CN109369163B - Preparation method of large solid quartz ceramic material - Google Patents
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- CN109369163B CN109369163B CN201811220088.2A CN201811220088A CN109369163B CN 109369163 B CN109369163 B CN 109369163B CN 201811220088 A CN201811220088 A CN 201811220088A CN 109369163 B CN109369163 B CN 109369163B
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Abstract
The invention relates to a preparation method of a large solid quartz ceramic material, belonging to the technical field of quartz ceramic products. The preparation method comprises the following steps: preparing a mixture: weighing the following substances in percentage by mass: 15-35% of quartz coarse particles, 20-40% of quartz fine particles, 0.99-5.66% of binding agent, 15-30% of quartz fine powder, 8-20% of quartz micro powder and 8-15% of spherical quartz micro powder, and uniformly mixing to form a mixture; isostatic pressing: filling the mixture obtained in the step 1 into a rubber mold, vacuumizing, and performing compression molding under isostatic pressure of 80-150MPa to form a blank; the firing process comprises the following steps: and (3) sintering the blank in the step (2) according to a sintering system, and cooling to room temperature along with the furnace after stopping the fire. The preparation method provided by the invention is scientific, reasonable, simple and feasible, and the prepared quartz ceramic material has the characteristics of good microstructure uniformity, low porosity, high volume density and high normal-temperature compressive strength.
Description
Technical Field
The invention relates to a preparation method of a large solid quartz ceramic material, belonging to the technical field of quartz ceramic products.
Background
The quartz glass ceramic is abbreviated as quartz ceramic, and has a small thermal expansion coefficient of only 0.54 × 10-6/° c, so that it has very excellent resistance to quenching and quenching heat; the quartz ceramic has extremely low thermal conductivity, and the thermal conductivity is only 2.1W/m.K, so the quartz ceramic is an ideal heat insulating material; the quartz ceramic has excellent chemical stability, hardly reacts with various metal melts, and has very good erosion resistance to various glass slags. Therefore, the gate brick, the cover brick, the breast wall brick and the ceramic crucible which are made of quartz glass as raw materials are widely applied to the melting of materials such as a float glass furnace, rare metals, special glass, polycrystalline silicon and the like. With the continuous expansion of the application range of fused quartz ceramics, the development of the molding methods for preparing the fused quartz ceramics by slip casting, gel casting and the like is faster, but the methods are more suitable for preparing the fused quartz ceramicsThe products prepared by the molding process generally have the defects of poor microstructure uniformity, long product production period caused by difficult dehydration, low efficiency of manufacturing large solid quartz ceramic blanks, easy blank sintering and cracking and the like, and are difficult to adapt to the requirement of large-scale industrial production of large solid quartz ceramic materials.
The cold isostatic pressing technology is an ideal method for forming high-performance and high-reliability ceramics at present. However, the fused silica ceramic material is glass material, so that the rigidity is high and the compressibility is low. The technology for isostatic pressing of fused silica ceramics disclosed in the prior art comprises the steps of drying a certain amount of fused silica powder, adding a certain amount of PVA solution, crushing, sieving, using powder granules of 150-30 meshes, and carrying out isostatic pressing molding in a small radome rubber mold under 110MPa, wherein the optimal sintering temperature is determined to be 1250 ℃ through experiments (see silicate report (ISSN1001-1625) No. 26, Vol. 4.26, 2007, No. 2 research on isostatic pressing of fused silica ceramics).
Chinese patent application No. 200610070310.6, discloses a method for preparing quartz ceramic by isostatic pressing: the preparation method comprises the steps of adding a dispersing agent, a binder, a pore-forming agent and a plasticizer into fused quartz to prepare slurry, controlling the particle size of fused quartz particles to be between 150 and 325 meshes, wherein the mass of the fused quartz particles is 0-60% of the total mass of the fused quartz, measuring d90 by a laser particle sizer to be less than 60 mu m, preparing 80-250-mesh particles by spray granulation for isostatic pressing, controlling the forming pressure to be between 20 and 300MPa, preparing products such as a quartz ceramic radome, a quartz ceramic flashboard brick and the like, and solving the problems of poor uniformity of all-powder injection-set forming and gel injection-molding microstructure, long production period of the products due to difficult dehydration and the like. However, for the quartz ceramic material containing the glassy coarse particles, the glassy fused quartz particles are easy to cut the rubber mold, so that the molding is difficult; and for large solid quartz ceramic materials, the sintering is fully carried out according to the prior art, the sintering heat preservation time needs to be prolonged, and the prolonging of the heat preservation time can cause cristobalite and influence the service performance of the fused quartz material. The search shows that the preparation method of the large solid quartz ceramic material is not found.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a large solid quartz ceramic material, which is scientific, reasonable, simple and feasible, and the prepared quartz ceramic material has the characteristics of low cristobalite conversion rate, good microstructure uniformity, low porosity, high volume density and high normal-temperature compressive strength.
