CN117229077B - High-strength refractory material based on ceramic micro powder and preparation method thereof - Google Patents
High-strength refractory material based on ceramic micro powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 180
- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- 239000011819 refractory material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002699 waste material Substances 0.000 claims abstract description 87
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 81
- 239000002131 composite material Substances 0.000 claims abstract description 69
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 41
- 238000002156 mixing Methods 0.000 claims abstract description 40
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000005011 phenolic resin Substances 0.000 claims abstract description 37
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 37
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 19
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 16
- 239000010431 corundum Substances 0.000 claims abstract description 16
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000013384 organic framework Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000011282 treatment Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 230000036571 hydration Effects 0.000 claims description 9
- 238000006703 hydration reaction Methods 0.000 claims description 9
- GJKFIJKSBFYMQK-UHFFFAOYSA-N lanthanum(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GJKFIJKSBFYMQK-UHFFFAOYSA-N 0.000 claims description 6
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000000197 pyrolysis Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005121 nitriding Methods 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 9
- 229910017109 AlON Inorganic materials 0.000 abstract description 6
- 239000011230 binding agent Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000000377 silicon dioxide Substances 0.000 abstract description 5
- AZJLMWQBMKNUKB-UHFFFAOYSA-N [Zr].[La] Chemical compound [Zr].[La] AZJLMWQBMKNUKB-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011247 coating layer Substances 0.000 abstract description 3
- 239000011258 core-shell material Substances 0.000 abstract description 3
- 238000005336 cracking Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000005253 cladding Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 15
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 102000020897 Formins Human genes 0.000 description 1
- 108091022623 Formins Proteins 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to the field of refractory materials, in particular to a high-strength refractory material based on ceramic micro powder and a preparation method thereof, wherein waste sanitary porcelain is used as a raw material, nano alumina and submicron aluminum nitride are introduced as cladding materials, carbothermal nitridation, oxidization and other processes are introduced to form a core-shell structure, and AlON powder is formed on the waste sanitary porcelain; treating the composite ceramic micro powder with citric acid and phenolic resin, and forming a phenolic resin coating layer on AlON in situ through adsorption and polymerization; mixing silicon micropowder, corundum powder, mullite powder and alumina powder as auxiliary agents to form rare earth modified corundum-mullite ceramic; nanometer silica is introduced into the refractory material in the form of silica sol and plays a role of partially replacing a binder, and the lanthanum-zirconium bimetallic organic framework is adopted to modify the silica sol, so that the refractory material is kept uniform, and the cracking resistance of the refractory material is improved.
Description
Technical Field
The invention relates to the field of refractory materials, in particular to a high-strength refractory material based on ceramic micro powder and a preparation method thereof.
Background
The narrow definition refractory refers to inorganic nonmetallic materials that are resistant to high temperatures above 1580 ℃ without softening and melting under no load. The broad sense refractory material refers to a material which can be used in a high temperature environment, and is widely applied in the industrial fields of metallurgy, chemical industry, petroleum, electric power, silicate, mechanical manufacturing and the like, and is a basic material for technical development in the fields.
Along with the development of industrialization, the exploitation and discarding of raw materials of refractory materials are both growing, waste ceramics occupy a relatively large area in waste refractory materials, how to change waste into valuables is the research focus in the field of preparing high-strength refractory materials by using the waste ceramics.
Disclosure of Invention
The invention aims to provide a high-strength refractory material based on ceramic micro powder and a preparation method thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a high-strength refractory material based on ceramic micropowder and a preparation method thereof comprise the following steps:
s1: pulverizing and sieving the waste sanitary porcelain, and dividing the waste sanitary porcelain into waste sanitary porcelain coarse powder, waste sanitary porcelain middle powder and waste sanitary porcelain fine powder;
s2: mixing the waste sanitary porcelain coarse powder and the waste sanitary porcelain middle powder, adding the modified silica sol, stirring, adding the mixed solution of the waste sanitary porcelain fine powder, the nano alumina, the submicron aluminum nitride and the modified silica sol, drying and then pyrolyzing to obtain a composite precursor;
s3: performing high Wen Tanre nitridation treatment, oxidization and ball milling on the composite precursor to obtain composite ceramic micro powder;
s4: performing hydration resistance treatment on the composite ceramic micro powder to obtain water-resistant composite ceramic micro powder;
s5: mixing silicon micropowder, corundum powder, mullite powder and alumina powder as an auxiliary agent;
s6: mixing the water-resistant composite ceramic micro powder, an auxiliary agent, modified silica sol and phenolic resin to obtain a green body, and drying, mould pressing and sintering the green body to obtain the high-strength refractory material based on the ceramic micro powder.
