CN102600767B - High-temperature insulation ceramic tube for synthesizing diamond with large cavity and manufacturing method thereof - Google Patents
High-temperature insulation ceramic tube for synthesizing diamond with large cavity and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature insulation ceramic tube for synthesizing diamond with a large cavity and a manufacturing method of the high-temperature insulation ceramic tube. The insulation ceramic tube is manufactured by pressing, molding and sintering dry ceramic powder, the ingredients of the dry powder comprises a-aluminum oxide or magnesium oxide with the purity higher than or equal to 99%, soapstone and/or kaolinite (being taken as sintering aids), magnesium stearate (being taken as a releasing agent) and polyvinyl alcohol (being taken as a binder), wherein the proportion of a-aluminum oxide or magnesium oxide, the sintering aids, the binder to magnesium stearate is (75-90):(10-25):(1-2):(1-2). The manufacturing method of the high-temperature insulation ceramic tube comprises the steps of preparing slurry by wet ball-milling process according to the proportion, conducting spray granulation on the slurry to prepare the dry ceramic powder; and pressing, molding and sintering the dry ceramic powder to prepare the high-temperature insulation ceramic tube. The high-temperature ceramic tube replaces dolomite to be used for the production of the diamond synthesized by a cubic press with the diameter of a cavity being more than or equal to 40mm, can avoid the gas release in the diamond synthesizing process so as to reduce the hammer explosion risk, and effectively reduces the loss rate of a tungsten carbide anvil.
Description
Technical field
The invention belongs to hexahedron top press high-pressure high temperature diamond synthesis technical field, be specifically related to a kind of in order to improve diamond synthesizing process stability, to reduce tungsten carbide top hammer loss and the high-temperature insulation earthenware and the preparation technology thereof that design.
Background technology
Since entering this century, the artificial Diamond Industry equipment of China has experienced three updates at least.Cubic hinge press cylinder diameter has developed into maximum 750mm, and 850mm at the experimental stage also.The increase of oil cylinder cylinder diameter, makes piston thrust larger, changes under necessary pressure condition meeting Graphite-diamond, can use the more larger sized tungsten carbide top hammer than in the past, expands the volume of synthetic cavity, has improved per unit area yield, has reduced energy consumption and cost.But due to the increase of synthetic cavity, the gas stool problems producing when pressure field uniformity that cylindrical synthetic cavity and cube briquetting shape difference cause, temperature homogeneity and high temperature becomes " top hammer killer ".Due to quick-fried hammer problem, the cylinder diameter 750mm cubic hinge press that many enterprises purchase almost cannot be produced by normal boot-strap.
Current most cubic hinge press diamond synthesis all adopts indirect mode.The heating of synthetic cavity is by tungsten carbide top hammer, to form with cavity heater element the form circuit of connecting with low-voltage and high-current.Take graphite matter tubing or electrothermal alloy as heating element heater indirect graphite synthetic rod.Graphite synthetic rod is wrapped among ferrous metal shell (steel bowl), to reduce nonhomogeneous deformation.Between heating element heater and shell, install insulation tube additional, avoid electric current to pass through graphite synthetic rod and ferrous metal shell leakage conductance.Diamond synthesis briquetting used is the pyrophillite powder with waterglass bonding, in the middle of cube briquetting, is cylindrical synthetic chamber, the dolomite insulating tube that liner 3-4mm is thick.In building-up process, heating element heater is close to dolomite insulating tube, temperature approximately 1450 degree; Briquetting is outside to be contacted with top hammer, and temperature is 220-250 degree.Between heating element heater and graphite synthetic rod overcoat steel bowl, it is the dolomite insulation tube of thinner thickness.For cylinder diameter 650mm press, cavity diameter 57mm, its generated time is about 30 minutes.Cylinder diameter 750mm press, cavity diameter 63mm, tests at present generated time and is about 40 minutes.
