CN114524673A - Preparation process of high-volume-density zirconia refractory material - Google Patents
Preparation process of high-volume-density zirconia refractory material Download PDFInfo
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- CN114524673A CN114524673A CN202111634205.1A CN202111634205A CN114524673A CN 114524673 A CN114524673 A CN 114524673A CN 202111634205 A CN202111634205 A CN 202111634205A CN 114524673 A CN114524673 A CN 114524673A
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 307
- 239000011819 refractory material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 119
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000005469 granulation Methods 0.000 claims abstract description 37
- 230000003179 granulation Effects 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000002844 melting Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 230000008018 melting Effects 0.000 claims abstract description 24
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 20
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 229910021532 Calcite Inorganic materials 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000007664 blowing Methods 0.000 claims description 20
- 238000007873 sieving Methods 0.000 claims description 17
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 17
- 239000002002 slurry Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 15
- 239000003381 stabilizer Substances 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 12
- 238000003723 Smelting Methods 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 238000010891 electric arc Methods 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000010431 corundum Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 9
- 229920002451 polyvinyl alcohol 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
- 238000004519 manufacturing process Methods 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 5
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 5
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 5
- 238000001238 wet grinding Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- NWBJYWHLCVSVIJ-UHFFFAOYSA-N N-benzyladenine Chemical compound N=1C=NC=2NC=NC=2C=1NCC1=CC=CC=C1 NWBJYWHLCVSVIJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 18
- 230000007547 defect Effects 0.000 abstract description 7
- 238000013461 design Methods 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- 239000000155 melt Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 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 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 238000009991 scouring Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- -1 zirconium ions Chemical class 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
A preparation process of a zirconia refractory material with high volume density comprises the following steps: (1) preparing electric melting zirconia powder; (2) preparing yttrium stable zirconia granulation powder; (3) mixing materials: adding the electric melting zirconia powder, yttrium stable zirconia granulation powder, SiC and nano eta-Al 2O3 into a high-speed mixing roll, and uniformly mixing and stirring; (4) pressing into a blank: pressing the mixture into a green body by a cold isostatic press under the pressure condition of 120-150 Mpa; (5) and (5) sintering and forming. The preparation process of the high-volume-density zirconia refractory material has reasonable design of process steps, perfects the crystal lattice development of the fused zirconia powder body, improves the surface performance of particles and eliminates defects through high-purity calcite and heat treatment,the electric melting zirconia powder and the yttrium stabilized zirconia granulation powder are taken as main materials, and SiC and nano eta-Al are added2O3The advantages of the electric melting zirconia powder and the yttrium stabilized zirconia granulation powder are combined, the fire resistance is excellent, the volume density is higher, the apparent porosity is smaller, and the preparation method is simple.
Description
Technical Field
The invention belongs to the technical field of zirconia products, and particularly relates to a preparation process of a zirconia refractory material with high volume density.
Background
The zirconium dioxide has the melting point of 2715 ℃, and the zirconium dioxide refractory material prepared by taking the zirconium dioxide as the main raw material has the advantages of stable chemical property at high temperature, ultrahigh use temperature (up to over 2400 ℃), suitability in oxidizing or reducing atmosphere and the like, and is the most mature refractory material for the ultrahigh-temperature field, which can be industrially produced and applied at present.
Currently, zirconia refractory materials can be classified into 3 general categories according to their thermal insulation properties: (1) a zirconia fiber product; (2) a high-purity zirconia hollow sphere heat insulation product; (3) a heavy zirconia article. The main material of the granule used by the zirconia heavy product is zirconia fused particles which are prepared by cooling and crushing fused zirconia melt, and the zirconia heavy product has the advantages of high structural strength, permeation resistance, scouring resistance and higher use temperature, has the defects of higher thermal conductivity and slightly poor heat insulation effect, and is mainly used for high-temperature reaction linings above 2000 ℃.
