CN109369163A - The preparation method of large-scale solid Quartz ceramic material - Google Patents
The preparation method of large-scale solid Quartz ceramic material Download PDFInfo
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- CN109369163A CN109369163A CN201811220088.2A CN201811220088A CN109369163A CN 109369163 A CN109369163 A CN 109369163A CN 201811220088 A CN201811220088 A CN 201811220088A CN 109369163 A CN109369163 A CN 109369163A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000010453 quartz Substances 0.000 title claims abstract description 55
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 29
- 239000007787 solid Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003595 mist Substances 0.000 claims abstract description 13
- 239000008187 granular material Substances 0.000 claims abstract description 12
- 238000010304 firing Methods 0.000 claims abstract description 9
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 8
- 230000003068 static effect Effects 0.000 claims abstract description 8
- 239000007767 bonding agent Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims 4
- 239000000919 ceramic Substances 0.000 abstract description 16
- 238000000748 compression moulding Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000011449 brick Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000005350 fused silica glass Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011236 particulate material Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004033 diameter control Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/54—Particle size related information
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- C04B2235/54—Particle size related information
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- C04B2235/602—Making the green bodies or pre-forms by moulding
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Abstract
The present invention relates to a kind of preparation methods of large-scale solid Quartz ceramic material, belong to quartz ceramic technical field.The preparation method, the following steps are included: preparing mixture: weigh the following substance of mass percent: quartzy coarse granule 15-35%, quartzy fine grained 20-40%, bonding agent 0.99-5.66%, quartzy fine powder 15-30%, quartz micropowder 8-20% and spherical quartz micro mist 8-15% form mixture after being kneaded uniformly；Isostatic pressing: vacuumizing after mixture in step 1 is packed into rubber mold, and the compression moulding in the case where waiting static pressure 80-150MPa forms green body；Firing process: green body in step 2 is sintered by calcining system, is cooled to room temperature with furnace after truce.Preparation method provided by the present invention is scientific and reasonable, simple and easy, and Quartz ceramic material uniform microstructure obtained is good, has the characteristics that the porosity is low, bulk density is high and cold crushing strength is high.
Description
Technical field
The present invention relates to a kind of preparation methods of large-scale solid Quartz ceramic material, belong to quartz ceramic technology neck
Domain.
Background technique
Ceramics quartz glass abbreviation quartz-ceramics, since its thermal expansion coefficient is small, only 0.54 × 10-6/ DEG C, so that it has
There is very good resistance to thermal shocks；The pyroconductivity of quartz-ceramics is especially low, and pyroconductivity is only 2.1W/m.K, therefore
It is a kind of ideal heat-barrier material；Quartz-ceramics have excellent chemical stability, hardly happen work with various metal baths
With also having extraordinary erosion resisting to various glass slags.Therefore, damper block, the cover board being made into using quartz glass as raw material
Brick, breast wall brick and pottery crucible, in the melting of the materials such as float glass furnace, rare metal, special glass and polysilicon
It is used widely.As fused quartz ceramic application range constantly expands, injection forming, note solidification forming and gel casting forming
Develop comparatively fast etc. the forming method for preparing fused quartz ceramic, but the product of these types of moulding process preparation is all in the prevalence of aobvious
Micro-structure uniformity is poor, and dehydration difficulty causes life cycle of the product long, manufactures large-scale solid quartz-ceramics green body low efficiency, base
Body is easy the disadvantages of firing cracking, it is difficult to adapt to the needs of large-scale industrial production large-scale solid Quartz ceramic material.
Cold isostatic compaction technology is current molding high-performance and the comparatively ideal method of high reliability ceramics.But due to melting
Quartz-ceramics material is frit, and rigidity is big, and compressibility is low.The skill of isostatic pressing fused quartz ceramic disclosed in the prior art
Art, including a certain amount of vitreous silica powder is dried, it adds after a certain amount of PVA solution is crushed and is sieved, with 150-30 mesh
Between powder particles material, formed in miniature antenna cover rubber mold with static pressure suppressions such as 110MPa, test and determine best firing
Temperature is 1250 DEG C (see " silicate notification " (ISSN1001-1625) in April, 2007 the 2nd phase " isostatic pressing melting of volume 26
The research of quartz-ceramics ").