Further, the size of the waste sanitary porcelain fine powder is 10-15 mu m, the size of the powder in the waste sanitary porcelain is 30-45 mu m, and the size of the waste sanitary porcelain coarse powder is 150-180 mu m.
Further, the working conditions of pyrolysis in step S2 are: in argon, the temperature is 890-900 ℃ and the time is 1-2h.
Further, in the step S2, the weight portions of the waste sanitary porcelain coarse powder are 20-25, the weight portions of the waste sanitary porcelain middle powder are 15-20, the weight portions of the modified silica sol are 1-3, the weight portions of the waste sanitary porcelain fine powder are 10-15, the weight portions of the nanometer alumina are 30-35, and the weight portions of the submicron aluminum nitride are 5-7.
Further, the working conditions of high Wen Tanre nitriding in step S3 are: in a nitrogen environment, heat preservation is carried out for 1h at 1700-1730 ℃, the working condition of oxidation in the step S3 is that the temperature is raised to 650-680 ℃ in the air, heat preservation is carried out for 1h, and the working condition of ball milling in the step S3 is that: ball milling was performed at 400r/min for 8 hours using a planetary ball mill.
Further, the preparation of the water-resistant composite ceramic micro powder comprises the following steps: mixing the composite ceramic micro powder with absolute ethyl alcohol, adding citric acid, phenolic resin and ethyl alcohol, mixing, ball milling and drying to obtain the water-resistant composite ceramic micro powder.
Further, the composition of the green body is as follows in parts by weight: 20-22 parts of water-resistant composite ceramic micro powder, 12-15 parts of auxiliary agent, 0.2-0.5 part of modified silica sol and 0.1 part of phenolic resin.
Further, the weight ratio of corundum powder, mullite powder, silicon micropowder and alumina powder in the auxiliary agent is 20:14:3:13.
further, the sum of the mass of the water-resistant composite ceramic micro powder and the mass of the auxiliary agent is a, the sum of the mass of the modified silica sol and the mass of the phenolic resin is b, and the mass ratio of b to a is 0.9% -1.6%.
Further, the preparation of the modified silica sol comprises the following steps:
1) Mixing lanthanum nitrate hexahydrate, zirconium chloride, 1,3, 5-trimesic acid and DMF, heating to 175-180 ℃, preserving heat for 22-24 hours, centrifuging, filtering, washing with DMF and ethanol for 3-5 times in sequence, and drying to obtain a bimetal organic frame;
2) And mixing and stirring the bimetal organic framework and the nano silica sol to obtain the modified silica sol.
Further, the sintering working conditions are as follows: heating to 680 ℃ at 4 ℃/min, preserving heat for 1h, and then heating to 1700-1780 ℃ at 8 ℃/min, preserving heat for 2h.
The invention has the beneficial effects that:
the invention provides a ceramic micropowder-based high-strength refractory material and a preparation method thereof, wherein waste sanitary porcelain is used as a raw material to prepare the ceramic micropowder-based high-strength refractory material with high fracture resistance and good erosion resistance.
Because the waste sanitary porcelain has the characteristics of high strength, granulation, no gas generation in the re-firing process and the like after high-temperature sintering, the invention takes the waste sanitary porcelain as a raw material, breaks and screens, and aims at the problems of complex components, difficult stripping of colored glaze materials and the like of the existing waste sanitary porcelain, nano aluminum oxide and submicron aluminum nitride are introduced as cladding materials, carbothermal nitridation, oxidization and other processes are introduced to form a core-shell structure, alON powder is formed on the waste sanitary porcelain, and the low-melting-point components in the waste sanitary porcelain are shielded and wrapped on the microstructure, so that the high-temperature performance in the waste sanitary porcelain is greatly improved, and waste materials are changed into valuable materials.
The composite ceramic micro powder is treated by citric acid and phenolic resin, and a phenolic resin coating layer is formed on AlON in situ through adsorption and polymerization, so that the hydration resistance of the composite ceramic micro powder is greatly improved.
