CN101323527B - Preparation of ceramic thermal protection tube - Google Patents
Preparation of ceramic thermal protection tube Download PDFInfo
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- CN101323527B CN101323527B CN2007100150102A CN200710015010A CN101323527B CN 101323527 B CN101323527 B CN 101323527B CN 2007100150102 A CN2007100150102 A CN 2007100150102A CN 200710015010 A CN200710015010 A CN 200710015010A CN 101323527 B CN101323527 B CN 101323527B
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Abstract
The invention provides a preparation method of a thermal protection tube of ceramics, which comprises the preparation, shaping and firing of suspended ceramic slurry. The preparation method is characterized in that: organic matters are dissolved in water in a certain proportion to prepare an organic solution which is mixed with a dispersant in a certain proportion, and the pH is adjusted to 8 to 11 to prepare a mixed organic solution; then ceramic powders are completely mixed with the mixed organic solution in a certain proportion to prepare into the suspended ceramic slurry, into which a 0.01 to 0.2 wt percent of initiator is added, and injected into a non-absorbent pattern after vacuum mixing treatment is carried out, and then the suspended ceramic slurry goes through gelatinization for shaping at 60 DEG C to 100 DEC G for 0.1 hour to 3 hours; demoulding and drying are carried out and dried body is fired under certain conditions. The preparation method of the invention adopts a gel-casting shaping technology and the prepared protection tube has compact structure, even density distribution of the tube and high binding strength of tube interface, can keep chemical stability at high temperature, can be repeatedly or continuously used in high temperature working environment which suffers thermal shock, oxidation or molten steel erosion, and the like, and has highly sensitive temperature measurement system.
Description
Affiliated technical field
The present invention relates to a kind of preparation method of ceramic thermal protection tube, belong to the special cermacis preparing technical field.
Background technology
Ceramic thermal protection tube be adopt slip casting, extrude and etc. traditional production method productions such as static pressure; produce ceramic thermal protection tube both at home and abroad because the restriction of forming method at present; the heat protective tube density distribution that forms is inhomogeneous and production cost is high; in use be easy to generate stress concentration, cause cracking.In addition, relatively poor as the resistance to air loss of heat protective tube zirconium diboride, must be used with the inner sleeve of aluminum oxide, therefore, reduced the sensitivity of temp measuring system.
Summary of the invention
The object of the present invention is to provide a kind ofly can overcome above-mentioned defective, to make the pipe density distribution of protective tube even and production cost is low, the preparation method of the ceramic thermal protection tube of product excellent working performance, its technical scheme is:
Comprise the preparation of suspension ceramic slurry, moulding and burning till, it is characterized in that: with the organism formation organic solution that is dissolved in the water by a certain percentage, organic solution and dispersion agent mix the back by a certain percentage and adjust pH to 8～11 and make mixed organic solvents, then with ceramic powder and mixed organic solvents by a certain percentage thorough mixing make the suspension ceramic slurry, the initiator vacuum stirring that adds 0.01～0.2wt% in the suspension ceramic slurry is handled the back inject non-suction mould, 60～100 ℃ of temperature, gelation moulding under the condition of 0.1～3 hour time, demoulding drying is then burnt till dried base substrate under certain condition.
The preparation method of described ceramic thermal protection tube, ceramic powder is that granularity is that zirconium diboride powder, 0.3～5 μ m of 0.5～5 μ m is alumina powder jointed, 0.5～5 μ m zirconium diboride and 0.3～5 μ m aluminum oxide composite granule.
The preparation method of described ceramic thermal protection tube; non-suction mould adopts the assembly combined isolating cylinder of cover; be provided with multilayer; wherein the suspension ceramic slurry ceramic powder of innermost layer injection is single alumina powder jointed; the suspension ceramic slurry ceramic powder that outermost layer injects is single zirconium diboride powder; the ceramic powder of the suspension ceramic slurry that injects in other layer is the composite granule of zirconium diboride and aluminum oxide; and from inside to outside, the alumina powder jointed ratio that contains in the composite granule is successively decreased successively, zirconium diboride powder ratio increases progressively successively.