Application No. is 200610070310.6 Chinese patents, disclose the method that isostatic pressing prepares quartz-ceramics:
With include vitreous silica is added to dispersing agent, slurry, vitreous silica grain diameter control is made in binder, pore former, plasticizer
System is in the 0-60% that the quality of 150 meshes to 325 meshes is vitreous silica gross mass, and laser particle analyzer surveys 60 μm of d90 <, with spray
Mist is granulated the particulate material that 80-250 mesh is made for isostatic pressing, and briquetting pressure is controlled in 20-300MPa, prepares quartz-ceramics
The products such as antenna house and petrographic examination solve full powder note solidification forming and gel casting forming uniform microstructure
Poor, dehydration difficulty leads to problems such as life cycle of the product long.But for the Quartz ceramic material containing glassy state coarse granule material,
Glassy state vitreous silica particle easily cuts rubber mold and causes difficult forming；And for large-scale solid Quartz ceramic material, by existing
There is technology to be sufficiently sintered, need to extend firing soaking time, extending soaking time will lead to cristobalite, influence tekite
The service performance of English material.Through retrieving, the preparation method of large-scale solid Quartz ceramic material is not found.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of preparation sides of large-scale solid Quartz ceramic material
Method, scientific and reasonable, simple and easy, Quartz ceramic material cristobalite conversion ratio obtained is low, uniform microstructure is good, has gas
The feature that porosity is low, bulk density is high and cold crushing strength is high.
The preparation method of large-scale solid Quartz ceramic material of the present invention, comprising the following steps:
1) it prepares mixture: weighing the following substance of mass percent: quartzy coarse granule 15-35%, quartzy fine grained 20-
40%, bonding agent 0.99-5.66%, quartzy fine powder 15-30%, quartz micropowder 8-20% and spherical quartz micro mist 8-15% are mixed
After refining uniformly, mixture is formed；
2) isostatic pressing: vacuumizing after mixture in step 1 is packed into rubber mold, in the case where waiting static pressure 80-150MPa
Compression moulding forms green body；
3) firing process: green body in step 2 is sintered, calcining system is as follows:
Room temperature is cooled to furnace after truce.
In the step 1, quartzy coarse granule partial size is 1-3mm；Quartzy fine grained partial size is 0.1-1mm；Quartzy fine powder
Partial size is to be less than or equal to 44 μm greater than 0；Quartz micropowder partial size is to be less than or equal to 5 μm greater than 0；Spherical quartz grain size of micropowder be greater than
0 is less than or equal to 2 μm.
Preferably, the quartz micropowder and spherical quartz micro mist mass ratio are 1:1, realize the grain composition of fine powder, energy
Blank sintering is effectively facilitated, the compaction rate of ceramic body is improved.
The bonding agent is one or both of PVA solution or silica solution.
In the step 1, after bonding agent is added in quartzy coarse granule, quartzy fine grained, it is kneaded 10-20 minutes, makes
It obtains bonding agent and is coated uniformly on vitreous silica coarse granule and the fine grain surface of vitreous silica, it is micro- to add quartzy fine powder, quartz
Powder and spherical quartz micro mist are kneaded 10-20 minutes, form mixture.
In the step 2, it is initially charged with the cardboard of 3-5mm thickness in rubber mold, is vacuumized after being reloaded into mixture, mixes
It closes material and is not directly contacted with mold.
Rubber mold liner cardboard solves vitreous silica particle in glassy state, has sharp corner, wait static pressure process
In the problem of easily cutting rubber mold, green body is caused the hydraulic system of static pressure such as to penetrate into unsuccessfully.
Wherein, isostatic pressing pressure is lower than 80MPa, and blank strength is low, and cracking is easy during mobile and loading of kiln.Pressure
Higher than 150Mpa, partial melting quartz particles are crushed, and blank strength is caused to decline, and are also easy out during mobile and loading of kiln
It splits.