In addition, the fused zirconia powder is easy to have crystallization defects in the cooling process, such as vacancies, crystal plane dislocations, glass states and the like in crystal lattices, which causes unstable performance of the fused zirconia powder, and meanwhile, the process of mechanically crushing the zirconia refractory product can cause rough surfaces of zirconia particles, irregular particle shapes and uneven particle size distribution, so that a high-density blank is not easy to prepare in the forming process, the densification process of the fused zirconia powder is influenced during sintering, and the volume density is reduced. Therefore, it is necessary to develop a process for preparing a zirconia refractory having a high bulk density to solve the above-mentioned technical problems.
Chinese patent application No. CN201911386761.4 discloses a zirconia-based refractory material and a preparation method thereof, wherein the zirconia-based refractory material comprises zirconia, silica, alumina, a stabilizer, a bonding agent and other raw materials, and is prepared and molded by a three-step method of mixing, blanking and sintering molding, and the volume density and the apparent porosity of the zirconia refractory material are not further improved.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention aims to provide a preparation process of a high-volume-density zirconia refractory material, which has reasonable design of process steps, perfects the lattice development of the fused zirconia powder, improves the surface performance of particles and eliminates the defects by high-purity calcite and heat treatment, takes the fused zirconia powder and the yttrium-stabilized zirconia granulation powder as main materials, adds SiC and nano eta-Al 2O3, combines the advantages of the fused zirconia powder and the yttrium-stabilized zirconia granulation powder, has excellent refractory performance, higher volume density and smaller apparent porosity, and has simple preparation method and wide prospect.
The purpose of the invention is realized by the following technical scheme:
a preparation process of a high-volume-density zirconia refractory material comprises the following steps:
(1) preparing electric smelting zirconia powder: uniformly mixing the fused monoclinic zirconium and the stabilizer high-purity calcite by using a stirrer to obtain mixed powder; putting the mixed powder into a three-phase electric arc furnace for smelting, refining for 0.5-1h after the mixed powder is completely molten in the three-phase electric arc furnace to obtain a molten mass, carrying out melt blowing on the molten mass to obtain zirconia hollow spheres, collecting the blown zirconia hollow spheres, and grinding to 325 meshes to obtain stable zirconia powder; putting the zirconia powder into a corundum crucible and putting the corundum crucible into a heat treatment furnace, heating the heat treatment furnace to 1100-1200 ℃ at the speed of 8-10 ℃/min, preserving heat for 3-5h, closing the heat treatment furnace, cooling along with the furnace, taking out the powder, wet-grinding the powder in a planetary ball mill at the speed of 500r/min for 5-6h, sieving with a 325-mesh sieve, and drying to obtain the fused zirconia powder;
(2) preparing yttrium stable zirconia granulation powder: carrying out nodular graphite treatment on yttria-stabilized zirconia powder, deionized water and a dispersing agent in a planetary ball mill at the speed of 300-400r/min to prepare slurry, adding a binder into the slurry, stirring for 4-6h by a stirrer, then carrying out spray granulation by a spray granulator, and sieving by a 325-mesh sieve to obtain yttria-stabilized zirconia granulation powder;
(3) mixing materials: adding the electric melting zirconia powder, yttrium stable zirconia granulation powder, SiC and nano eta-Al 2O3 into a high-speed mixing roll, mixing and stirring uniformly, and sieving with a 325-mesh sieve;
(4) pressing into a blank: filling the material in the mold by adopting a volume-controlled filling method, and pressing the material into a green body by a cold isostatic press under the pressure condition of 120-150 Mpa;
(5) sintering and forming: and (3) drying the molded green body for 8-12h at the temperature of 100-120 ℃ in a constant-temperature drying oven, then placing the green body in a lifting furnace, heating to 1500-1600 ℃ at the heating rate of 8-10 ℃/min, preserving heat for 4-6h, then closing the lifting furnace, and cooling the sample along with the furnace to obtain the zirconia refractory material.