Mixing silicon micropowder, corundum powder, mullite powder and alumina powder as an auxiliary agent, mixing the auxiliary agent with water-resistant composite ceramic micropowder and modified silica sol by controlling the content ratio of the auxiliary agent, and sintering to form rare earth modified corundum-mullite ceramic, wherein AlON in the water-resistant composite ceramic micropowder can compensate cracks generated by metal melting expansion, so that the volume density and the bending strength of the refractory material are effectively improved.
According to the invention, modified silica sol and phenolic resin are introduced as binders before sintering, and silica is introduced into the refractory material in the form of silica sol to play a role of partially replacing the binders, so that the high temperature resistance of the generated refractory material is effectively improved; in order to improve the compatibility between the silica sol and the phenolic resin and between the hydration-resistant ceramic micro powder and the auxiliary agent, the lanthanum-zirconium bimetal organic frame is adopted to carry out modification treatment on the nano silica sol, so that the refractory material is kept uniform, and the cracking resistance of the refractory material is improved.
The sum of the mass of the water-resistant composite ceramic micro powder and the mass of the auxiliary agent is a, the sum of the mass of the modified silica sol and the mass of the phenolic resin is b, the mass ratio of b to a is 0.9-1.6%, and La is formed when the refractory material is sintered 2+ 、Zr 2+ And the modified silica sol is sintered to form zirconia, lanthanum oxide and silicon oxide, so that the high-temperature fracture resistance of the refractory material is effectively improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely in connection with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, if directional indications such as up, down, left, right, front, and rear … … are involved in the embodiment of the present invention, the directional indications are merely used to explain a relative positional relationship, a movement condition, and the like between a certain posture such as the respective components, and if the certain posture is changed, the directional indications are changed accordingly. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The following description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
Example 1: a preparation method of a high-strength refractory material based on ceramic micro powder comprises the following steps:
s1: pulverizing and sieving the waste sanitary porcelain, and dividing the waste sanitary porcelain into waste sanitary porcelain coarse powder, waste sanitary porcelain middle powder and waste sanitary porcelain fine powder;
the size of the waste sanitary porcelain fine powder is 10 mu m, the size of the powder in the waste sanitary porcelain is 30 mu m, and the size of the waste sanitary porcelain coarse powder is 150 mu m;
s2: mixing the waste sanitary porcelain coarse powder and the waste sanitary porcelain middle powder, adding the modified silica sol, stirring, adding the mixed solution of the waste sanitary porcelain fine powder, the nano alumina, the submicron aluminum nitride and the modified silica sol, drying and then pyrolyzing to obtain a composite precursor;
the ceramic powder comprises, by mass, 20 parts of waste sanitary porcelain coarse powder, 15 parts of waste sanitary porcelain middle powder, 1 part of modified silica sol, 10 parts of waste sanitary porcelain fine powder, 30 parts of nano aluminum oxide and 5 parts of submicron aluminum nitride;
the working conditions of pyrolysis are: in argon, the temperature is 890 ℃ and the time is 2 hours;
s3: performing high Wen Tanre nitridation treatment, oxidization and ball milling on the composite precursor to obtain composite ceramic micro powder;
the working conditions of the high-temperature carbothermal nitridation are as follows: preserving heat for 1h at 1700 ℃ in a nitrogen environment; the oxidation working condition is that the temperature is raised to 650 ℃ in the air and the heat is preserved for 1h; the working conditions of ball milling are as follows: ball milling is carried out for 8 hours at 400r/min by using a planetary ball mill;
s4: performing hydration-resistant treatment on the composite ceramic micro powder to obtain the water-resistant composite ceramic micro powder, wherein the preparation method comprises the following steps of: mixing 5g of composite ceramic micro powder with 200mL of absolute ethyl alcohol, adding 3mmol of citric acid, 1mmol of phenolic resin and 100mL of ethyl alcohol, mixing, ball milling and drying to obtain water-resistant composite ceramic micro powder;
s5: mixing silicon micropowder, corundum powder, mullite powder and alumina powder as an auxiliary agent;
the weight ratio of corundum powder, mullite powder, silicon micropowder and alumina powder in the auxiliary agent is 20:14:3:13;
