CN116283322A - Large-scale structural ceramic formula - Google Patents
Large-scale structural ceramic formula Download PDFInfo
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- CN116283322A CN116283322A CN202310380561.8A CN202310380561A CN116283322A CN 116283322 A CN116283322 A CN 116283322A CN 202310380561 A CN202310380561 A CN 202310380561A CN 116283322 A CN116283322 A CN 116283322A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 66
- 239000010881 fly ash Substances 0.000 claims abstract description 48
- 239000002994 raw material Substances 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000003077 lignite Substances 0.000 claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 9
- MAKDTFFYCIMFQP-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti].[W] MAKDTFFYCIMFQP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 19
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 7
- 238000009472 formulation Methods 0.000 claims description 7
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 238000005245 sintering Methods 0.000 abstract description 19
- 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 abstract description 7
- 229910052863 mullite Inorganic materials 0.000 abstract description 7
- 239000011575 calcium Substances 0.000 abstract description 6
- 239000010456 wollastonite Substances 0.000 abstract description 6
- 229910052882 wollastonite Inorganic materials 0.000 abstract description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- MKTRXTLKNXLULX-UHFFFAOYSA-P pentacalcium;dioxido(oxo)silane;hydron;tetrahydrate Chemical compound [H+].[H+].O.O.O.O.[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O MKTRXTLKNXLULX-UHFFFAOYSA-P 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000010883 coal ash Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- -1 aluminum ion Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 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
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Abstract
The invention discloses a large-scale structural ceramic formula, which comprises a ceramic preparation raw material and a reinforced structural net, wherein the ceramic preparation raw material comprises fly ash, caO, naOH solution and fluxing agent, and the reinforced structural net is a net-shaped supporting frame made of tungsten-titanium alloy; the invention solves the problems of low yield and high raw material price of the ceramic powder with the structure at present, can improve the utilization rate of the accumulated fly ash in China, and lightens the huge environmental pressure in China; the wollastonite ceramic formed by sintering the raw materials synthesized by taking lignite fly ash as a silicon source and taking CaO as a calcium source in an NaOH alkaline medium shows the optimal performance, the sintering temperature is reduced by about 900 ℃, the temperature is reduced by 200 ℃ compared with the temperature in the prior art, the sintering temperature of the mullite ceramic formed by sintering the activated high-alumina fly ash as the raw material is reduced by about 1300 ℃ compared with the temperature in the prior art, and the load bearing limit of the structural ceramic is greatly improved after the reinforced structural network is added.
Description
Technical Field
The invention relates to the field of ceramic manufacture, in particular to a large-scale structural ceramic formula.
Background
The structural ceramic is a ceramic material with the performances of supernormal load bearing, high temperature bearing, wear resistance, corrosion resistance and the like, is widely applied to the fields of aerospace, machinery, chemical industry, energy sources, automobiles and the like, and common structural ceramics with better performances are wollastonite ceramics, mullite ceramics, silicon carbide ceramics and the like, however, although the quantity of ceramic manufacturing enterprises is considerable in China, the ceramic manufacturing enterprises still fall behind in a plurality of important production technical fields of the structural ceramics, and especially the yield of the structural ceramics is low and the quality is difficult to ensure, so that advanced structural ceramics still need to be imported from developed countries in a large amount, and the ceramic industry needs a transformation opportunity. On the other hand, the annual emission of the fly ash in China exceeds 5.5 hundred million tons, but the utilization rate is only 70 percent, so that the total accumulated amount of the fly ash exceeds 30 hundred million tons, and the main component of the fly ash is SiO 2 And Al 2 O 3 The ceramic material is very similar to the ceramic material in chemical composition and phase composition, so that how to make fly ash into the preparation material of the high-quality novel structural ceramic is a problem which needs to be considered.
Finally, ceramic articles are currently used in a variety of applications, but because ceramic articles are fragile and easily damaged, they are also highly consumable products in various applications.
In view of the foregoing, there is a need for a ceramic article that is inexpensive to manufacture and that can utilize fly ash as a raw material.
Disclosure of Invention
The invention provides a large-scale structural ceramic formula for solving the technical problems.
The technical scheme of the invention is realized as follows:
a large-scale structural ceramic formula comprises ceramic preparation raw materials and a reinforced structural net;
the reinforced structural net is a net-shaped supporting frame made of tungsten-titanium alloy, the net-shaped supporting frame is composed of a plurality of groups of pyramid-shaped supporting rods, 4 supporting rods forming a pyramid shape are arranged, a sphere is arranged at the top of the tower, a plurality of through holes are formed in the sphere, and the supporting rods are inserted into the through holes;
the ceramic preparation raw material uniformly covers the prefabricated reinforced structural net in a smearing way and is shaped by firing;
the ceramic preparation raw materials comprise fly ash, caO, naOH solution and auxiliary agent, wherein the fly ash comprises lignite fly ash and high-alumina fly ash, and SiO in the lignite fly ash 2 With Al 2 O 3 The mass ratio of the addition is higher than 75%.
Al in the high-alumina fly ash 2 O 3 The mass ratio of (2) is higher than 49%.