As everyone knows, dolomite is the carbonate of calcium magnesium, can be decomposed into oxide and the carbon dioxide of calcium, magnesium under normal pressure, high temperature.While making dolomite insulation tube and insulating tube, need to add part waterglass as binding agent.Due to the poor stability of dolomite under normal pressure, high temperature, manufacture the heating-up temperature of insulating tube and insulation tube not higher than 400 degree, this silica dioxide gel that waterglass is formed does not fully react with dolomite.Diamond synthesis is to carry out under high pressure (approximately 50,000 atmospheric pressure) and high temperature (1450 degree), and the source of pressure is that the extruding of tungsten carbide top hammer and 12 wedge-type seal limits of pyrophillite formation are limited in solid in synthetic cavity.Although pure dolomite is difficult to decompose under tens thousand of atmospheric high pressure, due to the existence of silicon gel, both at high temperature react and have just produced water and carbon dioxide.With regard to little cavity, the gas flow of generation is relatively less, and pyrophillite is sheet crystal structure (being different from metal) in addition, allows part micro-molecular gas to overflow along inter-level diffusion.After this just makes to have synthesized, top hammer can safety relief.But for large synthetic cavity, because graphite rod diameter increases, the heat time needs to extend.The thickness of insulating tube used and insulation tube and size strengthen, and the gas flow producing during heating increases.Therefore improved the risk of quick-fried hammer.
How to improve diamond synthesizing process stability, the particularly stability of the synthetic middle high temperature insulating material of large cavity diamond under high-temperature and high-pressure conditions, avoid the air release of these materials in diamond synthesis process, thereby improve the security of pressure leak process, reducing quick-fried hammer risk, is problem demanding prompt solution in current diamond synthesizing process and equipment.
Summary of the invention
The present invention is directed to current cubic hinge press diamond synthesis, particularly the diamond of synthetic cavity diameter >=40mm synthetic in existing the problems referred to above, aim to provide a kind of large cavity diamond synthesis high-temperature insulation earthenware and preparation method thereof, can avoid the air release of material therefor in diamond building-up process, improve pressure release security, reduce quick-fried hammer risk, reach the stability that improves diamond synthesizing process and equipment, reduce the effect of top hammer loss.
For achieving the above object, the present invention adopts following technical scheme:
A kind of large cavity diamond synthesis high-temperature insulation earthenware, it is characterized in that, described high-temperature insulation earthenware is made by the repressed moulding of ceramic powder, sintering, dry powder formulation comprises a-aluminium oxide or the magnesia of purity >=99%, sintering aid talcum and/or kaolinite, stearic acid release agent magnesium, and binding agent polyvinyl alcohol, wherein a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2.
In described sintering aid, transition metal ions is with Fe
2o
3quality meter <0.3%; Alkali metal ion is in sodium and potassium oxide mass <1%.
Described high-temperature insulation earthenware adopts following methods preparation: according to batching a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2, with a-aluminium oxide or the magnesia of purity >=99% be raw material, add one or both in talcum or kaolinite for sintering aid, dolomol is releasing agent, polyvinyl alcohol is binding agent, by wet ball grinding technique, make slurry, slurry mist projection granulating makes ceramic powder; Again that ceramic powder is compressing, sintering, makes described high-temperature insulation earthenware.
Transition metal ions in described sintering aid is with Fe
2o
3quality meter <0.3%; Alkali metal ion sodium and potassium are in oxide mass <1%.
In described method, in wet ball grinding technique, adopting corundum ball is abrasive media, described slurry particle diameter≤2 micron.
Described binding agent polyvinyl alcohol (PVA) molecular weight >=10000, preferably 10000～100000.
In described method, prilling temperature is not higher than 140 ℃.After granulation, dry powder particle diameter is 0.3-0.8mm.
In described method, ceramic powder is compressing under 200-400MPa at pressure.
In described method, sintering is that compressing pipe is placed in corundum sagger, then with schmigel fill, sintering at 850-1200 ℃.The optimum condition of sintering is with 3.5 ℃/min, to be warmed up to 550 ℃ of insulations and to come unstuck; With 5 ℃/min, be warming up to 850-1200 ℃ of sintering again.
