CN112299864A - Modified fused quartz sand and preparation process thereof - Google Patents
Modified fused quartz sand and preparation process thereof Download PDFInfo
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- CN112299864A CN112299864A CN202011259030.6A CN202011259030A CN112299864A CN 112299864 A CN112299864 A CN 112299864A CN 202011259030 A CN202011259030 A CN 202011259030A CN 112299864 A CN112299864 A CN 112299864A
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
Abstract
The invention provides modified fused quartz sand and a preparation process thereof, belonging to the technical field of quartz sand modification, wherein the modified fused quartz sand comprises the following components in parts by weight: fused quartz sand, aluminum oxide, boric acid and barium titanate; the preparation process of the modified fused quartz sand comprises the following processing steps: (1) preparing nano fused quartz sand: taking a fused quartz sand raw material for ball milling, and then sieving to obtain nano fused quartz sand; (2) and (3) granulation and forming: taking raw materials according to the weight ratio, adding an adhesive, granulating by using a granulator, and tabletting; (3) and (3) sintering: sintering by adopting a spark plasma technology to obtain the modified fused quartz sand. The modified fused quartz sand is used for modifying the fused quartz sand to improve the dielectric property of the fused quartz sand, and is wide in preparation process source, simple and convenient to operate and suitable for large-scale popularization and application.
Description
Technical Field
The invention belongs to the technical field of quartz sand modification, and particularly relates to modified fused quartz sand and a preparation process thereof.
Background
Fused silica is an amorphous (glassy) state of silica, which is a typical glass whose atomic structure is disordered long-range, providing its high use temperature and low coefficient of thermal expansion through three-dimensional structural cross-linking. The fused silica has a melting temperature of about 1713 ℃, a low thermal conductivity coefficient, a thermal expansion coefficient which is almost the minimum of all refractory materials, and extremely high thermal shock stability. Therefore, the fused silica shell is less likely to be cracked by the temperature change during the firing and casting processes, and is an ideal refractory for investment casting, as a refractory for a facing or backing coating, and as a sanding material. The relative dielectric constant of the fused quartz is 3.82, the fused quartz has a low dielectric constant, and in order to improve the dielectric property of the fused quartz and enhance the application of the fused quartz in microwave substrate materials, the fused quartz can be modified to enhance the dielectric property of the fused quartz.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the modified fused quartz sand and the preparation process thereof, the modified fused quartz sand is used for modifying the fused quartz sand so as to improve the dielectric property of the fused quartz sand, and the preparation process of the modified fused quartz sand has wide sources and simple and convenient operation, and is suitable for large-scale popularization and application.
In order to achieve the purpose, the invention is realized by the following technical scheme: the modified fused quartz sand comprises the following components in parts by weight: 85-90 parts of fused quartz sand, 5-10 parts of aluminum oxide, 1-5 parts of boric acid and 5-10 parts of barium titanate. The aluminum oxide can promote the growth of fused quartz sand grains, the gaps among the grains are smaller, and the compactness of the structure is improved; boric acid can effectively inhibit the formation of quartz crystal phase; barium titanate, a strong dielectric material, can significantly improve the dielectric properties of fused silica.
Further, the fused silica sand is nano fused silica sand, and the particle size of the fused silica sand is 10-20 microns. The nano fused silica sand can improve the mixing uniformity of the fused silica sand and other substances.
A preparation process of modified fused silica sand comprises the following processing steps:
(1) preparing nano fused quartz sand: ball-milling raw materials of fused quartz sand for 24 hours by using a ball mill, taking out and drying the raw materials, and sieving the dried raw materials to screen nano fused quartz sand with the particle size of 10-20 mu m;
(2) and (3) granulation and forming: adding a binding agent with the weight ratio of 1:0.5-1 into the raw materials according to the weight ratio, uniformly stirring, granulating by using a granulator, wherein the particle size is 5-10 mm, pressing the prepared powder into a sheet with the thickness of 3-5 mm by using a hydraulic machine, and tabletting under the pressure of 50 MPa;
(3) and (3) sintering: and (3) sintering the slices obtained in the step (2) by adopting a spark plasma technology to obtain the modified fused quartz sand. The spark plasma technology has the advantages of uniform sintering and heating, high temperature rise speed, low sintering temperature, short sintering time, high production efficiency, fine and uniform product tissue, capability of keeping the natural state of raw materials, capability of obtaining high-density materials, simple operation and no need of special skilled technology.
Further, the adhesive in the step (2) is epoxy resin. Has better adhesive property to raw materials.
Further, the working pressure of the sintering equipment in the step (3) is 15-25 MPa.
Further, the sintering temperature in the step (3) is 1100-. Sintering at the temperature can not only make the raw material fully coated on the surface of the fused quartz, but also avoid the fused quartz forming a crystalline phase.
