CN102503385A - Preparation method of low-crystallization fused quartz ceramic material - Google Patents
Preparation method of low-crystallization fused quartz ceramic material Download PDFInfo
- Publication number
- CN102503385A CN102503385A CN2011103091935A CN201110309193A CN102503385A CN 102503385 A CN102503385 A CN 102503385A CN 2011103091935 A CN2011103091935 A CN 2011103091935A CN 201110309193 A CN201110309193 A CN 201110309193A CN 102503385 A CN102503385 A CN 102503385A
- Authority
- CN
- China
- Prior art keywords
- fused quartz
- blank
- ceramic material
- base substrate
- lanthanum oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a preparation method of a low-crystallization fused quartz ceramic material, belonging to the field of high-temperature structural ceramic materials. The ceramic material is prepared from the raw materials in percentage by weight: 97-99% of fine fused quartz powder and 1-3% of nano lanthanum oxide. The preparation method of the ceramic material comprises the steps of: carrying out wet mixing on fine fused quartz powder with nano lanthanum oxide, drying, then adding a polyvinyl alcohol solution binding agent for wetting, screening, stirring, and aging to obtain a blank material for shaping a blank; shaping the blank by a hydraulic machine at the shaping pressure not less than 50 MPa; and drying, sintering the blank at high temperature of 1300-1400 DEG C, and maintaining the temperature for 1-3 hours to obtain the fused quartz ceramic material containing nano lanthanum oxide. The obtained ceramic material has a lower crystallization degree than pure fused quartz. According to the invention, a low-crystallization novel fused quartz ceramic material is provided for the fields of glass, steel, metallurgy, electronics, military missile, spacecrafts and the like in China, and the ceramic material has broad application prospects and the significance of consolidating the national defense.
Description
Technical field
The invention belongs to the high-temperature structural ceramics field, be specifically related to a kind of low crystallization fused quartz ceramic preparation methods.
Background technology
Fused quartz ceramic is meant that with silica glass or fused quartz be raw material, through fragmentation, moulding, the goods that the manufacture craft of series of ceramic prepares such as burn till.Fused quartz ceramic is called ceramics quartz glass, silica glass sintered article again.
Fused quartz ceramic is under high temperature life-time service condition more than 1300 ℃; Or experience when high temperature is chilled to the thermal shock process of room temperature more than 1300 ℃; Because of the fine fused quartz that constitutes fused quartz ceramic is the high vitreous state of energy state, it is cristobalite that the fused quartz particle is prone to crystallization, and then the thing in the fused quartz ceramic is converted into α-Fang Shiying by big of fused quartz; The low thermal expansion characteristics of fused quartz disappears basically; The volume effect of in phase transition process, following makes the intensity of fused quartz ceramic material reduce, and causes the material cracking, and big senior general is low for its safety in utilization safety.
Therefore, the crystallization effect when reducing the fused quartz ceramic material at high temperature and using seeks to suppress the technological approaches of fused quartz particle crystallization, improves the security and the safety of its use, becomes research that the fused quartz ceramic material require solves and uses problem.The foreign scholar is to the optical property of fused quartz and studying of aspects such as electric property and nuclearity ability, and the research that the fused silica material crystallization is suppressed is very few.Domestic part Study person once used the Al of conventional powder (particle diameter is greater than 5 microns)
2O
3, B
2O
3, Na
2O, H
3BO
3, Si
3N
4, P
2O
5, Y
2O
3, La
2O
3Crystallization suppressor factor as fused quartz ceramic.Though these additives have the effect of certain inhibition crystallization to fused quartz high temperature crystallization, it is unsatisfactory that crystallization suppresses effect, and when temperature was increased to more than 1300 ℃ temperature, significantly crystallization phenomenon still can appear in the fused quartz ceramic material.
The present invention adopts nano lanthanum oxide to be incorporated in the fused quartz ceramic material powder as the crystallization suppressor factor, and powder makes the fused quartz ceramic material that contains nano lanthanum oxide behind moulding and high temperature sintering.With the fused quartz ceramic material sample of the conventional powder lanthanum trioxide of introducing and the pure fused quartz ceramic material blank sample comparison of not introducing nano lanthanum oxide; This fused quartz ceramic material has advantages such as intensity height, crystallization degree is low, thermal expansivity is little, is the higher fused quartz ceramic material of a kind of security reliability standard.The present invention can be fields such as China's glass smelting, iron and steel and Non-ferrous Metallurgy, electronics, military project guided missile, spacecraft and a kind of new type high temperature structured material is provided, the meaning that has broad application prospects and consolidate national defence.
