CN117550906A - High-strength insulating ceramic and preparation method and application thereof - Google Patents
High-strength insulating ceramic and preparation method and application thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 116
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 70
- 239000003365 glass fiber Substances 0.000 claims abstract description 66
- 238000002156 mixing Methods 0.000 claims abstract description 42
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 37
- 239000000945 filler Substances 0.000 claims abstract description 36
- 239000010445 mica Substances 0.000 claims abstract description 35
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 35
- 238000005245 sintering Methods 0.000 claims abstract description 35
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 230
- 238000003756 stirring Methods 0.000 claims description 70
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- 235000019441 ethanol Nutrition 0.000 claims description 66
- 239000007788 liquid Substances 0.000 claims description 52
- 239000006185 dispersion Substances 0.000 claims description 50
- 239000007822 coupling agent Substances 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 39
- 239000010453 quartz Substances 0.000 claims description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 35
- 239000000725 suspension Substances 0.000 claims description 32
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 25
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 239000011812 mixed powder Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 13
- 238000007873 sieving Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000009775 high-speed stirring Methods 0.000 claims description 3
- 239000012212 insulator Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 9
- 238000009413 insulation Methods 0.000 abstract description 9
- 230000004048 modification Effects 0.000 abstract description 8
- 238000012986 modification Methods 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 230000032683 aging Effects 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 3
- 239000011810 insulating material Substances 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000243 solution Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000012767 functional filler Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Abstract
The invention relates to high-strength insulating ceramic, a preparation method and application thereof, belongs to the technical field of ceramic materials, and has the characteristics of high insulativity, wear resistance, corrosion resistance and aging resistance. According to the invention, the zirconium-containing ceramic fiber with high temperature resistance and insulation property is subjected to blending modification with the glass fiber subjected to surface treatment in a filler blending modification mode, so that the ceramic has higher-strength insulation property and aging resistance after blending modification, and mica powder and aluminum oxide with wear-resistant insulation property are added in the preparation process of the high-strength insulating material, so that the insulation property, wear resistance and corrosion resistance of the prepared ceramic material are improved under the action of a sintering aid, and the application range of the ceramic material in electronic products is enlarged.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and relates to high-strength insulating ceramic, and a preparation method and application thereof.
Background
The traditional concept of ceramics refers to all artificial industrial products which are prepared from inorganic nonmetallic minerals such as clay and the like, and comprise various products which are prepared by mixing, forming and calcining clay or a mixture containing clay. Modern ceramics are also called novel ceramics, fine ceramics or special ceramics, are commonly used as non-silicate chemical raw materials or artificial synthetic raw materials, such as oxide (alumina, zirconia, titania and the like) and non-oxide (silicon nitride, boron carbide and the like) manufacture, and the existing ceramics are of various types and are widely used in the chemical industry field, the electronic field and the like. Among them, alumina ceramics and barium titanate have excellent physicochemical properties, which are one of materials commonly used in the electrical field. In the prior art, the insulation resistance value prepared by alumina is low, the insulation performance is not high, and the durability of the product is reduced.
Therefore, developing an insulating ceramic material with high insulation, high temperature resistance, wear resistance, corrosion resistance and aging resistance is an important direction in the current electronic field.
Disclosure of Invention
The invention aims to provide high-strength insulating ceramic, a preparation method and application thereof, and the high-strength insulating ceramic has the characteristics of high insulativity, wear resistance, corrosion resistance and aging resistance.
The aim of the invention can be achieved by the following technical scheme:
the high-strength insulating ceramic comprises the following raw materials in parts by weight:
30-45 parts of mixed modified filler, 10-15 parts of mica powder, 2-7 parts of quartz powder, 5-10 parts of alumina, 5-10 parts of silicon nitride, 1-5 parts of sintering aid and 30-50 parts of deionized water.
As a preferable technical scheme of the invention, the mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering auxiliary agent is CaO-MgF in a ternary auxiliary agent 2 -SiO 2 、BaO-ZrO 2 -SiO 2 、MgO-SiO 2 -ZrO 2 And BaO-ZrO 2 -at least one of CaO.