s6: mixing the water-resistant composite ceramic micro powder, an auxiliary agent, modified silica sol and phenolic resin to obtain a green body, and drying, mould pressing and sintering to obtain a high-strength refractory material based on the ceramic micro powder;
the green body comprises the following components in parts by weight: 20 parts of water-resistant composite ceramic micro powder, 12 parts of auxiliary agent, 0.2 part of modified silica sol and 0.1 part of phenolic resin;
the mass sum of the water-resistant composite ceramic micro powder and the auxiliary agent is a, the mass sum of the modified silica sol and the phenolic resin is b, and the mass ratio of b to a is 0.9%;
the preparation of the modified silica sol comprises the following steps:
1) Mixing 3mmol of lanthanum nitrate hexahydrate, 6mmol of zirconium chloride, 3mmo1,3, 5-trimesic acid and 60mM of LDMF, heating to 175 ℃, preserving heat for 24 hours, centrifuging, filtering, washing with DMF and ethanol for 3 times in sequence, and drying to obtain a bimetal organic framework;
2) Mixing and stirring 1g of the bimetallic organic framework and 15g of nano silica sol to obtain modified silica sol;
the sintering working conditions are as follows: the temperature is raised to 680 ℃ at 4 ℃/min for 1h, and then raised to 1700 ℃ at 8 ℃/min for 2h.
Example 2: a preparation method of a high-strength refractory material based on ceramic micro powder comprises the following steps:
s1: pulverizing and sieving the waste sanitary porcelain, and dividing the waste sanitary porcelain into waste sanitary porcelain coarse powder, waste sanitary porcelain middle powder and waste sanitary porcelain fine powder;
the size of the waste sanitary porcelain fine powder is 12 mu m, the size of the powder in the waste sanitary porcelain is 40 mu m, and the size of the waste sanitary porcelain coarse powder is 170 mu m;
s2: mixing the waste sanitary porcelain coarse powder and the waste sanitary porcelain middle powder, adding the modified silica sol, stirring, adding the mixed solution of the waste sanitary porcelain fine powder, the nano alumina, the submicron aluminum nitride and the modified silica sol, drying and then pyrolyzing to obtain a composite precursor;
the ceramic powder comprises, by mass, 22 parts of waste sanitary porcelain coarse powder, 16 parts of waste sanitary porcelain middle powder, 2 parts of modified silica sol, 13 parts of waste sanitary porcelain fine powder, 32 parts of nano aluminum oxide and 6 parts of submicron aluminum nitride;
the working conditions of pyrolysis are: under argon, the temperature is 895 ℃ and the time is 1.5h;
s3: performing high Wen Tanre nitridation treatment, oxidization and ball milling on the composite precursor to obtain composite ceramic micro powder;
the working conditions of the high-temperature carbothermal nitridation are as follows: preserving heat for 1h at 1720 ℃ in a nitrogen environment; the oxidation working condition is that the temperature is raised to 660 ℃ in the air and the heat is preserved for 1h; the working conditions of ball milling are as follows: ball milling is carried out for 8 hours at 400r/min by using a planetary ball mill;
s4: performing hydration-resistant treatment on the composite ceramic micro powder to obtain the water-resistant composite ceramic micro powder, wherein the preparation method comprises the following steps of: mixing 5g of composite ceramic micro powder with 200mL of absolute ethyl alcohol, adding 3mmol of citric acid, 1mmol of phenolic resin and 100mL of ethyl alcohol, mixing, ball milling and drying to obtain water-resistant composite ceramic micro powder;
s5: mixing silicon micropowder, corundum powder, mullite powder and alumina powder as an auxiliary agent;
the weight ratio of corundum powder, mullite powder, silicon micropowder and alumina powder in the auxiliary agent is 20:14:3:13;
s6: mixing the water-resistant composite ceramic micro powder, an auxiliary agent, modified silica sol and phenolic resin to obtain a green body, and drying, mould pressing and sintering to obtain a high-strength refractory material based on the ceramic micro powder;
the green body comprises the following components in parts by weight: 21 parts of water-resistant composite ceramic micro powder, 13 parts of auxiliary agent, 0.3 part of modified silica sol and 0.1 part of phenolic resin;
the mass sum of the water-resistant composite ceramic micro powder and the auxiliary agent is a, the mass sum of the modified silica sol and the phenolic resin is b, and the mass ratio of b to a is 1.2%;
the preparation of the modified silica sol comprises the following steps:
1) Mixing 3mmol of lanthanum nitrate hexahydrate, 6mmol of zirconium chloride, 3mmo1,3, 5-trimesic acid and 60mM of LDMF, heating to 178 ℃, preserving heat for 23h, centrifuging, filtering, washing with DMF and ethanol for 4 times in sequence, and drying to obtain a bimetal organic framework;
2) Mixing and stirring 1g of the bimetallic organic framework and 15g of nano silica sol to obtain modified silica sol;
the sintering working conditions are as follows: heating to 680 ℃ at 4 ℃/min, preserving heat for 1h, and then heating to 1750 ℃ at 8 ℃/min, preserving heat for 2h.