Summary of the invention
The objective of the invention is to above-mentioned deficiency of the prior art, the high and low thermal expansion of a kind of intensity, thermal shock resistance is good, safe reliability is high fused quartz ceramic preparation methods are provided.
Technical scheme of the present invention and technical characterictic are:
The present invention is a kind of low crystallization fused quartz ceramic preparation methods, it is characterized in that this stupalith weight percent raw materials used and raw material is: fused quartz fine powder 97～99%, nano lanthanum oxide 1～3%.This ceramic material may further comprise the steps: the blank preparation; Blank forming; Body drying; Base substrate burns till.
The particle diameter of fused quartz fine powder is 0.010～0.060mm, and the weight percent of fused quartz fine powder purity is: SiO
2>=99.0%.Particle diameter＜the 100nm of nano lanthanum oxide, the weight percent of nano lanthanum oxide purity is: La
2O
3>=98.0%.
The blank preparation method: nano lanthanum oxide measures the back by weight ratio and added a certain amount of absolute ethyl alcohol and stirring 0.5～2 hour; Then under continuous whipped state progressively the fused quartz fine powder carry out wet mixing; Continue to mix that heating in water bath is stirred to dry powder after 0.5～2 hour; This powder is broken up the back progressively adds mass concentration 1.5～2% under continuous whipped state polyvinyl alcohol solution 5～7% (weight percents; Add) and place airtight plastics bag ageing mixture, but obtained the blank of voltage supply power moulding behind the ageing mixture through 4～6 hours.
The blank forming method: mix and adopt hydropress to be shaped to base substrate through the blank of ageing mixture above-mentioned, blank forming pressure is >=50MPa.
The body drying method: with base substrate after the moulding 20 ℃ of drying at room temperature 4～6 hours, afterwards 60 ℃～70 ℃ dryings 1～2 hour, after 100 ℃ of dryings obtained the dry base substrate that Gong to burn till in 1～2 hour.
The base substrate process for calcining: dried base substrate burns till through 1300～1400 ℃ of high temperature, is incubated the fused quartz ceramic material that obtains to contain nano-oxide after 1～3 hour.
Embodiment
Embodiment 1
Sample weight percent raw materials used and raw material is: particle diameter is the fused quartz fine powder 99% of 0.010～0.060mm, the nano lanthanum oxide 1% of particle diameter＜100nm.At first in the nano lanthanum oxide powder, added a certain amount of absolute ethyl alcohol and stirring 2 hours; Then under continuous whipped state progressively the fused quartz fine powder carry out wet mixing; Continue to mix that heating in water bath is stirred to dry loose condition (of surface) after 2 hours, again powder is crossed 80 mesh sieves, the back of sieving progressively adds the polyvinyl alcohol solution 7% (weight percent of mass concentration 2% under continuous whipped state; Add) place airtight plastics bag ageing mixture, but obtained the blank of voltage supply power moulding behind the ageing mixture through 4 hours.Blank adopts hydropress to be shaped to base substrate; Blank forming pressure is 50MPa; With base substrate after the moulding 20 ℃ of drying at room temperature 6 hours, afterwards 70 ℃ of dryings 1 hour, after 100 ℃ of dryings obtained the dry base substrate that Gong to burn till in 2 hours; Dried base substrate burns till through 1350 ℃ of high temperature, is incubated the fused quartz ceramic material that obtains to contain nano lanthanum oxide after 1 hour.
The folding strength of this stupalith is 36.0MPa; Coefficient of thermal expansion 0.03% (20～1000 ℃), and the folding strength of not introducing the fused quartz blank sample of nano lanthanum oxide is 8.6MPa; Coefficient of thermal expansion is 1% (20～1000 ℃).Comparative test result shows, contains the fused quartz ceramic material of 1% nano lanthanum oxide, and the fused quartz crystallization is that the degree of cristobalite is very little, and its coefficient of thermal expansion value is merely 3% of blank sample, has significant crystallization and suppresses effect.
Embodiment 2
Sample weight percent raw materials used and raw material is: particle diameter is the fused quartz fine powder 98% of 0.010～0.060mm, the nano lanthanum oxide 2% of particle diameter＜100nm.At first in the nano lanthanum oxide powder, added a certain amount of absolute ethyl alcohol and stirring 2 hours; Then under continuous whipped state progressively the fused quartz fine powder carry out wet mixing; Continue to mix that heating in water bath is stirred to dry loose condition (of surface) after 2 hours, again powder is crossed 80 mesh sieves, the back of sieving progressively adds the polyvinyl alcohol solution 7% (weight percent of mass concentration 2% under continuous whipped state; Add) place airtight plastics bag ageing mixture, but obtained the blank of voltage supply power moulding behind the ageing mixture through 5 hours.Blank adopts hydropress to be shaped to base substrate; Blank forming pressure is 50MPa; With base substrate after the moulding 20 ℃ of drying at room temperature 6 hours, afterwards 70 ℃ of dryings 2 hours, after 100 ℃ of dryings obtained the dry base substrate that Gong to burn till in 2 hours; Dried base substrate burns till through 1400 ℃ of high temperature, is incubated the fused quartz ceramic material that obtains to contain nano lanthanum oxide after 1 hour.
