CN116332664B - Large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate and preparation method thereof - Google Patents
Large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate and preparation method thereof Download PDFInfo
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- CN116332664B CN116332664B CN202310209751.3A CN202310209751A CN116332664B CN 116332664 B CN116332664 B CN 116332664B CN 202310209751 A CN202310209751 A CN 202310209751A CN 116332664 B CN116332664 B CN 116332664B
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- 239000000835 fiber Substances 0.000 title claims abstract description 255
- 239000000919 ceramic Substances 0.000 title claims abstract description 99
- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 229910018072 Al 2 O 3 Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000011159 matrix material Substances 0.000 claims abstract description 115
- 239000000843 powder Substances 0.000 claims abstract description 64
- 238000000498 ball milling Methods 0.000 claims abstract description 50
- 239000006185 dispersion Substances 0.000 claims abstract description 50
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 22
- 239000010703 silicon Substances 0.000 claims abstract description 22
- 238000009826 distribution Methods 0.000 claims abstract description 6
- 238000007580 dry-mixing Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 56
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 53
- 230000008569 process Effects 0.000 claims description 42
- 239000002994 raw material Substances 0.000 claims description 32
- 239000000395 magnesium oxide Substances 0.000 claims description 30
- 239000000126 substance Substances 0.000 claims description 30
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000011734 sodium Substances 0.000 claims description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 19
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 18
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 14
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 14
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 14
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 13
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 13
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 claims description 12
- 229910052590 monazite Inorganic materials 0.000 claims description 12
- 239000010427 ball clay Substances 0.000 claims description 11
- 239000000454 talc Substances 0.000 claims description 11
- 229910052623 talc Inorganic materials 0.000 claims description 11
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000440 bentonite Substances 0.000 claims description 9
- 229910000278 bentonite Inorganic materials 0.000 claims description 9
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 9
- 239000004575 stone Substances 0.000 claims description 9
- 238000004537 pulping Methods 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 238000003892 spreading Methods 0.000 claims description 6
- 230000007480 spreading Effects 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 54
- 239000000243 solution Substances 0.000 description 37
- 238000012360 testing method Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 21
- 238000010304 firing Methods 0.000 description 20
- 230000003014 reinforcing effect Effects 0.000 description 17
- 239000012071 phase Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- 235000012222 talc Nutrition 0.000 description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 description 9
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 239000012798 spherical particle Substances 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006355 external stress Effects 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 230000007847 structural defect Effects 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 238000009770 conventional sintering Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 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 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052656 albite Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910001597 celsian Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009036 growth inhibition Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000002648 laminated material Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 238000000643 oven drying 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
- 230000005501 phase interface Effects 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000010947 wet-dispersion method Methods 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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention relates to a large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate and its preparation method are provided. The preparation method comprises the following steps: zrO (ZrO) 2 Immersing chopped fibers into a pre-dispersion solution to obtain pre-dispersion ZrO with silicon-based interface layers wrapped by outer walls 2 Chopped fibers; pre-dispersing ZrO 2 Performing ball milling dry mixing after stacking distribution of chopped fibers and matrix powder to obtain a fiber/matrix mixture; pressing the fiber/matrix mixture into a ceramic blank, and sintering the ceramic blank to obtain the large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate.
Description
Technical Field
The invention belongs to the technical field of composite thin ceramic plates, and in particular relates to a large-size ZrO (high-performance ZrO) 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate and its preparation method are provided.
Background
At present, the defects of the traditional thin ceramic plate industry are gradually displayed: (1) A large amount of ore raw materials are mined, so that various environmental problems such as water and soil loss and the like occur; (2) The material system has low strength, is fragile in transportation and has extremely high cost; and (3) the production energy consumption is higher, and the emission of harmful tail gas exceeds the standard. In contrast, the thickness of the composite thin ceramic plate is only 3-5mm, which can save 30-50% of raw material consumption, reduce 20-40% of production emission and 20-30% of production energy consumption, and gradually becomes an important way for the future development of the traditional thin ceramic plate industry. However, with the reduction of the thickness of the traditional large-size thin ceramic plate, the mechanical strength of the ceramic large-size ceramic plate green body is suddenly reduced, so that the ceramic large-size ceramic plate green body is difficult to form and the daily home decoration and safety protection requirements are difficult to meet. Therefore, based on the characteristics of the traditional thin ceramic plate system, the development of systematic toughening research is a key for realizing the thinning of the traditional large-size thin ceramic plate.
Currently, the toughening research for traditional thin ceramic plates is largely divided into two ideas: (1) optimizing a ceramic matrix formulation system; (2) Introducing various reinforcing phases and constructing a multi-dimensional reinforcing system. The optimized ceramic matrix formula system mainly controls specific chemical reaction in the matrix by adjusting the formula composition in the matrix, so that the ceramic matrix generates internal reinforcing phases such as mullite, sepiolite and the like, and the comprehensive mechanical property of the traditional thin ceramic plate is further improved. However, the toughening effect of the mode has a large technical bottleneck because the defects of glass phase and mechanical vacancy in the traditional thin ceramic plate are more. The multi-dimensional reinforcing system is constructed mainly by introducing fiber bodies and dispersive particles into a traditional thin ceramic plate to serve as reinforcing phases, and supporting external stress by cooperating with the matrix phases, so that the comprehensive mechanical properties of the material are improved. However, the introduced reinforcing phase is easy to generate uncontrollable interface reaction with matrix phase with complex components at high temperature, so that the mechanical structure of the reinforcing body is destroyed, the material is embrittled, and the mechanical property of the material is reduced. In addition, reinforcing phases such as fibers and the like are difficult to uniformly disperse in a matrix by means of a traditional ball milling process, and agglomerated fibers can cause mechanical defects in the composite ceramic plate, so that the use safety and mechanical properties of the material are reduced. In conclusion, the method has great development potential and is expected to replace the current production process. However, the preparation technology of the raw materials is limited in China, the related researches are less, and a large technical gap exists between the raw materials and developed countries, so that the preparation technology is optimized.
Disclosure of Invention
Based on the research background, the invention introduces one-dimensional fiber ZrO into an optimized thin ceramic plate formula system 2 Fiber, two-dimensional flake Al 2 O 3 As a reinforcing phase, a large-sized ZrO was developed 2 Fiber/flake Al 2 O 3 The composite thin ceramic plate and the preparation method thereof realize the uniform dispersion of the multidimensional reinforcing phase in the matrix, effectively improve the comprehensive mechanical property of the thin ceramic plate, are hopeful to break the foreign technical barriers, provide important technical basis for the thinning of the traditional thin ceramic plate, have great development potential, and can be applied to the fields of building ceramics, military armor materials and the like. In addition, the preparation process is simple, the cost of the selected raw materials is low, and one-dimensional fiber bodies and two-dimensional flaky Al can be prepared 2 O 3 The ceramic plate is tightly combined with a ceramic matrix, and the prepared large-size thin ceramic plate has excellent mechanical properties and wide potential commercial market.
