CN109824353A - A kind of modified quartz-ceramics of the low porosity being effectively improved mechanical property - Google Patents
A kind of modified quartz-ceramics of the low porosity being effectively improved mechanical property Download PDFInfo
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- CN109824353A CN109824353A CN201910268712.4A CN201910268712A CN109824353A CN 109824353 A CN109824353 A CN 109824353A CN 201910268712 A CN201910268712 A CN 201910268712A CN 109824353 A CN109824353 A CN 109824353A
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Abstract
The present invention relates to electromagnetic wave transparent material technical fields, and disclose a kind of modified quartz-ceramics of the low porosity for being effectively improved mechanical property, the raw material including following parts by weight proportion: 40~60 parts of quartz powder materials, 5~15 parts of micron Si3N4Ceramics, 10~30 parts of nano Sis3N4Ceramics.The present invention solves existing quartz-ceramics electromagnetic wave transparent material, while with excellent electrical property, existing poor mechanical property and the high technical problem of porosity.
Description
Technical field
The present invention relates to electromagnetic wave transparent material technical field, specially a kind of modified stone of the low porosity for being effectively improved mechanical property
English ceramics.
Background technique
Quartz-ceramics are the systems through series of ceramic such as crushing, molding, sintering using vitreous silica or quartz glass as raw material
Make the product of technique preparation, most typical application is quartz pottery antenna covering.Quartz-ceramics have best thermal-shock resistance
Energy, optimal thermal protection ability, extremely low thermal expansion coefficient, excellent electrical property (permittivity ε 3.42, loss angle tangent
Tan δ be 0.0004), low-gravity (be less than 2.2g/cm3), but its poor mechanical property (bending strength 44MPa), and hole
Rate is high, so the easy moisture absorption, rainresistance is poor, and which limits quartz-ceramics electromagnetic wave transparent materials in outdoor application.
The present invention provides a kind of modified quartz-ceramics of the low porosity for being effectively improved mechanical property, it is intended to solve existing stone
English ceramic wave-transmitting material, while with excellent electrical property, existing poor mechanical property and the high technical problem of porosity.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of modified quartz of low porosity for being effectively improved mechanical property
Ceramics solve existing quartz-ceramics electromagnetic wave transparent material, while with excellent electrical property, existing poor mechanical property with
The high technical problem of porosity.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of modified quartz-ceramics of the low porosity being effectively improved mechanical property, the original including following parts by weight proportion
Material: 40~60 parts of quartz powder materials, 5~15 parts of micron Si3N4Ceramics, 10~30 parts of nano Sis3N4Ceramics.
Preferably, the micron Si3N4Average grain diameter≤10um.
Preferably, the nano Si3N4Average grain diameter≤100nm.
Preferably, the modified quartz-ceramics preparation method the following steps are included:
S101. 40~60g quartz powder materials are taken to be added in distilled water, ultrasonic disperse is uniform, and suspended nitride is prepared；
S102. 5~15 parts of micron Si are taken3N4Ceramics, 10~30 parts of nano Sis3N4Ceramics, it is spare；
S103. by the micron Si in step S1023N4Ceramics are placed in distilled water together with sodium metasilicate, and ultrasonic disperse is uniform；
S104. by the nano Si in step S1023N4Ceramics are placed in distilled water together with sodium metasilicate, and ultrasonic disperse is uniform；
S105. the suspended nitride in step S101 is added in the reactor equipped with agitating device and heating device,
Under the stirring rate of 600r/min, slowly by Si finely dispersed in step S1033N4Aqueous solution is added drop-wise in reactor, is added dropwise
After, slowly by Si finely dispersed in step S1043N4Aqueous solution is added drop-wise in reactor, after being added dropwise, in 800r/
2h is stirred under min, later, at 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed；
S106. 20g polyvinyl alcohol is taken to be added in 50mL distilled water, heating water bath fills polyvinyl alcohol to 65~85 DEG C