As a preferable technical scheme of the invention, the preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol, and performing ultrasonic dispersion to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent into absolute ethyl alcohol, adding a neutralizing agent, adjusting the pH value, and magnetically stirring for 20min to obtain coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion into the glass fiber ethanol dispersion, uniformly stirring while adding, ultrasonically dispersing, heating and stirring for 3 hours, and ending the reaction to obtain a surface modified glass fiber ethanol suspension;
(4) Dispersing zirconium-containing ceramic fibers into a sodium hydroxide aqueous solution, performing ultrasonic dispersion, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing under the conditions of constant temperature and high-speed stirring, stirring for reaction after uniform mixing, performing ultrasonic dispersion for 15-20min, heating and stirring for 30-40min, and filtering to obtain the mixed modified filler.
As a preferable technical scheme of the invention, in the step (1), the ultrasonic dispersion time is 15-20min.
As a preferable technical scheme of the invention, in the step (2), the neutralizer is 10-20% sodium hydroxide aqueous solution, and the pH value is adjusted to 7-8.
As a preferable technical scheme of the invention, in the step (3), the ultrasonic dispersion time is 30-40min.
As a preferable technical scheme of the invention, in the step (4), the ultrasonic dispersion time is 20-30min.
As a preferable technical scheme of the invention, in the step (5), the constant temperature is 70-80 ℃, the stirring speed of high-speed stirring is 500-700r/min, and the stirring reaction time is 2-3h.
As a preferable technical scheme of the invention, the preparation method of the high-strength insulating ceramic comprises the following steps:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving, adding mixed modified filler and sintering aid, adding deionized water, heating, ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating in a specified time, and preserving heat at the temperature; and then calcining at high temperature, preserving heat to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
As a preferable technical scheme of the invention, in the step S1, the number of the sieving screens is 300-400 meshes, and the temperature rise is 150-200 ℃.
As a preferable technical scheme of the invention, in the step S2, the specified time is 30-50min, the temperature rise range is 180-200 ℃ and the heat preservation time is 30-40min.
As a preferable technical scheme of the invention, in the step S2, the calcining temperature is 1300-1400 ℃ and the heat preservation time is 2-4h.
The invention has the beneficial effects that:
the high-strength insulating ceramic prepared by the invention utilizes the way of blending modification of the zirconium-containing ceramic fiber with insulating property and the glass fiber after surface treatment to carry out blending modification, and the zirconium-containing ceramic fiber and the glass fiber are added as functional filler after blending modification, so that the prepared ceramic material has the characteristics of higher-strength insulation, higher-temperature resistance and higher ageing resistance. And quartz powder, mica powder, silicon nitride and aluminum oxide are added in the preparation process of the high-strength insulating material, the quartz powder, the mica powder and the silicon nitride have high insulativity, wear resistance and corrosion resistance, the aluminum oxide has extremely strong high-temperature resistance, and various raw materials increase the insulativity, the wear resistance and the corrosion resistance of the prepared ceramic material under the synergistic effect of sintering aids, meanwhile, the product can keep higher smoothness for a long time, has higher temperature resistance, prolongs the service life of the product and has low replacement cost, so that the application of the ceramic material in electronic products is enlarged.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description of the specific embodiments, features and effects according to the present invention is given by way of examples.
Example 1
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
30 parts by weight of mixed modified filler, 15 parts by weight of mica powder, 5 parts by weight of quartz powder, 5 parts by weight of alumina, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid is CaO-MgF in a ternary aid 2 -SiO 2 。
The preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol (the weight ratio of the glass fiber to the absolute ethyl alcohol is 1:3), and performing ultrasonic dispersion for 15min to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent KH-550 into absolute ethyl alcohol (the coupling agent KH-550 and the absolute ethyl alcohol are mixed according to the weight ratio of 1:5), simultaneously adding a 10% sodium hydroxide aqueous solution, adjusting the pH value of the solution to 7.5, and magnetically stirring for 20min to obtain a coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion liquid into the glass fiber ethanol dispersion liquid (the volume ratio of the coupling agent ethanol dispersion liquid to the glass fiber ethanol dispersion liquid is 1:2), stirring uniformly while adding, performing ultrasonic dispersion for 30min, heating and stirring for 3h, and ending the reaction to obtain a surface modified glass fiber ethanol suspension liquid;
(4) Dispersing zirconium-containing ceramic fibers into a 10% sodium hydroxide aqueous solution (the weight ratio of the zirconium-containing ceramic fibers to the 10% sodium hydroxide aqueous solution is 1:4), performing ultrasonic dispersion for 20min, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing at the constant temperature of 80 ℃ and the stirring speed of 600r/min, stirring for 3h after uniform mixing, performing ultrasonic dispersion for 20min, heating and stirring at the temperature of 100 ℃ for 40min, and filtering to obtain the mixed modified filler.