In a first aspect, the present invention provides a large-sized ZrO 2 Fiber/flake Al 2 O 3 The preparation method of the composite thin ceramic plate comprises the following steps:
ZrO (ZrO) 2 Immersing chopped fibers into a fiber pre-dispersion solution containing sodium polyacrylate, aminopropyl triethoxysilane and sodium tripolyphosphate, pre-dispersing under heating and stirring, collecting fibers, and drying to obtain pre-dispersion ZrO with silicon-based interface layer wrapped by outer wall 2 Chopped fibers;
pre-dispersed ZrO with silicon-based interface layer wrapped on outer wall 2 After lamination type distribution of chopped fibers and matrix powder, ball milling dry mixing is carried outObtaining a fiber/matrix mixture; the mass ratio of the chemical components of the matrix powder is Al 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：La 2 O 3 ：Ce 2 O 3 ：Y 2 O 3 ：Na 3 PO 4 ＝(35-40)：(40-45)：(10-15)：(5-10)：(1-5)：(1-5)：(0.5-1)：(0.1-0.5)：(0.1-0.5)：(1.5-3)；
Pressing the fiber/matrix mixture into a ceramic blank, and sintering the ceramic blank to obtain the large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate.
Preferably, in the fiber pre-dispersion solution, sodium polyacrylate: aminopropyl triethoxysilane: sodium tripolyphosphate: the mass ratio of water is (20-30): (10-20): (10-20): (50-60); preferably, the pH of the fiber pre-dispersion solution is between 8.0 and 8.5.
Preferably, the ZrO 2 The ratio of chopped fibers to fiber pre-dispersion solution was 1g:25-100g; preferably, the ZrO 2 The chopped fiber has a length of 150-180 μm, a diameter of 3-5 μm, and an aspect ratio of 30-60. In some technical schemes, the pre-dispersion time is 2-3h.
Preferably, the outer wall is wrapped with pre-dispersed ZrO of the silicon-based interface layer 2 The chopped fiber is dried by vacuum freeze drying; preferably, the drying temperature is-80 to-120 ℃, the drying time is 6-8 hours, and the vacuum degree is 20-40Pa.
Preferably, the matrix raw materials are weighed according to the mass ratio of the chemical components of the matrix powder, and the matrix powder is obtained through crushing, pulping and spray granulation after being uniformly mixed; the mass ratio of each component of the matrix raw material is flaky alumina: magnesium oxide: black talc: monazite). Ball clay: bentonite: potassium feldspar: sodium tripolyphosphate = 30-35:8-13:9-14:21-26:14-19:7-12:12-17:1-3; preferably, the particle size of the flaky alumina is 1-2 mu m, the thickness is 50-100nm, the mesoporous pore diameter is 1-3nm, and the mesoporous rate is 10-20%.
Preferably, the pre-dispersed ZrO of the silicon-based interface layer wrapped by the outer wall in the ball milling process 2 Chopped fiber: matrix powderAnd (3) material: ball stone mass ratio= (1-5): (50-60): (80-100), the ball milling rotating speed is 50-80r/min, and the ball milling time is 2-5min.
Preferably, the specific operation of the laminated cloth is as follows: firstly, weighing matrix powder, spreading the matrix powder at the bottom of a ball milling tank, and then weighing pre-dispersed ZrO with the outer wall wrapped by a silicon-based interface layer 2 The chopped fibers are paved on the surface of the matrix powder, and the above procedures are alternately repeated until the chopped fibers and the matrix powder are all sent to a ball milling tank.
Preferably, the highest sintering temperature of sintering is 1250-1300 ℃, the sintering period is 20-30min, and the heat preservation time of the highest sintering temperature is 10-15min.
In a second aspect, the present invention provides a large-sized ZrO obtained by the above production method 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate. The bending strength of the composite thin ceramic plate is 160-170MPa, and the fracture toughness is 3.00-3.10MPa m 1/2 The water absorption rate is 0.15-0.25%, and the density is 2.90-3.00g/cm 3 . In some embodiments, the large-sized ZrO 2 Fiber/flake Al 2 O 3 The specification of the composite thin ceramic plate is 2350-2450mm long, 1150-1250mm wide and 2-5mm high.
In a third aspect, the present invention provides a large-sized ZrO 2 Fiber/flake Al 2 O 3 The preparation method of the composite thin ceramic plate comprises the following steps:
ZrO (ZrO) 2 Immersing chopped fibers into a fiber pre-dispersion solution containing sodium polyacrylate, aminopropyl triethoxysilane and sodium tripolyphosphate, pre-dispersing under heating and stirring, collecting fibers, and drying to obtain pre-dispersion ZrO with silicon-based interface layer wrapped by outer wall 2 Chopped fibers;
pre-dispersed ZrO with silicon-based interface layer wrapped on outer wall 2 Performing ball milling dry mixing after stacking distribution of chopped fibers and matrix powder to obtain a fiber/matrix mixture; the mass ratio of the raw materials of the matrix powder is flaky alumina: magnesium oxide: black talc: monazite). Ball clay: bentonite: potassium feldspar: sodium tripolyphosphate = 30-35:8-13:9-14:21-26:14-19:7-12:12-17：1-3；
Pressing the fiber/matrix mixture into a ceramic blank, and sintering the ceramic blank to obtain the large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate.
Advantageous effects
Currently, the traditional large-specification thin ceramic plate has the technical problems of poor mechanical strength and poor green body formability. The invention innovatively provides a large-size ZrO 2 Fiber/flake Al 2 O 3 The preparation method of the composite thin ceramic plate constructs a multi-dimensional composite reinforcing system by optimizing the formula of the traditional ceramic matrix. The toughness fiber body and the high-strength dispersive particles are introduced into a 'brittle' system of the traditional thin ceramic plate to serve as a reinforcing phase, so that the concentration of crack tip stress is restrained, an internal microcrack expansion path is deflected, and the composite thin ceramic plate with excellent mechanical properties is prepared by cooperatively bearing external stress with a matrix, so that the composite thin ceramic plate is expected to break a foreign technical barrier, and an important technical basis is provided for thinning of the traditional thin ceramic plate.
Drawings
FIG. 1 is a scanning electron microscope test chart of the zirconia chopped fiber raw material of example 1;
FIG. 2 is a scanning electron microscope test chart of the wet-dispersed (pre-dispersed) zirconia fiber of example 1;
FIG. 3 is a scanning electron microscope test chart of the zirconia fiber/matrix mixture D of example 1;
FIG. 4 is an XRD pattern of the thin fiber composite ceramic plate of example 2;
FIG. 5 is a scanning electron microscope test chart of a cross section of a fiber composite thin ceramic plate in example 3;
FIG. 6 is a scanning electron microscope test chart of the zirconia fiber interface in example 3;
FIG. 7 is a scanning electron microscope test chart of the wet-dispersed zirconia fiber of comparative example 1;
FIG. 8 is a scanning electron microscope test chart of the zirconia fiber/matrix mixture D of comparative example 2;
FIG. 9 is a scanning electron microscope test chart of the zirconia fiber/matrix mixture D of comparative example 3;
FIG. 10 is a scanning electron microscope test chart of a cross section of a fiber composite thin ceramic plate in comparative example 5;
FIG. 11 is a scanning electron microscope test chart of the zirconia fiber interface in comparative example 5.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
The large-sized ZrO of the present invention is exemplified as follows 2 Fiber/flake Al 2 O 3 A preparation method of a composite thin ceramic plate.