The folding strength of this stupalith is 45.8MPa; Coefficient of thermal expansion 1.00% (20～1000 ℃), and the folding strength of the blank sample of end introducing nano lanthanum oxide is 9.9MPa; Coefficient of thermal expansion is 1.6% (20～1000 ℃).Comparative test result shows, contains the fused quartz ceramic material of 2% nano lanthanum oxide, and the fused quartz crystallization is that the degree of cristobalite is little, and its coefficient of thermal expansion is merely 62.5% of blank sample, has tangible crystallization and suppresses effect.
Embodiment gathers
The embodiment summary sheet
Claims (7)
1. the present invention is characterized in that this stupalith weight percent raw materials used and raw material is: fused quartz fine powder 97～99%, nano lanthanum oxide 1～3% for low crystallization fused quartz ceramic preparation methods.This ceramic material may further comprise the steps: the blank preparation; Blank forming; Body drying; Base substrate burns till.
2. low crystallization fused quartz ceramic preparation methods as claimed in claim 1, the particle diameter that it is characterized in that used fused quartz powder is 0.010～0.060mm, the weight percent of fused quartz powder purity is: SiO
2>=99.0%.
3. low crystallization fused quartz ceramic preparation methods as claimed in claim 1 is characterized in that the particle diameter of used nano lanthanum oxide is＜100nm, and the weight percent of nano lanthanum oxide purity is: La
2O
3>=98.0%.
4. low crystallization fused quartz ceramic preparation methods as claimed in claim 1; The preparation method who it is characterized in that blank measures the back with nano lanthanum oxide to add a certain amount of absolute ethyl alcohol and stirring 0.5～2 hour by weight ratio; Then under continuous whipped state progressively the fused quartz fine powder carry out wet mixing; Continue to mix that heating in water bath is stirred to dry powder after 0.5～2 hour; This powder is broken up the back constantly progressively adding the polyvinyl alcohol solution 5～7% (weight percent adds) of mass concentration 1.5～2% and placing airtight plastics bag ageing mixture under the whipped state, but obtained the blank of voltage supply power moulding behind the ageing mixture through 4～6 hours.
5. low crystallization fused quartz ceramic preparation methods as claimed in claim 1, the forming method that it is characterized in that base substrate are to mix and adopt hydropress to be shaped to base substrate through the blank of ageing mixture above-mentioned, and blank forming pressure is >=50MPa.
6. low crystallization fused quartz ceramic preparation methods as claimed in claim 1; The drying means that it is characterized in that base substrate is 20 ℃ of drying at room temperature 4～6 hours with base substrate after the moulding; Afterwards 60 ℃～70 ℃ dryings 1～2 hour, after 100 ℃ of dryings obtained the dry base substrate that Gong to burn till in 1～2 hour.
7. low crystallization fused quartz ceramic preparation methods as claimed in claim 1; The process for calcining that it is characterized in that base substrate is that dried base substrate is burnt till through 1300～1400 ℃ of high temperature, is incubated the fused quartz ceramic material that obtains to contain nano lanthanum oxide after 1～3 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103091935A CN102503385A (en) | 2011-09-28 | 2011-09-28 | Preparation method of low-crystallization fused quartz ceramic material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103091935A CN102503385A (en) | 2011-09-28 | 2011-09-28 | Preparation method of low-crystallization fused quartz ceramic material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102503385A true CN102503385A (en) | 2012-06-20 |
Family
ID=46215536
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103091935A Pending CN102503385A (en) | 2011-09-28 | 2011-09-28 | Preparation method of low-crystallization fused quartz ceramic material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102503385A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183502A (en) * | 2013-03-26 | 2013-07-03 | 河北联合大学 | Preparation method of fused quartz ceramic material containing nanoscale ytterbium oxide |
| CN109320263A (en) * | 2018-11-13 | 2019-02-12 | 四川航天机电工程研究所 | Sintering aid and quartz-ceramics and its preparation and application method |
| CN113354422A (en) * | 2020-03-04 | 2021-09-07 | 中国科学院金属研究所 | Ceramic core for single crystal high-temperature alloy blade and preparation method thereof |
