CN111704458A - Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof - Google Patents
Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof Download PDFInfo
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- CN111704458A CN111704458A CN202010445252.0A CN202010445252A CN111704458A CN 111704458 A CN111704458 A CN 111704458A CN 202010445252 A CN202010445252 A CN 202010445252A CN 111704458 A CN111704458 A CN 111704458A
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- silicon dioxide
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- nanocrystal powder
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 74
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 73
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 51
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 13
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 13
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 11
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 26
- 235000015110 jellies Nutrition 0.000 claims description 14
- 239000008274 jelly Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000004115 Sodium Silicate Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011268 mixed slurry Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention relates to the field of ceramic materials, in particular to fine functional ceramic containing silicon dioxide nanocrystals and a preparation method thereof. The fine functional ceramic comprises the following components, by weight, 8-10 parts of silicon dioxide nanocrystal powder; 25-30 parts of barium titanate; 8-12 parts of aluminum hydroxide; 45-55 parts of zirconium dioxide; 10-18 parts of silicon carbide; 4-8 parts of hexamethyldisilazane; 2-5 parts of concentrated ammonia water; 12-18 parts of deionized water. The surface of the silicon dioxide nanocrystal is modified by hexamethyldisilazane and concentrated ammonia water, so that the surface of the silicon dioxide nanocrystal exists in an uneven atomic step form, and conditions are provided for the connection of the surface of the silicon dioxide nanocrystal and other components, so that the strength of the integral structure of the fine functional ceramic is increased, the fine functional ceramic has better structural strength, and the fine functional ceramic has longer service life.
Description
Technical Field
The invention relates to the field of ceramic materials, in particular to fine functional ceramic containing silicon dioxide nanocrystals and a preparation method thereof.
Background
Fine functional ceramics, broadly referred to as materials that utilize their non-mechanical properties primarily in their application, typically have one or more functions such as electrical, magnetic, optical, thermal, chemical, biological, etc., and some have coupling functions such as piezoelectric, piezomagnetic, thermoelectric, electro-optical, acousto-optical, magneto-optical, etc.
Specifically, piezoelectric ceramics, which is an emerging ceramic material, has been developed for over a hundred years. In the middle of the last century, the invention of PZT-based piezoelectric ceramics promoted the rapid development of electronic technology, so that various electronic products appeared in the front of us, and the piezoelectric ceramics, as an internal precise element, can convert electric energy into mechanical energy or mechanical energy into electric energy, and plays a key role in electronic products. In order to obtain high piezoelectric performance, doping modification is generally performed by using a soft additive, and although the method can make the piezoelectric ceramic performance active, the structural stability is poor, the service life is short, and the service life of an electronic product is finally affected.
Disclosure of Invention
In view of the above-mentioned drawbacks of the background art, the present invention provides a fine functional ceramic containing silica nanocrystals and a method for preparing the same.
The invention adopts the following technical scheme: a fine functional ceramic comprising silica nanocrystals, characterized in that: comprises the following components in parts by weight,
8-10 parts of silicon dioxide nanocrystal powder;
25-30 parts of barium titanate;
8-12 parts of aluminum hydroxide;
45-55 parts of zirconium dioxide;
10-18 parts of silicon carbide;
4-8 parts of hexamethyldisilazane;
2-5 parts of concentrated ammonia water;
12-18 parts of deionized water.
As a further improvement, the fine functional ceramic containing silica nanocrystals specifically comprises the following components in parts by weight, 10 parts of silica nanocrystal powder; 28 parts of barium titanate; 9 parts of aluminum hydroxide; 50 parts of zirconium dioxide; 4 parts of concentrated ammonia water; 15 parts of silicon carbide; 7 parts of hexamethyldisilazane; and 15 parts of deionized water.
As a further improvement, the silicon dioxide nano crystal powder comprises the following components in parts by weight, 8 parts of silicon dioxide nano crystal powder; 29 parts of barium titanate; 10 parts of aluminum hydroxide; 3 parts of concentrated ammonia water; 46 parts of zirconium dioxide; 15 parts of silicon carbide; 5 parts of hexamethyldisilazane; 16 parts of deionized water.