Example 3: a preparation method of a high-strength refractory material based on ceramic micro powder comprises the following steps:
s1: pulverizing and sieving the waste sanitary porcelain, and dividing the waste sanitary porcelain into waste sanitary porcelain coarse powder, waste sanitary porcelain middle powder and waste sanitary porcelain fine powder;
the size of the waste sanitary porcelain coarse powder is 15 mu m, the size of the powder in the waste sanitary porcelain is 45 mu m, and the size of the waste sanitary porcelain fine powder is 180 mu m;
s2: mixing the waste sanitary porcelain coarse powder and the waste sanitary porcelain middle powder, adding the modified silica sol, stirring, adding the mixed solution of the waste sanitary porcelain fine powder, the nano alumina, the submicron aluminum nitride and the modified silica sol, drying and then pyrolyzing to obtain a composite precursor;
the ceramic powder comprises, by mass, 25 parts of waste sanitary porcelain coarse powder, 20 parts of waste sanitary porcelain middle powder, 3 parts of modified silica sol, 15 parts of waste sanitary porcelain fine powder, 35 parts of nano alumina and 7 parts of submicron aluminum nitride;
the working conditions of pyrolysis are: in argon, the temperature is 900 ℃ and the time is 1h;
s3: performing high Wen Tanre nitridation treatment, oxidization and ball milling on the composite precursor to obtain composite ceramic micro powder;
the working conditions of the high-temperature carbothermal nitridation are as follows: preserving heat for 1h at 1730 ℃ in a nitrogen environment; the oxidation working condition is that the temperature is raised to 680 ℃ in the air and the heat is preserved for 1h; the working conditions of ball milling are as follows: ball milling is carried out for 8 hours at 400r/min by using a planetary ball mill;
s4: performing hydration-resistant treatment on the composite ceramic micro powder to obtain the water-resistant composite ceramic micro powder, wherein the preparation method comprises the following steps of: mixing 5g of composite ceramic micro powder with 200mL of absolute ethyl alcohol, adding 3mmol of citric acid, 1mmol of phenolic resin and 100mL of ethyl alcohol, mixing, ball milling and drying to obtain water-resistant composite ceramic micro powder;
s5: mixing silicon micropowder, corundum powder, mullite powder and alumina powder as an auxiliary agent;
the weight ratio of corundum powder, mullite powder, silicon micropowder and alumina powder in the auxiliary agent is 20:14:3:13;
s6: mixing the water-resistant composite ceramic micro powder, an auxiliary agent, modified silica sol and phenolic resin to obtain a green body, and drying, mould pressing and sintering to obtain a high-strength refractory material based on the ceramic micro powder;
the green body comprises the following components in parts by weight: 22 parts of water-resistant composite ceramic micro powder, 15 parts of auxiliary agent, 0.5 part of modified silica sol and 0.1 part of phenolic resin;
the mass sum of the water-resistant composite ceramic micro powder and the auxiliary agent is a, the mass sum of the modified silica sol and the phenolic resin is b, and the mass ratio of b to a is 1.6%;
the preparation of the modified silica sol comprises the following steps:
1) Mixing 3mmol of lanthanum nitrate hexahydrate, 6mmol of zirconium chloride, 3mmo1,3, 5-trimesic acid and 60mM of LDMF, heating to 180 ℃, preserving heat for 22 hours, centrifuging, filtering, washing with DMF and ethanol for 5 times in sequence, and drying to obtain a bimetal organic framework;
2) Mixing and stirring 1g of the bimetallic organic framework and 15g of nano silica sol to obtain modified silica sol;
the sintering working conditions are as follows: the temperature is raised to 680 ℃ at 4 ℃/min for 1h, and then raised to 1780 ℃ at 8 ℃/min for 2h.