The preparation method of the large solid quartz ceramic material comprises the following steps:
1) preparing a mixture: weighing the following substances in percentage by mass: 15-35% of quartz coarse particles, 20-40% of quartz fine particles, 0.99-5.66% of binding agent, 15-30% of quartz fine powder, 8-20% of quartz micro powder and 8-15% of spherical quartz micro powder, and uniformly mixing to form a mixture;
2) isostatic pressing: filling the mixture obtained in the step 1 into a rubber mold, vacuumizing, and performing compression molding under isostatic pressure of 80-150MPa to form a blank;
3) the firing process comprises the following steps: and (3) sintering the blank in the step (2), wherein the sintering system is as follows:
and (5) cooling to room temperature along with the furnace after stopping the fire.
In the step 1, the particle size of the quartz coarse particles is 1-3 mm; the particle size of the quartz fine particles is 0.1-1 mm; the grain size of the quartz fine powder is more than 0 and less than or equal to 44 mu m; the particle size of the quartz micro powder is more than 0 and less than or equal to 5 mu m; the particle size of the spherical quartz micro powder is more than 0 and less than or equal to 2 mu m.
Preferably, the mass ratio of the quartz micro powder to the spherical quartz micro powder is 1:1, so that the particle grading of the fine powder is realized, the sintering of a green body can be effectively promoted, and the compactness of the ceramic green body is improved.
The binding agent is one or two of PVA solution or silica sol.
In the step 1, after a bonding agent is added into the quartz coarse particles and the quartz fine particles, mixing is carried out for 10-20 minutes, so that the bonding agent is uniformly coated on the surfaces of the fused quartz coarse particles and the fused quartz fine particles, and then quartz fine powder, quartz micro powder and spherical quartz micro powder are added, and mixing is carried out for 10-20 minutes, so as to form a mixture.
In the step 2, a paperboard with the thickness of 3-5mm is firstly filled in the rubber mould, then the mixture is filled in the rubber mould, and then the rubber mould is vacuumized, wherein the mixture does not directly contact the mould.
The rubber mould lining paperboard solves the problems that molten quartz particles are in a glass state, have sharp corners, and easily cut the rubber mould in an isostatic pressing process, so that a blank body is permeated into an isostatic pressing hydraulic system and fails.
Wherein, the isostatic compaction pressure is lower than 80MPa, the strength of the blank is low, and the blank is easy to crack in the moving and kiln loading processes. Above 150Mpa, part of the fused silica particles are crushed, resulting in a decrease in the strength of the green body and also easily cracked during movement and kiln loading.
The length of the large solid quartz ceramic material is 600-3100mm, the thickness is 150-500mm, and the width is 400-1000 mm.
Preferably, the size of the large solid quartz ceramic material is 900-2000mm, the thickness is 200-500mm, and the width is 600-1000 mm.
SiO in the quartz coarse particles, the quartz fine powder, the quartz micro powder and the spherical quartz micro powder2The content of the cristobalite is more than or equal to 99.8 percent, and the conversion rate of the cristobalite is less than or equal to 3 percent.
The bulk density of the large solid quartz ceramic material is more than or equal to 1.88g/cm3The apparent porosity is less than or equal to 15 percent; SiO 22The content of the cristobalite is more than or equal to 99.8 percent, and the conversion rate of the cristobalite is less than or equal to 3 percent.