As a further improvement, the silicon dioxide nanocrystal powder is prepared from 65% of sodium silicate, 12% of absolute ethyl alcohol and 23% of deionized water.
The preparation method of the fine functional ceramic containing the silicon dioxide nanocrystals comprises the following steps:
s1: preparation of silica nanocrystal powder:
s2: pouring silicon dioxide nanocrystal powder, hexamethyldisilazane, concentrated ammonia water and water into a stirring container, and stirring for 5-10 min;
s3: filtering out water in the stirring container, and drying the silicon dioxide nanocrystal powder to obtain modified silicon dioxide nanocrystal powder;
s4: placing the modified silicon dioxide nanocrystal powder obtained in the step S3, barium titanate, aluminum hydroxide, zirconium dioxide, silicon carbide and deionized water into a stirring container for mixing to prepare mixed slurry;
s5: pouring the mixed slurry into a mold, and pressing and molding;
s6: opening the mold, taking out the green body formed by pressing, and putting the green body into a sintering furnace to sinter for 3-4 hours at the temperature of 1000-1150 ℃;
s7: and taking out the blank, naturally cooling, and polishing to obtain the fine functional ceramic.
As a further improvement of the above preparation method, the method for preparing the silica nanocrystal powder of step S1 includes the steps of,
s1-1: pouring sodium silicate, absolute ethyl alcohol and deionized water into a stirring container, stirring for 5-8 min, adding an ammonium chloride solution, and stirring for 15-20 min;
s1-2: heating the stirring container for 15-20 min at the temperature of 40-45 ℃ to obtain jelly;
s1-3: and drying the jelly, putting the jelly into an oven, and heating the jelly for 30-45 min at the temperature of 350-450 ℃ to obtain the silicon dioxide nanocrystal powder.
As a further improvement of the above preparation method, in step S1-1, the percentage of each component is 65% of sodium silicate, 12% of absolute ethyl alcohol, and 23% of deionized water.
As a further improvement of the above preparation method, in the step S2, in the step S2, water accounts for 8% of the total weight of the silica nanocrystal powder, hexamethyldisilazane, and concentrated ammonia water.
From the above description of the structure of the present invention, compared with the prior art, the present invention has the following advantages: according to the invention, the silicon dioxide nanocrystals are added into the components for preparing the fine functional ceramic, and the surface of the silicon dioxide nanocrystals is modified, so that the surface of the silicon dioxide nanocrystals exists in an uneven atomic step form, the contact surface of the chemical reaction of the silicon dioxide nanocrystals can be increased, and conditions are provided for the connection of the surface of the silicon dioxide nanocrystals and other components, thereby increasing the strength of the integral structure of the fine functional ceramic, and the polarity of the surface of the silicon dioxide can be weakened after the modification, the energy state of the surface of the silicon dioxide is reduced, the silicon dioxide nanocrystals are prevented from being agglomerated, the dispersibility of the silicon dioxide nanocrystals is improved, and the compatibility of the silicon dioxide nanocrystals with other substances (namely barium titanate and zirconium dioxide) is increased. Therefore, compared with the existing fine functional ceramic, the fine functional ceramic has better structural strength and longer service life.
Detailed Description
A fine functional ceramic containing silicon dioxide nano crystals comprises the following components in parts by weight: 8-10 parts of silicon dioxide nanocrystal powder; 25-30 parts of barium titanate; 8-12 parts of aluminum hydroxide; 45-55 parts of zirconium dioxide; 10-18 parts of silicon carbide; 4-8 parts of hexamethyldisilazane; 12-18 parts of deionized water. The silicon dioxide nanocrystal powder is prepared from 65% of sodium silicate, 12% of absolute ethyl alcohol and 23% of deionized water.
