CN102600767A - 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 the hammer loss of tungsten carbide top and the high-temperature insulation earthenware and the preparation technology thereof that design.
Background technology
Got into since this century, China's diamond industry equipment has experienced three updates at least.The cubic hinge press cylinder diameter has developed into maximum 750mm, and 850mm also at the experimental stage.The increase of oil cylinder cylinder diameter makes piston thrust bigger, changes under the necessary pressure condition satisfying graphite-diamond, can use the more larger sized tungsten carbide top hammer than in the past, enlarges the volume of synthetic cavity, has improved per unit area yield, has reduced energy consumption and cost.But because the increase of synthetic cavity, the gas stool problems that produces when the pressure field uniformity that cylindrical synthetic cavity and cube briquetting shape difference cause, temperature homogeneity and high temperature becomes " killer is hammered on the top into shape ".Because quick-fried hammer problem, the cylinder diameter 750mm cubic hinge press that many enterprises purchase almost can't normal boot-strap production.
Present most cubic hinge press diamond synthesis all adopts the indirect mode.The heating of synthetic cavity is to form connect form circuit through tungsten carbide top hammer with the cavity heater element with low-voltage and high-current.With graphite matter tubing or electrothermal alloy is heating element heater indirect graphite synthetic rod.The graphite synthetic rod is wrapped among the ferrous metal shell (steel bowl), to reduce nonhomogeneous deformation.Install insulation tube additional between heating element heater and the shell, avoid electric current to pass through graphite synthetic rod and ferrous metal shell leakage conductance.The used briquetting of diamond synthesis is the pyrophillite powder with the waterglass bonding, is cylindrical synthetic chamber in the middle of the cube briquetting, the dolomite insulating tube that liner 3-4mm is thick.Heating element heater is close to the dolomite insulating tube in building-up process, about 1450 degree of temperature; Briquetting is outside to be contacted with the top hammer, and temperature is the 220-250 degree.Between heating element heater and graphite synthetic rod overcoat steel bowl 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 generated time at present and is about 40 minutes.
As everyone knows, dolomite is the carbonate of calcium magnesium, under normal pressure, high temperature, can be decomposed into the oxide and the carbon dioxide of calcium, magnesium.When making dolomite insulation tube and insulating tube, need to add part waterglass as binding agent.Because the poor stability of dolomite under normal pressure, high temperature, the heating-up temperature of making insulating tube and insulation tube is not higher than 400 degree, and this silica dioxide gel that makes waterglass form does not fully react with dolomite.Diamond synthesis is under high pressure (about 50,000 atmospheric pressure) and high temperature (1450 degree), to carry out, 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 the synthetic cavity.Though pure dolomite is difficult to decompose under tens thousand of atmospheric high pressure, because 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 less relatively, and pyrophillite is sheet crystal structure (being different from metal) in addition, allows the part micro-molecular gas to overflow along inter-level diffusion.After this just made and synthesizes completion, the top hammer can safety relief.But,, need heat time heating time to prolong because the graphite rod diameter increases for big synthetic cavity.The thickness of used insulating tube and insulation tube and oversized, the gas flow that produces during heating increases.Therefore improved the risk of quick-fried hammer.
How to improve diamond synthesizing process stability; The stability of high temperature insulating material under high-temperature and high-pressure conditions during particularly big cavity diamond is synthetic; Avoid the gas of these materials in the diamond synthesis process to discharge; Thereby improving the security of pressure leak process, reduce quick-fried hammer risk, is problem demanding prompt solution in present diamond synthesizing process and the equipment.
Summary of the invention
The present invention is directed to present cubic hinge press diamond synthesis; Existing the problems referred to above during particularly the diamond of synthetic cavity diameter >=40mm synthesizes aim to provide a kind of big cavity diamond synthesis with high-temperature insulation earthenware and preparation method thereof, can avoid the gas of material therefor in the diamond building-up process to discharge; Improve the 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 realizing the foregoing invention purpose, the present invention adopts following technical scheme:
A kind of big cavity diamond synthesis is used the high-temperature insulation earthenware; It is characterized in that described high-temperature insulation earthenware is made through compression moulding, sintering by ceramic powder, dry powder formulation comprises the 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 the described sintering aid, transition metal ions is with Fe
2O
3The quality meter<0.3%; Alkali metal ion is in sodium and potassium oxide mass<1%.