The preparation process of the high-volume-density zirconia refractory material has reasonable process step design, the fused zirconia powder prepared by adopting the melting and blowing process undergoes the quenching process from a high-temperature melt to a solid zirconia hollow ball, so the growth process of the crystal grain is inhibited, the crystal grain of the obtained powder is smaller, the fused zirconia powder consists of two parts, one part is formed by replacing zirconium ions with calcium ions of high-purity calcite to form a replacement solid solution, the coulomb repulsion inside a tetragonal zirconia crystal lattice is reduced by introducing an oxygen vacancy, the stability of the tetragonal zirconia crystal lattice is improved, the tetragonal phase is stored to be in a room temperature state, and the other part is a pure zirconia crystal lattice without ion doping, and the metastable tetragonal phase can be kept at the room temperature because the crystal grain size is smaller than the phase change critical size.
The metastable tetragonal phase is removed through heat treatment, the heat treatment can perfect the lattice development and improve the surface performance of particles, eliminate defects, ensure that the shapes of the particles of the fused zirconia powder are more regular and the particle sizes are more uniformly distributed, is favorable for preparing a high-density blank in the forming process, solves the problem of cracking of the fused zirconia powder in the sintering process caused by the volume expansion effect in the subsequent heat treatment in the prior art, and improves the volume density.
The yttrium-stabilized zirconia granulation powder with high sintering activity is obtained by pulping yttrium-stabilized zirconia powder, deionized water, a dispersant and a binder and then performing spray granulation by a spray granulator.
The zirconia refractory material mainly comprises electric melting zirconia powder and yttrium-stabilized zirconia granulation powder, and combines the advantages of high strength, permeation resistance, scouring resistance, high use temperature, high sintering activity of the yttrium-stabilized zirconia granulation powder, self sintering shrinkage in a high-temperature sintering process, formation of a large number of closed shrinkage cavities or closed micro air holes in a product, low thermal conductivity and good heat insulation effect of the electric melting zirconia powder, by adding SiC and nano eta-Al 2O3, forming mullite crystals by taking SiO2 after SiC oxidation as a silicon source and taking nano eta-Al 2O3 as an aluminum source, and uniformly distributing the mullite crystals in the zirconia refractory material, the zirconia refractory material is favorable for having higher volume density and smaller apparent porosity, and because the yttrium-stabilized zirconia granulation powder contains a binder, no binder is added during material mixing.
Further, in the preparation process of the zirconia refractory material with high bulk density, in the step (1), the fused monoclinic zirconium and the high-purity calcite serving as the stabilizer are both 325 meshes, and the stabilizer is the high-purity calcite; the melting blowing adopts compressed air blowing and the pressure is 8-10 kg.
Further, in the above process for preparing a zirconia refractory having a high bulk density, in the step (1), the mass ratio of the fused monoclinic zirconia to the stabilizer is 96-97: 3-4.
Further, in the above preparation process of the zirconia refractory material with high bulk density, in the step (2), the yttria-stabilized zirconia powder includes a zirconia powder having a mass ratio of 94.74:5.23: 0.035: 0.0022 parts of zirconia, yttria, ferric oxide, titania; the dispersing agent is one or a mixture of more of ammonium polyacrylate, sodium polyacrylate, ammonium citrate, DS005, CE-64 and glycerol; the binder is one or a mixture of polyvinyl alcohol, polyethylene glycol, sodium carboxymethyl cellulose, B-1000 and B-1022.
Further, in the preparation process of the zirconia refractory material with high bulk density, in the step (2), the mass ratio of the yttria-stabilized zirconia powder, the deionized water, the dispersant and the binder is 100-.
Further, in the preparation process of the zirconia refractory material with high bulk density, in the step (3), the mass ratio of the electrofused zirconia powder, the yttrium-stabilized zirconia granulation powder, the SiC, and the nano η -Al2O3 is 20-30: 50-60: 5-10:2-5.