The preparation method of described ceramic thermal protection tube; organic solution is dissolved in by organism 1～75wt% in the water of 25～99wt% and forms; wherein organic component is N; N-methylene radical acrylamide and acrylamide; its weight percent is 1～10:90～99; organic solution adjusts to 8～11 with its pH value after mix 85～97:3～15 by weight percentage with dispersion agent again, promptly makes mixed organic solvents.
The preparation method of described ceramic thermal protection tube; dispersion agent adopts the polyacrylic acid ammonium solution; its concentration is 20～60wt%; it is that 40～60wt% ammoniacal liquor and concentration are lactic acid or the hydrochloric acid of 40～60wt% that the pH value is adjusted agent employing concentration; promptly to reduce the pH value of mixed organic solvents; it is 40～60wt% lactic acid or hydrochloric acid that the pH value is adjusted agent employing concentration, otherwise pH value adjustment agent employing concentration is 40～60wt% ammoniacal liquor.
The preparation method of described ceramic thermal protection tube, with ceramic powder with add ballstone after mixed organic solvents mixes according to weight ratio 70～85:15～30 and grind after, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
The preparation method of described ceramic thermal protection tube, it is the ammonium persulfate solution of 1～5wt% that initiator adopts concentration.
The preparation method of described ceramic thermal protection tube, the time that adds the stirring of initiator final vacuum was controlled in 0.5～3 minute, the suspension ceramic slurry was injected non-suction mould gelation moulding again, solidified demoulding drying then, made base substrate.
The preparation method of described ceramic thermal protection tube; the skimming temp of base substrate is 600 ℃～1300 ℃; degreasing time was not less than 0.5 hour; in 1700～1900 ℃ temperature range, burnt till in the hydrogen atmosphere 1 hour then, make the fine and close ceramic thermal protection tube of zirconium diboride-aluminum oxide gradient-structure high temperature.
The present invention compared with prior art, its advantage is:
1, suspension ceramic slurry of the present invention mainly is to adopt the zirconium diboride powder, or it is alumina powder jointed, or zirconium diboride and aluminum oxide composite granule are prepared from, this ceramic powder is evenly distributed in made suspension ceramic slurry, and then guarantee that heat protective tube base substrate microstructure, the density made are even, improve yield rate;
2, in present method owing to adopt the zirconium diboride powder, or it is alumina powder jointed, or zirconium diboride and aluminum oxide composite granule gradient-structure, the fine and close ceramic thermal protection tube interface bond strength of the zirconium diboride that makes-aluminum oxide gradient-structure high temperature height, compact structure, operating temperature range is widened greatly, temp measuring system highly sensitive;
3, because the fine and close ceramic thermal protection tube of the zirconium diboride that present method makes-aluminum oxide gradient-structure high temperature is high temperature resistant, its chemical stability of maintenance under hot conditions; so in high-temperature work environment; as be used for molten steel, brass, red copper melting; have performances such as heat shock resistance, anti-oxidant and anti-molten steel erosion because of it, can repeat or use continuously.
Embodiment
Embodiment 1: the preparation material is three layers of heat protective tube of alumina powder jointed, aluminum oxide and zirconium diboride composite granule, zirconium diboride powder
Step is:
1, preparation ceramic powder: ceramic powder has three kinds, first kind is that granularity is the alumina powder jointed of 1 μ m, second kind be granularity be the zirconium diboride powder of 5 μ m and alumina powder jointed weight ratio that granularity is 1 μ m with 1:1 mixed composite granule, the third is that granularity is the zirconium diboride powder of 5 μ m.
2, non-suction mould: adopt three layers of assembly combined isolating cylinder of cover.
3, preparation mixed organic solvents: with N, N-methylene radical acrylamide and acrylamide dissolve in the water with the mixed organism that gets of 2:98 weight percent, the weight percent of organism and water is 5:95, make organic solution, the polyacrylic acid ammonium solution dispersion agent that with organic solution and concentration is 40wt% again mixes with the weight ratio of 9:1, be that the ammoniacal liquor of 50wt% adjusts to 9 with the pH value of mixed solution with concentration then, promptly make mixed organic solvents.