ZrO (ZrO) 2 Immersing chopped fibers in a fiber pre-dispersion solution containing sodium polyacrylate, aminopropyl triethoxysilane and sodium tripolyphosphate, pre-dispersing under heating and stirring, collecting fibers, and drying to obtain pre-dispersed ZrO with silicon-based interface layer wrapped by outer wall 2 And (3) chopped fibers.
A fiber pre-dispersion solution was prepared. Sodium polyacrylate according to the mass ratio: aminopropyl triethoxysilane: sodium tripolyphosphate: water= (20-30): (10-20): (10-20): (50-60) preparing a mixed solution, and regulating the pH of the solution to 8.0-8.5 by using ammonia water with the concentration of 2-3mol/L to obtain a fiber pre-dispersion solution A. By preparing and selecting a mixed aqueous solution of sodium polyacrylate, aminopropyl triethoxysilane and sodium tripolyphosphate with specific mass ratio and pH=8.0-8.5 as ZrO 2 The liquid phase pre-mixing dispersion medium of the fiber develops a one-dimensional fiber wet chemical dispersion system. The components of the fiber pre-dispersion solution A are controlled within a specific mass proportion range, so that the solution is ensured to be in a stable state, adverse effects such as normal-temperature crystallization and solute suspension are prevented, the functions of the components can be fully exerted, and the maximization of the effect is realized.
Sodium tripolyphosphate is a water-soluble linear polyphosphate, and can be cooperated with sodium polyacrylate to dissociate active groups such as sodium ions and phosphoric acid by virtue of hydrolysis, and infiltrate ZrO 2 The outer surface of the fiber is provided with a negative electric layer so as to control the free water content in the water layer of the fiber interface and further adjust the interface negative ionsSub-potential, zrO beneficial to agglomerate and cross-linked structure 2 The fibers spontaneously disperse due to electrostatic repulsion.
At the same time, in a slightly alkaline environment with pH=8.0-8.5, the alkaline group can accelerate the dissolution of aminopropyl triethoxysilane, so that the aminopropyl triethoxysilane is fully wrapped in ZrO 2 An outer wall of the fiber. Meanwhile, the perfect combination of various active groups such as amino groups and the like and the structural attachment points of the outer wall can be promoted, the quality and the efficiency of the outer package of the fiber are improved, and the effect of guaranteeing the mechanical property of the fiber is achieved. The fiber outer wrapping coating is constructed, so that the thermodynamic damage of the fiber at high temperature by 40-60% can be reduced theoretically, and the comprehensive mechanical property of the composite sheet is ensured.
Taking ZrO 2 The chopped fibers are soaked into a fiber pre-dispersion solution A, and the ZrO 2 The ratio of chopped fibers to fiber pre-dispersion solution was 1g:25-100g; transferring to magnetic stirrer, pre-dispersing at 40-60deg.C at 400-500r/min for 2-3 hr, collecting fiber, and vacuum freeze drying to obtain pre-dispersed chopped fiber B (also called pre-dispersed ZrO with silicon-based interface layer wrapped by outer wall) 2 Chopped fibers). Wherein ZrO 2 The chopped fiber has a fiber length of 150-180 μm, a fiber diameter of 3-5 μm, and a fiber aspect ratio of 30-60. The freeze-drying temperature is-80 to-120 ℃, the drying time is 6-8h, and the vacuum degree is 20-40Pa.
The conventional drying process can cause secondary agglomeration, reduce chemical dispersion effect and prevent the fiber and the powder from being uniformly mixed in the subsequent steps. The invention develops a fiber dispersibility guarantee process, introduces a vacuum freeze drying process at first, and avoids ZrO 2 Secondary aggregation of the fiber possibly occurs in the drying process, and the silicon-based interface layer on the outer surface of the fiber is protected. The process can quickly freeze and remove free water on the surface of the fiber at the temperature of between 80 ℃ below zero and 120 ℃ below zero, so that the secondary aggregation of the fiber caused by strong hydrogen bonding action among water molecules is avoided, and the original chemical dispersion effect is destroyed. In addition, structural defects such as microcracks and layering occur in the silicon-based interface layer in a long-time heat-insulating environment. The invention adopts the vacuum freeze drying process, can effectively avoid the internal structural defect caused by temperature difference, and protects the silicon-based outside the fiberAnd the interface layer ensures the high-temperature protection effect.
Pre-dispersed ZrO with silicon-based interface layer wrapped on outer wall 2 And (3) carrying out ball milling dry mixing after stacking distribution of the chopped fibers and the matrix powder to obtain a fiber/matrix mixture.
Preparing matrix powder. Raw materials such as flaky alumina, magnesia, black talcum, monazite, ball clay, bentonite, potassium feldspar, sodium tripolyphosphate and the like are prepared according to Al 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：La 2 O 3 ：Ce 2 O 3 ：Y 2 O 3 ：Na 3 PO 4 = (35-40): (40-45): (10-15): (5-10): (1-5): (1-5): (0.5-1): (0.1-0.5): (0.1-0.5): and (1.5-3) weighing and uniformly mixing the specific chemical components according to the mass ratio, and then crushing, pulping, spray granulating and other working procedures to obtain the matrix powder C with the water content of 10-15%. In some technical schemes, the mass ratio of each component of the matrix raw material is flake aluminum oxide: magnesium oxide: black talc: monazite). Ball clay: bentonite: potassium feldspar: sodium tripolyphosphate = 30-35:8-13:9-14:21-26:14-19:7-12:12-17:1-3. In this technical scheme, al 2 O 3 、SiO 2 、MgO、CaO、Na 2 O、K 2 O、La 2 O 3 、Ce 2 O 3 、Y 2 O 3 Refers to the mass ratio of the corresponding chemical components of the other raw materials except sodium tripolyphosphate. The matrix powder C is spherical particles, and the particle size is preferably 2-5 mu m. Wherein the particle diameter of the flaky alumina is 1-2 mu m, the thickness is 50-100nm, the mesoporous aperture is 1-3nm, and the mesoporous rate is 10-20%. The alumina with lower diameter-thickness ratio has poor toughening effect, and the alumina with higher diameter-thickness ratio has high cost. The process adopts an optimized dry ball milling process, and the powder with specific water content is obtained through a high-efficiency spray granulation process, so that the matrix powder C with specific mass fraction can be obtained in the subsequent process steps conveniently, and the matrix powder C directly participates in a forming process, and the process steps are simple. In some embodiments, the chemical composition of the black talc may include: in mass percent, al 2 O 3 ：15-20％，SiO 2 ：50-55％，MgO：4-8％，CaO：6-11％，Na 2 O：2-7％，K 2 O:3-8%; the chemical composition of the monazite comprises: in mass percent, al 2 O 3 ：13-18％，SiO 2 ：46-51％，MgO：3-7％，CaO：4-9％，Na 2 O：2-6％，K 2 O：1-5％，La 2 O 3 ：3-5％，Ce 2 O 3 ：1-3％，Y 2 O 3 :1-3%; the chemical composition of the ball clay comprises: in mass percent, al 2 O 3 ：12-17％，SiO 2 ：47-52％，MgO：5-10％，CaO：3-8％，Na 2 O：5-10％，K 2 O：1-5％。
The 'alumina-magnesia-rare earth' system is a high strength blank formulation system, compared with the traditional thin ceramic plate blank formulation, the formulation system disclosed by the invention creatively introduces flaky Al 2 O 3 Low cost raw materials such as magnesia, monazite, etc. Wherein rare earth elements can be introduced into the monazite. On one hand, the magnesium oxide and rare earth elements can be absorbed in the molten alumina interface layer and penetrate into alumina crystal lattice to form solid solution, so that the sintering temperature of the system is reduced. Rare earth elements can be distributed at alumina grain boundary to prevent flaky Al 2 O 3 Irregular growth and creep occur in the subsequent solid phase reaction process, so that the reinforcing effect is reduced; on the other hand, rare earth elements are introduced, which can cooperate with K in solid phase reaction 2 O、Na 2 O and other low-melting-point substances promote the matrix to form molten glass phase at 650-750 ℃ in advance, thereby effectively promoting the internal liquid phase mass transfer rate, greatly reducing the densification temperature of the system and saving the production cost.