Divide dissolution to get polyvinyl alcohol water solution is arrived；
S107., slurry finely dispersed in step S106 is poured into the reactor equipped with high speed agitator and heating device
In, at 65~85 DEG C of temperature, stirring rate 300r/min, the polyvinyl alcohol water solution being slowly added in step S107 is added dropwise
After, reaction is until solvent evaporating completely at 120 DEG C of temperature, stirring rate 800r/min；
S108. the powder in step S107 is fitted into etc. in static pressure rubber mold, the compression moulding under 110MPa pressure, is risen
Temperature keeps the temperature 2h to 1500 DEG C, and under 1500 DEG C, 5MPa, and modified quartz-ceramics are prepared.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
Present invention doped micron-size Si in quartz-ceramics base-material in the micron-scale3N4With nanoscale Si3N4Two kinds of different-grain diameters
Filling-modified phase, micron order Si3N4With nanoscale Si3N4Filling in quartz ceramic-base material, can effectively realize drop in the micron-scale
The technical effect of the porosity of low quartz ceramic matrix；
The modification quartz-ceramics prepared of the present invention after tested, at 25 DEG C, 10GHz, permittivity ε is 3.93~
4.08, losstangenttanδ is 0.0009~0.0014, and bending strength is 186~194MPa；
With quartz-ceramics in the prior art, at 25 DEG C, 10GHz, permittivity ε 3.42, losstangenttanδ
It is 0.0004, bending strength is compared for 44MPa, achieves the technical effect for significantly improving quartz-ceramics mechanical property, simultaneously
Electrical property of the invention has been substantially achieved goes up same technical effect with quartz-ceramics substantially.
Specific embodiment
By 200g vitreous silica powder, ball milling prepares screened stock together with 50mL dehydrated alcohol, be heated to 80 DEG C evaporate it is anhydrous
Ethyl alcohol, by remaining dried material, by the sieve of 10000 mesh numbers, extracting screen underflow is to get arriving average grain diameter≤1.3um quartz
Powder；
Wherein, vitreous silica powder, glass phase 100%, true specific gravity 2.2g/cm3, the mass percent of chemical composition
Content are as follows: 99.85%SiO2, 0.11%Al2O3, 0.0041%Fe2O3, 0.0061%Na2O, 0.0053%K2O, 0.0013%
CaO, 0.0011%MgO, 0.002%Li2O, 0.01% other；
Quartz powder materials used in the following embodiment are prepared by the above method.
Embodiment one:
S101. 40g quartz powder materials are taken to be added in 50mL distilled water, ultrasonic disperse is uniform, and suspended nitride is prepared；
S102. 15g average grain diameter≤10um Si is taken3N4, 10g average grain diameter≤100nm Si3N4, spare；
S103. by average grain diameter≤10um Si in step S1023N4It is placed in together with 1mL sodium metasilicate in 10mL distilled water,
Ultrasonic disperse is uniform；
S104. by average grain diameter≤100nm Si in step S1023N420mL distilled water is placed in together with 2mL sodium metasilicate
In, ultrasonic disperse is uniform；
S105. the suspended nitride in step S101 is added in the reactor equipped with agitating device and heating device,
Under the stirring rate of 600r/min, slowly by Si finely dispersed in step S1033N4Aqueous solution is added drop-wise in reactor, is added dropwise
After, slowly by Si finely dispersed in step S1043N4Aqueous solution is added drop-wise in reactor, after being added dropwise, in 800r/
2h is stirred under min, later, at 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed；
S106. 20g polyvinyl alcohol is taken to be added in 50mL distilled water, heating water bath fills polyvinyl alcohol to 65~85 DEG C
Divide dissolution to get polyvinyl alcohol water solution is arrived；Wherein, the alcoholysis degree of polyvinyl alcohol is 87~89%, viscosity is 40.0~65.0；
S107., slurry finely dispersed in step S106 is poured into the reactor equipped with high speed agitator and heating device
In, at 65~85 DEG C of temperature, stirring rate 300r/min, the polyvinyl alcohol water solution being slowly added in step S107 is added dropwise
After, reaction is until solvent evaporating completely at 120 DEG C of temperature, stirring rate 800r/min；
S108. the powder in step S107 is fitted into etc. in static pressure rubber mold, the compression moulding under 110MPa pressure, then
Being placed in preheating temperature is in 600 DEG C of vacuum drying oven, with the heating rate of 10 DEG C/min, is warming up to 1500 DEG C, and in 1500 DEG C,
2h is kept the temperature under 5MPa, later with the annealing rate of 5 DEG C/min, modified quartz-ceramics are prepared in taking-up when being cooled to room temperature.