For a large solid quartz ceramic material blank, the sintering temperature is raised to 750-900 ℃ and the heat is preserved for 12-36h, and the sintering qualification rate of the blank can reach more than 90%. The added organic PVA solution is completely removed by burning loss at the temperature, so that the sintering qualification rate of the blank is greatly improved, and the spherical quartz micro powder with the grain diameter less than or equal to 5 mu m or the grain diameter less than or equal to 2 mu m is primarily sintered to the surface of large grains at the temperature, thereby integrally improving the medium-temperature strength of the blank. In addition, in the heat preservation process of 750-900 ℃ for 12-36h, the porosity of the product can be obviously reduced, and the volume density and the normal-temperature compressive strength can be improved.
Compared with the prior art, the invention has the following beneficial effects:
1. the quartz coarse particles, the quartz fine powder, the quartz micro powder and the spherical quartz micro powder which are sold in the market are mixed, the sintering of the blank body under the medium temperature is effectively promoted through the particle grading of the fine powder and the micro powder, and the problem of cristobalite caused by prolonging the sintering heat preservation time of a large blank body is solved;
2. for a large solid ceramic material blank, the temperature is kept at 750-;
3. the problem that the rubber mold is damaged because the glass-state fused quartz particles are easy to cut the rubber mold in the processes of loading and isostatic pressing is solved by adopting the rubber mold lining paperboard;
4. the preparation method provided by the invention is scientific and reasonable, simple and feasible, has high production efficiency, and is beneficial to popularization and application.
Detailed Description
The present invention will be further described with reference to the following examples.
In the invention, the particle size of the powder is measured by a laser particle sizer, and the median diameter refers to the corresponding particle size when the cumulative particle size distribution percentage of a sample reaches 50%. Its physical meaning is that the particle size is greater than 50% of its particles and less than 50% of its particles, but does not relate to the aspect ratio of the particles.
In the invention, the volume density and the porosity are measured by GB/T2997-2000 test methods of the volume density, the apparent porosity and the true porosity of the compact shaped refractory product. The normal temperature compressive strength is measured by a GB/T5072.1-1998 test method for the normal temperature compressive strength of the compact shaped refractory product. The chemical components are measured by a GB-T21114-2007 refractory material X-ray fluorescence spectrum chemical analysis fusion-cast glass sheet method. The cristobalite proportion is detected by referring to a YB/T172-2000 silica brick quantitative analysis X-ray diffraction method.
Example 1
1) Preparing a mixture: the quartz material adopts SiO with the purity of commercial products according to mass percentage2Fused quartz particles with content of more than 99.9 percentWeighing 35% of quartz coarse particles, 30% of quartz fine particles, 1-3mm of quartz coarse particles and 0.1-1mm of quartz fine particles according to weight percentage, adding 2% of PVA solution into a stirrer, stirring for 15 minutes, then adding 17% of quartz fine powder with the particle size of more than 0 and less than or equal to 44 microns, 8% of quartz fine powder with the particle size of more than 0 and less than or equal to 5 microns and 8% of spherical quartz fine powder with the particle size of more than 0 and less than 2 microns, and stirring for 15 minutes to form a mixture;
2) a 3mm thick paperboard is lined in the rubber mold, the paperboard is tightly attached to the rubber mold, the mixture is filled, and after the vacuum pumping is carried out for 40 minutes, the paperboard is pressed and formed under 120MPa isostatic pressure; the green body obtained by pressing had a dimension of 2100mm in length, 370mm in thickness and 750mm in width.
3) Taking out the formed blank body, and carefully cleaning the paperboard attached to the surface of the blank body;
4) loading into a gas kiln, and sintering according to the following sintering schedule:
and cooling along with the furnace after stopping the fire.
And cutting a sample after the blank is cooled to room temperature, and detecting the volume density, the apparent porosity, the room-temperature compressive strength and the cristobalite proportion. The quartz ceramic materials described in examples 2 to 8 were prepared in the same manner as in example 1, using the raw materials in the amounts indicated in Table 1; the molding pressure and the firing system are shown in Table 2; examples 1-2 the rate of temperature rise was the same as in example 1, and examples 3-4 were as follows:
cooling along with the furnace after stopping the fire;
examples 5-6 the rate of temperature rise is as follows:
cooling along with the furnace after stopping the fire;
examples 7-8 the rate of temperature rise was as follows:
cooling along with the furnace after stopping the fire;
the data for the tests of examples 1-8 are shown in Table 3.