Chopped fiber B according to the following mass ratio: matrix powder C: ball stone (grinding ball) = (1-5): (50-60): (80-100) weighing, mixing and moving to a ball mill, setting the ball milling rotation speed to be 50-80r/min and the ball milling time to be 2-5min, then sieving the product through a 60-mesh screen, collecting the screen blanking and drying to obtain a fiber/matrix mixture D with the water content of 5-10 wt%. The control of the mass proportion of the grinding raw materials not only can ensure higher mixing efficiency of the three materials, but also can grind the matrix powder to smaller granularity, thereby improving the toughness of the fiberEffects. The mixing is carried out in a ball milling tank, and the specific mode is as follows: firstly weighing 10-20% of the total mass of the matrix powder C, spreading the matrix powder C at the bottom of a ball milling tank, then weighing chopped fibers B with the same mass fraction, spreading the chopped fibers B on the surface of the matrix powder C, alternately repeating the above processes until the chopped fibers B and the matrix powder C are all sent to the tank, and finally uniformly spreading and arranging the ball stones at the uppermost layer. Compared with the traditional ball milling mixing process, the method has the advantages that the fiber reinforcement and the powder are premixed through the laminated cloth, the ball milling efficiency is improved, and ZrO caused by long-time ball milling can be avoided 2 The fibers undergo structural abrasion, damaging their mechanical properties.
The traditional ball milling process is wet ball milling, the obtained slurry can be sieved, dried and sieved to obtain ceramic powder, the process is complex, and the fibers and the matrix which are originally uniformly dispersed are easily rearranged and agglomerated, so that the method is not suitable for the invention. This is because conventional dispersion uses a wet mixing process to facilitate stripping of the silicon-based interface layer under the impact and abrasion of the liquid medium. The invention adopts a dry mixing process, can effectively protect the wet chemical dispersion process from ZrO 2 The silicon-based interface layer wrapped on the surface of the fiber further ensures the protection effect on the fiber at high temperature. In addition, through setting up reasonable ball-milling compounding time, both can avoid leading to dispersion inhomogeneous because of the short time ball-milling compounding, can avoid leading to the fiber to take place the grain dissociation because of long-time ball-milling compounding again.
Pressing the fiber/matrix mixture D into a ceramic blank, and sintering the ceramic blank to obtain the large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate.
Forming the fiber/matrix mixture D into a composite thin ceramic plate blank by means of a ten-thousand-ton press under the forming pressure of 80-120MPa, and then transferring the composite thin ceramic plate blank into a roller kiln for sintering to obtain the large-size ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate. Wherein, the length, width and height specification parameters of the composite ceramic sheet blank can be 2350-2450mm, 1150-1250mm and 2-5mm. The highest firing temperature of the roller kiln is 1250-1300 ℃, the firing period is 20-30min, and the time for staying at the highest firing temperature is 10-15min。
In solid phase sintering, heat is an important driving force for densification of ceramic materials, namely, a sintering system can influence the strength and density of a traditional thin ceramic plate blank. The invention breaks through the limitation of the conventional sintering technology by reasonably adjusting the formula composition and optimizing the sintering process, and develops a rapid sintering system based on morphology regulation. Conventional sintering process has long period and flaky Al 2 O 3 The invention adopts a sintering system of 'high temperature and quick firing', and cooperates with the growth inhibition effect of magnesium oxide and rare earth elements to protect flaky Al 2 O 3 The specific morphology of the steel is convenient for the steel to exert the strengthening and toughening mechanism of enhancing the diffusion of particles. In addition, the silicon-based interface layer is introduced as a fiber protection layer to prevent ZrO at high temperature 2 The fibers impair mechanical properties due to thermodynamic creep. The traditional sintering system period is 40-50min, and the densification of the sheet blank can be realized only in 20-30min, so that the production period is shortened by 40-50%, the production cost can be saved by 10-20%, and the method has a high popularization value.
The invention is realized by introducing dispersed one-dimensional ZrO 2 Fiber, adjusting raw material proportion composition, constructing one-dimensional fiber ZrO 2 Platelet-shaped Al 2 O 3 Synergistic enhancement system. In contrast, conventional processes have difficulty in incorporating ZrO 2 The fibers are distributed in the matrix material in a single form, and the agglomerated ZrO 2 The contact specific surface area of the fiber and the matrix is small, so that structural defects such as air holes and the like appear at the periphery, and the mechanical strength of the fiber is greatly reduced. The invention innovatively selects flaky Al with the grain diameter of 1-2 mu m and the thickness of 50-100nm 2 O 3 And one-dimensional ZrO dispersed in a chemical medium 2 The fiber is used as a reinforcing body, and the fiber and the reinforcing body are uniformly mixed by means of a ball milling mixing process. Flake Al 2 O 3 、ZrO 2 The fiber can effectively prevent crack expansion in the matrix, and exert reinforcing mechanisms such as particle diffusion enhancement, fiber breakage-extraction and the like. Namely, when the material bears external load, two reinforcing bodies which are uniformly distributed can effectively deflect the expansion path of cracks, and cooperatively absorb more external impact energy, so that the fracture mode of the material is changed from original brittlenessThe fracture is converted into ductile fracture, and the maximum lifting amplitude of the bending strength and fracture toughness of the material can reach 50% and 60% respectively.