Embodiment two:
S101. 60g quartz powder materials are taken to be added in 50mL distilled water, ultrasonic disperse is uniform, and suspended nitride is prepared；
S102. 5g average grain diameter≤10um Si is taken3N4, 30g average grain diameter≤100nm Si3N4, spare；
S103. by average grain diameter≤10um Si in step S1023N4It is placed in together with 1mL sodium metasilicate in 10mL distilled water,
Ultrasonic disperse is uniform；
S104. by average grain diameter≤100nm Si in step S1023N420mL distilled water is placed in together with 2mL sodium metasilicate
In, ultrasonic disperse is uniform；
S105. the suspended nitride in step S101 is added in the reactor equipped with agitating device and heating device,
Under the stirring rate of 600r/min, slowly by Si finely dispersed in step S1033N4Aqueous solution is added drop-wise in reactor, is added dropwise
After, slowly by Si finely dispersed in step S1043N4Aqueous solution is added drop-wise in reactor, after being added dropwise, in 800r/
2h is stirred under min, later, at 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed；
S106. 20g polyvinyl alcohol is taken to be added in 50mL distilled water, heating water bath fills polyvinyl alcohol to 65~85 DEG C
Divide dissolution to get polyvinyl alcohol water solution is arrived；Wherein, the alcoholysis degree of polyvinyl alcohol is 87~89%, viscosity is 40.0~65.0；
S107., slurry finely dispersed in step S106 is poured into the reactor equipped with high speed agitator and heating device
In, at 65~85 DEG C of temperature, stirring rate 300r/min, the polyvinyl alcohol water solution being slowly added in step S107 is added dropwise
After, reaction is until solvent evaporating completely at 120 DEG C of temperature, stirring rate 800r/min；
S108. the powder in step S107 is fitted into etc. in static pressure rubber mold, the compression moulding under 110MPa pressure, then
Being placed in preheating temperature is in 600 DEG C of vacuum drying oven, with the heating rate of 10 DEG C/min, is warming up to 1500 DEG C, and in 1500 DEG C,
2h is kept the temperature under 5MPa, later with the annealing rate of 5 DEG C/min, modified quartz-ceramics are prepared in taking-up when being cooled to room temperature.
Embodiment three:
S101. 50g quartz powder materials are taken to be added in 50mL distilled water, ultrasonic disperse is uniform, and suspended nitride is prepared；
S102. 10g average grain diameter≤10um Si is taken3N4, 20g average grain diameter≤100nm Si3N4, spare；
S103. by average grain diameter≤10um Si in step S1023N4It is placed in together with 1mL sodium metasilicate in 10mL distilled water,
Ultrasonic disperse is uniform；
S104. by average grain diameter≤100nm Si in step S1023N420mL distilled water is placed in together with 2mL sodium metasilicate
In, ultrasonic disperse is uniform；
S105. the suspended nitride in step S101 is added in the reactor equipped with agitating device and heating device,
Under the stirring rate of 600r/min, slowly by Si finely dispersed in step S1033N4Aqueous solution is added drop-wise in reactor, is added dropwise
After, slowly by Si finely dispersed in step S1043N4Aqueous solution is added drop-wise in reactor, after being added dropwise, in 800r/
2h is stirred under min, later, at 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed；
S106. 20g polyvinyl alcohol is taken to be added in 50mL distilled water, heating water bath fills polyvinyl alcohol to 65~85 DEG C
Divide dissolution to get polyvinyl alcohol water solution is arrived；Wherein, the alcoholysis degree of polyvinyl alcohol is 87~89%, viscosity is 40.0~65.0；
S107., slurry finely dispersed in step S106 is poured into the reactor equipped with high speed agitator and heating device
In, at 65~85 DEG C of temperature, stirring rate 300r/min, the polyvinyl alcohol water solution being slowly added in step S107 is added dropwise
After, reaction is until solvent evaporating completely at 120 DEG C of temperature, stirring rate 800r/min；
S108. the powder in step S107 is fitted into etc. in static pressure rubber mold, the compression moulding under 110MPa pressure, then
Being placed in preheating temperature is in 600 DEG C of vacuum drying oven, with the heating rate of 10 DEG C/min, is warming up to 1500 DEG C, and in 1500 DEG C,
2h is kept the temperature under 5MPa, later with the annealing rate of 5 DEG C/min, modified quartz-ceramics are prepared in taking-up when being cooled to room temperature.