Described high-temperature insulation earthenware adopts the preparation of following method: according to batching a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2; Use the a-aluminium oxide or the magnesia of purity >=99% to be raw material; In adding talcum or the kaolinite one or both are sintering aid, and dolomol is a releasing agent, and polyvinyl alcohol is a binding agent; Make slurry through wet ball grinding technology, the slurry mist projection granulating makes ceramic powder; With ceramic powder compression moulding, sintering makes described high-temperature insulation earthenware again.
Transition metal ions in the described sintering aid is with Fe
2O
3The quality meter<0.3%; Alkali metal ion sodium and potassium are in oxide mass<1%.
In the described method, adopting the corundum ball in the wet ball grinding technology is abrasive media, described slurry particle diameter≤2 microns.
Described binding agent polyvinyl alcohol (PVA) molecular weight >=10000, preferred 10000～100000.
In the described method, prilling temperature is not higher than 140 ℃.The dry powder particle diameter is 0.3-0.8mm after the granulation.
In the described method, ceramic powder is the moulding of 200-400MPa pressed at pressure.
In the described method, sintering is that the pipe with compression moulding places in the corundum saggar, fills with schmigel, at 850-1200 ℃ of following sintering again.The optimum condition of sintering is to be warmed up to 550 ℃ of insulations with 3.5 ℃/min and to come unstuck; Be warming up to 850-1200 ℃ of sintering with 5 ℃/min again.
Big cavity diamond synthesis of the present invention is used the high-temperature insulation earthenware; Adopt the high temperature insulating material (like powders such as corundum, magnesia) of high temperatures to add the insulating ceramic materials that talcum (or kaolinite) makes through compression moulding, sintering; Can be made into insulating tube and insulation tube, avoided the gas of these materials in the diamond synthesis process to discharge.Be used for the cubic hinge press diamond synthesis; Particularly in the suitability for industrialized production of the big 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.
Concrete feature and advantage of the present invention comprise at least:
1) high-temperature insulation pottery of the present invention uses a-aluminium oxide or magnesia to be main material, and talcum (or kaolinite) is a sintering aid, and polyvinyl alcohol is a molding adhesive, and dolomol is a releasing agent, is made through compression moulding, sintering by dry powder.Adopt the high temperature insulating material (like powders such as corundum, magnesia) of high temperatures to process earthenware, and it is carried out high annealing, avoided the gas of material in the diamond synthesis process to discharge.Transition metal ions and sodium in the raw material, potassium class alkali metal ion content measured are very low, and the insulation tube of this feedstock production is good insulation preformance at high temperature.
2) become required tubular blank by pressed by powder in the preparation process, tubular blank is placed in the corundum saggar, fill with schmigel again, at 850-1200 ℃ of following sintering.Bury powder on the one hand and limited the earthenware diametric contraction deformation in edge in the sintering process, guaranteed the diameter uniformity and the caliber size of pipe; On the other hand, high temperature sintering has been removed volatile material (like the hydroxyl in the raw material, moisture, organic binder bond), has avoided prepared insulation tube or insulating tube under the high pressure-temperature condition of diamond synthesis, to produce gas; The 3rd, through sintering process, the density of insulation tube is bigger, and intensity is high, is difficult for fragmentation, helps the 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 when temperature is higher than 1450 ℃; Owing to having generated a small amount of cordierite (or blue or green spinelle) suitable plasticity is arranged; Help the pressure transmission under the synthetic hot environment of diamond, thereby improved the pressure uniformity; Thereby can improve a distributing homogeneity and a concentration degree that the footpath distributes of diamond particles in the graphite post.
The specific embodiment
Big cavity diamond synthesis of the present invention is used the high-temperature insulation earthenware, with a-aluminium oxide (Chun Du>99%) or magnesia (Chun Du>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 the sintering aid is with Fe for sintering aid
2O
3The quality meter<0.3%; Alkali metal ion is in sodium, potassium oxide mass<1%), polyvinyl alcohol is a binding agent; Make the slurry of particle diameter≤2 micron through wet ball grinding technology, 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 method preparation:
1) with a-aluminium oxide (Chun Du>99%) or magnesia (Chun Du>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 the auxiliary agent is with Fe for sintering aid
2O
3The quality meter<0.3%; Alkali metal ion sodium, potassium are in oxide mass<1%), dolomol is a releasing agent; With a-aluminium oxide or magnesia, sintering aid and dolomol according to 75～90:10～25:1～2 ball grinder of packing into; According to mass ratio (a-aluminium oxide or magnesia+sintering aid): corundum ball: water=100:400:200～250 add the corundum balls, and (commercial production is with diameter 15-70mm corundum ball; The laboratory is with diameter 5-20mm corundum ball) and water; Ball milling 8～24 hours makes particle diameter less than 2 microns slurry.