3, preparation suspension ceramic slurry: with three kinds of ceramic powders of step 1 gained respectively with add the ballstone grinding after mixed organic solvents that step 2 makes mixes according to the weight ratio of 4:1 after, vacuum-treat does not have bubble to overflow to slurry again, make three kinds of even suspension ceramic slurries respectively, i.e. alumina slurry, zirconium diboride-aluminum oxide composite granule slurry and zirconium diboride slurry.
4, blank forming: with the concentration that adds 0.01wt% in three kinds of suspension ceramic slurries respectively is the ammonium persulfate solution initiator of 4wt%, vacuum stirring 2 minutes, be injected in three layers of non-suction mould by zirconium diboride slurry, zirconium diboride-aluminum oxide composite granule slurry, alumina slurry are corresponding from outside to inside then, and gelation moulding under 90 ℃ of temperature, the condition of 0.5 hour time, the dry base substrate that forms of the demoulding then.
5, base substrate degreasing: with base substrate 650 ℃ of degreasings 1 hour.
6, burn till: the base substrate after the degreasing is fired in 1800 ℃, hydrogen atmosphere burnt till in 1 hour, make the fine and close ceramic thermal protection tube of zirconium diboride-aluminum oxide gradient-structure high temperature.
The purity of testing used proportion material is technical pure.
The pyroceramic heat protective tube intensity that obtains is 150MPa., 2000 ℃ of heatproofs.
Embodiment 2: the preparation material is four layers of heat protective tube of alumina powder jointed, aluminum oxide and zirconium diboride composite granule, zirconium diboride powder
Step is:
1, preparation ceramic powder: ceramic powder has four kinds, first kind is that granularity is the alumina powder jointed of 1 μ m, the alumina powder jointed weight ratio that zirconium diboride powder that second kind of granularity is 5 μ m and granularity are 1 μ m with 3:7 mixed composite granule, the third granularity be the zirconium diboride powder of 5 μ m and alumina powder jointed weight ratio that granularity is 1 μ m with 7:3 mixed composite granule, the 4th kind is that granularity is the zirconium diboride powder of 5 μ m.
2, non-suction mould: adopt four layers of assembly combined isolating cylinder of cover.
3, preparation mixed organic solvents: with N, N-methylene radical acrylamide and acrylamide dissolve in the water with the mixed organism that gets of 5:95 weight percent, the weight ratio of organism and water is 1:4, make organic solution, the polyacrylic acid ammonium solution dispersion agent that with organic solution and concentration is 60wt% again mixes with the weight percent of 97:3, be that the ammoniacal liquor of 60wt% adjusts to 10 with the pH value of mixed solution with concentration then, promptly make mixed organic solvents.
3, preparation suspension ceramic slurry: with four kinds of ceramic powders of step 1 gained respectively with add the ballstone grinding after mixed organic solvents that step 2 makes mixes according to the weight ratio of 7:3 after, vacuum-treat does not have bubble to overflow to slurry again, make four kinds of even suspension ceramic slurries respectively, i.e. alumina slurry, two kinds of zirconium diboride-aluminum oxide composite granule slurries and zirconium diboride slurry.
4, blank forming: with the concentration that adds 0.1wt% in four kinds of suspension ceramic slurries respectively is the ammonium persulfate solution initiator of 2wt%, vacuum stirring 2 minutes, press the zirconium diboride slurry then, zirconium diboride powder and alumina powder jointed ratio are zirconium diboride-aluminum oxide composite granule slurry of 7:3, zirconium diboride powder and alumina powder jointed ratio are zirconium diboride-aluminum oxide composite granule slurry of 3:7, alumina slurry is corresponding from outside to inside to be injected in four layers of non-suction mould, and 90 ℃ of temperature, gelation moulding under the condition of 1 hour time, the dry base substrate that forms of the demoulding then.
5, base substrate degreasing: with base substrate 1000 ℃ of degreasings 1 hour.
6, burn till: the base substrate after the degreasing is fired in 1700 ℃, hydrogen atmosphere burnt till in 1 hour, make the fine and close ceramic thermal protection tube of zirconium diboride-aluminum oxide gradient-structure high temperature.