Comparative example 1: in the case of example 3 as a control group, no nano-alumina and submicron aluminum nitride were added in step S2, and the other steps were normal.
Comparative example 2: with example 3 as a control group, the water-resistant composite ceramic micropowder was replaced with the composite ceramic micropowder, and the other procedures were normal.
Comparative example 3: taking the example 3 as a control group, the weight ratio of corundum powder, mullite powder, silicon micropowder and alumina powder in the auxiliary agent is 20:10:1:19, other steps are normal.
Comparative example 4: with example 3 as a control group, the modified silica sol was replaced with the nano silica sol, and the other procedures were normal.
Comparative example 5: taking example 3 as a control group, the composition of the green body in parts by weight is: 22 parts of water-resistant composite ceramic micro powder, 15 parts of auxiliary agent, 0.5 part of modified silica sol and 0.2 part of phenolic resin; the sum of the mass of the water-resistant composite ceramic micro powder and the mass of the auxiliary agent is a, the sum of the mass of the modified silica sol and the mass of the phenolic resin is b, the mass ratio of b to a is 1.9%, and other working procedures are normal.
Comparative example 6: taking example 3 as a control group, the composition of the green body in parts by weight is: 22 parts of water-resistant composite ceramic micro powder, 53 parts of auxiliary agent, 0.5 part of modified silica sol and 0.1 part of phenolic resin; the sum of the mass of the water-resistant composite ceramic micro powder and the mass of the auxiliary agent is a, the sum of the mass of the modified silica sol and the mass of the phenolic resin is b, the mass ratio of b to a is 0.8%, and other working procedures are normal.
The raw material sources are as follows:
the main components of the waste sanitary porcelain powder are as follows: 66.1% of silicon dioxide, 24.1% of aluminum oxide, 0.31% of magnesium oxide, 2.2% of ferric oxide, 1.01% of calcium oxide, 0.41% of titanium oxide, 2.32% of potassium oxide and 2.12% of sodium oxide; corundum powder 325F (99.3%): new electric smelting corundum plant in spring and yang city of Henan province; mullite powder (45 μm): jingzhou Hua Xin mullite limited; alumina powder 1344-28-1: zhejiang nanometer technology Co., ltd; nano silica sol VK-S01A: xuan Chengjing Rui New Material Co., ltd; nanometer alumina A299287, submicron aluminum nitride A432362, silicon micropowder S131649, citric acid C108869, lanthanum nitrate hexahydrate L106046, zirconium chloride Z109459, 1,3, 5-trimesic acid T109692, DMF (N, N-dimethylformamide) D111999, phenolic resin P195710: ala Ding Shiji; absolute ethanol, analytically pure: national drug group reagent.
Performance test: performance tests were conducted on the refractory bricks produced in examples 1 to 3 and comparative examples 1 to 6:
the refractory materials in the examples and comparative examples were sized to 250mm by 150mm by 60mm;
testing the bending strength of three points by a high-temperature fatigue tester;
thermal shock resistance: carrying out thermal shock circulation experiment on a sample by adopting a box-type resistance furnace, and firstly, carrying out a thermal shock circulation experiment on the sample by adopting the resistance furnace at the temperature of 5 ℃ for min -1 Heating to 1100 ℃, placing the sample in the sample, preserving the temperature for 15min, taking out the sample, performing air cooling to room temperature to finish one thermal shock, circulating for 5 times, testing the flexural strength before and after the circulation, and calculating the flexural strength retention rate;
crack resistance: detecting alkali resistance by adopting an alkali-dissolving crucible method, drilling a hole with the diameter of 50mm multiplied by 20mm in the refractory material, filling 20g of pure potassium carbonate into the hole, heating to 1200 ℃, preserving heat for 4 hours, and detecting whether cracks are generated after natural cooling; the results are shown in the following table;
| flexural Strength (MPa) | Flexural strength retention (%) | Crack resistance | |
| Example 1 | 338 | 71.9 | No crack |
| Example 2 | 342 | 72.4 | No crack |
| Example 3 | 346 | 73.1 | No crack |
| Comparative example 1 | 221 | 50.6 | Crack occurrence |
| Comparative example 2 | 292 | 59.5 | Crack occurrence |
| Comparative example 3 | 284 | 56.9 | Crack occurrence |
| Comparative example 4 | 232 | 51.4 | Crack occurrence |
| Comparative example 5 | 283 | 58.7 | Crack occurrence |
| Comparative example 6 | 271 | 57.2 | Crack occurrence |
The invention provides a high-strength refractory material based on ceramic micro powder and a preparation method thereof, and the refractory material prepared according to the invention has the advantages of 338-342MPa of bending strength, 71.9-73.1% of flexural strength retention rate, no crack in an alkali-dissolving crucible method, and high fracture resistance and good erosion resistance.