Large cavity diamond synthesis high-temperature insulation earthenware of the present invention, adopt the repressed moulding of high temperature insulating material (as powders such as corundum, magnesia) interpolation talcum (or kaolinite) of high temperatures, the insulating ceramic materials that sintering makes, can be made into insulating tube and insulation tube, avoided the air release of these materials in diamond synthesis process.For cubic hinge press diamond synthesis, particularly in the suitability for industrialized production of the large cavity cubic hinge press diamond synthesis of synthetic cavity diameter >=40mm, alternative dolomite can improve the security of pressure leak process, reduces quick-fried hammer risk, effectively reduces the proportion of goods damageds of tungsten carbide top hammer.
Specific features of the present invention and advantage at least comprise:
1) high-temperature insulation pottery of the present invention is main material with a-aluminium oxide or magnesia, and talcum (or kaolinite) is sintering aid, and polyvinyl alcohol is molding adhesive, and dolomol is releasing agent, by the repressed moulding of dry powder, sintering, is made.Adopt the high temperature insulating material (as powders such as corundum, magnesia) of high temperatures to make earthenware, and it is carried out to high annealing, avoided the air release of material in diamond synthesis process.Transition metal ions and sodium in raw material, potassium class alkali metal ion content measured are very low, at high temperature good insulation preformance of insulation tube prepared by this raw material.
2) in preparation process, by pressed by powder, become required tubular blank, tubular blank be placed in corundum sagger, then with schmigel fill, sintering at 850-1200 ℃.Buried powder has limited earthenware in sintering process and, along diametric contraction deformation, has guaranteed diameter uniformity and the caliber size of pipe on the one hand; On the other hand, high temperature sintering has been removed volatile material (as the hydroxyl in raw material, moisture, organic binder bond), has avoided prepared insulation tube or insulating tube to produce gas under the high pressure-temperature condition of diamond synthesis; The 3rd, by sintering process, the density of insulation tube is larger, and intensity is high, is difficult for fragmentation, is conducive to packaging technology operation, reduces the breakage rate of transportation.
3) high-temperature insulation earthenware of the present invention, the ceramic material that adds talcum (or kaolinite) is in temperature during higher than 1450 ℃, owing to having generated a small amount of cordierite (or blue or green spinelle), there is suitable plasticity, be conducive to the pressure transmission under the synthetic hot environment of diamond, thereby improved pressure uniformity; Thereby can improve the distributing homogeneity of diamond particles in graphite column and the concentration degree that a footpath distributes.
The specific embodiment
Large cavity diamond synthesis high-temperature insulation earthenware of the present invention, using a-aluminium oxide (purity >99%) or magnesia (purity >99%) is raw material, talcum [Mg
3(Si
4o
10) (OH)
2)] and kaolinite [Al
2si
2o
5(OH)
4] in one or both be that (transition metal ions in sintering aid is with Fe for sintering aid
2o
3quality meter <0.3%; Alkali metal ion is in sodium, potassium oxide mass <1%), polyvinyl alcohol is binding agent; The slurry that makes particle diameter≤2 micron by wet ball grinding technique, it is 0.3-0.8mm dry powder that mist projection granulating makes particle diameter; Again through dry-pressing formed, be sintered into earthenware.Material prescription is: a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2.
The common thickness of described pipe fitting is 1.0-1.5mm, height 10-70mm, the external profile diameter 30-70mm of pipe.