The purity of testing used proportion material is technical pure.
The pyroceramic heat protective tube intensity that obtains is 200MPa., 1700 ℃ of heatproofs.
Embodiment 3: the preparation material is three layers of heat protective tube of alumina powder jointed, aluminum oxide and zirconium diboride composite granule, zirconium diboride powder
Step is:
1, preparation ceramic powder: ceramic powder has three kinds, first kind is that granularity is the alumina powder jointed of 0.3 μ m, the alumina powder jointed weight ratio that zirconium diboride powder that second kind of granularity is 3 μ m and granularity are 0.3 μ m with 4:1 mixed composite granule, the third is that granularity is the zirconium diboride powder of 3 μ m.
2, non-suction mould: adopt three layers of assembly combined isolating cylinder of cover.
3, preparation mixed organic solvents: with N, N-methylene radical acrylamide and acrylamide dissolve in the water with the mixed organism that gets of 10:90 weight percent, the weight percent of organism and water is 70:30, make organic solution, the polyacrylic acid ammonium solution dispersion agent that with organic solution and concentration is 20wt% again mixes with the weight percent of 85:15, be that the ammoniacal liquor of 40wt% adjusts to 8 with the pH value of mixed solution with concentration then, promptly make mixed organic solvents.
3, preparation suspension ceramic slurry: with three kinds of ceramic powders of step 1 gained respectively with add the ballstone grinding after mixed organic solvents that step 2 makes mixes according to the weight ratio of 17:3 after, vacuum-treat does not have bubble to overflow to slurry again, make three kinds of even suspension ceramic slurries respectively, i.e. alumina slurry, zirconium diboride-aluminum oxide composite granule slurry and zirconium diboride slurry.
4, blank forming: with the concentration that adds 0.2wt% in three kinds of suspension ceramic slurries respectively is the ammonium persulfate solution initiator of 1wt%, vacuum stirring 1.5 minutes, be injected in three layers of non-suction mould by zirconium diboride slurry, zirconium diboride-aluminum oxide composite granule slurry, alumina slurry are corresponding from outside to inside then, and gelation moulding under 90 ℃ of temperature, the condition of 0.5 hour time, the dry base substrate that forms of the demoulding then.
5, base substrate degreasing: with base substrate 1300 ℃ of degreasings 1 hour.
6, burn till: the base substrate after the degreasing is fired in 1900 ℃, hydrogen atmosphere burnt till in 1 hour, make the fine and close ceramic thermal protection tube of zirconium diboride-aluminum oxide gradient-structure high temperature.
The purity of testing used proportion material is technical pure.
The pyroceramic heat protective tube intensity that obtains is 100MPa., 2000 ℃ of heatproofs.
Claims (7)
1. the preparation method of a ceramic thermal protection tube, comprise the preparation of suspension ceramic slurry, moulding and burning till, it is characterized in that: ceramic powder is that granularity is the zirconium diboride powder of 0.5～5 μ m, 0.3～5 μ m are alumina powder jointed, 0.5～5 μ m zirconium diborides and 0.3～5 μ m aluminum oxide composite granule, organic component is N, N-methylene radical acrylamide and acrylamide, with organism 1～75: 25～99 formation organic solutions that are dissolved in the water by weight percentage, organic solution and dispersion agent mix back and adjust pH to 8～11 make mixed organic solvents by weight percentage at 85～97: 3～15, then with ceramic powder and mixed organic solvents according to weight percent 70～85: 15～30 thorough mixing are made the suspension ceramic slurry, the initiator vacuum stirring that adds 0.01～0.2wt% in the suspension ceramic slurry is handled the back inject non-suction mould, 60～100 ℃ of temperature, gelation moulding under the condition of 0.1～3 hour time, demoulding drying then, dried base substrate was burnt till in the hydrogen atmosphere 1 hour in 1700～1900 ℃ temperature range, make the fine and close ceramic thermal protection tube of zirconium diboride-aluminum oxide gradient-structure high temperature; Wherein non-suction mould adopts the assembly combined isolating cylinder of cover, be provided with multilayer, wherein the suspension ceramic slurry ceramic powder of innermost layer injection is single alumina powder jointed, the suspension ceramic slurry ceramic powder that outermost layer injects is single zirconium diboride powder, the ceramic powder of the suspension ceramic slurry that injects in other layer is the composite granule of zirconium diboride and aluminum oxide, and from inside to outside, the alumina powder jointed ratio that contains in the composite granule is successively decreased successively, zirconium diboride powder ratio increases progressively successively.