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding mixed modified filler and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Example 2
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
35 parts by weight of mixed modified filler, 15 parts by weight of mica powder, 5 parts by weight of quartz powder, 7 parts by weight of alumina, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid isBaO-ZrO in ternary assistants 2 -SiO 2 。
The preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol (the weight ratio of the glass fiber to the absolute ethyl alcohol is 1:3), and performing ultrasonic dispersion for 15min to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent KH-550 into absolute ethyl alcohol (the coupling agent KH-550 and the absolute ethyl alcohol are mixed according to the weight ratio of 1:5), simultaneously adding a 10% sodium hydroxide aqueous solution, adjusting the pH value of the solution to 7.5, and magnetically stirring for 20min to obtain a coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion liquid into the glass fiber ethanol dispersion liquid (the volume ratio of the coupling agent ethanol dispersion liquid to the glass fiber ethanol dispersion liquid is 1:2), stirring uniformly while adding, performing ultrasonic dispersion for 30min, heating and stirring for 3h, and ending the reaction to obtain a surface modified glass fiber ethanol suspension liquid;
(4) Dispersing zirconium-containing ceramic fibers into a 10% sodium hydroxide aqueous solution (the weight ratio of the zirconium-containing ceramic fibers to the 10% sodium hydroxide aqueous solution is 1:4), performing ultrasonic dispersion for 20min, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing at the constant temperature of 80 ℃ and the stirring speed of 600r/min, stirring for 3h after uniform mixing, performing ultrasonic dispersion for 20min, heating and stirring at the temperature of 100 ℃ for 40min, and filtering to obtain the mixed modified filler.
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding mixed modified filler and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Example 3
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
40 parts by weight of mixed modified filler, 15 parts by weight of mica powder, 5 parts by weight of quartz powder, 8 parts by weight of alumina, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid is MgO-SiO in ternary aids 2 -ZrO 2 。
The preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol (the weight ratio of the glass fiber to the absolute ethyl alcohol is 1:3), and performing ultrasonic dispersion for 15min to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent KH-550 into absolute ethyl alcohol (the coupling agent KH-550 and the absolute ethyl alcohol are mixed according to the weight ratio of 1:5), simultaneously adding a 10% sodium hydroxide aqueous solution, adjusting the pH value of the solution to 7.5, and magnetically stirring for 20min to obtain a coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion liquid into the glass fiber ethanol dispersion liquid (the volume ratio of the coupling agent ethanol dispersion liquid to the glass fiber ethanol dispersion liquid is 1:2), stirring uniformly while adding, performing ultrasonic dispersion for 30min, heating and stirring for 3h, and ending the reaction to obtain a surface modified glass fiber ethanol suspension liquid;
(4) Dispersing zirconium-containing ceramic fibers into a 10% sodium hydroxide aqueous solution (the weight ratio of the zirconium-containing ceramic fibers to the 10% sodium hydroxide aqueous solution is 1:4), performing ultrasonic dispersion for 20min, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing at the constant temperature of 80 ℃ and the stirring speed of 600r/min, stirring for 3h after uniform mixing, performing ultrasonic dispersion for 20min, heating and stirring at the temperature of 100 ℃ for 40min, and filtering to obtain the mixed modified filler.
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding mixed modified filler and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Example 4
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
45 parts by weight of mixed modified filler, 15 parts by weight of mica powder, 5 parts by weight of quartz powder, 10 parts by weight of alumina, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid is BaO-ZrO in a ternary aid 2 -CaO。
The preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol (the weight ratio of the glass fiber to the absolute ethyl alcohol is 1:3), and performing ultrasonic dispersion for 15min to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent KH-550 into absolute ethyl alcohol (the coupling agent KH-550 and the absolute ethyl alcohol are mixed according to the weight ratio of 1:5), simultaneously adding a 10% sodium hydroxide aqueous solution, adjusting the pH value of the solution to 7.5, and magnetically stirring for 20min to obtain a coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion liquid into the glass fiber ethanol dispersion liquid (the volume ratio of the coupling agent ethanol dispersion liquid to the glass fiber ethanol dispersion liquid is 1:2), stirring uniformly while adding, performing ultrasonic dispersion for 30min, heating and stirring for 3h, and ending the reaction to obtain a surface modified glass fiber ethanol suspension liquid;
(4) Dispersing zirconium-containing ceramic fibers into a 10% sodium hydroxide aqueous solution (the weight ratio of the zirconium-containing ceramic fibers to the 10% sodium hydroxide aqueous solution is 1:4), performing ultrasonic dispersion for 20min, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing at the constant temperature of 80 ℃ and the stirring speed of 600r/min, stirring for 3h after uniform mixing, performing ultrasonic dispersion for 20min, heating and stirring at the temperature of 100 ℃ for 40min, and filtering to obtain the mixed modified filler.