More specifically and optimally, high-temperature insulation earthenware of the present invention adopts following methods preparation:
1) with a-aluminium oxide (purity >99%) or magnesia (purity >99%), be raw material, talcum [Mg
3(Si
4o
10) (OH)
2)] and kaolinite [Al
2si
2o
5(OH)
4] in one or both be that (transition metal ions in auxiliary agent is with Fe for sintering aid
2o
3quality meter <0.3%; Alkali metal ion sodium, potassium are in oxide mass <1%), dolomol is releasing agent; According to 75～90:10～25:1～2, pack a-aluminium oxide or magnesia, sintering aid and dolomol into ball grinder; According to mass ratio (a-aluminium oxide or magnesia+sintering aid): corundum ball: water=100:400:200～250 add corundum ball (industrial production diameter 15-70mm corundum ball, use for laboratory diameter 5-20mm corundum ball) and water, ball milling 8～24 hours, makes the slurry that particle diameter is less than 2 microns.
2) in gained slurry, press (a-aluminium oxide or magnesia+sintering aid): polyvinyl alcohol mass ratio is that 100:1～2 add binding agent polyvinyl alcohol (PVA, molecular weight >=10000) aqueous solution, be made into dry powder with atomizing granulating technology, prilling temperature is not higher than 140 ℃; After granulation, dry powder particle diameter is 0.3～0.8mm.
3) take required powder, it is filling in mould, at pressure, be under 200～400MPa, to be pressed into required tubular blank.
4) tubular blank vertical pendulum is put in corundum sagger, then with schmigel, fills inside and the surrounding space of pipe, until pipe is buried; Saggar is warmed up to 550 ℃ of insulations with 3.5 ℃/min to come unstuck for 1 hour; With 5 ℃/min, be warmed up to 850-1200 ℃, sintering 1 hour, makes described high-temperature insulation earthenware again.
Embodiment 1
In the steel ball grinder of length 2.5m, the diameter 1.5m of liner nylon, by a-aluminium oxide, talcum, water, dolomol in mass ratio: 85/15/200/2 packs ball grinder into.With raw material (aluminium oxide+talcum)/corundum ball mass ratio 100/400, pack corundum ball into; The mass ratio of different-diameter corundum ball is: diameter 15-20mm corundum ball: diameter 20-40mm corundum ball: diameter 40-70mm corundum ball=3:2:1.With 20 turn/min ball milling 24 hours.Isolate after corundum ball, by slip in pond standing 1 hour, at the bottom of allowing and mailing a small amount of in ball grinder liner nylon sheet gap and do not sunk to pond by levigate bulky grain sandstone; Upper strata slip is sent into dosing chamber with slush pump, by (aluminium oxide+talcum)/polyvinyl alcohol mass ratio, is the aqueous solution that 100:1.5 adds polyvinyl alcohol, after stirring, with stainless steel mist projection granulating tower, carries out granulation.Granulation tower gas flow temperature is 120 ℃.After granulation, powder ball particle diameter is 0.3-0.7mm.
According to the thickness of earthenware, diameter and altitude information, take required powder, it is filling in carbide alloy (YG18～YG20) mould, at pressure, be under 400MPa, to be pressed into required tubular blank, the length of pipe is conventionally than the allowance for shrinkage in the large 5～8%(sintering of design size).Pipe vertical pendulum is put in corundum sagger, then uses inside and the surrounding space of schmigel filling tube, until pipe is buried.Saggar is placed in to Muffle furnace (or tunnel cave), with 3.5 ℃/min, is warmed up to 550 ℃, insulation is come unstuck 1 hour, except no-bonder; With 5 ℃/min, be warmed up to 850～1200 ℃ again, be incubated 1 hour.Naturally coolingly can make high-temperature insulation earthenware.
For diameter 42mm earthenware, the shrinkage factor of its length direction and the relation of sintering temperature are as table 1:
The shrinkage factor of table 1 42mm earthenware length direction and the relation of sintering temperature
| Temperature | 850 | 900 | 1000 | 1050 | 1100 | 1150 | 1200 |
| Shrinkage factor % | 2.2 | 2.8 | 3.4 | 4.6. | 6.5 | 7.6 | 8 |
| The weightless % of sintering | 6 | 6 | 6 | 6.1 | 6.1 | 6.1 | 6.1 |
| Compression strength/MPa | 321 | 345 | 414 | 530 | 941 | 1130 | 1400 |
Substitute dolomite insulation tube with the high-temperature insulation earthenware making, after assembling in cubic hinge press diamond synthesis, by catalyst: graphite=25%:75% batching is prepared graphite column and carried out diamond and synthesize, and synthesis condition is: 1450 ℃, 28min.