Further, in the preparation process of the high-volume-density zirconia refractory material, 1500# SiC is adopted as the SiC, and the grain diameter is 10 μm; the purity of the nano eta-Al 2O3 is 99.5%, and the particle size is 20 nm.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation process of the high-volume-density zirconia refractory material has reasonable design of process steps, the fused zirconia powder prepared by adopting the melting and blowing process undergoes the quenching process from high-temperature melt to solid zirconia hollow spheres, so the growth process of the crystal grains is inhibited, the crystal grains of the obtained powder are smaller, the fused zirconia powder consists of two parts, one part is formed by replacing zirconium ions with calcium ions of high-purity calcite to form a replacement solid solution, the coulomb repulsion inside a tetragonal zirconia crystal lattice is reduced by introducing an oxygen vacancy, the stability of the tetragonal zirconia crystal lattice is improved, the tetragonal phase is stored to be in a room temperature state, and the other part is a pure zirconia crystal lattice without ion doping, and the metastable tetragonal phase can be kept at the room temperature because the size of the crystal grains is smaller than a phase-change critical size;
(2) according to the preparation process of the high-volume-density zirconia refractory material, the metastable tetragonal phase is removed through heat treatment, the heat treatment can perfect the lattice development and improve the surface performance of particles, and defects are eliminated, so that the particle shape of the fused zirconia powder is more regular, the particle size is more uniformly distributed, a high-density blank is favorably prepared in the forming process, the problem of cracking of the fused zirconia powder in the sintering process caused by the volume expansion effect in the subsequent heat treatment in the prior art is solved, and the volume density is improved;
(3) the preparation process of the high-volume-density zirconia refractory material mainly comprises the steps of taking the electric-melting zirconia powder and the yttrium-stabilized zirconia granulation powder as main materials, combining the advantages of high strength, permeation resistance, scouring resistance, high use temperature, high sintering activity of the yttrium-stabilized zirconia granulation powder, self sintering shrinkage in the high-temperature sintering process, formation of a large number of closed shrinkage cavities or closed micro air holes in the product, low heat conductivity and good heat insulation effect, adding SiC and nano eta-Al 2O3, taking SiO2 after SiC oxidation as a silicon source and nano eta-Al 2O3 as an aluminum source to form mullite crystals which are uniformly distributed in the zirconia refractory material, and being beneficial to the zirconia refractory material to have higher volume density and smaller apparent porosity.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described in the embodiments with reference to specific experimental data, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following examples 1, 2, 3, and 1 provide a process for preparing a zirconia refractory having a high bulk density.
Wherein the fused monoclinic zirconium and the stabilizer high-purity calcite are 325 meshes; the yttria-stabilized zirconia powder comprises the following components in a mass ratio of 94.74:5.23: 0.035: 0.0022 parts of zirconia, yttria, ferric oxide, titania; the dispersing agent is one or a mixture of more of ammonium polyacrylate, sodium polyacrylate, ammonium citrate, DS005, CE-64 and glycerol; the binder is one or a mixture of polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, B-1000 and B-1022; the SiC adopts 1500# SiC, and the particle size is 10 mu m; the purity of the nano eta-Al 2O3 is 99.5%, and the particle size is 20 nm.