The CaO gives a Ca/(Al+Si) molar ratio of 1 in the raw material mixture.
The concentration of the NaOH solution is 50g/L and 100 g/L.
The auxiliary agent comprises an antioxidant and a fluxing agent.
The antioxidant comprises titanate and silicon nitride.
The fluxing agent is rare metal oxide Y 2 O 3 、V 2 O 5 、La 2 O 3 And CeO 2 One or more of the following.
The invention solves the problems of low yield and high raw material price of the ceramic powder with the structure at present, can improve the utilization rate of the accumulated fly ash in China, and lightens huge environmental pressure in China; the sintering temperature of the wollastonite ceramic which is formed by sintering the raw materials synthesized by taking lignite coal ash as a silicon source and taking CaO as a calcium source in an NaOH alkaline medium shows the optimal performance is about 900 ℃, the sintering temperature is reduced by 200 ℃ compared with the temperature in the prior art, the sintering temperature of the mullite ceramic which is formed by sintering the activated high-alumina coal ash as the raw material shows the optimal performance is below 1300 ℃, the temperature is reduced by about 150 ℃ compared with the temperature in the prior art, and the load bearing limit of the structural ceramic is greatly improved after the reinforced structural network is added; therefore, the invention has great market popularization value.
Drawings
FIG. 1 is a schematic structural view of a reinforced structural web of the present invention.
FIG. 2 is a second schematic structural view of the reinforced structural net of the present invention.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples are not representative of all implementations consistent with the present disclosure. Rather, they are merely examples of apparatus consistent with some aspects of the disclosure as detailed in the accompanying claims.
1-2, a large structural ceramic formulation comprising ceramic preparation raw materials and a reinforced structural mesh;
the reinforced structural net is a net-shaped supporting frame made of tungsten-titanium alloy, the net-shaped supporting frame is composed of a plurality of groups of pyramid-shaped supporting rods, 4 supporting rods which form a pyramid shape are arranged, a spherical ball is arranged at the top of the tower, a plurality of through holes are formed in the spherical ball, the supporting rods are inserted into the through holes, and the reinforced structural net is prefabricated for standby;
the ceramic preparation raw material uniformly covers the reinforced structural net in a smearing way and is shaped by firing;
the ceramic preparation raw materials comprise fly ash, caO, naOH solution, an auxiliary agent, weight-reducing balls and a dispersing agent, wherein the weight-reducing balls are hollow metal balls, particularly tungsten-titanium alloy hollow balls, the dispersing agent is a leveling agent, so that the weight-reducing balls can be uniformly distributed, the fly ash comprises lignite fly ash and high-alumina fly ash, the lignite fly ash is used as raw materials for manufacturing wollastonite ceramic, the high-alumina fly ash is used as raw materials for manufacturing mullite ceramic, and SiO in the lignite fly ash is used as a raw material for manufacturing the mullite ceramic 2 With Al 2 O 3 The added mass ratio is higher than 75 percent, and the Al in the chemical components of the high-alumina fly ash 2 O 3 The mass ratio is higher than 50%.
The CaO gives a Ca/(Al+Si) molar ratio of 1 in the raw material mixture.
The concentration of the NaOH solution is 50g/L and 100 g/L.
The auxiliary agent comprises an antioxidant and a fluxing agent, wherein the antioxidant comprises titanate and silicon nitride, and the fluxing agent is rare metal oxide Y 2 O 3 、V 2 O 5 、La 2 O 3 And CeO 2 The mass ratio of the auxiliary agent to the mixture is 5%.
Example 1
A large-scale structural ceramic formula comprises ceramic preparation raw materials and a reinforced structural net;
the reinforced structural net is a net-shaped supporting frame made of tungsten-titanium alloy, the net-shaped supporting frame is composed of a plurality of groups of pyramid-shaped supporting rods, 4 supporting rods forming a pyramid shape are arranged, a sphere is arranged at the top of the tower, a plurality of through holes are formed in the sphere, and the supporting rods are inserted into the through holes;
the ceramic preparation raw material uniformly covers the reinforced structural net in a smearing way and is shaped by firing;
the ceramic preparation raw materials comprise fly ash, caO, naOH solution and auxiliary agent, wherein the fly ash comprises lignite fly ash and high-alumina fly ash, and SiO in the lignite fly ash 2 With Al 2 O 3 The mass ratio of the addition is higher than 75%.
