CN118145986A - Aluminum titanate ceramic nozzle material - Google Patents
Aluminum titanate ceramic nozzle material Download PDFInfo
- Publication number
- CN118145986A CN118145986A CN202410185748.7A CN202410185748A CN118145986A CN 118145986 A CN118145986 A CN 118145986A CN 202410185748 A CN202410185748 A CN 202410185748A CN 118145986 A CN118145986 A CN 118145986A
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- Prior art keywords
- oxide
- parts
- aluminum titanate
- ceramic nozzle
- nozzle material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910000505 Al2TiO5 Inorganic materials 0.000 title claims abstract description 46
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 title claims abstract description 46
- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 29
- 229920001661 Chitosan Polymers 0.000 claims abstract description 22
- 239000004005 microsphere Substances 0.000 claims abstract description 19
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 15
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 10
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 10
- 150000003254 radicals Chemical class 0.000 claims abstract description 10
- 238000004132 cross linking Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 34
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 18
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 14
- 239000005751 Copper oxide Substances 0.000 claims description 14
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 14
- 229910000431 copper oxide Inorganic materials 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000395 magnesium oxide Substances 0.000 claims description 14
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 14
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 12
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 9
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 9
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000009849 vacuum degassing Methods 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- ZQMIGQNCOMNODD-UHFFFAOYSA-N diacetyl peroxide Chemical compound CC(=O)OOC(C)=O ZQMIGQNCOMNODD-UHFFFAOYSA-N 0.000 claims 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 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229940057995 liquid paraffin Drugs 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052580 B4C Inorganic materials 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 10
- 239000011812 mixed powder Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/478—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on aluminium titanates
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Abstract
The invention relates to the field of ceramic materials, in particular to an aluminum titanate ceramic nozzle material which is prepared from the following raw materials in parts by weight: 70-90 parts of aluminum titanate, 5-10 parts of non-metal carbide, 15-30 parts of metal oxide, 4-8 parts of N-methylol acrylamide, 1-3 parts of octavinyl-POSS, 3-6 parts of carboxymethyl chitosan crosslinking microsphere, 0.1-0.5 part of dispersing agent, 0.1-0.5 part of free radical initiator and 200-300 parts of solvent.
Description
Technical Field
The invention relates to the field of ceramic materials, in particular to an aluminum titanate ceramic nozzle material.
Background
Aluminum titanate is the only stable compound of Al 2O3-TiO2, has the characteristics of high melting point, good impact resistance and thermal shock resistance, and is a novel ceramic material with low expansibility and high melting point.
The conventional forming methods of aluminum titanate ceramics mainly comprise slip casting, compression molding and isostatic pressing, and the forming methods have the advantages of long production period, low efficiency, uneven green body density and easiness in cracking, and are difficult to meet the production requirements of people. Gel casting is a novel ceramic forming technology newly developed in the last thirty years, the gel casting technology can realize the preparation of a blank with a complex shape at normal temperature and normal pressure, the obtained blank has uniform density and high mechanical strength, and the report of preparing aluminum titanate ceramic by gel casting is also available at present, but the mechanical strength of the prepared aluminum titanate ceramic is difficult to meet the use requirement.
Disclosure of Invention
The invention aims to: aiming at the technical problems, the invention provides an aluminum titanate ceramic nozzle material.
The technical scheme adopted is as follows:
The aluminum titanate ceramic nozzle material is prepared from the following raw materials in parts by weight:
70-90 parts of aluminum titanate, 5-10 parts of non-metal carbide, 15-30 parts of metal oxide, 4-8 parts of N-methylol acrylamide, 1-3 parts of octavinyl-POSS, 3-6 parts of carboxymethyl chitosan crosslinking microsphere, 0.1-0.5 part of dispersing agent, 0.1-0.5 part of free radical initiator and 200-300 parts of solvent.
Further, the nonmetallic carbide is any one or a combination of more than one of silicon carbide, boron carbide and nitrogen carbide.