2) press (a-aluminium oxide or magnesia+sintering aid) in the gained slurry: the 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 ℃; The dry powder particle diameter is 0.3～0.8mm after the granulation.
3) taking by weighing required powder, in mould, is that 200～400MPa press down process required tubular blank at pressure with its can.
4) the tubular blank vertical pendulum is put in the corundum saggar, fills the inside and the surrounding space of pipe again with schmigel, up to pipe is buried; Saggar is warmed up to 550 ℃ of insulations with 3.5 ℃/min to come unstuck in 1 hour; Be warmed up to 850-1200 ℃ with 5 ℃/min, sintering 1 hour makes described high-temperature insulation earthenware again.
Embodiment 1
In the steel ball grinder of the length 2.5m of liner nylon, diameter 1.5m, with a-aluminium oxide, talcum, water, dolomol by mass ratio: 85/15/200/2 ball grinder of packing into.With raw material (aluminium oxide+talcum)/corundum ball mass ratio 100/400 corundum ball of packing 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 commentaries on classics/min ball millings 24 hours.After isolating the corundum ball, slip was left standstill in the pond 1 hour, let mail a small amount of in ball grinder liner nylon sheet gap and do not sunk to the pond by levigate bulky grain sandstone at the bottom of; The upper strata slip is sent into dosing chamber with slush pump, is the aqueous solution that 100:1.5 adds polyvinyl alcohol by (aluminium oxide+talcum)/polyvinyl alcohol mass ratio, and granulation is carried out with stainless steel mist projection granulating tower in the back that stirs.The granulation tower gas flow temperature is 120 ℃.The powder ball particle diameter is 0.3-0.7mm after the granulation.
Thickness, diameter and altitude information according to earthenware; Take by weighing required powder; (in the mould of YG18～YG20), be that 400MPa presses down and processes required tubular blank at pressure, the length of pipe is usually than design size big by 5～8% (allowance for shrinkage in the sintering) in carbide alloy with its can.The pipe vertical pendulum is put in the corundum saggar, fills the inside and the surrounding space of pipe again with schmigel, up to pipe is buried.Saggar is placed Muffle furnace (or tunnel cave), be warmed up to 550 ℃ with 3.5 ℃/min, insulation was come unstuck 1 hour, removed binding agent; Be warmed up to 850～1200 ℃ with 5 ℃/min again, be incubated 1 hour.The nature cooling can make the high-temperature insulation earthenware.
For diameter 42mm earthenware, the shrinkage factor of its length direction and the relation such as the table 1 of sintering temperature:
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 the dolomite insulation tube with the high-temperature insulation earthenware that makes, assembling back diamond synthesis in cubic hinge press, by catalyst: graphite=25%:75% batching preparation graphite post carries out diamond and synthesizes, and synthesis condition is: 1450 ℃, 28min.
The result is as shown in table 2 below.
Table 2 dolomite insulated with material pipe and alumina insulation pipe (1000 ℃) diamond synthesis effect relatively
Dolomite insulation tube diamond synthesizing technology is implemented six months 2/platform of average top hammer spoilage, and alumina insulation pipe diamond synthesizing technology is implemented hammer spoilage＜1, average top/platform of six months.
Embodiment 2
For cylinder diameter 750mm diamond synthesis press, cavity diameter 60mm.Method by embodiment 1 prepares diameter 56mm insulation tube, the shrinkage factor of its length direction and the relation such as the table 3 of sintering temperature.
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 the dolomite insulation tube with the high-temperature insulation earthenware that makes, assembling back diamond synthesis in cubic hinge press, by catalyst: graphite=25%:75% batching preparation graphite post carries out diamond and synthesizes, and synthesis condition is: 1450 ℃, 28min.
The result is as shown in table 4 below.
The diamond synthesis effect of table 4 dolomite insulated with material pipe and alumina insulation pipe (1000 ℃) relatively
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 adopting alumina insulation pipe diamond synthesizing technology steady production of the present invention 1 month, quick-fried hammer phenomenon does not appear.
Embodiment 3
According to embodiment 1 essentially identical prepared powder, wherein the batching be: magnesia, talcum, water, dolomol mass ratio 85/15/250/2.The ball grinder of packing into was with 10 commentaries on classics/min ball millings 16 hours.The powder ball particle diameter is 0.3-0.8mm after the granulation.
The moulding of pipe, sintering condition are identical with embodiment 1, make the high-temperature insulation earthenware.