The molecular weight of the sodium polyacrylate used in the examples is 3000 to 5000.
Example 1
Large-scale ZrO 2 Fiber/flake Al 2 O 3 The preparation method of the composite thin ceramic plate comprises the following steps:
1) Sodium polyacrylate according to the mass ratio: aminopropyl triethoxysilane: sodium tripolyphosphate: water = 20:10:10:60 preparing a mixed solution, and regulating the pH value of the mixed solution to 8.5 by ammonia water to obtain a fiber pre-dispersion solution A. Wherein the concentration of the ammonia water solution is 3mol/L.
2) Taking ZrO 2 Immersing chopped fibers into a fiber pre-dispersion solution A, and soaking the chopped fibers into the fiber pre-dispersion solution A to obtain ZrO 2 The mass ratio of the chopped fiber to the fiber pre-dispersion solution A is 1:25, transferring to a magnetic stirrer, pre-dispersing for 3 hours at the temperature of 60 ℃ at the rotating speed of 500r/min, collecting the fibers, and vacuum freeze-drying to obtain pre-dispersed chopped fibers B. Wherein ZrO 2 The chopped fibers had a fiber length of 180 μm, a fiber diameter of 3 μm and a fiber aspect ratio of 60. The freeze-drying temperature is-120 ℃, the drying time is 8 hours, and the vacuum degree is 40Pa.
3) Weighing 35g of flaky alumina, 8g of magnesia, 14g of black talcum, 24g of monazite, 14g of ball clay, 8g of bentonite, 16g of potassium feldspar and 1g of sodium tripolyphosphate, wherein the chemical components of the raw materials are compared with Al by mass 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：La 2 O 3 ：Ce 2 O 3 ：Y 2 O 3 ：Na 3 PO 4 =40: 40:10:5:1:1:0.5:0.5:0.5:1.5. wherein Al is 2 O 3 、SiO 2 、MgO、CaO、Na 2 O、K 2 O、La 2 O 3 、Ce 2 O 3 、Y 2 O 3 Refers to the mass ratio of the corresponding chemical components of the other raw materials except sodium tripolyphosphate. Uniformly mixing the above raw materials, and performing crushing, pulping and spray granulation to obtain a water content of 15% of matrix powder C. The particle size of the flaky alumina is 2 mu m, the thickness is 100nm, the mesoporous pore diameter is 3nm, and the mesoporous rate is 10%. The matrix powder C is spherical particles with the particle size of 5 mu m.
4) Chopped fiber B according to the following mass ratio: matrix powder C: ball stone = 5:60:100, weighing, mixing and moving to a ball mill, setting the ball milling rotation speed to be 80r/min and the ball milling time to be 5min, then sieving the product through a 60-mesh screen, collecting the screen blanking, and drying to obtain a fiber/matrix mixture D with the water content of 10 wt%. Wherein, the mixing is carried out in a ball milling tank, firstly, matrix powder C with the mass fraction of 20% is weighed and paved at the bottom, then chopped fiber B with the same mass fraction is weighed and paved on the surface of the matrix powder C, and the above processes are alternately repeated until the chopped fiber B and the matrix powder C are all sent into the tank.
5) Forming the fiber/matrix mixture D into a composite thin ceramic plate blank by means of a ten-thousand-ton press under the forming pressure of 120MPa, and then transferring the composite thin ceramic plate blank into a roller kiln for sintering to obtain the large-size ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate. Wherein, the length, width and height specification parameters of the composite thin ceramic plate blank are 2450mm, 1250mm and 2mm. The highest firing temperature of the roller kiln is 1300 ℃, the firing period is 20min, and the time for staying at the highest firing temperature is 10min.
Example 2
Large-scale ZrO 2 Fiber/flake Al 2 O 3 The preparation method of the composite thin ceramic plate comprises the following steps:
1) Sodium polyacrylate according to the mass ratio: aminopropyl triethoxysilane: sodium tripolyphosphate: water = 20:10:20:50 preparing a mixed solution, and regulating the pH value of the solution to 8.0 by using an ammonia water solution to obtain a fiber pre-dispersion solution A. Wherein the concentration of the ammonia water solution is 2mol/L.
2) Taking ZrO 2 Immersing chopped fibers into a fiber pre-dispersion solution A, and soaking the chopped fibers into the fiber pre-dispersion solution A to obtain ZrO 2 The mass ratio of the chopped fiber to the fiber pre-dispersion solution A is 1:100, moving to a magnetic stirrer, pre-dispersing for 2h at the rotation speed of 400r/min and the temperature of 40 ℃, collecting the fibers, and performing vacuum freeze drying to obtain pre-dispersed chopped fibersB. Wherein ZrO 2 The chopped fibers had a fiber length of 150 μm, a fiber diameter of 5 μm and a fiber aspect ratio of 30. The freeze-drying temperature is-80 ℃, the drying time is 6 hours, and the vacuum degree is 20Pa.
3) Weighing 30g of flaky alumina, 8g of magnesia, 11g of black talcum, 26g of monazite, 15g of ball clay, 10g of bentonite, 12g of potassium feldspar and 1.5g of sodium tripolyphosphate, wherein the mass ratio of the chemical components of the raw materials is Al 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：La 2 O 3 ：Ce 2 O 3 ：Y 2 O 3 ：Na 3 PO 4 =35: 45:10:5:1:1:1:0.2:0.2:1.6. wherein Al is 2 O 3 、SiO 2 、MgO、CaO、Na 2 O、K 2 O、La 2 O 3 、Ce 2 O 3 、Y 2 O 3 Refers to the mass ratio of the corresponding chemical components of the other raw materials except sodium tripolyphosphate. The raw materials are evenly mixed, and the base powder C with the water content of 10% is obtained through crushing, pulping and spray granulation processes. The particle size of the flaky alumina is 1 mu m, the thickness is 50nm, the mesoporous pore diameter is 1nm, and the mesoporous rate is 20%. The matrix powder C is spherical particles with the particle size of 2 mu m.
4) Chopped fiber B according to the following mass ratio: matrix powder C: ball stone = 1:50:80 weighing, mixing and moving to a ball mill, setting the ball milling rotation speed to be 50r/min and the ball milling time to be 2min, then sieving the product through a 60-mesh screen, collecting the screen blanking, and drying to obtain a fiber/matrix mixture D with the water content of 5 wt%. Wherein, the mixing is carried out in a ball milling tank, firstly, matrix powder C with the mass fraction of 10% is weighed and paved at the bottom, then chopped fiber B with the same mass fraction is weighed and paved on the surface of the matrix powder C, and the above processes are alternately repeated until the chopped fiber B and the matrix powder C are all sent into the tank.