Performance test:
The modification quartz-ceramics prepared in above-described embodiment and comparative example are tested for the property, performance data such as following table
Shown in 1.
Table 1
Claims (4)
1. a kind of modified quartz-ceramics of the low porosity for being effectively improved mechanical property, which is characterized in that including following parts by weight
The raw material of proportion: 40~60 parts of quartz powder materials, 5~15 parts of micron Si3N4Ceramics, 10~30 parts of nano Sis3N4Ceramics.
2. modified quartz-ceramics according to claim 1, which is characterized in that the micron Si3N4Average grain diameter≤
10um。
3. modified quartz-ceramics according to claim 1, which is characterized in that the nano Si3N4Average grain diameter≤
100nm。
4. modified quartz-ceramics according to claim 1, which is characterized in that the preparation method packet of the modified quartz-ceramics
Include following steps:
S101. 40~60g quartz powder materials are taken to be added in distilled water, ultrasonic disperse is uniform, and suspended nitride is prepared；
S102. 5~15 parts of micron Si are taken3N4Ceramics, 10~30 parts of nano Sis3N4Ceramics, it is spare；
S103. by the micron Si in step S1023N4Ceramics are placed in distilled water together with sodium metasilicate, and ultrasonic disperse is uniform；
S104. by the nano Si in step S1023N4Ceramics are placed in distilled water together with sodium metasilicate, and ultrasonic disperse is uniform；
S105. the suspended nitride in step S101 is added in the reactor equipped with agitating device and heating device, in 600r/
Under the stirring rate of min, slowly by Si finely dispersed in step S1033N4Aqueous solution is added drop-wise in reactor, is added dropwise
Afterwards, slowly by Si finely dispersed in step S1043N4Aqueous solution is added drop-wise in reactor, after being added dropwise, under 800r/min
2h is stirred, later, at 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed；
S106. 20g polyvinyl alcohol is taken to be added in 50mL distilled water, heating water bath keeps polyvinyl alcohol sufficiently molten to 65~85 DEG C
Solution to get arrive polyvinyl alcohol water solution；
S107. slurry finely dispersed in step S106 is poured into the reactor equipped with high speed agitator and heating device,
Under 65~85 DEG C of temperature, stirring rate 300r/min, the polyvinyl alcohol water solution being slowly added in step S107 is added dropwise
Afterwards, it reacts at 120 DEG C of temperature, stirring rate 800r/min until solvent evaporating completely；
S108. the powder in step S107 is fitted into etc. in static pressure rubber mold, the compression moulding under 110MPa pressure is warming up to
1500 DEG C, and 2h is kept the temperature under 1500 DEG C, 5MPa, modified quartz-ceramics are prepared.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569743A (en) * | 2004-04-23 | 2005-01-26 | 山东工业陶瓷研究设计院 | Silicon nitride - boron nitride- silicon dioxide ceramic wave-transparent material and preparation process thereof |
| CN108911520A (en) * | 2018-08-02 | 2018-11-30 | 晶科能源有限公司 | A kind of production method of silicon nitride coating |
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2019
- 2019-04-04 CN CN201910268712.4A patent/CN109824353A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569743A (en) * | 2004-04-23 | 2005-01-26 | 山东工业陶瓷研究设计院 | Silicon nitride - boron nitride- silicon dioxide ceramic wave-transparent material and preparation process thereof |
| CN108911520A (en) * | 2018-08-02 | 2018-11-30 | 晶科能源有限公司 | A kind of production method of silicon nitride coating |
Non-Patent Citations (1)
| Title |
|---|
| 高芳等: "氮化硅增强石英陶瓷天线罩复合材料的研究", 《陶瓷》 * |
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Application publication date: 20190531 |