The length of the large-scale solid Quartz ceramic material is 600-3100mm, and with a thickness of 150-500mm, width is
400-1000mm。
Preferably, it is 900-2000mm that the size of the large-scale solid Quartz ceramic material, which is length, with a thickness of 200-
500mm, width 600-1000mm.
SiO in the quartzy coarse granule, quartzy fine grained, quartzy fine powder, quartz micropowder and spherical quartz micro mist2Contain
All >=99.8%, cristobalite conversion ratio is all≤3% for amount.
Bulk density >=1.88g/cm of the large-scale solid Quartz ceramic material3, apparent porosity≤15%；SiO2's
Content >=99.8%, cristobalite conversion ratio≤3%.
For large-scale solid Quartz ceramic material green body, firing is warming up to 750-900 DEG C of heat preservation 12-36h, and green body firing is closed
Lattice rate can reach 90% or more.It adds organic PVA solution and burns mistake exclusion completely at such a temperature, make green body sintering qualified rate
It greatly improves, and the spherical quartz micro mist of partial size≤5 μm or partial size≤2 μm is at such a temperature, is tentatively sintered to bulky grain table
Face is integrally improved green body medium temperature intensity.In addition, can significantly reduce product in 750-900 DEG C of heat preservation 12-36h insulating process
The porosity, improve bulk density and cold crushing strength.
Compared with prior art, the invention has the following beneficial effects:
1. being mixed with commercially available quartzy coarse granule, quartzy fine grained, quartzy fine powder, quartz micropowder and spherical quartz micro mist
Material, by the grain composition of fine powder, micro mist, has effectively facilitated the sintering of green body under medium temperature, solves large-scale green body and extends firing
Soaking time, the problem of leading to cristobalite；
2. temperature is reached in 750-900 DEG C of heat preservation 12-36h, green body sintering qualified rate for large-scale solid ceramic material green body
To 90% or more, while it can significantly reduce the porosity of product, improving bulk density and cold crushing strength, and microstructure
Uniformity is good；
3. use rubber mold liner cardboard, solve glassy state vitreous silica particulate material charging, etc. static pressure during
The problem of easily cutting rubber mold, leading to burn failure；
4. preparation method of the present invention is scientific and reasonable, simple and easy, high production efficiency, be conducive to promote and apply.
Specific embodiment
The present invention will be further explained with reference to the examples below.
In the present invention, powder particle size is measured with laser particle analyzer, and meso-position radius refers to the cumulative particle sizes distribution of sample
Percentage reaches partial size corresponding when 50%.Its physical significance is that partial size is greater than its particle and accounts for 50%, less than its
Grain also accounts for 50%, but is not related to the draw ratio of particle.
In the present invention, bulk density and the porosity use GB/T2997-2000 densification shaping refractory product bulk density, show
The porosity and the measurement of true porosity test method.Cold crushing strength uses GB/T5072.1-1998 densification shaping refractory product
The measurement of cold crushing strength test method.Chemical component is using GB-T 21114-2007 refractory material X-ray fluorescence spectra chemistry
Analyze the measurement of founding sheet glass method.Cristobalite ratio is detected referring to YB/T172-2000 silica brick quantitative analysis X-ray diffraction method.
Embodiment 1
1) mixture is prepared: SiO of the quartz material using commercially available purity by mass percentage2Content is greater than 99.9%
Vitreous silica particle, quartzy fine powder, quartz micropowder and spherical quartz micro mist weigh quartzy coarse granule in percentage by weight
35%, quartzy fine grained 30%, quartzy coarse granule partial size are 1-3mm, and quartzy fine grained partial size is 0.1-1mm, add 2% PVA
Solution is into blender, after stirring 15 minutes, adds the quartzy fine powder 17% that partial size is less than or equal to 44 μm greater than 0, partial size is big
It is less than or equal to 5 μm of quartz micropowder 8% in 0, the spherical quartz micro mist 8% greater than 0 less than 2 μm stirs 15 minutes, forms mixing
Material；
2) in rubber mold liner 3mm thickness cardboard, be tightly attached on rubber mold, be packed into mixture, vacuumize after 40
After minute, formed in static pressure suppressions such as 120MPa；Suppress green body dimensions length be 2100mm, with a thickness of 370mm, width is
750mm。
3) green body after molding is taken out, carefully cleaning is attached to the cardboard of billet surface；
4) it is packed into gas-combustion kiln, is sintered by following calcining system:
Cool down after truce with furnace.