| CN114907133A (en) * | 2022-05-07 | 2022-08-16 | 中国联合重型燃气轮机技术有限公司 | Silicon-based ceramic core material, preparation method and silicon-based ceramic core |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101767983A (en) * | 2009-12-25 | 2010-07-07 | 河北理工大学 | Fused silica ceramic material containing ytterbium oxide and preparation method thereof |
| CN101767984A (en) * | 2010-01-06 | 2010-07-07 | 河北理工大学 | Fused silica ceramic material containing holmium oxide and preparation method thereof |
-
2011
- 2011-09-28 CN CN2011103091935A patent/CN102503385A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101767983A (en) * | 2009-12-25 | 2010-07-07 | 河北理工大学 | Fused silica ceramic material containing ytterbium oxide and preparation method thereof |
| CN101767984A (en) * | 2010-01-06 | 2010-07-07 | 河北理工大学 | Fused silica ceramic material containing holmium oxide and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 南守宇 等: "熔融石英晶化抑制与烧结性能", 《河北理工大学学报(自然科学版)》, vol. 31, no. 3, 31 August 2009 (2009-08-31), pages 95 - 98 * |
| 卜景龙 等: "熔融石英陶瓷材料的晶化抑制研究", 《稀有金属材料与工程》, vol. 36, 31 August 2007 (2007-08-31), pages 357 - 360 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183502A (en) * | 2013-03-26 | 2013-07-03 | 河北联合大学 | Preparation method of fused quartz ceramic material containing nanoscale ytterbium oxide |
| CN103183502B (en) * | 2013-03-26 | 2015-02-11 | 河北联合大学 | Preparation method of fused quartz ceramic material containing nanoscale ytterbium oxide |
| CN109320263A (en) * | 2018-11-13 | 2019-02-12 | 四川航天机电工程研究所 | Sintering aid and quartz-ceramics and its preparation and application method |
| CN113354422A (en) * | 2020-03-04 | 2021-09-07 | 中国科学院金属研究所 | Ceramic core for single crystal high-temperature alloy blade and preparation method thereof |
| CN114907133A (en) * | 2022-05-07 | 2022-08-16 | 中国联合重型燃气轮机技术有限公司 | Silicon-based ceramic core material, preparation method and silicon-based ceramic core |
| CN114907133B (en) * | 2022-05-07 | 2024-02-27 | 中国联合重型燃气轮机技术有限公司 | Silicon-based ceramic core material, preparation method and silicon-based ceramic core |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101767983B (en) | Fused silica ceramic material containing ytterbium oxide and preparation method thereof | |
| Chen et al. | Mullite whisker network reinforced ceramic with high strength and lightweight | |
| CN101948316B (en) | Preparation method of ceramic filtration supporter | |
| CN102276276B (en) | Alumina hollow ball insulation product | |
| CN102285799B (en) | Novel wave-transmission and thermal-insulation combined SiO2-Si3N4 composite material and preparation method thereof | |
| CN107935575B (en) | High-purity low-creep fused mullite brick and preparation method thereof | |
| CN102746013A (en) | Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof | |
| CN102775163A (en) | Silicon carbide-cordierite composite ceramic kiln furniture and preparation method thereof | |
| CN103073269A (en) | Alumina ceramic and preparation method thereof | |
| CN102617180B (en) | Porous foamed ceramic and preparation method thereof | |
| CN105236945B (en) | A kind of high-strength temperature-resistant shake push pedal and preparation method thereof | |
| CN101767984B (en) | Fused silica ceramic material containing holmium oxide and preparation method thereof | |
| CN103011870B (en) | Forsterite refractory and production method thereof | |
| CN102503385A (en) | Preparation method of low-crystallization fused quartz ceramic material | |
| CN102503144B (en) | Method for preparing fused quartz ceramic material containing nanometer zinc oxide | |
| CN103467078B (en) | Preparation method of cordierite material | |
| CN102503143A (en) | Preparation method of fused quartz ceramic material containing nano yttrium oxide | |
| CN105036167A (en) | Calcium hexaluminate and preparation method thereof | |
| CN102503146B (en) | Preparation method of fused silica ceramic material containing boron carbide and ytterbium oxide | |
| CN103183502B (en) | Preparation method of fused quartz ceramic material containing nanoscale ytterbium oxide | |
| CN102503147A (en) | Method for preparing fused silica ceramic material containing nano cerium oxide | |
| Soykan | Low-temperature fabrication of steatite ceramics with boron oxide addition | |
| CN104557056A (en) | Bauxite homogenizing material as Sialon raw material and production method of bauxite homogenizing material | |
| CN104357693A (en) | Preparation method of floating bead/AZ91D magnesium alloy composite material | |
| Wang et al. | A new strategy to realize phase structure and morphology of BaTiO3 nanowires controlled in ZnO-B2O3-SiO2 glass |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120620 |