Fused quartz ceramic material and preparation method thereof

Abstract

The invention discloses a fused quartz ceramic material and a preparation method thereof, and relates to the technical field of fused quartz ceramics. The preparation method comprises the following steps: adding deionized water, a dispersing agent and a crystallization inhibitor into high-purity fused quartz (SiO2 content is greater than or equal to 99.9%) grading powder, mixing, grinding and drying to obtain fused quartz dry powder, adding a binder into the fused quartz dry powder, manually grinding and granulating to obtain granulated powder, and carrying out compression molding, glue discharging and sintering to obtain the fused quartz ceramic material. Through the three-stage grain composition design, the synergistic crystallization inhibitor and the two-stage sintering process, the technical defects that existing fused quartz ceramic is low in strength, poor in thermal shock resistance and prone to crystallization at the high temperature are overcome, the volume density of the prepared material is larger than or equal to 2.0 g / cm < 3 >, the bending strength is larger than or equal to 70 MPa, the water-cooling thermal shock resistance at the temperature of 1050 DEG C is larger than or equal to 50 times, and the thermal shock resistance is larger than or equal to 90%. The method is suitable for manufacturing precision structural parts in the fields of aerospace, semiconductors and the like.

Description

Technical Field

[0001] This invention relates to the field of inorganic non-metallic materials technology, specifically to a fused silica ceramic material and its preparation method. Background Technology

[0002] Fused silica ceramics are amorphous ceramic materials with high-purity silicon dioxide (SiO2 content ≥ 99.9%) as the main component, and have a low coefficient of thermal expansion (5.4 × 10⁻⁶). -7 With its low dielectric constant (3.0~3.9), excellent high-temperature resistance (long-term operating temperature ≤1200℃), and chemical stability, it has broad application prospects in high-end fields such as aero-engine combustion chambers and semiconductor wafer carriers. However, existing technologies have the following core problems: (1) Insufficient density and strength: Traditional fused silica powder has a single particle size distribution and low bulk density, resulting in high porosity of ceramic green bodies (usually ≥10%) and flexural strength generally below 70MPa, making it difficult to withstand high mechanical loads. (2) High-temperature crystallization degradation: When used above 1200℃, amorphous silica is easily converted into cristobalite (density 2.32 g / cm³). 3 This, accompanied by volume expansion (approximately 3.8%), leads to material cracking; (3) Poor thermal shock stability: Existing materials can only be ≤30 times of water cooling at 1050℃, which cannot meet the requirements of use in extreme temperature environments.

[0003] In existing technologies, although crystallization inhibitors such as zirconium oxide are added, the particle size distribution is not optimized, resulting in limited improvement in density. Furthermore, despite employing a two-stage sintering process, the matching relationship between heating rate and holding time is not clearly defined, leading to poor process stability. Therefore, developing a method for preparing fused silica ceramic materials and systems that balances high density, high strength, and thermal shock resistance is of significant technological value. Summary of the Invention

[0004] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a fused silica ceramic material, the raw materials of which include the following components by weight: 90-95 parts of high-purity fused silica graded powder, 1-2 parts of dispersant, 1-2 parts of binder, and 2-5 parts of crystallization inhibitor.

[0005] Furthermore, the dispersant is one of acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer, TH-908, ammonium citrate, and sodium dodecyl sulfate.

[0006] Furthermore, the adhesive is polyvinyl alcohol with a concentration of 5 wt%.

[0007] Further, the crystallization inhibitor is one or more of boron carbide, silicon oxynitride, calcium oxide, magnesium oxide, calcium carbonate, strontium oxide, barium oxide, yttrium oxide, zirconium oxide, aluminum oxide.