Further, the sintering process in the step (3) comprises a first temperature rise process, a second temperature rise process and a heat preservation process. The first temperature rise process adopts rapid temperature rise, so that other impurities in the raw materials can be removed; the second temperature rise process has a slow temperature rise rate, so that the added raw materials can be melted to be uniformly coated on the surface of the fused quartz.
Further, the first temperature raising process is to raise the temperature to 520-550 ℃ at a temperature raising rate of 150-200 ℃/min.
Further, the second temperature-raising process is to raise the temperature to 1100-1200 ℃ at a temperature-raising rate of 50-100 ℃/min.
Further, the heat preservation process is to preserve heat for 5-10 min at 1100-1200 ℃. The heat preservation process promotes the fusion of the raw materials and the fused quartz.
Has the advantages that: compared with the prior art, the invention has the following advantages: the modified fused quartz sand and the preparation process thereof have the advantages that the preparation process of the modified fused quartz sand has wide sources, is simple and convenient to operate, and is suitable for large-scale popularization and application; the aluminum oxide can promote the growth of fused quartz sand grains, the gaps among the grains are smaller, and the compactness of the structure is improved; boric acid can effectively inhibit the formation of quartz crystal phase; barium titanate, a strong dielectric material, can significantly improve the dielectric properties of fused silica.
Detailed Description
The invention will now be further illustrated by reference to the following specific examples.
Example 1
A preparation process of modified fused silica sand comprises the following processing steps:
(1) preparing nano fused quartz sand: ball-milling raw materials of fused quartz sand for 24 hours by using a ball mill, taking out and drying the raw materials, and sieving the dried raw materials to screen nano fused quartz sand with the particle size of 15 mu m;
(2) and (3) granulation and forming: taking 87 parts of fused quartz sand, 7 parts of alumina and epoxy resin in a weight ratio of 1:0.5, uniformly stirring, granulating by using a granulator, wherein the particle size is 7 mm, pressing the prepared powder into a sheet with the thickness of 4 mm by using a hydraulic machine, and tabletting under the pressure of 50 MPa;
(3) and (3) sintering: and (3) sintering the slices obtained in the step (2) by adopting a spark plasma technology, wherein the working pressure of sintering equipment is 20 Mpa, the sintering process comprises a first heating process, a second heating process and a heat preservation process, the first heating process is carried out by heating to 530 ℃ at a heating rate of 170 ℃/min, the second heating process is carried out by heating to 1100 ℃ at a heating rate of 75 ℃/min, the heat preservation process is carried out by heat preservation for 7 min at 1100 ℃, and the slices are taken out and naturally cooled to obtain the modified fused quartz sand.
The dielectric constant of the modified fused silica sand prepared in this example was 3.3, and it was found in the experiment that the dielectric property was the best when the alumina content was controlled to 5-10 parts and the dielectric constant was at most 3.3 for 87 parts of fused silica sand.
Example 2
A preparation process of modified fused silica sand comprises the following processing steps:
(1) preparing nano fused quartz sand: ball-milling raw materials of fused quartz sand for 24 hours by using a ball mill, taking out and drying the raw materials, and sieving the dried raw materials to screen nano fused quartz sand with the particle size of 10-20 mu m;
(2) and (3) granulation and forming: taking 87 parts of fused quartz sand and 3 parts of boric acid, adding epoxy resin in a weight ratio of 1:0.7, uniformly stirring, granulating by using a granulator until the particle size is 7 mm, pressing the prepared powder into a sheet with the thickness of 4 mm by using a hydraulic machine, and tabletting under the pressure of 50 MPa;
(3) and (3) sintering: and (3) sintering the slices obtained in the step (2) by adopting a spark plasma technology, wherein the working pressure of sintering equipment is 20 Mpa, the sintering process comprises a first heating process, a second heating process and a heat preservation process, the first heating process is carried out by heating to 530 ℃ at a heating rate of 170 ℃/min, the second heating process is carried out by heating to 1100 ℃ at a heating rate of 75 ℃/min, the heat preservation process is carried out by heat preservation for 7 min at 1100 ℃, and the slices are taken out and naturally cooled to obtain the modified fused quartz sand.
The dielectric constant of the modified fused silica sand obtained in this example was found to be 3.43, and it was found in the experiment that the dielectric properties were the best when the boric acid content was controlled to 1-5 parts and the dielectric constant was at most 3.43 for 87 parts of fused silica sand.
Example 3
A preparation process of modified fused silica sand comprises the following processing steps:
(1) preparing nano fused quartz sand: ball-milling raw materials of fused quartz sand for 24 hours by using a ball mill, taking out and drying the raw materials, and sieving the dried raw materials to screen nano fused quartz sand with the particle size of 15 mu m;
(2) and (3) granulation and forming: adding 87 parts of fused quartz sand and 7 parts of barium titanate into epoxy resin in a weight ratio of 1:0.7, uniformly stirring, granulating by using a granulator until the particle size is 7 mm, pressing the prepared powder into a sheet with the thickness of 4 mm by using a hydraulic machine, and tabletting under the pressure of 50 MPa;
(3) and (3) sintering: and (3) sintering the slices obtained in the step (2) by adopting a discharge plasma technology, wherein the working pressure of sintering equipment is 20 Mpa, the sintering process comprises a first heating process, a second heating process and a heat preservation process, the first heating process is carried out at a heating rate of 170 ℃/min to 530 ℃, the second heating process is carried out at a heating rate of 75 ℃/min to 1400 ℃, the heat preservation process is carried out at 1400 ℃ for 7 min, and the modified fused quartz sand is obtained after being taken out and naturally cooled.