Result is as shown in table 2 below.
The comparison of table 2 dolomite material insulation tube and alumina insulation pipe (1000 ℃) diamond synthesis effect
Dolomite insulation tube diamond synthesizing technology is implemented the 2/platform of average top hammer spoilage of six months, and alumina insulation pipe diamond synthesizing technology is implemented the 1/platform of average top hammer spoilage < of six months.
Embodiment 2
For cylinder diameter 750mm diamond synthesis press, cavity diameter 60mm.By the method for embodiment 1, prepare diameter 56mm insulation tube, the shrinkage factor of its length direction and the relation of sintering temperature are as table 3.
The shrinkage factor of table 3 56mm earthenware length direction and the relation of sintering temperature
| Temperature | 850 | 900 | 1000 | 1050 | 1100 | 1150 | 1200 |
| Shrinkage factor % | 2.3 | 2.8 | 3.5 | 4.6. | 6.6 | 7.65 | 8 |
| The weightless % of sintering | 6 | 6 | 6 | 6.1 | 6.1 | 6.1 | 6.1 |
| Compression strength/MPa | 321 | 345 | 414 | 530 | 941 | 1130 | 1400 |
Substitute dolomite insulation tube with the high-temperature insulation earthenware making, after assembling in cubic hinge press diamond synthesis, by catalyst: graphite=25%:75% batching is prepared graphite column and carried out diamond and synthesize, and synthesis condition is: 1450 ℃, 28min.
Result is as shown in table 4 below.
The diamond synthesis effect comparison of table 4 dolomite material insulation tube and alumina insulation pipe (1000 ℃)
For cylinder diameter 750mm, the synthetic cubic hinge press of cavity diameter 60mm diamond, dolomite insulation tube diamond synthesizing technology is implemented 5 times, whole quick-fried hammers.And adopt alumina insulation pipe diamond synthesizing technology steady production of the present invention 1 month, there is not quick-fried hammer phenomenon.
Embodiment 3
According to technique substantially the same manner as Example 1, prepare powder, wherein batching is: magnesia, talcum, water, dolomol mass ratio 85/15/250/2.Pack ball grinder into, with 10 turn/min ball milling 16 hours.After granulation, powder ball particle diameter is 0.3-0.8mm.
Moulding, the sintering condition of pipe are identical with embodiment 1, make high-temperature insulation earthenware.
For diameter 38mm earthenware, the shrinkage factor of its length direction and the relation of sintering temperature are as table 5:
The shrinkage factor of table 5 38mm earthenware length direction and the relation of sintering temperature
| Temperature | 850 | 900 | 1000 | 1050 | 1100 | 1150 | 1200 |
| Shrinkage factor % | 2.2 | 2.8 | 3.4 | 4.6. | 6.5 | 7.6 | 8 |
| Sintering weightlessness | 11.3 | 11.3 | 11.3 | 11.3 | 11.7 | 12 | 12 |
| Compression strength/MPa | 412 | 437 | 457 | 510 | 608 | 732 | 740 |
Substitute dolomite insulation tube with the high-temperature insulation earthenware making, after assembling in cubic hinge press diamond synthesis, by catalyst: graphite=25%:75% batching is prepared graphite column and carried out diamond and synthesize, and synthesis condition is: 1450 ℃, 28min.
Implement 6 months continuously, result is as following table 6.
The diamond synthesis effect comparison of table 6 dolomite material insulation tube and alumina insulation pipe
Dolomite insulation tube diamond synthesizing technology is implemented the 1.5/platform of average top hammer spoilage of six months, and magnesium oxide insulated pipe diamond synthesizing technology is implemented the 0.8/platform of average top hammer spoilage < of six months.