2. the preparation method of ceramic thermal protection tube as claimed in claim 1, it is characterized in that: N, the weight percent of N-methylene radical acrylamide and acrylamide are 1～10: 90～99.
3. the preparation method of ceramic thermal protection tube as claimed in claim 1; it is characterized in that: dispersion agent adopts the polyacrylic acid ammonium solution; its concentration is 20～60wt%; it is that 40～60wt% ammoniacal liquor and concentration are lactic acid or the hydrochloric acid of 40～60wt% that the pH value is adjusted agent employing concentration; promptly to reduce the pH value of mixed organic solvents; it is 40～60wt% lactic acid or hydrochloric acid that the pH value is adjusted agent employing concentration, otherwise pH value adjustment agent employing concentration is 40～60wt% ammoniacal liquor.
4. the preparation method of ceramic thermal protection tube as claimed in claim 1 is characterized in that: with ceramic powder with add ballstone after mixed organic solvents mixes and grind after, vacuum-treat does not have bubble to overflow to slurry again, makes even suspension ceramic slurry.
5. the preparation method of ceramic thermal protection tube as claimed in claim 1 is characterized in that: it is the ammonium persulfate solution of 1～5wt% that initiator adopts concentration.
6. the preparation method of ceramic thermal protection tube as claimed in claim 1; it is characterized in that: the time that adds the stirring of initiator final vacuum was controlled in 0.5～3 minute; again the suspension ceramic slurry is injected non-suction mould gelation moulding, solidify demoulding drying then, make base substrate.
7. the preparation method of ceramic thermal protection tube as claimed in claim 1, it is characterized in that: the skimming temp of base substrate is 600 ℃～1300 ℃, and degreasing time was not less than 0.5 hour.
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| CN2007100150102A CN101323527B (en) | 2007-06-13 | 2007-06-13 | Preparation of ceramic thermal protection tube |
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| CN2007100150102A CN101323527B (en) | 2007-06-13 | 2007-06-13 | Preparation of ceramic thermal protection tube |
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| CN101323527B true CN101323527B (en) | 2011-03-02 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4717692A (en) * | 1984-04-27 | 1988-01-05 | Aluminum Company Of America | Composites comprising one or more interwoven matrix compositions each containing a refractory hard metal and method of forming same |
| EP0500093A1 (en) * | 1991-02-20 | 1992-08-26 | Sumitomo Electric Industries, Ltd. | Ceramic composite material and process for producing the same |
| CN1629100A (en) * | 2003-12-18 | 2005-06-22 | 山东理工大学 | Method for producing large-aperture porous ceramic element |
| CN1629097A (en) * | 2003-12-18 | 2005-06-22 | 山东理工大学 | Method for producing metal-ceramic gradient materials |
-
2007
- 2007-06-13 CN CN2007100150102A patent/CN101323527B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4717692A (en) * | 1984-04-27 | 1988-01-05 | Aluminum Company Of America | Composites comprising one or more interwoven matrix compositions each containing a refractory hard metal and method of forming same |
| EP0500093A1 (en) * | 1991-02-20 | 1992-08-26 | Sumitomo Electric Industries, Ltd. | Ceramic composite material and process for producing the same |
| CN1629100A (en) * | 2003-12-18 | 2005-06-22 | 山东理工大学 | Method for producing large-aperture porous ceramic element |
| CN1629097A (en) * | 2003-12-18 | 2005-06-22 | 山东理工大学 | Method for producing metal-ceramic gradient materials |
Non-Patent Citations (1)
| Title |
|---|
| 唐竹兴.注凝成型制备硼化锆-氧化铝复合材料.《硅酸盐通报》.2007,第26卷(第6期),全文. * |
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