The preparation method of the fine functional ceramic containing the silicon dioxide nanocrystals comprises the following steps:
s1: the silica nanocrystal powder was prepared as follows:
s1-1: weighing 65% of sodium silicate, 12% of absolute ethyl alcohol and 23% of deionized water in percentage by weight, pouring the sodium silicate, the absolute ethyl alcohol and the deionized water into a stirring container, stirring for 5-8 min, adding an ammonium chloride solution, and stirring for 15-20 min, wherein the ammonium chloride solution accounts for 8% of the total amount of the components in the stirring container;
s1-2: heating the stirring container for 15-20 min at the temperature of 40-45 ℃ to obtain jelly;
s1-3: and drying the jelly, wherein the jelly can be placed on a tray in a drying mode and then placed in an oven for baking, specifically, the jelly can be baked at the temperature of 120 ℃ for 15-20 min, then the temperature of the oven is changed to the temperature of 350-450 ℃, the jelly is heated for 30-45 min, and preferably heated at the temperature of 420 ℃ for 40min, so that the silicon dioxide nanocrystal powder can be obtained.
S2: pouring the silicon dioxide nanocrystal powder, hexamethyldisilazane, concentrated ammonia water and water into a stirring container, and stirring for 5-10 min, wherein the water accounts for 8% of the total weight of the silicon dioxide nanocrystal powder, the hexamethyldisilazane and the concentrated ammonia water. In the process, the surface of the silicon dioxide is modified by hexamethyldisilazane, and the silicon dioxide is an acidic oxide, so that the purpose that the silicon dioxide nanocrystal powder can not be modified due to the hydrolysis of a large amount of hexamethyldisilazane is avoided by adding alkaline concentrated ammonia water to neutralize the pH value of liquid in the stirring container.
S3: and (3) filtering water in the stirring container, and drying the silicon dioxide nanocrystal powder, wherein the drying mode can be natural air drying or the drying mode is consistent with the drying mode of the jelly in the step S1-1, and the modified silicon dioxide nanocrystal powder can be obtained after drying. The modified silicon dioxide nanocrystal surface exists in an uneven atomic step form, so that the contact surface of chemical reaction can be increased, a condition is provided for the connection of the surface of the silicon dioxide nanocrystal and other inorganic matters, the polarity of the silicon dioxide surface can be weakened after modification, the energy state of the silicon dioxide surface is reduced, the silicon dioxide nanocrystal is prevented from being aggregated, and the dispersibility of the silicon dioxide nanocrystal and the compatibility of the silicon dioxide nanocrystal and other substances (namely barium titanate and zirconium dioxide) are improved.
S4: and (4) placing the modified silicon dioxide nanocrystal powder obtained in the step (S3), barium titanate, aluminum hydroxide, zirconium dioxide, silicon carbide and deionized water into a stirring container for mixing to prepare mixed slurry.
S5: and pouring the mixed slurry into a mold, and pressing and molding.
S6: and opening the mold, taking out the blank formed by pressing, and putting the blank into a sintering furnace to be sintered for 3-4 hours at the temperature of 1000-1150 ℃, particularly preferably 1100 ℃ for 3 hours.
S7: and taking out the blank, naturally cooling, and polishing to obtain the fine functional ceramic.
Referring to the above-described preparation method of fine functional ceramics of silica nanocrystals, fine functional ceramics were prepared using examples of the following composition (1) in which silica nanocrystals, hexamethyldisilazane and concentrated ammonia were not included in the composition of example three, respectively, in different weight parts, and thus were directly performed according to steps S4 to S7.
Watch (1)
The fine functional ceramics prepared in the above three examples were respectively tested for compressive strength and fracture toughness and again after 12 months, and the test results were compared as shown in the following table (2)
Watch (2)
Referring to the above table (2), it can be seen that the physical strength of the first and second examples is significantly higher than that of the third example, and the first and second examples are superior in stability to the third example, while the first, second and third examples are different in that the three components of silica nanocrystals, hexamethyldisilazane and concentrated ammonia are not present, so that the fine functional ceramic of the present invention has better structural strength and longer service life than the existing functional ceramic.