TABLE 1 weight percentages of the raw materials used in examples 1-8
TABLE 2 examples 1-8 Molding pressure and firing schedule
Table 3 results of performance testing of examples 1-8
Claims (6)
1. A preparation method of a large solid quartz ceramic material is characterized by comprising the following steps: the method comprises the following steps:
1) preparing a mixture: weighing the following substances in percentage by mass: 15-35% of quartz coarse particles, 20-40% of quartz fine particles, 0.99-5.66% of binding agent, 15-30% of quartz fine powder, 8-20% of quartz micro powder and 8-15% of spherical quartz micro powder, and uniformly mixing to form a mixture;
2) isostatic pressing: filling the mixture obtained in the step 1 into a rubber mold, vacuumizing, and performing compression molding under isostatic pressure of 80-150MPa to form a blank;
3) the firing process comprises the following steps: and (3) sintering the blank in the step (2), wherein the sintering system is as follows:
in the step 1, the particle size of quartz coarse particles is 1-3 mm; the particle size of the quartz fine particles is 0.1-1 mm; the grain size of the quartz fine powder is more than 0 and less than or equal to 44 mu m; the particle size of the quartz micro powder is more than 0 and less than or equal to 5 mu m; the particle size of the spherical quartz micro powder is more than 0 and less than or equal to 2 mu m;
in step 2, a paperboard with the thickness of 3-5mm is filled in the rubber mold, then the mixture is filled in the rubber mold, and then the rubber mold is vacuumized, wherein the mixture does not directly contact the mold.
2. The method for preparing a large solid quartz ceramic material according to claim 1, wherein: the bonding agent is one or two of PVA solution or silica sol.
3. The method for preparing a large solid quartz ceramic material according to claim 1, wherein: the length of the large solid quartz ceramic material is 600-3100mm, the thickness is 150-500mm, and the width is 400-1000 mm.
4. The method for preparing a large solid quartz ceramic material according to claim 3, wherein: the large solid quartz ceramic material has the dimensions of 900-2000mm in length, 200-500mm in thickness and 600-1000mm in width.
5. The method for preparing a large solid quartz ceramic material according to claim 1, wherein: coarse quartz particles, fine quartz powder, quartzSiO in micro powder and spherical quartz micro powder2The content of the cristobalite is more than or equal to 99.8 percent, and the conversion rate of the cristobalite is less than or equal to 3 percent.
6. The method for preparing a large solid quartz ceramic material according to claim 1, wherein: the volume density of the large solid quartz ceramic material is more than or equal to 1.88g/cm3The apparent porosity is less than or equal to 15 percent; SiO 22The content of the cristobalite is more than or equal to 99.8 percent, and the conversion rate of the cristobalite is less than or equal to 3 percent.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0787699A2 (en) * | 1993-09-16 | 1997-08-06 | Btg International Limited | Milled fired material usable in whiteware ceramics |
| CN105777153A (en) * | 2016-03-01 | 2016-07-20 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing large-size refractory bricks |
| CN107935608A (en) * | 2017-11-17 | 2018-04-20 | 淄博工陶耐火材料有限公司 | The method that zircon brick is prepared using compact zircon aggregate |
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| CN100528809C (en) * | 2007-02-02 | 2009-08-19 | 淄博工陶耐火材料有限公司 | Large compact zircon overflow brick and manufacturing method thereof |
| CN101851107B (en) * | 2010-05-06 | 2013-04-17 | 广州市石基耐火材料厂 | Compact zircon brick with low alkali content, hole fusion rate and stress and manufacturing method thereof |
| CN102030546B (en) * | 2010-10-28 | 2013-03-06 | 中钢集团洛阳耐火材料研究院有限公司 | Zircon product containing special zircon particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0787699A2 (en) * | 1993-09-16 | 1997-08-06 | Btg International Limited | Milled fired material usable in whiteware ceramics |
| CN105777153A (en) * | 2016-03-01 | 2016-07-20 | 中钢集团洛阳耐火材料研究院有限公司 | Method for manufacturing large-size refractory bricks |
| CN107935608A (en) * | 2017-11-17 | 2018-04-20 | 淄博工陶耐火材料有限公司 | The method that zircon brick is prepared using compact zircon aggregate |
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