Example 1
The preparation process of the zirconia refractory material with high volume density comprises the following steps:
(1) preparing electric smelting zirconia powder: the mass ratio of the electric melting monoclinic zirconium to the stabilizer is 96.5: 3.5, uniformly mixing the fused monoclinic zirconium and the stabilizer high-purity calcite by using a stirrer to obtain mixed powder; putting the mixed powder into a three-phase electric arc furnace for smelting, refining for 1h after the mixed powder is completely molten in the three-phase electric arc furnace to obtain a molten mass, carrying out melt blowing on the molten mass to obtain a zirconia hollow sphere, wherein the melt blowing adopts compressed air for blowing and the pressure is 8 kilograms, collecting the blown zirconia hollow sphere, and grinding to 325 meshes to obtain stable zirconia powder; putting the zirconia powder into a corundum crucible, putting the corundum crucible into a heat treatment furnace, heating the heat treatment furnace to 1150 ℃ at the speed of 10 ℃/min, preserving heat for 4 hours, closing the heat treatment furnace, cooling along with the furnace, taking out the powder, wet-grinding the powder in a planetary ball mill at the speed of 450r/min for 6 hours, sieving with a 325-mesh sieve, and drying to obtain the fused zirconia powder;
(2) preparing yttrium stable zirconia granulation powder: the mass ratio of the yttria-stabilized zirconia powder to the deionized water to the CE-64 to the 10 wt% PVA solution is 100:125:0.22:1.8, carrying out ball milling on the yttria-stabilized zirconia powder, the deionized water and the CE-64 in a planetary ball mill at the speed of 300r/min to prepare slurry, adding the 10 wt% PVA solution into the slurry, stirring for 5 hours by a stirrer, then carrying out spray granulation by a spray granulator, and sieving by a 325-mesh sieve to obtain yttrium-stabilized zirconia granulated powder;
(3) mixing materials: the mass ratio of the electric melting zirconia powder, the yttrium stable zirconia granulation powder, the SiC to the nano eta-Al 2O3 is 30: 50: 10:5, adding the electric melting zirconia powder, the yttrium stabilized zirconia granulation powder, SiC and nano eta-Al 2O3 into a high-speed mixing roll, mixing and stirring uniformly, and sieving with a 325-mesh sieve;
(4) pressing into a blank: filling the material in the mould by adopting a volume-controlled filling normal method, and pressing the material into a green body by a cold isostatic press under the pressure condition of 130 Mpa;
(5) sintering and forming: and (3) drying the molded green body for 12h at 110 ℃ in a constant-temperature oven, then placing the green body in a lifting furnace, heating to 1550 ℃ at the heating rate of 10 ℃/min, preserving heat for 5h, then closing the lifting furnace, and cooling the sample along with the furnace to obtain the zirconia refractory material.
Example 2
The preparation process of the zirconia refractory material with high volume density comprises the following steps:
(1) preparing electric smelting zirconia powder: the mass ratio of the electric melting monoclinic zirconium to the stabilizer is 97: 3, uniformly mixing the fused monoclinic zirconium and the stabilizer high-purity calcite by using a stirrer to obtain mixed powder; putting the mixed powder into a three-phase electric arc furnace for smelting, refining for 45min after the mixed powder is completely molten in the three-phase electric arc furnace to obtain a molten mass, performing melt blowing on the molten mass to obtain a zirconia hollow sphere, wherein the melt blowing adopts compressed air for blowing and the pressure is 10 kilograms, collecting the blown zirconia hollow sphere, and grinding to 325 meshes to obtain stable zirconia powder; putting the zirconia powder into a corundum crucible, putting the corundum crucible into a heat treatment furnace, heating the heat treatment furnace to 1200 ℃ at the speed of 9 ℃/min, preserving heat for 3.5 hours, closing the heat treatment furnace, cooling along with the furnace, taking out the powder, wet-grinding the powder in a planetary ball mill at the speed of 400r/min for 5 hours, sieving with a 325-mesh sieve, and drying to obtain the fused zirconia powder;
(2) preparing yttrium stable zirconia granulation powder: the method comprises the following steps of (1) carrying out ball milling on yttria-stabilized zirconia powder, deionized water and a dispersing agent (a mixture of sodium polyacrylate and DS005, wherein the mass ratio of sodium polyacrylate to DS005 is 3:2) and a 10 wt% sodium carboxymethylcellulose solution is 100:130:0.3: 1.6) in a planetary ball mill at the speed of 300-400r/min to prepare slurry, adding 10 wt% sodium carboxymethylcellulose solution into the slurry, stirring for 6 hours by a stirrer, then carrying out spray granulation by a spray granulator, and sieving by a 325-mesh sieve to obtain yttria-stabilized zirconia granulated powder;
(3) mixing materials: the mass ratio of the electric melting zirconia powder, the yttrium stable zirconia granulation powder, the SiC and the nano eta-Al 2O3 is 30: 55: 6:4, adding the electric melting zirconia powder, the yttrium stabilized zirconia granulation powder, SiC and the nano eta-Al 2O3 into a high-speed mixing roll, mixing and stirring uniformly, and sieving with a 325-mesh sieve;
(4) pressing into a blank: filling the material in the mould by adopting a volume-controlled filling method, and pressing the material into a green body by a cold isostatic press under the pressure condition of 120 Mpa;
(5) sintering and forming: and (3) drying the molded green body at 120 ℃ for 12h in a constant-temperature oven, then placing the green body in a lifting furnace, heating to 1580 ℃ at the rate of heating to 8 ℃/min, preserving heat for 5h, then closing the lifting furnace, and cooling the sample along with the furnace to obtain the zirconia refractory material.