For diameter 38mm earthenware, the shrinkage factor of its length direction and the relation such as the table 5 of sintering temperature:
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 is weightless | 11.3 | 11.3 | 11.3 | 11.3 | 11.7 | 12 | 12 |
| Compression strength/MPa | 412 | 437 | 457 | 510 | 608 | 732 | 740 |
Substitute the dolomite insulation tube with the high-temperature insulation earthenware that makes, assembling back diamond synthesis in cubic hinge press, by catalyst: graphite=25%:75% batching preparation graphite post carries out diamond and synthesizes, and synthesis condition is: 1450 ℃, 28min.
Implemented 6 months result such as following table 6 continuously.
The diamond synthesis effect of table 6 dolomite insulated with material pipe and alumina insulation pipe relatively
Dolomite insulation tube diamond synthesizing technology is implemented six months 1.5/platform of average top hammer spoilage, and magnesia insulation tube diamond synthesizing technology is implemented hammer spoilage＜0.8, average top/platform of six months.
Embodiment 4
According to preparing the high-temperature insulation earthenware with embodiment 1 essentially identical method, 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 such as the table 7 of sintering temperature:
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 is weightless | 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 the dolomite insulation tube with the high-temperature insulation earthenware that makes, assembling back diamond synthesis in cubic hinge press, by catalyst: graphite=25%:75% batching preparation graphite post carries out diamond and synthesizes, and synthesis condition is: 1450 ℃, 28min.Implemented 6 months continuously, effect and embodiment 1 are similar, but synthetic chamber deformation uniformity is not so good as the former slightly, and the type variable is big.
Embodiment 5
According to preparing the high-temperature insulation earthenware with embodiment 1 essentially identical method, 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 such as the table 8 of sintering temperature:
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 is weightless | 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 the dolomite insulation tube with the high-temperature insulation earthenware that makes, assembling back diamond synthesis in cubic hinge press, by catalyst: graphite=25%:75% batching preparation graphite post carries out diamond and synthesizes, and synthesis condition is: 1450 ℃, 28min.Implemented 6 months continuously, effect and embodiment 1 are similar, building-up process lumen deformation good uniformity, and the shape conservation rate is high, but synthesis pressure (oil pressure) will improve 5-8%, explains that the pressure transmission ability has decline slightly.
Claims (10)
1. one kind big cavity diamond synthesis is used the high-temperature insulation earthenware; It is characterized in that described high-temperature insulation earthenware is made through compression moulding, sintering by ceramic powder, dry powder formulation comprises the 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 the described sintering aid, transition metal ions is with Fe
2O
3The quality 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 the preparation of following method: according to quality batching a-aluminium oxide or magnesia: sintering aid: binding agent: dolomol=75～90:10～25:1～2:1～2, and use the a-aluminium oxide of purity>=99% or magnesia to be raw material, one or both in adding talcum or the kaolinite are sintering aid; Dolomol is a releasing agent; Polyvinyl alcohol is a binding agent, makes the slurry of particle diameter≤2 micron through wet ball grinding technology, and the slurry mist projection granulating makes the ceramic powder that particle diameter is 0.3～0.8mm; With the moulding of ceramic powder 200～400MPa pressed, make behind 850～1200 ℃ of sintering again.
4. one kind big cavity diamond synthesis is with the preparation method of 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 are raw material with the a-aluminium oxide or the magnesia of purity >=99%, and adding in talcum or the kaolinite one or both is sintering aid; Dolomol is a releasing agent; Polyvinyl alcohol is a binding agent, makes slurry through wet ball grinding technology, and the slurry mist projection granulating makes ceramic powder; With ceramic powder compression moulding, sintering makes described high-temperature insulation earthenware again.
5. the preparation method of high-temperature insulation earthenware according to claim 4 is characterized in that, the transition metal ions in the described sintering aid is with Fe
2O
3The quality 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 the described method, adopting the corundum ball in the wet ball grinding technology is abrasive media, described slurry particle diameter≤2 microns.
7. the preparation method of high-temperature insulation earthenware according to claim 4 is characterized in that, in the described method, prilling temperature is not higher than 140 ℃, and the ceramic powder particle diameter is 0.3～0.8mm after the granulation.
8. the preparation method of high-temperature insulation earthenware according to claim 4 is characterized in that, in the described method, ceramic powder is the moulding of 200～400MPa pressed at pressure.
9. the preparation method of high-temperature insulation earthenware according to claim 4 is characterized in that, in the described method, sintering is that the pipe with compression moulding places in the corundum saggar, fills with schmigel, at 850～1200 ℃ of following sintering again.