Green body cuts sample, detection bulk density, apparent porosity, cold crushing strength and cristobalite ratio after being cooled to room temperature
Example.The preparation method of Quartz ceramic material described in embodiment 2-8 is same as Example 1, raw materials used weight percent ginseng
Number is shown in Table 1；Briquetting pressure and calcining system are shown in Table 2；Embodiment 1-2 heating rate is same as Example 1, embodiment
3-4 heating rate is as follows:
Cool down after truce with furnace；
Embodiment 5-6 heating rate is as follows:
Cool down after truce with furnace；
Embodiment 7-8 heating rate is as follows:
Cool down after truce with furnace；
Embodiment 1-8 detection data is shown in Table the testing result in 3.
The 1 raw materials used weight percent of embodiment 1-8 of table
2 embodiment 1-8 briquetting pressure of table and calcining system
3 embodiment 1-8 the performance test results of table
Claims (8)
1. a kind of preparation method of large-scale solid Quartz ceramic material, it is characterised in that: the following steps are included:
1) it prepares mixture: weighing the following substance of mass percent: quartzy coarse granule 15-35%, quartzy fine grained 20-
40%, bonding agent 0.99-5.66%, quartzy fine powder 15-30%, quartz micropowder 8-20% and spherical quartz micro mist 8-15% are mixed
After refining uniformly, mixture is formed；
2) isostatic pressing: vacuumizing after mixture in step 1 is packed into rubber mold, suppresses in the case where waiting static pressure 80-150MPa
Molding forms green body；
3) firing process: green body in step 2 is sintered, calcining system is as follows:
2. the preparation method of large-scale solid Quartz ceramic material according to claim 1, it is characterised in that: in step 1, stone
English coarse granule partial size is 1-3mm；Quartzy fine grained partial size is 0.1-1mm；Quartzy fine powder partial size is to be less than or equal to 44 μm greater than 0；
Quartz micropowder partial size is to be less than or equal to 5 μm greater than 0；Spherical quartz grain size of micropowder is to be less than or equal to 2 μm greater than 0.
3. the preparation method of large-scale solid Quartz ceramic material according to claim 1, it is characterised in that: bonding agent is
One or both of PVA solution or silica solution.
4. the preparation method of large-scale solid Quartz ceramic material according to claim 1, it is characterised in that: in step 2,
It is initially charged with the cardboard of 3-5mm thickness in rubber mold, is vacuumized after being reloaded into mixture, mixture is not directly contacted with mold.
5. the preparation method of large-scale solid Quartz ceramic material according to claim 1, it is characterised in that: large-scale solid stone
The length of English ceramic material is 600-3100mm, with a thickness of 150-500mm, width 400-1000mm.
6. the preparation method of large-scale solid Quartz ceramic material according to claim 5, it is characterised in that: large-scale solid stone
The size of English ceramic material is that length is 900-2000mm, with a thickness of 200-500mm, width 600-1000mm.
7. the preparation method of large-scale solid Quartz ceramic material according to claim 1, it is characterised in that: thick of quartz
SiO in grain, quartzy fine grained, quartzy fine powder, quartz micropowder and spherical quartz micro mist2Content all >=99.8%, cristobalite turn
Rate is all≤3%.
8. the preparation method of large-scale solid Quartz ceramic material according to claim 1, it is characterised in that: large-scale solid stone
Bulk density >=1.88g/cm of English ceramic material3, apparent porosity≤15%；SiO2Content >=99.8%, cristobalite conversion ratio
≤ 3%.
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| CN116874292A (en) * | 2023-08-03 | 2023-10-13 | 西安交通大学 | High-strength high-purity silicon dioxide ceramic and manufacturing method thereof |
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