Example 3
The preparation process of the zirconia refractory material with high volume density comprises the following steps:
(1) preparing electric smelting zirconia powder: the mass ratio of the electric melting monoclinic zirconium to the stabilizer is 96.2: 3.8, uniformly mixing the electrofused monoclinic zirconium and the stabilizer high-purity calcite by using a stirrer to obtain mixed powder; putting the mixed powder into a three-phase electric arc furnace for smelting, refining for 1h after the mixed powder is completely molten in the three-phase electric arc furnace to obtain a molten mass, carrying out melt blowing on the molten mass to obtain a zirconia hollow sphere, wherein the melt blowing adopts compressed air for blowing and the pressure is 9 kilograms, collecting the blown zirconia hollow sphere, and grinding to 325 meshes to obtain stable zirconia powder; putting the zirconia powder into a corundum crucible, putting the corundum crucible into a heat treatment furnace, heating the heat treatment furnace to 1180 ℃ at the speed of 9 ℃/min, preserving heat for 4 hours, closing the heat treatment furnace, cooling along with the furnace, taking out the powder, wet-grinding the powder in a planetary ball mill at the speed of 450r/min for 6 hours, sieving with a 325-mesh sieve, and drying to obtain the fused zirconia powder;
(2) preparing yttrium stable zirconia granulation powder: carrying out nodular graphite treatment on the yttria-stabilized zirconia powder, deionized water and a dispersing agent (a mixture of sodium polyacrylate and DS005, the mass ratio of the sodium polyacrylate to the DS005 is 1:1) and a 10 wt% PVA solution is 100:125:0.25:2 in a planetary ball mill at the speed of 400r/min to prepare slurry, adding the 10 wt% PVA solution into the slurry, stirring the slurry for 5 hours by a stirrer, then carrying out spray granulation by a spray granulator, and sieving the slurry by a 325-mesh sieve to obtain yttria-stabilized zirconia granulated powder;
(3) mixing materials: the mass ratio of the electric melting zirconia powder, the yttrium stable zirconia granulation powder, the SiC to the nano eta-Al 2O3 is 30: 50: 6:3, adding the electric melting zirconia powder, the yttrium stabilized zirconia granulation powder, SiC and nano eta-Al 2O3 into a high-speed mixing roll, mixing and stirring uniformly, and sieving with a 325-mesh sieve;
(4) pressing into a blank: filling the material in the mould by adopting a volume-controlled filling method, and pressing the material into a green body by a cold isostatic press under the pressure condition of 120 Mpa;
(5) sintering and forming: and (3) drying the molded green body for 12 hours at 110 ℃ in a constant-temperature oven, then placing the green body in a lifting furnace, heating to 1590 ℃ at the heating rate of 8 ℃/min, keeping the temperature for 5 hours, then closing the lifting furnace, and cooling the sample along with the furnace to obtain the zirconia refractory material.