[0008] Further, a preparation method of a fused quartz ceramic material, the preparation steps are as follows: (1) The high-purity fused quartz powder is sieved into three particle size distribution range powders, namely coarse particles, medium particles and fine particles. According to the closest packing principle of powder engineering, Dinger-Funk model and measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing is calculated, and the three powders are mechanically mixed uniformly according to the optimal ratio to obtain a high-purity fused quartz graded powder; (2) According to weight parts, 1-2 parts of a dispersing agent is added to deionized water, stirred at 300-500 r / min for 10-20 min to prepare a premix, then 90-95 parts of the high-purity fused quartz graded powder, 2-5 parts of a crystallization inhibitor, zirconium oxide grinding balls and the prepared premix are poured into a ball mill tank, placed in a high-energy ball mill at a speed of 200-300 r / min, and ball milled for 4-6 h to obtain a fused quartz slurry. The fused quartz slurry is dried in an electric heating air drying oven at 80-100℃ for 18-24 h to obtain a fused quartz dry powder; (3) According to weight parts, 1-2 parts of a binder is added to the above fused quartz dry powder, and a granulating powder is obtained by hand grinding. The granulating powder is evenly laid in a metal mold cavity and pressed into a quartz blank by a tablet press. The quartz blank is placed in a corundum crucible, heated to 600-800℃ at a heating rate of 1℃ / min, and then heated to 1200-1250℃ at a heating rate of 3℃ / min, and held for 2-6 h to obtain a fused quartz ceramic.

[0009] Further, in step (1), the high-purity fused quartz graded powder has a mass percentage of (66-74%): (14-20%): (10-18%) for coarse particles, medium particles and fine particles, respectively. The particle size of the coarse particles is 20-35 um, the particle size of the medium particles is 5-8 um, and the particle size of the fine particles is 0.5-2 um.

[0010] Further, in step (1), the distribution coefficient of the Dinger-Funk model is 0.3-0.5.

[0011] Further, in step (2), the mass ratio of high-purity fused quartz graded powder: zirconium oxide grinding balls: deionized water is 3:4:7.

[0012] Further, in step (3), the parameters of the tablet press are: pressure 6-8 MPa, and pressure holding time 1-2 min.

[0013] Further, the two-stage pressureless sintering in step (3) is: heating to 600-800℃ at a heating rate of 1℃ / min, keeping for 1-2h, then heating to 1200-1250℃ at a heating rate of 3℃ / min, keeping for 2-6h.

[0014] Compared with the prior art, the present application has the beneficial effects that: (1) The present application adopts a two-stage pressureless sintering process, and in the low-temperature stage, the gradient heating mode is used for degreasing and glue removal, the decomposition products of the organic binder are slowly released, the internal stress caused by the sudden aggregation of gas in the body is avoided, and the defects such as cracking and delamination are effectively inhibited; in the high-temperature stage, during the holding process, the crystallization process is significantly delayed by hindering the lattice rearrangement of the amorphous network of silicon dioxide to cristobalite / tridymite through the preset crystallization inhibitor in the system, and the structural stability and density of the ceramic matrix at high temperature are ensured.

[0015] (2) The present application improves the flowability of the granulated particles by grading the particle size of the purified fused quartz ceramic, solves the problems of bridging and uneven density of raw materials during dry pressing, improves the density of the body, reduces the voids between particles, reduces the sintering shrinkage, improves the thermal shock resistance of the fused quartz ceramic, and the mutual support of the graded particles can improve the compressive strength of the composite material. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 SEM photos of the cross sections of fused quartz ceramics prepared at different sintering temperatures and holding times, (a) 1250℃ / 2h, (b) 1250℃ / 6h, (c) 1275℃ / 2h, (d) 1275℃ / 6h, (e) 1300℃ / 2h, (f) 1300℃ / 6h. DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0018] Example 1; (1) high-purity fused quartz powder is sieved into three kinds of particle size distribution range, namely coarse particles, medium particles and fine particles, according to the principle of powder engineering closest packing, Dinger-Funk model and the measured powder particle size distribution curve to calculate the optimal ratio of three kinds of powder to achieve the closest packing, according to the optimal ratio of three kinds of powder is mixed uniformly to get high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles and fine particles is 66%:16%:18%; (2) according to the weight part, 1 part of TH-908 is added in deionized water, stirred at 300 r / min for 20 min to prepare a premix, then 90 parts of high-purity fused quartz graded powder, 2 parts of silicon oxynitride, zirconium oxide grinding ball (d=10mm) and the prepared premix are poured into the ball mill tank, and placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconium oxide grinding ball: deionized water is 3:4:7, the rotation speed of high-energy ball mill is 200 r / min, and the ball milling time is 4 h, to obtain a fused quartz slurry, and the fused quartz slurry is placed in an electric heating air drying oven at 100℃ for 24 h to obtain a fused quartz dry powder; (3) according to the weight part, 1 part of polyvinyl alcohol is added in the above fused quartz dry powder, and the granulation powder is obtained by hand grinding, which is uniformly laid in the metal mold cavity and pressed into a tablet by a tablet press with a pressure of 6 MPa and a pressure holding time of 1 min to obtain a quartz blank; the quartz blank is placed in a corundum crucible, heated to 600℃ at a heating rate of 1℃ / min, and kept for 1 h, then heated to 1250℃ at a heating rate of 3℃ / min, and kept for 2 h to obtain a fused quartz ceramic.