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding mixed modified filler and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Comparative example 1
Comparative example 1 differs from example 1 in that the mixed modified filler was replaced with surface modified glass fiber.
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
30 parts by weight of surface modified glass fiber, 15 parts by weight of mica powder, 5 parts by weight of quartz powder, 5 parts by weight of alumina, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid is CaO-MgF in a ternary aid 2 -SiO 2 。
The preparation method of the surface modified glass fiber comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol (the weight ratio of the glass fiber to the absolute ethyl alcohol is 1:3), and performing ultrasonic dispersion for 15min to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent KH-550 into absolute ethyl alcohol (the coupling agent KH-550 and the absolute ethyl alcohol are mixed according to the weight ratio of 1:5), simultaneously adding a 10% sodium hydroxide aqueous solution, adjusting the pH value of the solution to 7.5, and magnetically stirring for 20min to obtain a coupling agent ethanol dispersion liquid for later use;
(3) Adding the coupling agent ethanol dispersion liquid into the glass fiber ethanol dispersion liquid (the volume ratio of the coupling agent ethanol dispersion liquid to the glass fiber ethanol dispersion liquid is 1:2), stirring uniformly while adding, performing ultrasonic dispersion for 30min, heating and stirring for 3h, ending the reaction, standing and filtering to obtain the surface modified glass fiber.
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding surface modified glass fiber and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Comparative example 2
Comparative example 2 differs from example 1 in that the mixed modified filler was directly replaced with zirconium-containing ceramic fiber.
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
30 parts by weight of zirconium-containing ceramic fiber, 15 parts by weight of mica powder, 5 parts by weight of quartz powder, 5 parts by weight of alumina, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid is CaO-MgF in a ternary aid 2 -SiO 2 。
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding zirconium-containing ceramic fiber and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Comparative example 3
Comparative example 3 differs from example 1 in that no mixed modified filler was added. The high-strength insulating ceramic comprises the following raw materials in parts by weight:
30 parts by weight of mica powder, 15 parts by weight of quartz powder, 10 parts by weight of aluminum oxide, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid is CaO-MgF in a ternary aid 2 -SiO 2 。
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding a sintering aid and deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Comparative example 4
Comparative example 4 differs from example 1 in that no mica powder was added.
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
30 parts by weight of mixed modified filler, 10 parts by weight of quartz powder, 15 parts by weight of alumina, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The size of the quartz powder is 200 meshes; the sintering aid is CaO-MgF in a ternary aid 2 -SiO 2 。
The preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol (the weight ratio of the glass fiber to the absolute ethyl alcohol is 1:3), and performing ultrasonic dispersion for 15min to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent KH-550 into absolute ethyl alcohol (the coupling agent KH-550 and the absolute ethyl alcohol are mixed according to the weight ratio of 1:5), simultaneously adding a 10% sodium hydroxide aqueous solution, adjusting the pH value of the solution to 7.5, and magnetically stirring for 20min to obtain a coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion liquid into the glass fiber ethanol dispersion liquid (the volume ratio of the coupling agent ethanol dispersion liquid to the glass fiber ethanol dispersion liquid is 1:2), stirring uniformly while adding, performing ultrasonic dispersion for 30min, heating and stirring for 3h, and ending the reaction to obtain a surface modified glass fiber ethanol suspension liquid;
(4) Dispersing zirconium-containing ceramic fibers into a 10% sodium hydroxide aqueous solution (the weight ratio of the zirconium-containing ceramic fibers to the 10% sodium hydroxide aqueous solution is 1:4), performing ultrasonic dispersion for 20min, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing at the constant temperature of 80 ℃ and the stirring speed of 600r/min, stirring for 3h after uniform mixing, performing ultrasonic dispersion for 20min, heating and stirring at the temperature of 100 ℃ for 40min, and filtering to obtain the mixed modified filler.