Comparative example 1
The preparation process of the zirconia refractory material comprises the following steps:
(1) preparing electric melting zirconia powder: putting the fused monoclinic zirconium into a three-phase electric arc furnace for smelting, refining for 1h after the fused monoclinic zirconium is completely molten to obtain a molten mass, carrying out melt blowing on the molten mass to prepare a zirconia hollow sphere, wherein the melt blowing adopts compressed air for blowing and the pressure is 9 kg, collecting the blown zirconia hollow sphere, and grinding to 325 meshes to obtain fused zirconia powder;
(2) preparing yttrium stable zirconia granulation powder: carrying out nodular graphite treatment on the yttria-stabilized zirconia powder, deionized water and a dispersing agent (a mixture of sodium polyacrylate and DS005, the mass ratio of the sodium polyacrylate to the DS005 is 1:1) and a 10 wt% PVA solution is 100:125:0.25:2 in a planetary ball mill at the speed of 400r/min to prepare slurry, adding the 10 wt% PVA solution into the slurry, stirring the slurry for 5 hours by a stirrer, then carrying out spray granulation by a spray granulator, and sieving the slurry by a 325-mesh sieve to obtain yttria-stabilized zirconia granulated powder;
(3) mixing materials: the mass ratio of the electric melting zirconia powder to the yttrium stable zirconia granulation powder is 3: 5, adding the electric melting zirconia powder and the yttrium stabilized zirconia granulation powder into a high-speed mixing roll, mixing and stirring uniformly, and sieving with a 325-mesh sieve;
(4) pressing into a blank: filling the material in the mould by adopting a volume-controlled filling method, and pressing the material into a green body by a cold isostatic press under the pressure condition of 120 Mpa;
(5) sintering and forming: and (3) drying the molded green body for 12h at 110 ℃ in a constant-temperature oven, then placing the green body in a lifting furnace, heating to 1590 ℃ at the heating rate of 8 ℃/min, preserving heat for 5h, then closing the lifting furnace, and cooling the sample along with the furnace to obtain the zirconia refractory material.
Effect verification:
the zirconia refractories obtained in example 1, example 2, example 3, and comparative example 1 were prepared as sample 1, sample 2, sample 3, and sample 4, respectively, and the performance of sample 1, sample 2, sample 3, and sample 4 was examined.
1. Volume density, apparent porosity: calculated according to GB/T2997-2015 standard. The method comprises the following specific steps: (1) mass measurement of the sample in air: and (3) respectively placing the samples to be tested 1-4 in a drying oven for drying treatment at 110 ℃ for 24 hours, removing fine particles on the surfaces of the samples 1-4, and testing the mass (m1) of each sample. Then placing the samples 1-4 in a vacuum device, keeping the constant pressure for 5min when the internal pressure is less than 0.08MPa, then injecting impregnation liquid until the samples 1-4 are submerged, and keeping the constant pressure for 30min to fully saturate the samples 1-4; (2) and (3) measuring the apparent mass of a saturated sample: soaking the sample 1-4 for 30min, putting the sample into a container with an overflow nozzle, and weighing the suspended mass (m2) of the sample 1-4 after the indication is stable; (3) and (3) saturated sample mass determination: the samples 1 to 4 were taken out from the immersion liquid, droplets on the surface of the samples 1 to 4 were wiped off with a saturated wet towel, and then the mass of the saturated samples 1 to 4 in the air was measured (m 3). The test data are shown in Table 1.
The calculation formula is as follows:
volume density m1 × (density of immersion liquid at experimental temperature)/m 3-m2
The apparent porosity is (m3-m1)/(m3-m 2). times.100%
2. Normal temperature flexural strength: and (4) determining the limit stress which can be borne when the sample to be tested 1-4 is pressurized on a three-point bending device without being broken under the room temperature according to the GB/T6569-2006 standard. The equipment used in the experiment is a digital display electric bending resistance instrument. The span is 4cm, and the loading speed is 0.5 mm/min. The test data are shown in table 1.