Comparing example 3 with comparative example 1, aiming at the problems of complex components, difficult stripping of colored glaze materials and the like of the existing waste sanitary porcelain, nano aluminum oxide and submicron aluminum nitride are introduced as coating materials, carbothermal nitridation, oxidization and other processes are introduced to form a core-shell structure, alON powder is formed on the waste sanitary porcelain, and the low-melting-point components in the waste sanitary porcelain are shielded and wrapped on the microstructure, so that the high-temperature performance in the waste sanitary porcelain is greatly improved, and waste is changed into valuable.
Comparing example 3 with comparative example 2, the composite ceramic micro powder is treated by citric acid and phenolic resin, and a phenolic resin coating layer is formed on AlON in situ through adsorption and polymerization, so that the hydration resistance of the composite ceramic micro powder is greatly improved, and the strength of the refractory material is improved.
Comparing the embodiment 3 with the comparative example 3, mixing silicon micropowder, corundum powder, mullite powder and alumina powder as auxiliary agents, and by controlling the content ratio of the auxiliary agents, mixing the auxiliary agents with water-resistant composite ceramic micropowder and modified silica sol and sintering to form rare earth modified corundum-mullite ceramic, wherein AlON in the water-resistant composite ceramic micropowder can compensate cracks generated by metal melting expansion, so that the volume density and the bending strength of the refractory material are effectively improved.
Comparing example 3 with comparative example 4, the modified silica sol and phenolic resin are introduced as binders before sintering, nano silica is introduced into the refractory material in the form of nano silica sol, and the nano silica plays a role of partially replacing the binders, so that the high temperature resistance of the generated refractory material is effectively improved; in order to improve the compatibility between the silica sol and the phenolic resin and between the hydration-resistant ceramic micro powder and the auxiliary agent, the lanthanum-zirconium bimetal organic frame is adopted to carry out modification treatment on the silica sol, so that the refractory material is kept uniform, and the cracking resistance of the refractory material is improved.
Comparing example 3 with comparative example 5 and comparative example 6, the water resistant composite ceramic microThe mass sum of the powder and the auxiliary agent is a, the mass sum of the modified silica sol and the phenolic resin is b, the mass ratio of b to a is 0.9-1.6%, and La is generated when the refractory material is sintered 2+ 、Zr 2+ And the modified silica sol is sintered to form zirconia, lanthanum oxide and silicon oxide, so that the high-temperature fracture resistance of the refractory material is effectively improved.