5) Forming the fiber/matrix mixture D into a composite thin ceramic plate blank by means of a ten-thousand-ton press under the forming pressure of 80MPa, and then transferring the composite thin ceramic plate blank into a roller kiln for sintering to obtain the large-size ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate. Which is a kind ofThe length, width and height specification parameters of the composite thin ceramic plate blank are 2350mm, 1150mm and 5mm. The highest firing temperature of the roller kiln is 1250 ℃, the firing period is 30min, and the time for staying at the highest firing temperature is 15min.
Example 3
Large-scale ZrO 2 Fiber/flake Al 2 O 3 The preparation method of the composite thin ceramic plate comprises the following steps:
1) Sodium polyacrylate according to the mass ratio: aminopropyl triethoxysilane: sodium tripolyphosphate: water = 24:12:11:53 preparing a mixed solution, and adjusting the pH of the solution to 8.2 by using an ammonia water solution to obtain a fiber pre-dispersion solution A. Wherein the concentration of the ammonia water solution is 2.5mol/L.
2) Taking ZrO 2 Immersing chopped fibers into a fiber pre-dispersion solution A, and soaking the chopped fibers into the fiber pre-dispersion solution A to obtain ZrO 2 The mass ratio of the chopped fiber to the fiber pre-dispersion solution A is 1:50, transferring to a magnetic stirrer, pre-dispersing for 2.4 hours at the rotating speed of 450r/min and the temperature of 50 ℃, collecting the fibers, and performing vacuum freeze drying to obtain the pre-dispersed chopped fibers B. Wherein ZrO 2 The chopped fibers had a fiber length of 160 μm, a fiber diameter of 4 μm and a fiber aspect ratio of 40. The freeze-drying temperature was-100deg.C, the drying time was 7 hours, and the vacuum degree was 30Pa.
3) Weighing 32g of flaky alumina, 9g of magnesia, 11g of black talcum, 24g of monazite, 19g of ball clay, 12g of bentonite, 15g of potassium feldspar and 3g of sodium tripolyphosphate, wherein the chemical components of the raw materials are compared with Al by mass 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：La 2 O 3 ：Ce 2 O 3 ：Y 2 O 3 ：Na 3 PO 4 =36: 41:11:6:1.2:1.3:0.6:0.2:0.1:2.6. wherein Al is 2 O 3 、SiO 2 、MgO、CaO、Na 2 O、K 2 O、La 2 O 3 、Ce 2 O 3 、Y 2 O 3 Refers to the mass ratio of the corresponding chemical components of the other raw materials except sodium tripolyphosphate. Uniformly mixing the above raw materials, crushing, pulping, and spray granulating to obtain matrix with water content of 12%Powder C. The particle size of the flaky alumina is 1.6 mu m, the thickness is 80nm, the mesoporous aperture is 1.8nm, and the mesoporous rate is 15%. The matrix powder C is spherical particles with the particle size of 3 mu m.
4) Chopped fiber B according to the following mass ratio: matrix powder C: ball stone = 2:58:95 weighing, mixing and moving to a ball mill, setting the ball milling rotation speed to be 60r/min and the ball milling time to be 3min, then sieving the product through a 60-mesh screen, collecting the screen blanking, and drying to obtain a fiber/matrix mixture D with the water content of 8 wt%. Wherein, the mixing is carried out in a ball milling tank, firstly, matrix powder C with the mass fraction of 15% is weighed and paved at the bottom, then chopped fiber B with the same mass fraction is weighed and paved on the surface of the matrix powder C, and the above processes are alternately repeated until the chopped fiber B and the matrix powder C are all sent into the tank.
5) Forming the fiber/matrix mixture D into a composite thin ceramic plate blank by a ten-thousand-ton press under the forming pressure of 100MPa, and then transferring the composite thin ceramic plate blank into a roller kiln for sintering to obtain the large-size ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate. Wherein, the length, width and height specification parameters of the composite thin ceramic plate blank body are 2400mm, 1200mm and 4mm. The highest firing temperature of the roller kiln is 1275 ℃, the firing period is 25min, and the time for staying at the highest firing temperature is 13min.
Comparative example 1
Substantially the same as in example 1, the main difference is that: the vacuum freeze-drying in step 2) is replaced by oven-drying. Wherein the drying temperature is 60 ℃ and the drying time is 6 hours.
Comparative example 2
The preparation method of the composite thin ceramic plate comprises the following steps:
1) 34g of flaky alumina, 12g of magnesia, 13g of black talcum, 23g of monazite, 18g of ball clay, 10g of bentonite, 16g of potassium feldspar and 3g of sodium tripolyphosphate are weighed, and the chemical components of the raw materials are compared with Al by mass 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：La 2 O 3 ：Ce 2 O 3 ：Y 2 O 3 ：Na 3 PO 4 ＝40：40：14：8:5:1:1:0.4:0.5:3. wherein Al is 2 O 3 、SiO 2 、MgO、CaO、Na 2 O、K 2 O、La 2 O 3 、Ce 2 O 3 、Y 2 O 3 Refers to the mass ratio of the corresponding chemical components of the other raw materials except sodium tripolyphosphate. The raw materials are evenly mixed, and the base powder A with the water content of 12% is obtained through crushing, pulping and spray granulation processes. The particle size of the flaky alumina is 1.8 mu m, the thickness is 65nm, the mesoporous pore diameter is 2.5nm, and the mesoporous rate is 12%. The matrix powder A is spherical particles with the particle size of 4 mu m.
2) ZrO (ZrO) 2 The chopped fibers were used as the chopped fibers B. ZrO (ZrO) 2 The chopped fibers had a fiber length of 176 μm, a fiber diameter of 4 μm and a fiber aspect ratio of 44. ZrO in the following mass ratio 2 Chopped fiber B: matrix powder a: ball stone = 3:58:87, weighing, mixing and moving to a ball mill, setting the ball milling rotation speed to be 76r/min and the ball milling time to be 4min, then sieving the product through a 60-mesh screen, collecting the screen blanking, and drying to obtain the fiber/matrix mixture C with the water content of 9 wt%. Firstly weighing matrix powder A with the mass fraction of 13% and laying the matrix powder A at the bottom, then weighing chopped fibers B with the same mass fraction and laying the chopped fibers B on the surface of the matrix powder A, and repeating the above processes alternately until the chopped fibers B and the matrix powder A are all sent to the tank.
3) And forming the fiber/matrix mixture C into a composite thin ceramic plate blank by means of a ten-thousand-ton press under the forming pressure of 110MPa, and then transferring the composite thin ceramic plate blank into a roller kiln for sintering to obtain the composite thin ceramic plate. Wherein, the length, width and height specification parameters of the composite thin ceramic plate blank are 2450mm, 1250mm and 3mm. The highest firing temperature of the roller kiln is 1290 ℃, the firing period is 26min, and the time for staying at the highest firing temperature is 14min.
Comparative example 3
Substantially the same as in example 1, the main difference is that: step 4) adopting one-step direct ball milling.
4) Chopped fiber B according to the following mass ratio: matrix powder C: ball stone = 1:50:80 is weighed and directly transferred to a ball mill, the ball milling speed is set to be 50r/min, the ball milling time is set to be 2min, then the product is sieved by a 60-mesh screen, the screen is collected for discharging, and the mixture is dried, so that a fiber/matrix mixture D with the water content of 5wt% is obtained.