Table 1 results of performance testing
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (7)
1. A preparation process of a high-volume-density zirconia refractory material is characterized by comprising the following steps of:
(1) preparing electric smelting zirconia powder: uniformly mixing the fused monoclinic zirconium and the stabilizer high-purity calcite by using a stirrer to obtain mixed powder; putting the mixed powder into a three-phase electric arc furnace for smelting, refining for 0.5-1h after the mixed powder is completely molten in the three-phase electric arc furnace to obtain a molten mass, carrying out melt blowing on the molten mass to obtain zirconia hollow spheres, collecting the blown zirconia hollow spheres, and grinding to 325 meshes to obtain stable zirconia powder; putting the zirconia powder into a corundum crucible and putting the corundum crucible into a heat treatment furnace, heating the heat treatment furnace to 1100-1200 ℃ at the speed of 8-10 ℃/min, preserving heat for 3-5h, closing the heat treatment furnace, cooling along with the furnace, taking out the powder, wet grinding the powder in a planetary ball mill at the speed of 400-500r/min for 5-6h, sieving by a 325-mesh sieve, and drying to obtain the fused zirconia powder;
(2) preparing yttrium stable zirconia granulation powder: carrying out nodular graphite treatment on yttria-stabilized zirconia powder, deionized water and a dispersing agent in a planetary ball mill at the speed of 300-400r/min to prepare slurry, adding a binder into the slurry, stirring for 4-6h by a stirrer, then carrying out spray granulation by a spray granulator, and sieving by a 325-mesh sieve to obtain yttria-stabilized zirconia granulation powder;
(3) mixing materials: mixing the above electrically-fused zirconia powder, yttrium stabilized zirconia granulated powder, SiC, and nano eta-Al2O3Adding into a high-speed mixing roll, mixing and stirring uniformly, and sieving with a 325-mesh sieve;
(4) pressing into a blank: filling the material in the mold by adopting a volume-controlled filling method, and pressing the material into a green body by a cold isostatic press under the pressure condition of 120-150 Mpa;
(5) sintering and forming: and (3) drying the molded green body for 8-12h at the temperature of 100-120 ℃ in a constant-temperature drying oven, then placing the green body in a lifting furnace, heating to 1500-1600 ℃ at the heating rate of 8-10 ℃/min, preserving heat for 4-6h, then closing the lifting furnace, and cooling the sample along with the furnace to obtain the zirconia refractory material.
2. The process for preparing a high bulk density zirconia refractory according to claim 1, wherein in step (1), the electrofused monoclinic zirconium and the stabilizer high purity calcite are 325 mesh; the melting blowing adopts compressed air blowing and the pressure is 8-10 kg.
3. The process for preparing a high bulk density zirconia refractory according to claim 1, wherein in the step (1), the mass ratio of the electrofused monoclinic zirconia to the stabilizer is 96-97: 3-4.
4. The process according to claim 1, wherein in the step (2), the yttria-stabilized zirconia powder comprises a zirconia powder having a mass ratio of 94.74:5.23: 0.035: 0.0022 parts of zirconia, yttria, ferric oxide, and titania; the dispersing agent is one or a mixture of more of ammonium polyacrylate, sodium polyacrylate, ammonium citrate, DS005, CE-64 and glycerol; the binder is one or a mixture of polyvinyl alcohol, polyethylene glycol, sodium carboxymethyl cellulose, B-1000 and B-1022.
5. The process for preparing a high bulk density zirconia refractory as claimed in claim 1, wherein in the step (2), the mass ratio of the yttria-stabilized zirconia powder, the deionized water, the dispersant and the binder is 100-110:120-130:0.2-0.3: 1.5-2.5.
6. The process for preparing a high bulk density zirconia refractory according to claim 1, wherein in the step (3), the electrofused zirconia powder, the yttrium-stabilized zirconia granulated powder, SiC, or nano η -Al is used2O3The mass ratio of (A) to (B) is 20-30: 50-60: 5-10:2-5.
7. The process for producing a high bulk density zirconia refractory according to claim 1, wherein 1500# SiC is used as the SiC, and the grain size is 10 μm; the purity of the nano eta-Al 2O3 is 99.5%, and the particle size is 20 nm.
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| CN115124073A (en) * | 2022-07-07 | 2022-09-30 | 郑州振中电熔新材料有限公司 | Method for preparing fused yttrium stabilized zirconium by using waste zirconia material |
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