[0019] Example 2; (1) high-purity fused quartz powder is sieved into three kinds of particle size distribution range, namely coarse particles, medium particles and fine particles, according to the principle of powder engineering closest packing, Dinger-Funk model and the measured powder particle size distribution curve to calculate the optimal ratio of three kinds of powder to achieve the closest packing, according to the optimal ratio of three kinds of powder is mixed uniformly to get high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles and fine particles is 68%:15%:17%; (2) according to weight parts, 1.5 parts of TH-908 is added in deionized water, stirred at 400 r / min for 15 min to prepare a premix, then 92 parts of high-purity fused quartz graded powder, 3 parts of silicon oxynitride, zirconia grinding balls (d=10 mm) and the prepared premix are poured into a ball mill tank, which is placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconia grinding ball: deionized water is 3:4:7, the rotation speed of the high-energy ball mill is 250 r / min, and the ball milling is carried out for 5 h to obtain a fused quartz slurry, and the fused quartz slurry is placed in an electric heating air drying oven at 100℃ for 24 h to obtain a fused quartz dry powder; (3) according to weight parts, 1.5 parts of polyvinyl alcohol is added in the above fused quartz dry powder, which is ground by hand to obtain a granulated powder, the granulated powder is evenly laid in a metal mold cavity, and a tablet press is used to press and form, the pressure is 7 MPa, and the pressure holding time is 1.5 min to obtain a quartz blank; the quartz blank is placed in a corundum crucible, first heated to 650℃ at a heating rate of 1℃ / min, and then heated to 1250℃ at a heating rate of 3℃ / min, and kept for 6 h to obtain a fused quartz ceramic.

[0020] Example 3; (1) high-purity fused quartz powder is sieved into three particle size distribution range powders, namely coarse particles, medium particles and fine particles, according to the powder engineering closest packing principle, Dinger-Funk model and measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing is calculated, and the three powders are mechanically mixed according to the optimal ratio to obtain high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles and fine particles is 70%:20%:10%; (2) according to weight parts, 2 parts of TH-908 is added in deionized water, stirred at 500 r / min for 20 min to prepare a premix, then 95 parts of high-purity fused quartz graded powder, 5 parts of silicon oxynitride, zirconia grinding balls (d=10 mm) and the prepared premix are poured into a ball mill tank, which is placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconia grinding ball: deionized water is 3:4:7, the rotation speed of the high-energy ball mill is 300 r / min, and the ball milling is carried out for 6 h to obtain a fused quartz slurry, and the fused quartz slurry is placed in an electric heating air drying oven at 100℃ for 24 h to obtain a fused quartz dry powder; (3) According to the weight parts, 2 parts of polyvinyl alcohol is added to the above fused quartz dry powder, which is ground by hand to obtain a granulating powder. The granulating powder is evenly laid in the metal mold cavity and pressed into shape by a tablet press with a pressure of 8 MPa and a pressure holding time of 2 min to obtain a quartz blank. The quartz blank is placed in a corundum crucible, heated to 700℃ at a heating rate of 1℃ / min first, and then heated to 1275℃ at a heating rate of 3℃ / min, and kept for 2h, to obtain a fused quartz ceramic.