Comparative example 4
Substantially the same as in example 1, the main difference is that: the composition of the matrix powder C in step 3) is different.
3) 34g of kaolin, 21g of water-washed ball clay, 15g of albite, 18g of potassium feldspar, 8g of black mud, 11g of talcum, 6g of clay and 1.5g of sodium tripolyphosphate are weighed. The chemical composition of clay includes: in mass percent, al 2 O 3 ：SiO 2 ：MgO：Fe 2 O 3 ：CaO：TiO 2 ：Na 2 O：K 2 O=13%: 58%:2%:6%:5%:3%:5%:8%. The mass ratio of the chemical components of the raw materials to Al 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：Na 3 PO 4 =36: 58:5:8:6:4:4. wherein Al is 2 O 3 、SiO 2 、MgO、CaO、Na 2 O、K 2 O refers to the mass ratio of the corresponding chemical components of the other raw materials except sodium tripolyphosphate. The raw materials are evenly mixed, and the base powder C with the water content of 12% is obtained through crushing, pulping and spray granulation processes. The matrix powder C is spherical particles with the particle size of 4 mu m.
Comparative example 5
Substantially the same as in example 1, the main difference is that: the firing schedule in step 5) is different.
The highest firing temperature of the roller kiln in the step 5) is 1350 ℃, the firing period is 60min, and the time for staying at the highest firing temperature is 35min.
Comparative example 6
Substantially the same as in example 1, the main difference is that: the pH of the pre-dispersion solution of fibers in step 1) is different.
1) Sodium polyacrylate according to the mass ratio: aminopropyl triethoxysilane: sodium tripolyphosphate: water = 25:20:15:50 preparing a mixed solution, and regulating the pH value of the solution to 10.5 by using an ammonia water solution to obtain a fiber pre-dispersion solution A. Wherein the concentration of the ammonia water solution is 3mol/L.
Comparative example 7
Substantially the same as in example 1, the main difference is that: zrO selected in step 2) 2 The chopped fibers vary in size.
In step 2), the ZrO selected 2 The chopped fibers had a fiber length of 860 μm, a fiber diameter of 8.6 μm and a fiber aspect ratio of 100.
The mechanical experiment is carried out on the composite thin ceramic plate on a universal tensile testing machine. The water absorption was measured by a conventional boiling saturation method. The density was tested using a liquid drainage method.
Table 1 lists the mechanical property test data for examples 1-3 and comparative examples 1-7:
table 1 comparison of mechanical properties of examples and comparative examples
FIG. 1 is a scanning electron microscope test chart of the zirconia chopped strand feedstock of example 1. As can be seen from FIG. 1, the zirconia chopped fibers are in an agglomerated state as a whole, and the fibers are crosslinked with each other, so that the overall dispersibility is poor.
FIG. 2 is a scanning electron microscope test chart of the wet dispersed (pre-dispersed) zirconia fiber of example 1. As can be seen from comparison of fig. 1 and 2, the dispersibility of the zirconia chopped fibers is greatly improved after the dispersion by the wet process, and the agglomeration phenomenon is obviously reduced, which indicates that the dispersibility of the zirconia chopped fibers can be effectively improved by the wet dispersion process.
FIG. 3 is a scanning electron microscope test chart of the zirconia fiber/matrix mixture D of example 1. As can be seen from fig. 3, the apparent structure of the zirconia fiber is not significantly destroyed due to the reasonable time setting of the ball milling dispersion process. As can be seen by combining the mechanical property analysis in the table 1, by means of the laminated material distribution ball milling mixing process, the zirconia fibers can be uniformly distributed in the ceramic matrix, so that the defects of internal mechanical structures such as holes and the like are reduced, and the comprehensive mechanical property of the material is improved.
Fig. 4 is an XRD test pattern of the fiber composite thin ceramic plate in example 2. From the diffraction peak positions in fig. 4, it can be inferred that the product has a crystal phase of mullite, zirconia, quartz, celsian, or the like. In addition, the diffraction peak is sharp and the half-peak width is smaller, which indicates that the sintering process is reasonable in arrangement, the formed crystalline phase substance has good orientation and high purity, the content of brittle substances such as internal glass phase is reduced, and the mechanical strength of the material is improved.
Fig. 5 is a scanning electron microscope test chart of a cross section of the fiber composite thin ceramic plate in example 3, and fig. 6 is a scanning electron microscope test chart of a zirconia fiber interface in example 3. As can be seen from FIG. 5, the ceramic matrix at the section has compact structure, the zirconia chopped fibers are uniformly distributed, and no obvious structural creep is seen on the surface, which indicates that the sintering process of the invention is reasonably arranged. In addition, as shown in fig. 6, an obvious interface layer exists between the fiber and the matrix, and it is proved that the silicon-based interface layer can be wrapped outside the fiber interface by establishing a one-dimensional fiber wet chemical dispersion system, so that the thermodynamic damage of high temperature to the fiber is reduced, and the comprehensive mechanical property of the composite sheet is ensured. Meanwhile, part of flaky alumina particles and zirconia fibers are 'pinned' into a ceramic matrix, so that crack expansion can be effectively prevented when external stress is born, and mechanical enhancement mechanisms such as particle diffuse enhancement, fiber fracture-extraction and the like are exerted, so that the mechanical property characterization results in Table 1 are verified.
Fig. 7 is a scanning electron microscope test chart of the wet-dispersed zirconia fiber of comparative example 1. As can be seen by comparing fig. 2 and 7, the zirconia fiber aggregation phenomenon is serious in the conventional drying process, and the zirconia fiber dispersibility is good in the vacuum freeze drying process.
FIG. 8 is a scanning electron microscope test chart of the zirconia fiber/matrix mixture D of comparative example 2. As can be seen by comparing fig. 3 and 8, the zirconia fiber cannot be uniformly distributed in the matrix mixture D by only a single ball-milling dispersion process, and part of the fibers still show an interweaved state, which indicates that the dispersion effect of adopting the one-dimensional fiber wet chemical dispersion is superior to that of the conventional ball-milling dispersion process.
FIG. 9 is a scanning electron microscope test chart of the zirconia fiber/matrix mixture D of comparative example 3. As can be seen by comparing fig. 3 and 9, the fibers in fig. 9 are uniformly distributed and have a similar length-diameter ratio, but the fibers are distributed and dispersed in the matrix and have a dense stacking trend, so that the dispersion effect of the laminated cloth ball milling mixing process in the invention is superior to that of the one-step conventional ball milling process.