Further, the metal oxide is any one or a combination of more of magnesium oxide, aluminum oxide, calcium oxide, zirconium oxide, zinc oxide, copper oxide, yttrium oxide, iron oxide, lanthanum oxide and cerium oxide.
Further, the metal oxide is a combination of magnesium oxide, zirconium oxide, copper oxide, iron oxide and cerium oxide;
The weight ratio of the magnesium oxide to the zirconium oxide to the copper oxide to the iron oxide to the cerium oxide is 1-5:1-5:0.1-1:0.1-1:5-15.
Further, the preparation method of the carboxymethylated chitosan crosslinked microsphere comprises the following steps:
adding carboxymethyl chitosan into sodium hydroxide aqueous solution, stirring to fully swell, adding liquid paraffin, stirring to emulsify to form water-in-oil solution, dropwise adding epichlorohydrin under the protection of nitrogen, reacting in water bath at 50-60 ℃ for 4-10h, centrifuging, collecting the obtained precipitate, and drying.
Further, the dispersing agent is any one or a combination of more than one of polymethacrylamide, polyacrylamide, polyacrylic acid, sodium polyacrylate and polyvinyl alcohol.
Further, the free radical initiator is any one or a combination of more of benzoyl peroxide, acetyl peroxide, ammonium persulfate and sodium persulfate.
Further, the solvent is a mixed solution consisting of tetrahydrofuran and water;
the volume fraction of tetrahydrofuran in the mixed solution is more than or equal to 50 percent.
The preparation method of the aluminum titanate ceramic nozzle material comprises the following steps:
Mixing aluminum titanate, nonmetallic carbide and metal oxide, ball milling, drying, uniformly mixing with N-methylolacrylamide, octavinyl-POSS, carboxymethyl chitosan crosslinking microsphere, a dispersing agent and a solvent to obtain slurry, adding a free radical initiator, fully stirring, uniformly mixing, vacuum degassing, injecting into a mould, curing and forming to obtain a blank, and finally drying, degreasing and sintering.
Further, the sintering temperature is 1450-1550 ℃ and the sintering time is 1-3h.
The invention has the beneficial effects that:
The invention provides an aluminum titanate ceramic nozzle material, nonmetallic carbide can reduce grain size and microcrack size through pinning effect, prevent abnormal grain growth and microcrack expansion, improve sintered compact density, improve mechanical strength, form liquid phase in sintering process of metal oxide, increase matrix fluidity, increase ion exchange speed, facilitate aluminum titanate ceramic sintering property improvement, realize aluminum titanate ceramic dynamic stability, in cooling process, liquid phase can bond surrounding grains together to improve ceramic material strength, octavinyl-POSS can polymerize with N-methylolacrylamide as cross-linking agent to form three-dimensional network structure, so ceramic powder in situ solidification forming green body, siO 2,Si4+ can form solid solution in situ during sintering, stability of aluminum titanate can be improved, sintering is promoted, carboxymethyl chitosan crosslinking microsphere forms three-dimensional network skeleton in green body interior and surface, contact degree of N-methylolacrylamide molecule and oxygen in air is promoted, monomer polymerization is promoted, green body is effectively prevented from being polymerized together due to oxygen inhibition polymerization in gel injection molding forming, the difference between external strength and thermal strength of the ceramic is improved, and the invention has high thermal density is higher than that of the ceramic is prepared to 65 MPa.
Drawings
FIG. 1 is an SEM image of an aluminum titanate ceramic nozzle material prepared in example 1.
Detailed Description
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention. The technology not mentioned in the present invention refers to the prior art, and unless otherwise indicated, the following examples and comparative examples are parallel tests, employing the same processing steps and parameters.
