafluoroethylene emulsion (purchased from Dajin company D210, 60%) and 50g of water for 25min to obtain a blend B;
s2) pouring the blend B obtained in the step S2 into a tray, baking the blend B for 30min at 80 ℃, heating the blend B to 250 ℃, and baking the blend B for 15min to obtain powder;
s3), sieving the powder in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 5min to obtain the composite ceramic filler.
The treatment method of the treated ceramic filler comprises the following steps: 1000g of fine silica powder (particle size D of 10 μm), 25g of trehalose fatty acid monoester and 25kg of ethanol were ultrasonically dispersed for 3.5 hours, and then dried under vacuum for 10 hours.
The preparation method of the sheet material made of the composite ceramic filler comprises the following steps:
mixing the composite ceramic filler and polytetrafluoroethylene (powder) according to the weight ratio of 1: 1, die pressing into a sheet with the thickness of 1.0mm, and then sintering at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler.
The difference from example 4 is that step S1 of example 1 is not performed.
Comparative example 3 sheet made with composite ceramic Filler
The preparation method of the composite ceramic filler comprises the following steps:
s1) putting 1000g of the treated ceramic filler into a mixing device, stirring for 5min, then injecting 10g of coupling agent (coupling agent KH550) into the mixing device in a spray mode, stirring for 10min, heating to 150 ℃, and stirring for 10min to obtain a blend A;
s2) pouring the blend B obtained in the step S2 into a tray, baking the blend B for 30min at 80 ℃, heating the blend B to 250 ℃, and baking the blend B for 15min to obtain powder;
s3), sieving the powder in the step S2 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 5min to obtain the composite ceramic filler.
The treatment method of the treated ceramic filler comprises the following steps: 1000g of fine silica powder (particle size D of 10 μm), 25g of trehalose fatty acid monoester and 25kg of ethanol were ultrasonically dispersed for 3.5 hours, and then dried under vacuum for 10 hours.
The preparation method of the sheet material made of the composite ceramic filler comprises the following steps:
mixing the composite ceramic filler and polytetrafluoroethylene (powder) according to the weight ratio of 1: 1, die pressing into a sheet with the thickness of 1.0mm, and then sintering at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler.
The difference from example 4 is that step S2 of example 1 is not performed.
Comparative example 4 a sheet made with a composite ceramic filler
The method comprises the following steps:
s1) putting 1000g of ceramic filler (silicon powder (the particle size range D is 10 mu m)) into a mixing device, stirring for 5min, then injecting 10g of coupling agent (KH550) into the mixing device in a spray form, stirring for 10min, heating to 150 ℃, and stirring for 10min to obtain a blend A;
s2) mixing and stirring 100g of the blend A obtained in the step S1, 10g of polytetrafluoroethylene emulsion (purchased from Dajin company D210, 60%) and 50g of water for 25min to obtain a blend B;
s3) pouring the blend B obtained in the step S2 into a tray, baking the blend B for 30min at 80 ℃, heating the blend B to 250 ℃, and baking the blend B for 15min to obtain powder;
s4), sieving the powder in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 5min to obtain the composite ceramic filler.
Mixing the composite ceramic filler and polytetrafluoroethylene (powder) according to the weight ratio of 1: 1, die pressing into a sheet with the thickness of 1.0mm, and then sintering at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler.
The difference compared to example 1 is that the ceramic filler was not treated.
Comparative example 5 sheet made with composite ceramic Filler
Compared with the example 4, the difference is that the treated ceramic filler in the composite ceramic filler, the silicon powder: sucrose ester: water 1: 0.025: 25, other parameters are the same as in example 4.
Comparative example 6A sheet made of a composite ceramic Filler
Compared with the example 4, the difference is that the treated ceramic filler in the composite ceramic filler, the silicon powder: sucrose ester: ethanol ═ 1: 0.025: 25, other parameters are the same as in example 4.
Comparative example 7 sheet made of composite ceramic Filler
Compared with the example 4, the difference is that the treated ceramic filler in the composite ceramic filler, the silicon powder: trehalose glycolipid fatty acid monoester: water 1: 0.025: 25, other parameters are the same as in example 4.
Test I, sheet appearance detection
The test method comprises the following steps: a center line is drawn on the surface of the sheet, the center line is divided into four points on average, the thicknesses of the sheet at the four points are measured, and the average value is calculated.
TABLE 1 sheet thickness calculation results
As can be seen from Table 1, the sheet thicknesses of examples 4-6 were close to 1.0mm, indicating that the sheet thicknesses were relatively uniform. While the sheet thicknesses of comparative examples 1-6 differ significantly from 1.0 mm.
Test II, sheet Performance test
TABLE 2 sheet Performance test results
| Group of | Density (g/cm)3) | Flexural strength (Mpa) | Water absorption (%) |
| Example 4 | 2.335 | 50 | 0.01 |
| Example 5 | 2.331 | 50 | 0.02 |
| Example 6 | 2.323 | 49 | 0.01 |
| Comparative example 1 | 2.211 | 15 | 1.05 |
| Comparative example 2 | 2.305 | 30 | 0.21 |
| Comparative example 3 | 2.295 | 35 | 0.13 |
| Comparative example 4 | 2.273 | 35 | 0.15 |
| Comparative example 5 | 2.288 | 38 | 0.12 |
| Comparative example 6 | 2.329 | 49 | 0.03 |
| Comparative example 7 | 2.309 | 39 | 0.11 |
When the density of the sheet is high, the bending strength is high, the water absorption is low, and the interface bonding performance of the composite ceramic filler and the polytetrafluoroethylene blend between the inner parts of the sheets is good. As can be seen from Table 2, the interfacial bonding property of the composite ceramic filler and the polytetrafluoroethylene blend between the interiors of the sheets in the examples 4-6 is good, so that the sheets have high bending strength and low water absorption, wherein the example 4 is the best example of the invention.