[0021] Example 4; (1) The high-purity fused quartz powder is sieved into three particle size distribution range powders, namely coarse particles, medium particles and fine particles. According to the principle of powder engineering closest packing, the Dinger-Funk model and the measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing is calculated. The three powders are mechanically mixed according to the optimal ratio to obtain a high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles and fine particles is 72%:14%:14%; (2) According to the weight parts, 1.3 parts of TH-908 is added to deionized water, stirred at 400 r / min for 15 min to prepare a premix solution. Then 91 parts of high-purity fused quartz graded powder, 3.5 parts of silicon oxynitride, and zirconium oxide grinding balls (d=10mm) are poured into a ball mill tank, which is placed in a high-energy ball mill. The mass ratio of high-purity fused quartz graded powder: zirconium oxide grinding ball: deionized water is 3:4:7. The rotation speed of the high-energy ball mill is 250 r / min. The ball milling is carried out for 4h to obtain a fused quartz slurry. The fused quartz slurry is dried in an electric heating air drying oven at 100℃ for 24h to obtain a fused quartz dry powder; (3) According to the weight parts, 1.2 parts of polyvinyl alcohol is added to the above fused quartz dry powder, which is ground by hand to obtain a granulating powder. The granulating powder is evenly laid in the metal mold cavity and pressed into shape by a tablet press with a pressure of 7 MPa and a pressure holding time of 1.5 min to obtain a quartz blank. The quartz blank is placed in a corundum crucible, heated to 720℃ at a heating rate of 1℃ / min first, and then heated to 1275℃ at a heating rate of 3℃ / min, and kept for 6h, to obtain a fused quartz ceramic.

[0022] Example 5; (1) The high-purity fused quartz powder is sieved into three particle size distribution range powders, namely coarse particles, medium particles and fine particles. According to the principle of powder engineering closest packing, the Dinger-Funk model and the measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing is calculated. The three powders are mechanically mixed according to the optimal ratio to obtain a high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles and fine particles is 66%:15%:19%; (2) according to weight parts, 1.8 parts of TH-908 is added in deionized water, stirred at 400 r / min for 15 min to prepare a premix, then 93 parts of high-purity fused quartz graded powder, 4 parts of silicon oxynitride, zirconia grinding balls (d=10 mm) and the prepared premix are poured into a ball mill tank, which is placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconia grinding ball: deionized water is 3:4:7, the rotation speed of the high-energy ball mill is 300 r / min, and the ball milling is carried out for 5 h to obtain a fused quartz slurry, and the fused quartz slurry is placed in an electric heating air drying oven at 100℃ for 20 h to obtain a fused quartz dry powder; (3) according to weight parts, 1.9 parts of polyvinyl alcohol is added in the above fused quartz dry powder, which is ground by hand to obtain a granulated powder, the granulated powder is uniformly laid in a metal mold cavity, and a tablet press is used to press and form, the pressure is 7 MPa, and the pressure holding time is 1.7 min to obtain a quartz blank; the quartz blank is placed in a corundum crucible, first heated to 750℃ at a heating rate of 1℃ / min, and then heated to 1300℃ at a heating rate of 3℃ / min, and kept for 2 h to obtain a fused quartz ceramic.