Aluminum titanate: 800 mesh, qing river county Ruijiang metal materials Co., ltd;
Silicon carbide: 2000 mesh, ultra-tai metal materials limited in the Qing river county;
Magnesium oxide: nanoscale, hebei magnesium science and technology, inc.;
Zirconia: 2000 mesh, eastern mountain chinese and new materials limited;
copper oxide: 325 mesh, beijing Gaokao New Material technologies Co., ltd;
Iron oxide: 800 mesh, langfang Peng color fine chemical Co., ltd;
cerium oxide: 800 mesh, mountain Dongchang Yao New Material Co., ltd;
n-methylolacrylamide: shandong Star sea chemical Co.Ltd
Octavinyl-POSS: hubei ferry chemical Co., ltd;
carboxymethylated chitosan crosslinked microspheres: self-making;
sodium polyacrylate: guangdong Weng Jiang chemical Co., ltd;
Ammonium persulfate: guangdong Weng Jiang chemical Co., ltd;
tetrahydrofuran: guangdong Weng Jiang chemical Co., ltd;
Water: deionized water.
Example 1:
The aluminum titanate ceramic nozzle material is prepared from the following raw materials in parts by weight:
80 parts of aluminum titanate, 10 parts of silicon carbide, 2.5 parts of magnesium oxide, 2.5 parts of zirconium oxide, 0.5 part of copper oxide, 0.5 part of ferric oxide, 12 parts of cerium oxide, 7 parts of N-methylolacrylamide, 2.5 parts of octavinyl-POSS, 4 parts of carboxymethyl chitosan crosslinking microsphere, 0.3 part of sodium polyacrylate, 0.25 part of ammonium persulfate and 250 parts of tetrahydrofuran/water solution.
The preparation method of the carboxymethyl chitosan crosslinked microsphere comprises the following steps:
Adding 2g of carboxymethylated chitosan into 30ml of 0.067mol/L sodium hydroxide aqueous solution, stirring for 30min to fully swell, adding 60ml of liquid paraffin, stirring for 1.5h to emulsify to form water-in-oil solution, then dropwise adding 1ml of cross-linking agent epichlorohydrin under the protection of nitrogen, performing water bath reaction at 50 ℃ for 6h, centrifuging, and collecting and drying the obtained precipitate.
The aluminum titanate ceramic nozzle materials are as follows:
Tetrahydrofuran and deionized water are mixed according to a volume ratio of 2: mixing evenly to obtain tetrahydrofuran/water solution, mixing aluminum titanate, silicon carbide, magnesium oxide, zirconium oxide, copper oxide, iron oxide and cerium oxide, ball milling for 10 hours, drying to obtain mixed powder, wherein the rotating speed is 250r/min, the ball milling medium is absolute ethyl alcohol, mixing the obtained mixed powder, N-methylolacrylamide, octavinyl-POSS, carboxymethyl chitosan crosslinked microsphere, dispersing agent sodium polyacrylate and tetrahydrofuran/water solution evenly to obtain slurry, adding a free radical initiator ammonium persulfate into the slurry, fully stirring, vacuum degassing for 5 minutes, injecting into a die, curing and molding at room temperature for 5 hours, demoulding to obtain a blank with smooth and flat surface and without peeling and dent, finally drying the obtained blank at 40 ℃ for 24 hours, placing the blank in a sintering furnace, degreasing at the temperature of 700 ℃ for 2 hours at the speed of 5 ℃/min, and sintering at the temperature of 1500 ℃ for 2 hours.
Example 2:
The aluminum titanate ceramic nozzle material is prepared from the following raw materials in parts by weight:
90 parts of aluminum titanate, 10 parts of silicon carbide, 2.5 parts of magnesium oxide, 2.5 parts of zirconium oxide, 0.5 part of copper oxide, 0.5 part of ferric oxide, 12 parts of cerium oxide, 8 parts of N-methylolacrylamide, 3 parts of octavinyl-POSS, 6 parts of carboxymethyl chitosan crosslinked microsphere, 0.5 part of sodium polyacrylate, 0.2 part of ammonium persulfate and 250 parts of tetrahydrofuran/water solution.