The dielectric constant of the modified fused silica sand prepared in the embodiment is 890, and because barium titanate is difficult to sinter, a small amount of barium titanate is adopted in the method so that the barium titanate is uniformly coated on the surface of the fused silica sand.
Example 4
A preparation process of modified fused silica sand comprises the following processing steps:
(1) preparing nano fused quartz sand: ball-milling raw materials of fused quartz sand for 24 hours by using a ball mill, taking out and drying the raw materials, and sieving the dried raw materials to screen nano fused quartz sand with the particle size of 15 mu m;
(2) and (3) granulation and forming: adding 87 parts of fused quartz sand, 7 parts of aluminum oxide, 3 parts of boric acid and 7 parts of barium titanate into epoxy resin with the weight ratio of 1:0.7, uniformly stirring, granulating by using a granulator, wherein the particle size is 7 mm, pressing the prepared powder into a sheet with the thickness of 4 mm by using a hydraulic machine, and the tabletting pressure is 50 MPa;
(3) and (3) sintering: and (3) sintering the slices obtained in the step (2) by adopting a discharge plasma technology, wherein the working pressure of sintering equipment is 20 Mpa, the sintering process comprises a first temperature rise process, a second temperature rise process and a heat preservation process, the first temperature rise process is carried out by raising the temperature to 540 ℃ at a temperature rise rate of 170 ℃/min, the second temperature rise process is carried out by raising the temperature to 1150 ℃ at a temperature rise rate of 75 ℃/min, the heat preservation process is carried out for 7 min at 1150 ℃, and the modified fused quartz sand is obtained by taking out and naturally cooling.
The dielectric constant of the modified fused silica sand prepared in this example was determined to be 893.
The foregoing is directed to embodiments of the present invention and, more particularly, to a method and apparatus for controlling a power converter in a power converter, including a power converter, a power converter.
Claims (10)
1. A modified fused silica sand, characterized in that: comprises the following components in parts by weight: 85-90 parts of fused quartz sand, 5-10 parts of aluminum oxide, 1-5 parts of boric acid and 5-10 parts of barium titanate.
2. The modified fused quartz sand of claim 1, wherein: the fused quartz sand is nano fused quartz sand, and the particle size of the fused quartz sand is 10-20 mu m.
3. A process for preparing a modified fused silica sand according to claim 1 or 2, wherein: the method comprises the following processing steps:
(1) preparing nano fused quartz sand: ball-milling raw materials of fused quartz sand for 24 hours by using a ball mill, taking out and drying the raw materials, and sieving the dried raw materials to screen nano fused quartz sand with the particle size of 10-20 mu m;
(2) and (3) granulation and forming: adding a binding agent with the weight ratio of 1:0.5-1 into the raw materials according to the weight ratio, uniformly stirring, granulating by using a granulator, wherein the particle size is 5-10 mm, pressing the prepared powder into a sheet with the thickness of 3-5 mm by using a hydraulic machine, and tabletting under the pressure of 50 MPa;
(3) and (3) sintering: and (3) sintering the slices obtained in the step (2) by adopting a spark plasma technology to obtain the modified fused quartz sand.
4. The process according to claim 3, wherein the modified fused silica sand is prepared by the following steps: the adhesive in the step (2) is epoxy resin.
5. The process according to claim 3, wherein the modified fused silica sand is prepared by the following steps: and (4) the working pressure of the sintering equipment in the step (3) is 15-25 Mpa.
6. The process according to claim 3, wherein the modified fused silica sand is prepared by the following steps: the sintering temperature in the step (3) is 1100-1200 ℃.
7. The process according to claim 3 or 6, wherein the modified fused silica sand comprises: the sintering process of the step (3) comprises a first temperature rise process, a second temperature rise process and a heat preservation process.
8. The process according to claim 7, wherein the modified fused silica sand comprises: the first temperature raising process is to raise the temperature to 520 ℃ and 550 ℃ at a temperature raising rate of 150 ℃ and 200 ℃/min.
9. The process according to claim 7, wherein the modified fused silica sand comprises: the second temperature rise process is to rise to 1100-1200 ℃ at a temperature rise rate of 50-100 ℃/min.
10. The process according to claim 7, wherein the modified fused silica sand comprises: the heat preservation process is to preserve heat for 5-10 min at 1100-1200 ℃.
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Application publication date: 20210202 |