[0023] Example 6: (1) high-purity fused quartz powder is sieved into three particle size distribution range powders, namely coarse particles, medium particles and fine particles, according to the powder engineering closest packing principle, Dinger-Funk model and measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing is calculated, and the three powders are mechanically mixed according to the optimal ratio to obtain high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles and fine particles is 74%:14%:12%; (2) according to weight parts, 1.5 parts of TH-908 is added in deionized water, stirred at 400 r / min for 20 min to prepare a premix, then 92 parts of high-purity fused quartz graded powder, 3 parts of silicon oxynitride, zirconia grinding balls (d=10 mm) and the prepared premix are poured into a ball mill tank, which is placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconia grinding ball: deionized water is 3:4:7, the rotation speed of the high-energy ball mill is 300 r / min, and the ball milling is carried out for 6 h to obtain a fused quartz slurry, and the fused quartz slurry is placed in an electric heating air drying oven at 100℃ for 24 h to obtain a fused quartz dry powder; (3) 1.1 parts of polyvinyl alcohol by weight was added to the above fused quartz dried powder, and hand grinding was performed to obtain granulation powder. The granulation powder was uniformly laid in a metal mold cavity, and a tablet press was used for compression molding, with a pressure of 7 MPa and a pressure holding time of 1 min, to obtain a quartz blank. The quartz blank was placed in a corundum crucible, heated to 800°C at a heating rate of 1°C / min, and held for 2 h, and then heated to 1300°C at a heating rate of 3°C / min, and held for 6 h, to obtain a fused quartz ceramic.

[0024] Comparative Example 1; (1) 1.8 parts of TH-908 was added to deionized water, stirred at 400 r / min for 15 min to prepare a premix solution, and then 93 parts of high-purity fused quartz powder, 4 parts of silicon oxynitride, and zirconia grinding balls (d = 10 mm) were added to a ball mill tank, which was placed in a high-energy ball mill. The mass ratio of high-purity fused quartz powder: zirconia grinding balls: deionized water was 3:4:7, and the rotation speed of the high-energy ball mill was 300 r / min. Ball milling was performed for 5 h, and then the fused quartz slurry was dried in an electric heating air drying oven at 100°C for 20 h to obtain a fused quartz dried powder; (2) 1.9 parts of polyvinyl alcohol by weight was added to the above fused quartz dried powder, and hand grinding was performed to obtain granulation powder. The granulation powder was uniformly laid in a metal mold cavity, and a tablet press was used for compression molding, with a pressure of 7 MPa and a pressure holding time of 1.7 min, to obtain a quartz blank. The quartz blank was placed in a corundum crucible, heated to 750°C at a heating rate of 1°C / min, and held for 1.5 h, and then heated to 1300°C at a heating rate of 3°C / min, and held for 2 h, to obtain a fused quartz ceramic.

[0025] Comparative Example 2; (1) The high-purity fused quartz powder was sieved into three particle size distribution ranges, i.e. coarse particles, medium particles and fine particles. According to the principle of closest packing of powder engineering, Dinger-Funk model and actual measurement of powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing was calculated, and the three powders were mechanically mixed uniformly according to the optimal ratio to obtain a high-purity fused quartz graded powder. The mass percentage of coarse particles, medium particles and fine particles was 66%:15%:19%. (2) according to weight parts, 1.8 parts of TH-908 is added in deionized water, stirred at 400 r / min for 15 min to prepare a premix solution, then 93 parts of high-purity fused quartz graded powder, zirconia grinding balls (d=10 mm) and the prepared premix solution are poured into a ball mill tank, and placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconia grinding ball: deionized water is 3:4:7, the rotation speed of the high-energy ball mill is 300 r / min, and the ball milling is carried out for 5 h to obtain a fused quartz slurry, and the fused quartz slurry is placed in an electric heating air drying oven at 100℃ for 20 h to obtain a fused quartz dry powder; (3) according to weight parts, 1.9 parts of polyvinyl alcohol is added in the above fused quartz dry powder, and hand grinding is carried out to obtain a granulated powder, which is uniformly laid in a metal mold cavity and pressed into a shape by a tablet press with a pressure of 7 MPa and a pressure holding time of 1.7 min to obtain a quartz blank; the quartz blank is placed in a corundum crucible, heated to 750℃ at a heating rate of 1℃ / min first, and then heated to 1300℃ at a heating rate of 3℃ / min, and kept for 2 h to obtain a fused quartz ceramic.