Embodiment 4
According to method substantially the same manner as Example 1, prepare high-temperature insulation earthenware, wherein batching is: a-aluminium oxide, talcum, water, dolomol mass ratio 75/25/200/1, (aluminium oxide+talcum)/polyvinyl alcohol mass ratio is 100:2.
For diameter 38mm earthenware, the shrinkage factor of its length direction and the relation of sintering temperature are as table 7:
The shrinkage factor of table 7 38mm earthenware length direction and the relation of sintering temperature
| Temperature | 850 | 900 | 1000 | 1050 | 1100 | 1150 | 1200 |
| Shrinkage factor % | 4.1 | 4.2 | 5.4 | 5.6. | 7.5 | 8.1 | 8.4 |
| Sintering weightlessness | 6.4 | 6.4 | 6.4 | 6.5 | 6.8 | 6.8 | 6.8 |
| Compression strength/MPa | 352 | 375 | 488 | 551 | 944 | 1151 | 1412 |
Substitute dolomite insulation tube with the high-temperature insulation earthenware making, after assembling in cubic hinge press diamond synthesis, by catalyst: graphite=25%:75% batching is prepared graphite column and carried out diamond and synthesize, and synthesis condition is: 1450 ℃, 28min.Implement 6 months continuously, effect is similar to Example 1, but synthetic chamber deformation uniformity is slightly not so good as the former, and type variable is large.
Embodiment 5
According to method substantially the same manner as Example 1, prepare high-temperature insulation earthenware, wherein batching is: a-aluminium oxide, kaolinite, water, dolomol mass ratio 90/10/200/1, (aluminium oxide+kaolinite)/polyvinyl alcohol mass ratio is 100:1.
For diameter 38mm earthenware, the shrinkage factor of its length direction and the relation of sintering temperature are as table 8:
The shrinkage factor of table 8 38mm earthenware length direction and the relation of sintering temperature
| Temperature | 850 | 900 | 1000 | 1050 | 1100 | 1150 | 1200 |
| Shrinkage factor % | <0.2 | <0.2 | 0.4 | 0.6 | 0.6 | 1.8 | 2.3 |
| Sintering weightlessness | 5.1 | 5.1 | 5.1 | 5.1 | 5.2 | 5.2 | 5.2 |
| Compression strength/MPa | 302 | 324 | 387 | 430 | 472 | 671 | 845 |
Substitute dolomite insulation tube with the high-temperature insulation earthenware making, after assembling in cubic hinge press diamond synthesis, by catalyst: graphite=25%:75% batching is prepared graphite column and carried out diamond and synthesize, and synthesis condition is: 1450 ℃, 28min.Implement 6 months continuously, effect is similar to Example 1, building-up process lumen deformation good uniformity, and shape conservation rate is high, but synthesis pressure (oil pressure) will improve 5-8%, illustrates that pressure transmission ability slightly declines.
Claims (10)
1. a large cavity diamond synthesis high-temperature insulation earthenware, it is characterized in that, described high-temperature insulation earthenware is compressing under 200～400MPa by ceramic powder, 850～1200 ℃ of sintering make, dry powder formulation comprises a-aluminium oxide or the magnesia of purity >=99%, sintering aid talcum and/or kaolinite, stearic acid release agent magnesium, and binding agent polyvinyl alcohol, wherein mass ratio a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2.
2. high-temperature insulation earthenware according to claim 1, is characterized in that, in described sintering aid, transition metal ions is with Fe
2o
3quality meter <0.3%; Alkali metal ion is in sodium and potassium oxide mass <1%.
3. high-temperature insulation earthenware according to claim 1, it is characterized in that, described high-temperature insulation earthenware adopts following methods preparation: according to quality batching a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2, with a-aluminium oxide or the magnesia of purity >=99% be raw material, add one or both in talcum or kaolinite for sintering aid, dolomol is releasing agent, polyvinyl alcohol is binding agent, by wet ball grinding technique, make the slurry of particle diameter≤2 micron, slurry mist projection granulating makes the ceramic powder that particle diameter is 0.3～0.8mm, by compressing under ceramic powder 200～400MPa, after 850～1200 ℃ of sintering, make again.