The preparation method of the carboxymethylated chitosan crosslinked microsphere is the same as that of example 1;
The aluminum titanate ceramic nozzle materials are as follows:
Tetrahydrofuran and deionized water are mixed according to a volume ratio of 2: mixing evenly to obtain tetrahydrofuran/water solution, mixing aluminum titanate, silicon carbide, magnesium oxide, zirconium oxide, copper oxide, iron oxide and cerium oxide, ball milling for 10 hours, drying to obtain mixed powder, wherein the rotating speed is 250r/min, the ball milling medium is absolute ethyl alcohol, mixing the obtained mixed powder, N-methylolacrylamide, octavinyl-POSS, carboxymethyl chitosan crosslinked microsphere, dispersing agent sodium polyacrylate and tetrahydrofuran/water solution evenly to obtain slurry, adding a free radical initiator ammonium persulfate into the slurry, fully stirring, vacuum degassing for 5 minutes, injecting into a die, curing and molding at room temperature for 5 hours, demoulding to obtain a blank with smooth and flat surface and without peeling and dent, finally drying the obtained blank at 40 ℃ for 24 hours, placing the blank in a sintering furnace, degreasing at the temperature of 700 ℃ for 2 hours at the speed of 5 ℃/min, and sintering at the temperature of 1550 ℃ for 2 hours.
Example 3:
The aluminum titanate ceramic nozzle material is prepared from the following raw materials in parts by weight:
70 parts of aluminum titanate, 5 parts of silicon carbide, 2.5 parts of magnesium oxide, 2.5 parts of zirconium oxide, 0.5 part of copper oxide, 0.5 part of ferric oxide, 12 parts of cerium oxide, 4 parts of N-methylolacrylamide, 2 parts of octavinyl-POSS, 4 parts of carboxymethyl chitosan crosslinked microsphere, 0.5 part of sodium polyacrylate, 0.1 part of ammonium persulfate and 250 parts of tetrahydrofuran/water solution.
The preparation method of the carboxymethylated chitosan crosslinked microsphere is the same as that of example 1;
The aluminum titanate ceramic nozzle materials are as follows:
Tetrahydrofuran and deionized water are mixed according to a volume ratio of 2: mixing evenly to obtain tetrahydrofuran/water solution, mixing aluminum titanate, silicon carbide, magnesium oxide, zirconium oxide, copper oxide, iron oxide and cerium oxide, ball milling for 10 hours, drying to obtain mixed powder, wherein the rotating speed is 250r/min, the ball milling medium is absolute ethyl alcohol, mixing the obtained mixed powder, N-methylolacrylamide, octavinyl-POSS, carboxymethyl chitosan crosslinked microsphere, dispersing agent sodium polyacrylate and tetrahydrofuran/water solution evenly to obtain slurry, adding a free radical initiator ammonium persulfate into the slurry, fully stirring, vacuum degassing for 5 minutes, injecting into a die, curing and molding at room temperature for 5 hours, demoulding to obtain a blank with smooth and flat surface and no peeling and concave, finally drying the obtained blank at 40 ℃ for 24 hours, placing the blank in a sintering furnace, degreasing at the temperature of 650 ℃ for 2 hours at the speed of 5 ℃/min, and sintering at the temperature of 1450 ℃ for 3 hours.
Comparative example 1:
substantially the same as in example 1, except that silicon carbide was not added.
Comparative example 2:
Substantially the same as in example 1, except that no magnesium oxide was added.
Comparative example 3:
Substantially the same as in example 1, except that zirconia was not added.
Comparative example 4:
substantially the same as in example 1, except that copper oxide was not added.
Comparative example 5:
Substantially the same as in example 1, except that no iron oxide was added.
Comparative example 6:
substantially the same as in example 1, except that cerium oxide was not added.
Comparative example 7:
Substantially the same as in example 1, except that octavinyl-POSS was not added.
Comparative example 8:
substantially the same as in example 1, except that the carboxymethylated chitosan crosslinked microspheres were not added.