[0026] Comparative Example 3: (1) high-purity fused quartz powder is sieved into three particle size distribution range powders, namely coarse particles, medium particles and fine particles, according to the powder engineering closest packing principle, Dinger-Funk model and the measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing is calculated, and the three powders are mechanically mixed uniformly according to the optimal ratio to obtain high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles and fine particles is 66%:15%:19%; (2) according to weight parts, 1.8 parts of TH-908 is added in deionized water, stirred at 400 r / min for 15 min to prepare a premix solution, then 93 parts of high-purity fused quartz graded powder, 4 parts of boron carbide, zirconia grinding balls (d=10 mm) and the prepared premix solution are poured into a ball mill tank, and placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconia grinding ball: deionized water is 3:4:7, the rotation speed of the high-energy ball mill is 300 r / min, and the ball milling is carried out for 5 h to obtain a fused quartz slurry, and the fused quartz slurry is placed in an electric heating air drying oven at 100℃ for 20 h to obtain a fused quartz dry powder; (3) 1.9 parts of polyvinyl alcohol by weight was added to the above fused quartz dry powder, and hand grinding was performed to obtain granulated powder. The granulated powder was uniformly laid in a metal mold cavity, and a tablet press was used for compression molding, with a pressure of 7 MPa and a pressure holding time of 1.7 min, to obtain a quartz blank. The quartz blank was placed in a corundum crucible, heated to 750°C at a heating rate of 1°C / min, and held for 1.5 h, and then heated to 1300°C at a heating rate of 3°C / min, and held for 2 h, to obtain a fused quartz ceramic.

[0027] Comparative Example 4; (1) high-purity fused quartz powder was sieved into three particle size distribution ranges, namely coarse particles, medium particles, and fine particles. According to the principle of powder engineering closest packing, the Dinger-Funk model, and the measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing was calculated. The three powders were mechanically mixed uniformly according to the optimal ratio to obtain a high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles, and fine particles was 66%:15%:19%; (2) 1.8 parts of sodium dodecyl sulfate by weight was added to deionized water, stirred at 400 r / min for 15 min to prepare a premix solution. Then 93 parts of high-purity fused quartz graded powder, 4 parts of yttrium oxide, and zirconium oxide grinding balls (d=10 mm) were added to a ball mill tank, and placed in a high-energy ball mill. The mass ratio of high-purity fused quartz graded powder: zirconium oxide grinding balls: deionized water was 3:4:7. The rotation speed of the high-energy ball mill was 300 r / min, and the ball milling time was 5 h. The fused quartz slurry was obtained and dried in an electric heating air drying oven at 100°C for 20 h to obtain a fused quartz dry powder; (3) 1.9 parts of polyvinyl alcohol by weight was added to the above fused quartz dry powder, and hand grinding was performed to obtain granulated powder. The granulated powder was uniformly laid in a metal mold cavity, and a tablet press was used for compression molding, with a pressure of 7 MPa and a pressure holding time of 1.7 min, to obtain a quartz blank. The quartz blank was placed in a corundum crucible, heated to 750°C at a heating rate of 1°C / min, and held for 1.5 h, and then heated to 1300°C at a heating rate of 3°C / min, and held for 2 h, to obtain a fused quartz ceramic.