4. the preparation method of a large cavity diamond synthesis use high-temperature insulation earthenware, it is characterized in that, according to quality batching a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2, take the a-aluminium oxide of purity >=99% or magnesia as raw material, add one or both in talcum or kaolinite for sintering aid, dolomol is releasing agent, polyvinyl alcohol is binding agent, by wet ball grinding technique, make slurry, slurry mist projection granulating makes ceramic powder; Again that ceramic powder is compressing, sintering, makes described high-temperature insulation earthenware.
5. the preparation method of high-temperature insulation earthenware according to claim 4, is characterized in that, the transition metal ions in described sintering aid is with Fe
2o
3quality meter <0.3%; Alkali metal ion is in sodium and potassium oxide mass <1%.
6. the preparation method of high-temperature insulation earthenware according to claim 4, is characterized in that, in described method, in wet ball grinding technique, adopting corundum ball is abrasive media, described slurry particle diameter≤2 micron.
7. the preparation method of high-temperature insulation earthenware according to claim 4, is characterized in that, in described method, prilling temperature is not higher than 140 ℃, and after granulation, ceramic powder particle diameter is 0.3～0.8mm.
8. the preparation method of high-temperature insulation earthenware according to claim 4, is characterized in that, in described method, ceramic powder is compressing under 200～400MPa at pressure.
9. the preparation method of high-temperature insulation earthenware according to claim 4, is characterized in that, in described method, sintering is that compressing pipe is placed in corundum sagger, then with schmigel fill, sintering at 850～1200 ℃.
10. the preparation method of high-temperature insulation earthenware according to claim 4, is characterized in that, said method comprising the steps of:
1) with a-aluminium oxide or magnesia, be raw material, talcum and/or kaolinite are sintering aid, and dolomol is releasing agent; According to 75～90:10～25:1～2, pack the a-aluminium oxide of purity >=99% or magnesia, sintering aid talcum and/or kaolinite and dolomol into ball grinder; According to mass ratio (a-aluminium oxide or magnesia+sintering aid): corundum ball: water=100:400:200～250 add corundum ball and water, ball milling 8～24 hours, makes the slurry that particle diameter is less than 2 microns;
2) in gained slurry by (a-aluminium oxide or magnesia+sintering aid): polyvinyl alcohol mass ratio is that 100:1～2 add binding agent polyvinyl alcohol water solution, is made into dry powder with atomizing granulating technology, and prilling temperature is not higher than 140 ℃; After granulation, dry powder particle diameter is 0.3～0.8mm;
3) take required powder, it is filling in mould, at pressure, be under 200～400MPa, to be pressed into required tubular blank;
4) tubular blank vertical pendulum is put in corundum sagger, then with schmigel, fills inside and the surrounding space of pipe, until pipe is buried; Saggar is warmed up to 550 ℃ of insulations with 3.5 ℃/min to come unstuck for 1 hour; With 5 ℃/min, be warmed up to 850～1200 ℃, sintering 1 hour, makes described high-temperature insulation earthenware again.
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| CN101348372A (en) * | 2008-09-03 | 2009-01-21 | 山东硅苑新材料科技股份有限公司 | Production method of electrovacuum ceramic tube envelope |
| CN102145993A (en) * | 2011-05-12 | 2011-08-10 | 安徽理工大学 | Low-temperature quick sintered high-strength aluminum oxide ceramic and preparation method thereof |
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| CN101348372A (en) * | 2008-09-03 | 2009-01-21 | 山东硅苑新材料科技股份有限公司 | Production method of electrovacuum ceramic tube envelope |
| CN102145993A (en) * | 2011-05-12 | 2011-08-10 | 安徽理工大学 | Low-temperature quick sintered high-strength aluminum oxide ceramic and preparation method thereof |
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