Fig. 10 is a scanning electron microscope test chart of a cross section of the fiber composite thin ceramic plate of comparative example 5, and fig. 11 is a scanning electron microscope test chart of a zirconia fiber interface of comparative example 5. As can be seen from FIGS. 10 and 11, the matrix of comparative example 5 has a remarkable structure of mechanical defects such as pores and the like, and the internal grains are remarkably enlarged. In addition, the fused holes and broken fiber structures are visible at the phase interface of the fiber and the matrix, which shows that the sintering system set in comparative example 5 is unreasonable, and long-time heat preservation promotes the surface of the fiber to creep, damages the original compact structure of the fiber, and causes the fiber to become brittle and the mechanical property to be greatly reduced. Therefore, the bending strength of the composite material under the process system is only 38.96MPa, and the fracture toughness is only 1.38 MPa.m 1/2 。
Claims (7)
1. Large-sized ZrO 2 Fiber/flake Al 2 O 3 The preparation method of the composite thin ceramic plate is characterized by comprising the following steps:
ZrO (ZrO) 2 Immersing chopped fibers into a fiber pre-dispersion solution containing sodium polyacrylate, aminopropyl triethoxysilane and sodium tripolyphosphate, wherein the pH of the fiber pre-dispersion solution is 8.0-8.5, pre-dispersing under the conditions of heating and stirring, collecting fibers, and vacuum freeze-drying to obtain pre-dispersion ZrO with silicon-based interface layer wrapped by outer wall 2 Chopped fibers; the ZrO 2 The length of the chopped fiber is 150-180 mu m, the diameter is 3-5 mu m, and the length-diameter ratio is 30-60;
pre-dispersed ZrO with silicon-based interface layer wrapped on outer wall 2 Performing ball milling dry mixing after stacking distribution of chopped fibers and matrix powder to obtain a fiber/matrix mixture; the base isThe mass ratio of the chemical components of the bulk powder is Al 2 O 3 ：SiO 2 ：MgO：CaO：Na 2 O：K 2 O：La 2 O 3 ：Ce 2 O 3 ：Y 2 O 3 ：Na 3 PO 4 = (35-40): (40-45): (10-15): (5-10): (1-5): (1-5): (0.5-1): (0.1-0.5): (0.1-0.5): (1.5-3); weighing the matrix raw materials according to the mass ratio of the chemical components of the matrix powder, uniformly mixing, and crushing, pulping and spray granulating to obtain the matrix powder; the mass ratio of each component of the matrix raw material is flaky alumina: magnesium oxide: black talc: monazite). Ball clay: bentonite: potassium feldspar: sodium tripolyphosphate = 30-35:8-13:9-14:21-26:14-19:7-12:12-17:1-3; the specific operation of the laminated cloth is as follows: firstly, weighing matrix powder, spreading the matrix powder at the bottom of a ball milling tank, and then weighing pre-dispersed ZrO with the outer wall wrapped by a silicon-based interface layer 2 Spreading the chopped fibers on the surface of the matrix powder, and alternately repeating the above processes until the chopped fibers and the matrix powder are all sent to a ball milling tank;
pressing the fiber/matrix mixture into a ceramic blank, and sintering the ceramic blank to obtain the large-sized ZrO 2 Fiber/flake Al 2 O 3 Composite thin ceramic plate; the highest sintering temperature of sintering is 1250-1300 ℃, the sintering period is 20-30min, and the heat preservation time of the highest sintering temperature is 10-15min.
2. The method of claim 1, wherein the sodium polyacrylate, in the pre-dispersion solution of fibers: aminopropyl triethoxysilane: sodium tripolyphosphate: the mass ratio of water is (20-30): (10-20): (10-20): (50-60).
3. The method according to claim 1, wherein the ZrO 2 The ratio of chopped fibers to fiber pre-dispersion solution was 1g:25-100g.
4. The method according to claim 1, wherein the drying temperature of vacuum freeze-drying is-80 to-120 ℃, the drying time of vacuum freeze-drying is 6-8 hours, and the vacuum degree of vacuum freeze-drying is 20-40Pa.
5. The preparation method according to claim 1, wherein the particle size of the flaky alumina is 1-2 μm, the thickness is 50-100nm, the mesoporous pore diameter is 1-3nm, and the mesoporous rate is 10-20%.
6. The method of claim 1, wherein the pre-dispersed ZrO of the silicon-based interface layer is surrounded by the outer wall during the ball milling process 2 Chopped fiber: matrix powder: ball stone mass ratio= (1-5): (50-60): (80-100), the ball milling rotating speed is 50-80r/min, and the ball milling time is 2-5min.
7. A large-sized ZrO obtained by the production method according to claim 1 2 Fiber/flake Al 2 O 3 The composite thin ceramic plate is characterized in that the bending strength of the composite thin ceramic plate is 160-170MPa, and the fracture toughness is 3.00-3.10MPa.m 1/2 The water absorption rate is 0.15-0.25%, and the density is 2.90-3.00g/cm 3 。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113124A (en) * | 2013-02-04 | 2013-05-22 | 西安交通大学 | Preparation method of fiber-toughened SiC ceramic-based composite material three-dimensional member |
| CN105753460A (en) * | 2016-02-03 | 2016-07-13 | 蒙娜丽莎集团股份有限公司 | Low-shrinkage high-strength large-scale ceramic plate and preparation method thereof |
| CN110330350A (en) * | 2019-07-25 | 2019-10-15 | 武汉理工大学 | A kind of preparation method of fiber reinforced alumina ceramics |
| CN110483085A (en) * | 2019-08-01 | 2019-11-22 | 广东工业大学 | A kind of whisker reinforcement alumina composite ceramic and the preparation method and application thereof |
| WO2021012448A1 (en) * | 2019-07-23 | 2021-01-28 | 南充三环电子有限公司 | Zirconia compounded alumina ceramic sintered body, preparation method therefor and use thereof |
| CN113896555A (en) * | 2021-10-26 | 2022-01-07 | 厦门大学 | Particle-reinforced fiber woven composite material and preparation method thereof |
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| CN109053206B (en) * | 2018-08-31 | 2021-07-23 | 中国科学院金属研究所 | Short fiber reinforced oriented MAX phase ceramic matrix composite material and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113124A (en) * | 2013-02-04 | 2013-05-22 | 西安交通大学 | Preparation method of fiber-toughened SiC ceramic-based composite material three-dimensional member |
| CN105753460A (en) * | 2016-02-03 | 2016-07-13 | 蒙娜丽莎集团股份有限公司 | Low-shrinkage high-strength large-scale ceramic plate and preparation method thereof |
| WO2021012448A1 (en) * | 2019-07-23 | 2021-01-28 | 南充三环电子有限公司 | Zirconia compounded alumina ceramic sintered body, preparation method therefor and use thereof |
| CN110330350A (en) * | 2019-07-25 | 2019-10-15 | 武汉理工大学 | A kind of preparation method of fiber reinforced alumina ceramics |
| CN110483085A (en) * | 2019-08-01 | 2019-11-22 | 广东工业大学 | A kind of whisker reinforcement alumina composite ceramic and the preparation method and application thereof |
| CN113896555A (en) * | 2021-10-26 | 2022-01-07 | 厦门大学 | Particle-reinforced fiber woven composite material and preparation method thereof |
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