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding mixed modified filler and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
Comparative example 5
Comparative example 5 differs from example 1 in that no alumina was added.
The high-strength insulating ceramic comprises the following raw materials in parts by weight:
30 parts by weight of mixed modified filler, 15 parts by weight of mica powder, 10 parts by weight of quartz powder, 8 parts by weight of silicon nitride, 3 parts by weight of sintering aid and 45 parts by weight of deionized water.
The mesh number of the mica powder is 200 meshes, and the whiteness is 80; the size of the quartz powder is 200 meshes; the sintering aid is CaO-MgF in a ternary aid 2 -SiO 2 。
The preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol (the weight ratio of the glass fiber to the absolute ethyl alcohol is 1:3), and performing ultrasonic dispersion for 15min to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent KH-550 into absolute ethyl alcohol (the coupling agent KH-550 and the absolute ethyl alcohol are mixed according to the weight ratio of 1:5), simultaneously adding a 10% sodium hydroxide aqueous solution, adjusting the pH value of the solution to 7.5, and magnetically stirring for 20min to obtain a coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion liquid into the glass fiber ethanol dispersion liquid (the volume ratio of the coupling agent ethanol dispersion liquid to the glass fiber ethanol dispersion liquid is 1:2), stirring uniformly while adding, performing ultrasonic dispersion for 30min, heating and stirring for 3h, and ending the reaction to obtain a surface modified glass fiber ethanol suspension liquid;
(4) Dispersing zirconium-containing ceramic fibers into a 10% sodium hydroxide aqueous solution (the weight ratio of the zirconium-containing ceramic fibers to the 10% sodium hydroxide aqueous solution is 1:4), performing ultrasonic dispersion for 20min, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing at the constant temperature of 80 ℃ and the stirring speed of 600r/min, stirring for 3h after uniform mixing, performing ultrasonic dispersion for 20min, heating and stirring at the temperature of 100 ℃ for 40min, and filtering to obtain the mixed modified filler.
A high strength insulating ceramic, the method of preparing the high strength insulating ceramic comprising the steps of:
s1, weighing mica powder, quartz powder and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving with a 300-mesh screen, adding mixed modified filler and sintering aid, adding deionized water, heating to 170 ℃, carrying out ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating to 200 ℃ within 30min, and preserving heat for 40min at the temperature; and then calcining at the high temperature of 1300 ℃ for 1h, preserving heat for 3h to obtain a ceramic blank, demoulding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
The high-strength insulating ceramics prepared in examples 1 to 4 and comparative examples 1 to 5 of the present invention were used as test samples for dielectric constant and breakdown voltage, and the results are shown in Table 1 below.
TABLE 1
| Breakdown voltage/KV | Insulation resistance/omega | Surface condition after 3 years of use | |
| Example 1 | 56.7 | 4.8×10 11 | Smooth and glossy |
| Example 2 | 58.7 | 5.2×10 11 | Smooth and glossy |
| Example 3 | 58.2 | 5.1×10 11 | Smooth and glossy |
| Example 4 | 59.1 | 5.5×10 11 | Smooth and glossy |
| Comparative example 1 | 46.3 | 4.2×10 11 | Roughness of |
| Comparative example 2 | 46.5 | 4.1×10 11 | Smooth and glossy |
| Comparative example 3 | 42.7 | 3.8×10 11 | Etching point |
| Comparative example 4 | 50.6 | 3.9×10 11 | Roughness of |
| Comparative example 5 | 52.8 | 4.0×10 11 | Etching point |
As can be seen from the results in Table 1, the high-strength insulating ceramic prepared by the invention has the advantages that under the combined action of the glass fiber and the zirconium-containing ceramic fiber modified blend serving as functional filler and various raw materials such as mica powder, alumina and the like, the insulating property of the ceramic is obviously improved, the breakdown phenomenon can not occur even under the action of strong electricity, and the safety performance of the product is improved; meanwhile, the wear resistance and corrosion resistance of the product are effectively improved, the product can keep higher smoothness for a long time, the service life is greatly prolonged, and the aging degree is reduced, so that the replacement cost is reduced, and the ceramic insulator is widely applied to the electronic field as an insulator in the insulating ceramic material.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (6)