[0028] Comparative Example 5; (1) high-purity fused quartz powder was sieved into three particle size distribution ranges, namely coarse particles, medium particles, and fine particles. According to the principle of powder engineering closest packing, the Dinger-Funk model, and the measured powder particle size distribution curve, the optimal ratio of the three powders to achieve the closest packing was calculated. The three powders were mechanically mixed uniformly according to the optimal ratio to obtain a high-purity fused quartz graded powder, wherein the mass percentage of coarse particles, medium particles, and fine particles was 66%:15%:19%; (2) 1.8 parts of acrylic acid-2-acrylamide-2-methylpropane sulfonic acid copolymer was added in deionized water according to weight parts, and a premix liquid was prepared by stirring at 400 r / min for 15 min, then 93 parts of high-purity fused quartz graded powder, 4 parts of calcium oxide, and zirconium oxide grinding balls (d = 10 mm) and the prepared premix liquid were poured into a ball mill tank, which was placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz graded powder: zirconium oxide grinding balls: deionized water was 3:4:7, the rotation speed of the high-energy ball mill was 300 r / min, and the ball milling was performed for 5 h to obtain a fused quartz slurry, which was dried in an electric heating air drying oven at 100℃ for 20 h to obtain a fused quartz dry powder; (3) 1.9 parts of polyvinyl alcohol was added in the above fused quartz dry powder according to weight parts, and a granulation powder was obtained by manual grinding, which was uniformly laid in a metal mold cavity and molded by a tablet press with a pressure of 7 MPa and a pressure holding time of 1.7 min to obtain a quartz blank; the quartz blank was placed in a corundum crucible, heated to 750℃ at a heating rate of 1℃ / min first, and then heated to 1300℃ at a heating rate of 3℃ / min, and kept for 2 h to obtain a fused quartz ceramic.

[0029] Comparative Example 6: (1) 1.8 parts of TH-908 was added in deionized water according to weight parts, and a premix liquid was prepared by stirring at 400 r / min for 15 min, then 93 parts of high-purity fused quartz powder, zirconium oxide grinding balls (d = 10 mm) and the prepared premix liquid were poured into a ball mill tank, which was placed in a high-energy ball mill, wherein the mass ratio of high-purity fused quartz powder: zirconium oxide grinding balls: deionized water was 3:4:7, the rotation speed of the high-energy ball mill was 300 r / min, and the ball milling was performed for 5 h to obtain a fused quartz slurry, which was dried in an electric heating air drying oven at 100℃ for 20 h to obtain a fused quartz dry powder; (3) 1.9 parts of polyvinyl alcohol was added in the above fused quartz dry powder according to weight parts, and a granulation powder was obtained by manual grinding, which was uniformly laid in a metal mold cavity and molded by a tablet press with a pressure of 7 MPa and a pressure holding time of 1.7 min to obtain a quartz blank; the quartz blank was placed in a corundum crucible, heated to 750℃ at a heating rate of 1℃ / min first, and then heated to 1300℃ at a heating rate of 3℃ / min, and kept for 2 h to obtain a fused quartz ceramic.

[0030] Effect Example Test method: The bulk density was tested according to GB / T4100-2015 standard, the total porosity was tested according to GB / T25995-2010 standard, the bending strength was tested according to GB / T4741-1999 standard, the dielectric constant was tested according to GB / T11310-1989 standard, the linear expansion coefficient was tested according to GB / T3810.8-2006 standard, the thermal shock resistance was tested according to GB / T3810.9-2016 standard, and the results are shown in Table 1.

[0031] Table 1

[0032] From the data results of Examples 1-6 and Comparative Examples 1-6 and Table 1, it can be seen that the fused quartz ceramic material prepared in the present application exhibits good comprehensive performance at 1300℃ without pressure sintering for 2h, has better high temperature stability (linear expansion coefficient = 7.11x10 -7 / ℃), excellent density (total porosity = 5.5%, bulk density = 2.11g / cm 3 , and at the same time has good strength and is not easy to crack (bending strength 91.5MPa, thermal shock resistance 1050℃ water cooling 57 times).

[0033] It is obvious to those skilled in the art that the present application is not limited to the details of the above exemplary embodiments, and the present application can be implemented in other specific forms without departing from the spirit or essential characteristics of the present application. Therefore, the embodiments should be regarded as exemplary and non-limiting in any respect, and the scope of the present application is defined by the appended claims rather than the above description, and therefore all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present application. Any mark in the claims should not be regarded as limiting the involved claims.

Claims

1. A fused quartz ceramic material, characterized by, The fused quartz ceramic material comprises the following components by weight: high-purity fused quartz graded powder 90-95 parts, dispersing agent 1-2 parts, binder 1-2 parts, and crystallization inhibitor 2-5 parts.