Compared with example 4, comparative example 1 is a direct mixing mode, and the obtained sheet has low density and high absorption rate, which indicates that the composite ceramic filler and the polytetrafluoroethylene are not mixed in the sheet, namely, gaps are formed, and water can enter the sheet through the gaps. When a step of the manufacturing method is eliminated, such as comparative example 2 and comparative example 3, the composite ceramic filler and polytetrafluoroethylene are not mixed in the sheet. Comparative example 5 the ceramic filler was treated with silica micropowder: sucrose ester: water 1: 0.025: the treatment of 25 can suitably improve the mixing of the composite ceramic filler and polytetrafluoroethylene in the sheet, but the improvement is not so large. When comparative example 6 is used for treating the ceramic filler, the silica powder: sucrose ester: ethanol ═ 1: 0.025: 25 treatment, further improving the mixing of the composite ceramic filler and the polytetrafluoroethylene in the sheet, which is similar to that of the example 4.
Test III, stability test
3.1 dimensional stability test: the test was carried out according to the method of IPC-TM-650-2.4.4.
3.2 thermal stability test: the sheet to be tested was heated to 250 ℃ in a thermomechanical analyzer (TMA) and held at that temperature for 10 minutes, and then the thermal expansion coefficient between 240 ℃ and 100 ℃ was determined at a cooling rate of 5 ℃/min.
Table 3 stability test results
As can be seen from Table 3, when the composite ceramic filler and polytetrafluoroethylene were mixed in the sheet material and the interfacial adhesiveness was good, the thermal expansion coefficient was low and the dimensional stability was good. On the contrary, the thermal expansion coefficient is high and the dimensional stability is not good. However, the inventors found that comparative example 6 was similar to example 4 in the performance test, whereas a large difference was found from example 4 in the dimensional stability test and the thermal stability test, particularly that the thermal expansion coefficient thereof was much larger than that of example 4.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. The preparation method of the composite ceramic filler is characterized by comprising the following steps of:
s1) putting the treated ceramic filler into mixing equipment, stirring for 3-7 min, then injecting the coupling agent into the mixing equipment in a spraying mode, stirring for 10-15 min, heating to 150 ℃, and stirring for 10-15 min to obtain a blend A;
s2) mixing and stirring the blend A, the fluorine-containing resin emulsion and the water in the step S1 for 10-30 min to obtain a blend B;
s3) pouring the blend B obtained in the step S2 into a tray, baking for 5-60 min at 80-120 ℃, heating to 250-300 ℃, and baking for 5-60 min to obtain powder;
s4) sieving the powder obtained in the step S3 by a 110-mesh vibrating screen, and sintering at 380 ℃ for 5-10 min to obtain the composite ceramic filler;
the treatment method of the treated ceramic filler comprises the following steps: taking the ceramic filler, the seaweed glycolipid fatty acid monoester and ethanol, carrying out ultrasonic dispersion for 2-5 h, and drying for 8-10 h under vacuum;
the mass ratio of the ceramic filler to the seaweed glycolipid fatty acid monoester to the ethanol is 1 (0.025-0.05): 25.
2. the method for preparing the composite ceramic filler according to claim 1, wherein the mass ratio of the ceramic filler treated in the step S1 to the coupling agent is 1000: (5-15).
3. The method for preparing the composite ceramic filler according to claim 1, wherein the ceramic filler comprises at least one of silica, titanium dioxide, barium titanate, glass fiber yarn, graphite, aluminum oxide and silica micropowder.
4. The method for preparing the composite ceramic filler according to claim 1 or 2, wherein the coupling agent comprises at least one of a silane coupling agent, a titanate coupling agent, and a zirconate coupling agent.
5. The preparation method of the composite ceramic filler according to claim 1, wherein the mass ratio of the blend A, the fluorine-containing resin emulsion and the water in the step S2 is (75-55): (5-25): (20-40).
6. The method of claim 1 or 5, wherein the fluorine-containing resin emulsion comprises at least one of polytetrafluoroethylene emulsion, polyperfluoroethylpropylene emulsion, and polyperfluoroalkylether emulsion.
7. A sheet material made of a composite ceramic filler is characterized in that the composite ceramic filler is prepared by the preparation method of any one of claims 1 to 6, and the mass ratio of the composite ceramic filler to polytetrafluoroethylene is 1: 1, preparing the composition.
8. A method of making a sheet, comprising the steps of: mixing a composite ceramic filler and polytetrafluoroethylene, molding the mixture into a sheet with the thickness of 1.0mm, and sintering the sheet at 100 ℃ for 30min, 300 ℃ for 30min and 380 ℃ for 120min to obtain the sheet made of the composite ceramic filler, wherein the composite ceramic filler is prepared by the preparation method of any one of claims 1 to 6.
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| CN103102627A (en) * | 2013-01-23 | 2013-05-15 | 广东生益科技股份有限公司 | PTFE (polytetrafluoroethylene) base material with high filler content and preparation and application thereof |
| CN109456051A (en) * | 2018-11-28 | 2019-03-12 | 电子科技大学 | A kind of preparation method of polytetrafluoroethylene (PTFE) based composite ceramic material |
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