The foregoing description is only exemplary embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (5)
1. The preparation method of the high-strength refractory material based on the ceramic micro powder is characterized by comprising the following steps of:
s1: pulverizing and sieving the waste sanitary porcelain, and dividing the waste sanitary porcelain into waste sanitary porcelain coarse powder, waste sanitary porcelain middle powder and waste sanitary porcelain fine powder;
s2: mixing the waste sanitary porcelain coarse powder and the waste sanitary porcelain middle powder, adding the modified silica sol, stirring, adding the mixed solution of the waste sanitary porcelain fine powder, the nano alumina, the submicron aluminum nitride and the modified silica sol, drying and then pyrolyzing to obtain a composite precursor;
s3: performing high Wen Tanre nitridation treatment, oxidization and ball milling on the composite precursor to obtain composite ceramic micro powder;
s4: performing hydration resistance treatment on the composite ceramic micro powder to obtain water-resistant composite ceramic micro powder;
s5: mixing silicon micropowder, corundum powder, mullite powder and alumina powder as an auxiliary agent;
s6: mixing the water-resistant composite ceramic micro powder, an auxiliary agent, modified silica sol and phenolic resin to obtain a green body, and drying, mould pressing and sintering to obtain a high-strength refractory material based on the ceramic micro powder;
the preparation of the water-resistant composite ceramic micro powder comprises the following steps: mixing the composite ceramic micro powder with absolute ethyl alcohol, adding citric acid, phenolic resin and ethyl alcohol, mixing, ball milling and drying to obtain water-resistant composite ceramic micro powder;
the green body comprises the following components in parts by weight: 20-22 parts of water-resistant composite ceramic micro powder, 12-15 parts of auxiliary agent, 0.2-0.5 part of modified silica sol and 0.1 part of phenolic resin;
the weight ratio of corundum powder, mullite powder, silicon micropowder and alumina powder in the auxiliary agent is 20:14:3:13;
the mass sum of the water-resistant composite ceramic micro powder and the auxiliary agent is a, the mass sum of the modified silica sol and the phenolic resin is b, and the mass ratio of b to a is 0.9% -1.6%;
the preparation of the modified silica sol comprises the following steps:
1) Mixing lanthanum nitrate hexahydrate, zirconium chloride, 1,3, 5-trimesic acid and DMF, heating to 175-180 ℃, preserving heat for 22-24 hours, centrifuging, filtering, washing with DMF and ethanol for 3-5 times in sequence, and drying to obtain a bimetal organic frame;
2) And mixing and stirring the bimetal organic framework and the nano silica sol to obtain the modified silica sol.
2. The preparation method of the high-strength refractory material based on the ceramic micro powder, as claimed in claim 1, is characterized in that the size of the waste sanitary porcelain fine powder is 10-15 mu m, the size of the powder in the waste sanitary porcelain is 30-45 mu m, and the size of the waste sanitary porcelain coarse powder is 150-180 mu m.
3. The method for preparing a ceramic micropowder-based high-strength refractory according to claim 1, wherein the pyrolysis in step S2 is performed under the following conditions: in argon, the temperature is 890-900 ℃ and the time is 1-2h.
4. The method for preparing a ceramic micropowder-based high-strength refractory according to claim 1, wherein the working conditions of nitriding high Wen Tanre in step S3 are as follows: in a nitrogen environment, preserving heat for 1h at 1700-1730 ℃; the oxidation conditions in step S3 are: heating to 650-680 deg.c in air and maintaining for 1 hr; the working conditions of ball milling in the step S3 are as follows: ball milling was performed at 400r/min for 8 hours using a planetary ball mill.
5. A ceramic micropowder-based high strength refractory material, characterized in that it is produced by the production method according to any one of claims 1 to 4.
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| WO2017075865A1 (en) * | 2015-11-06 | 2017-05-11 | 武汉科技大学 | Lightweight slightly-closed-pore corundum composite refractory material and method for preparing same |
| CN110467443A (en) * | 2019-09-19 | 2019-11-19 | 广东工业大学 | A kind of aluminium nitride/Toughened Alumina Ceramics and preparation method thereof |
| WO2022100249A1 (en) * | 2020-11-12 | 2022-05-19 | 广东工业大学 | Slurry and preparation method for high-performance aluminum nitride ceramic substrate |
| CN115160001A (en) * | 2022-07-21 | 2022-10-11 | 郑州金河源耐火材料有限公司 | Multi-base composite low-heat-conduction refractory brick for garbage incinerator |
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| WO2017075865A1 (en) * | 2015-11-06 | 2017-05-11 | 武汉科技大学 | Lightweight slightly-closed-pore corundum composite refractory material and method for preparing same |
| CN110467443A (en) * | 2019-09-19 | 2019-11-19 | 广东工业大学 | A kind of aluminium nitride/Toughened Alumina Ceramics and preparation method thereof |
| WO2022100249A1 (en) * | 2020-11-12 | 2022-05-19 | 广东工业大学 | Slurry and preparation method for high-performance aluminum nitride ceramic substrate |
| CN115160001A (en) * | 2022-07-21 | 2022-10-11 | 郑州金河源耐火材料有限公司 | Multi-base composite low-heat-conduction refractory brick for garbage incinerator |
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