Performance test:
The aluminum titanate ceramic nozzle materials prepared in examples 1 to 3 and comparative examples 1 to 8 of the present invention were used as test samples for performance test;
Measuring the volume density of the sample by adopting an Archimedes drainage method;
The bending strength of a sample is tested by adopting a CREE-8003A three-point bending resistant material testing machine, the size of the sample is 3mm multiplied by 4mm multiplied by 35mm, the testing span is 30mm, and the loading speed is 0.5mm/min;
measuring the thermal expansion coefficient of a sample by using a German relaxation-resistant DIL 402C/7 thermal expansion instrument, wherein the size of the sample is 3mm multiplied by 4mm multiplied by 35mm, and the heating rate is 5 ℃/min;
The test results are shown in table 1 below:
Table 1:
As shown in the table 1, the aluminum titanate ceramic nozzle material prepared by the invention has higher density and lower thermal expansion coefficient, and the bending strength is as high as more than 65 MPa.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The aluminum titanate ceramic nozzle material is characterized by being prepared from the following raw materials in parts by weight:
70-90 parts of aluminum titanate, 5-10 parts of non-metal carbide, 15-30 parts of metal oxide, 4-8 parts of N-methylol acrylamide, 1-3 parts of octavinyl-POSS, 3-6 parts of carboxymethyl chitosan crosslinking microsphere, 0.1-0.5 part of dispersing agent, 0.1-0.5 part of free radical initiator and 200-300 parts of solvent.
2. The aluminum titanate ceramic nozzle material of claim 1, wherein the non-metal carbide is any one or a combination of silicon carbide, boron carbide, nitrogen carbide.
3. The aluminum titanate ceramic nozzle material of claim 1, wherein the metal oxide is any one or more of magnesium oxide, aluminum oxide, calcium oxide, zirconium oxide, zinc oxide, copper oxide, yttrium oxide, iron oxide, lanthanum oxide, cerium oxide.
4. An aluminum titanate ceramic nozzle material as in claim 3 wherein said metal oxide is a combination of magnesium oxide, zirconium oxide, copper oxide, iron oxide, cerium oxide;
The weight ratio of the magnesium oxide to the zirconium oxide to the copper oxide to the iron oxide to the cerium oxide is 1-5:1-5:0.1-1:0.1-1:5-15.
5. The aluminum titanate ceramic nozzle material of claim 1, wherein the preparation method of the carboxymethylated chitosan crosslinked microspheres comprises the following steps:
adding carboxymethyl chitosan into sodium hydroxide aqueous solution, stirring to fully swell, adding liquid paraffin, stirring to emulsify to form water-in-oil solution, dropwise adding epichlorohydrin under the protection of nitrogen, reacting in water bath at 50-60 ℃ for 4-10h, centrifuging, collecting the obtained precipitate, and drying.
6. The aluminum titanate ceramic nozzle material of claim 1, wherein the dispersant is any one or a combination of more of polymethacrylamide, polyacrylamide, polyacrylic acid, sodium polyacrylate, polyvinyl alcohol.
7. The aluminum titanate ceramic nozzle material of claim 1, wherein the free radical initiator is any one or a combination of more of benzoyl peroxide, acetyl peroxide, ammonium persulfate, sodium persulfate.
8. The aluminum titanate ceramic nozzle material of claim 1 wherein the solvent is a mixed solution of tetrahydrofuran and water;
the volume fraction of tetrahydrofuran in the mixed solution is more than or equal to 50 percent.
9. The aluminum titanate ceramic nozzle material of claim 1, wherein the specific preparation method comprises the following steps:
Mixing aluminum titanate, nonmetallic carbide and metal oxide, ball milling, drying, uniformly mixing with N-methylolacrylamide, octavinyl-POSS, carboxymethyl chitosan crosslinking microsphere, a dispersing agent and a solvent to obtain slurry, adding a free radical initiator, fully stirring, uniformly mixing, vacuum degassing, injecting into a mould, curing and forming to obtain a blank, and finally drying, degreasing and sintering.
10. The aluminum titanate ceramic nozzle material of claim 9, wherein the sintering temperature is 1450-1550 ℃ and the sintering time is 1-3 hours.
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