1. A high strength insulating ceramic, characterized in that: the high-strength insulating ceramic comprises the following raw materials in parts by weight: 30-45 parts by weight of mixed modified filler, 10-15 parts by weight of mica powder, 2-7 parts by weight of quartz powder, 5-10 parts by weight of alumina, 5-10 parts by weight of silicon nitride, 1-5 parts by weight of sintering aid and 30-50 parts by weight of deionized water;
wherein the preparation method of the mixed modified filler comprises the following steps:
(1) Adding the dried glass fiber into absolute ethyl alcohol, and performing ultrasonic dispersion to obtain glass fiber ethanol dispersion liquid for later use;
(2) Adding a coupling agent into absolute ethyl alcohol, adding a neutralizing agent, adjusting the pH value, and magnetically stirring for 20min to obtain coupling agent ethanol dispersion liquid for later use;
(3) Adding a coupling agent ethanol dispersion into the glass fiber ethanol dispersion, uniformly stirring while adding, ultrasonically dispersing, heating and stirring for 3 hours, and ending the reaction to obtain a surface modified glass fiber ethanol suspension;
(4) Dispersing zirconium-containing ceramic fibers into a sodium hydroxide aqueous solution, performing ultrasonic dispersion, and stirring to obtain a zirconium-containing ceramic fiber suspension for later use;
(5) Mixing the surface modified glass fiber ethanol suspension and the zirconium-containing ceramic fiber suspension according to the weight ratio of 1:3, mixing under the conditions of constant temperature and high-speed stirring, stirring for reaction after uniform mixing, performing ultrasonic dispersion for 15-20min, heating and stirring for 30-40min, and filtering to obtain the mixed modified filler.
2. A high strength insulating ceramic according to claim 1, wherein: the mesh size of the mica powder is 200 meshes, and the whiteness is 80.
3. A high strength insulating ceramic according to claim 1, wherein: the size of the quartz powder is 200 meshes.
4. A high strength insulating ceramic according to claim 1, wherein: the sintering aid is CaO-MgF in a ternary aid 2 -SiO 2 、BaO-ZrO 2 -SiO 2 、MgO-SiO 2 -ZrO 2 And BaO-ZrO 2 -at least one of CaO.
5. A method of producing the high-strength insulating ceramic according to any one of claims 1 to 4, characterized in that: the preparation method of the high-strength insulating ceramic comprises the following steps:
s1, weighing mica powder, quartz powder, aluminum oxide and silicon nitride according to parts by weight, putting into a grinder for grinding, sieving, adding mixed modified filler and sintering aid, adding deionized water, heating, ultrasonic mixing, uniformly stirring, processing in a granulator to obtain mixed powder, and drying for later use;
s2, placing the mixed powder in a die under the protection of nitrogen, heating in a specified time, preserving heat at the temperature, calcining at a high temperature, preserving heat to obtain a ceramic blank, demolding and cutting the blank, and cooling to obtain the high-strength insulating ceramic.
6. Use of a high strength insulating ceramic according to any of claims 1-4, characterized in that: the high-strength insulating ceramic is applied to insulators.
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| CN109095913A (en) * | 2018-09-26 | 2018-12-28 | 李少伟 | A kind of high heat conductive insulating ceramics and preparation method thereof |
| CN113480907A (en) * | 2021-07-01 | 2021-10-08 | 江西东维电气有限公司 | Preparation method of spherical stain-resistant pin insulator |
| CN113956059A (en) * | 2021-11-16 | 2022-01-21 | 江西凯佳电瓷电器有限公司 | High-strength suspension insulator for high-voltage transmission line |
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| US6043172A (en) * | 1998-01-14 | 2000-03-28 | Global Consulting, Inc. | Ceramic fiber insulation material |
| CN106591745A (en) * | 2016-12-07 | 2017-04-26 | 苏州洛特兰新材料科技有限公司 | Pressure resistant and heat resistant ceramic composite material and preparation method thereof |
| CN107382295A (en) * | 2017-07-26 | 2017-11-24 | 合肥同佑电子科技有限公司 | A kind of IC substrate insulating ceramics and preparation method thereof |
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| CN113480907A (en) * | 2021-07-01 | 2021-10-08 | 江西东维电气有限公司 | Preparation method of spherical stain-resistant pin insulator |
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