2. A fused quartz ceramic material according to claim 1, wherein The dispersing agent is one of acrylic acid-2-acrylamide-2-methylpropane sulfonic acid copolymer, TH-908, ammonium citrate, and sodium dodecyl sulfate.

3. The fused quartz ceramic material of claim 1, wherein The binder is polyvinyl alcohol with a concentration of 5wt%.

4. The fused quartz ceramic material of claim 1, wherein The crystallization inhibitor is one or a mixture of more than one of boron carbide, silicon oxynitride, calcium oxide, magnesium oxide, calcium carbonate, strontium oxide, barium oxide, yttrium oxide, zirconium oxide, and aluminum oxide.

5. A method of making the fused quartz ceramic material of claim 1, wherein, The preparation steps include: (1) The high-purity fused quartz powder is sieved into three kinds of particle size distribution range, i.e. coarse particles, medium particles, and fine particles. According to the closest packing principle of powder engineering, Dinger-Funk model, and the measured powder particle size distribution curve, the optimal ratio of the three kinds of powder to achieve the closest packing is calculated, and the three kinds of powder are mechanically mixed uniformly according to the optimal ratio to obtain high-purity fused quartz graded powder; (2) According to the weight, 1-2 parts of dispersing agent is added to deionized water, stirred at 300-500 r / min for 10-20 min to prepare a premix, then 90-95 parts of high-purity fused quartz graded powder and 2-5 parts of crystallization inhibitor, zirconium oxide grinding balls, and the prepared premix are poured into a ball mill tank, placed in a high-energy ball mill at a speed of 200-300 r / min, and ball milled for 4-6 h to obtain a fused quartz slurry. The fused quartz slurry is dried in an electric heating air drying oven at 80-100℃ for 18-24 h to obtain a fused quartz dry powder; (3) According to the weight, 1-2 parts of binder is added to the above fused quartz dry powder, which is ground by hand to obtain granulating powder. The granulating powder is evenly laid in a metal mold cavity and pressed into a tablet by a tablet press to obtain a quartz blank. The quartz blank is placed in a corundum crucible and subjected to two-stage pressureless sintering to obtain a fused quartz ceramic.

6. The method of claim 5, wherein the fused quartz ceramic material is prepared by the steps of: In step (1), the mass percentage of the coarse particles, medium particles, and fine particles of the high-purity fused quartz graded powder is (66-74%):(14-20%):(10-18%), the particle size of the coarse particles is 20-35 um, the particle size of the medium particles is 5-8 um, and the particle size of the fine particles is 0.5-2 um.

7. The method of claim 5, wherein the fused quartz ceramic material is prepared by the steps of: providing a fused quartz substrate; and coating the fused quartz substrate with a coating layer of a ceramic material. In step (1), the distribution coefficient of the Dinger-Funk model is 0.3-0.

5.

8. The method of claim 5, wherein the fused quartz ceramic material is prepared by the steps of: providing a fused quartz material; and doping the fused quartz material with a dopant selected from the group consisting of aluminum, boron, phosphorous, and combinations thereof. In step (2), the mass ratio of high-purity fused quartz: zirconium oxide grinding balls: deionized water is 3:4:

7.

9. The method of claim 5, wherein the fused quartz ceramic material is prepared by the steps of: providing a fused quartz material; and doping the fused quartz material with a dopant selected from the group consisting of aluminum, boron, phosphorous, and combinations thereof. In step (3), the parameters of the tablet press are: pressure 6-8 MPa, and pressure holding time 1-2 min.

10. The method of claim 5, wherein the fused quartz ceramic material is prepared by the steps of: providing a fused quartz material; and doping the fused quartz material with a dopant selected from the group consisting of aluminum, boron, phosphorous, and combinations thereof. In step (3), the two-stage pressureless sintering is: heating to 600-800℃ at a rate of 1℃ / min, holding for 1-2 h, then heating to 1250-1300℃ at a rate of 3℃ / min, and holding for 2-6 h.

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