10. the preparation method of high-temperature insulation earthenware according to claim 4 is characterized in that, said method comprising the steps of:
1) use a-aluminium oxide or magnesia to be raw material, talcum and/or kaolinite are sintering aid, and dolomol is a releasing agent; With the a-aluminium oxide of purity >=99% or magnesia, sintering aid talcum and/or kaolinite and dolomol according to 75～90:10～25:1～2 ball grinder of packing into; According to mass ratio (a-aluminium oxide or magnesia+sintering aid): corundum ball: water=100:400:200～250 add corundum ball and water, and ball milling 8～24 hours makes particle diameter less than 2 microns slurry;
2) press (a-aluminium oxide or magnesia+sintering aid) in the gained slurry: the polyvinyl alcohol mass ratio is that 100:1～2 add the binding agent polyvinyl alcohol water solutions, is made into dry powder with atomizing granulating technology, and prilling temperature is not higher than 140 ℃; The dry powder particle diameter is 0.3～0.8mm after the granulation;
3) taking by weighing required powder, in mould, is that 200～400MPa press down process required tubular blank at pressure with its can;
4) the tubular blank vertical pendulum is put in the corundum saggar, fills the inside and the surrounding space of pipe again with schmigel, up to pipe is buried; Saggar is warmed up to 550 ℃ of insulations with 3.5 ℃/min to come unstuck in 1 hour; Be warmed up to 850～1200 ℃ with 5 ℃/min, sintering 1 hour makes described high-temperature insulation earthenware again.
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| CN104103387A (en) * | 2014-06-17 | 2014-10-15 | 宁国新博能电子有限公司 | Insulating sleeve |
| CN107159060A (en) * | 2017-04-05 | 2017-09-15 | 河南黄河旋风股份有限公司 | A kind of method of diamond synthesis and the dolomite bushing pipe of diamond synthesis |
| CN109966994A (en) * | 2019-04-26 | 2019-07-05 | 河南省力量钻石股份有限公司 | A kind of diamond synthesizing compound block for transmitting pressure and preparation method thereof |
| CN113813875A (en) * | 2021-08-27 | 2021-12-21 | 中南钻石有限公司 | Pressure transmission sealing medium raw material for synthesis of cubic press and preparation method and application thereof |
| CN116813312A (en) * | 2023-07-11 | 2023-09-29 | 聊城冠县尚敖超硬材料有限公司 | High-heat-insulation material for diamond synthesis and preparation process thereof |
| CN118437230A (en) * | 2024-07-08 | 2024-08-06 | 吉林大学 | Preparation method of hexagonal diamond and cubic-hexagonal heterostructure |
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| 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 |
| KR101046264B1 (en) * | 2011-02-01 | 2011-07-08 | 주식회사 비앤비 | Ceramic powder coating composion, steel pipe pile coated the same and process for preparing the same |
| 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 |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011782A (en) * | 2013-01-17 | 2013-04-03 | 宁夏天宇光电太阳能科技有限公司 | Method for preparing alumina ceramic tube used for sodium-nickel battery |
| CN104103387A (en) * | 2014-06-17 | 2014-10-15 | 宁国新博能电子有限公司 | Insulating sleeve |
| CN104103387B (en) * | 2014-06-17 | 2016-12-28 | 青岛燕园海洋生物科技有限公司 | A kind of insulated sleeve |
| CN107159060A (en) * | 2017-04-05 | 2017-09-15 | 河南黄河旋风股份有限公司 | A kind of method of diamond synthesis and the dolomite bushing pipe of diamond synthesis |
| CN109966994A (en) * | 2019-04-26 | 2019-07-05 | 河南省力量钻石股份有限公司 | A kind of diamond synthesizing compound block for transmitting pressure and preparation method thereof |
| CN113813875A (en) * | 2021-08-27 | 2021-12-21 | 中南钻石有限公司 | Pressure transmission sealing medium raw material for synthesis of cubic press and preparation method and application thereof |
| CN116813312A (en) * | 2023-07-11 | 2023-09-29 | 聊城冠县尚敖超硬材料有限公司 | High-heat-insulation material for diamond synthesis and preparation process thereof |
| CN118437230A (en) * | 2024-07-08 | 2024-08-06 | 吉林大学 | Preparation method of hexagonal diamond and cubic-hexagonal heterostructure |
| CN118437230B (en) * | 2024-07-08 | 2024-09-24 | 吉林大学 | Preparation method of hexagonal diamond and cubic-hexagonal heterostructure |
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