The above description is only an embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications made by using the design concept should fall within the scope of infringing the present invention.
Claims (8)
1. A fine functional ceramic comprising silica nanocrystals, characterized in that: comprises the following components in parts by weight,
8-10 parts of silicon dioxide nanocrystal powder;
25-30 parts of barium titanate;
8-12 parts of aluminum hydroxide;
45-55 parts of zirconium dioxide;
10-18 parts of silicon carbide;
4-8 parts of hexamethyldisilazane;
2-5 parts of concentrated ammonia water;
12-18 parts of deionized water.
2. The fine functional ceramic containing silica nanocrystals according to claim 1, wherein: the silicon dioxide nano-crystal powder comprises the following components in parts by weight, namely 10 parts of silicon dioxide nano-crystal powder; 28 parts of barium titanate; 9 parts of aluminum hydroxide; 50 parts of zirconium dioxide; 15 parts of silicon carbide; 7 parts of hexamethyldisilazane; 4 parts of concentrated ammonia water; and 15 parts of deionized water.
3. The fine functional ceramic containing silica nanocrystals according to claim 1, wherein: comprises the following components, by weight, 8 parts of silicon dioxide nanocrystal powder; 29 parts of barium titanate; 10 parts of aluminum hydroxide; 46 parts of zirconium dioxide; 15 parts of silicon carbide; 5 parts of hexamethyldisilazane; 3 parts of concentrated ammonia water; 16 parts of deionized water.
4. The fine functional ceramic containing silica nanocrystals according to any one of claims 1 to 3, wherein: the silicon dioxide nanocrystal powder is prepared from 65% of sodium silicate, 12% of absolute ethyl alcohol and 23% of deionized water.
5. A method for preparing a fine functional ceramic containing silica nanocrystals, comprising the steps of:
s1: preparation of silica nanocrystal powder:
s2: pouring silicon dioxide nanocrystal powder, hexamethyldisilazane, concentrated ammonia water and water into a stirring container, and stirring for 5-10 min;
s3: filtering out water in the stirring container, and drying the silicon dioxide nanocrystal powder to obtain modified silicon dioxide nanocrystal powder;
s4: placing the modified silicon dioxide nanocrystal powder obtained in the step S3, barium titanate, aluminum hydroxide, zirconium dioxide, silicon carbide and deionized water into a stirring container for mixing to prepare mixed slurry;
s5: pouring the mixed slurry into a mold, and pressing and molding;
s6: opening the mold, taking out the green body formed by pressing, and putting the green body into a sintering furnace to sinter for 3-4 hours at the temperature of 1000-1150 ℃;
s7: and taking out the blank, naturally cooling, and polishing to obtain the fine functional ceramic.
6. The method for preparing a fine functional ceramic containing silica nanocrystals according to claim 5, wherein: the method for preparing the silica nanocrystal powder of step S1 includes the steps of,
s1-1: pouring sodium silicate, absolute ethyl alcohol and deionized water into a stirring container, stirring for 5-8 min, adding an ammonium chloride solution, and stirring for 15-20 min;
s1-2: heating the stirring container for 15-20 min at the temperature of 40-45 ℃ to obtain jelly;
s1-3: and drying the jelly, putting the jelly into an oven, and heating the jelly for 30-45 min at the temperature of 350-450 ℃ to obtain the silicon dioxide nanocrystal powder.
7. The method for preparing a fine functional ceramic containing silica nanocrystals according to claim 6, wherein: in the step S1-1, the percentage of each component is 65% of sodium silicate, 12% of absolute ethyl alcohol and 23% of deionized water.
8. The method for preparing a fine functional ceramic containing silica nanocrystals according to claim 5, wherein: in the step S2, water accounts for 8% of the total weight of the silica nanocrystal powder, hexamethyldisilazane, and concentrated ammonia water.
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