When wollastonite ceramic needs to be synthesized, the preparation flow of the invention is as follows:
firstly, preparing a prefabricated reinforced structural net, then preparing a green body, adding lignite fly ash, caO and NaOH solution with the concentration of 50g/L into a reaction kettle, wherein the reaction condition is that the molar ratio of Ca/(Al+Si) is 1, the liquid-solid ratio is 35mL/g, the reaction temperature is 225 ℃, and the reaction time is 110min. The silicate structure and mineral crystal structure in the lignite fly ash are destroyed in alkaline hydrothermal environment, so that SiO 2 Reacting with CaO to generate tobermorite type calcium silicate hydrate, wherein the reaction formula is as follows:
5CaO+6SiO 2 +5H 2 O=5CaO·6SiO 2 ·5H 2 O
at the same time due to Si 4+ And Al 3+ Similar structure, al in the process of tobermorite synthesis 3+ Can partially replace Si 4+ Forming the aluminum ion replacement type tobermorite. The tobermorite powder, titanate and Y synthesized by the reaction 2 O 3 And V 2 O 5 Mixing and grinding the mixture and deionized water uniformly in a ball mill, mixing the mixture and deionized water according to a mass ratio of 11:2, then forming the mixed mixture and a prefabricated tungsten-titanium alloy reinforced structural net on a single-shaft hydraulic press together, enabling the reinforced structural net to be attached to the surface of a green body, forming four green bodies without the reinforced structural net, namely a first sample, a second sample, a third sample and a fourth sample, respectively, wherein the forming pressure is 20MPa, putting the formed green bodies into an oven, and drying the green bodies for 12 hours at a temperature of 110 ℃. The next step is ceramic firing, sintering the dried green body, wherein the sintering temperatures of the sample I, the sample II, the sample III, the sample IV and the sample V are respectively 800 ℃, 900 ℃, 1000 ℃, 1100 ℃ and 900 ℃, the heating speed in the firing process is 10 ℃/min, the heat preservation time is 2h, the cooling speed is 1 ℃/min, and the performance test is carried out after the finished product is obtained, and the experimental results are as follows:
sintering temperature | Flexural Strength | Porosity of the porous material | Bulk density of | |
Sample one | 800℃ | 52.37MPa | 9.23% | 2.02g/cm 3 |
Sample two | 900℃ | 53.68MPa | 8.98% | 2.26g/cm 3 |
Sample three | 1000℃ | 50.61MPa | 9.39% | 2.11g/cm 3 |
Sample four | 1100℃ | 50.32MPa | 9.54% | 2.09g/cm 3 |
As is clear from the above table, the wollastonite ceramic which is formed by sintering the raw materials synthesized by taking lignite fly ash as a silicon source and taking CaO as a calcium source in NaOH alkaline medium shows the best performance, the sintering temperature is about 900 ℃, the temperature is reduced by 200 ℃ compared with the temperature in the prior art, the flexural strength reaches 53.68MPa under the condition of not adding reinforced structural mesh sintering, the porosity is 8.98%, and the volume density is 2.26g/cm 3 。
Example two
A large-scale structural ceramic formula comprises ceramic preparation raw materials and a reinforced structural net;
the reinforced structural net is a net-shaped supporting frame made of tungsten-titanium alloy, the net-shaped supporting frame is composed of a plurality of groups of pyramid-shaped supporting rods, 4 supporting rods forming a pyramid shape are arranged, a sphere is arranged at the top of the tower, a plurality of through holes are formed in the sphere, and the supporting rods are inserted into the through holes;
the ceramic preparation raw material uniformly covers the reinforced structural net in a smearing way and is shaped by firing;
the ceramic preparation raw materials comprise fly ash, caO, naOH solution and auxiliary agent, wherein the fly ash comprises lignite fly ash and high-alumina fly ash, and SiO in the lignite fly ash 2 With Al 2 O 3 The mass ratio of the addition is higher than 75%.
When mullite ceramic is needed to be synthesized, the preparation flow of the invention is as follows:
firstly, preparing a prefabricated reinforced structural net, then, performing alkali activation and desilication reaction of the high-alumina fly ash in a beaker heated by a water bath, adding the high-alumina fly ash and a NaOH solution with the concentration of 100g/L into the beaker, wherein the liquid-solid ratio is 5mL/g, the stirring speed is 250rpm, the reaction temperature is 98 ℃, and the reaction time is 3.5h. The alkali activated high alumina fly ash, titanate and La obtained by the reaction 2 O 3 And CeO 2 Mixing and grinding the mixture and deionized water uniformly in a ball mill, mixing the mixture and deionized water according to a mass ratio of 11:2, then forming the mixed mixture and a prefabricated tungsten-titanium alloy reinforced structural net on a single-shaft hydraulic press together, enabling the reinforced structural net to be attached to the surface of a green body, forming four green bodies without the reinforced structural net as a sample five, forming the four green bodies without the reinforced structural net as a sample one, a sample two, a sample three and a sample four respectively, wherein the forming pressure is 20MPa, putting the formed green bodies into an oven, and drying the formed green bodies for 12 hours in a temperature environment of 110 ℃. The next step is that the ceramic is sintered, the sintering temperature of the dried green body is 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃ and 1300 ℃ respectively, the heating speed in the sintering process is 5 ℃/min, the heat preservation time is 2h, and the temperature is reducedThe temperature speed is 2 ℃/min, and the performance test is carried out after the finished product is obtained, and the experimental result is as follows:
as is clear from the above table, the mullite ceramic sintered from activated high alumina fly ash as raw material shows the best performance, the sintering temperature is lower than 1300 ℃, the temperature is reduced by about 150 ℃ compared with the temperature in the prior art, the flexural strength reaches 110.72MPa under the condition of sintering without adding a reinforced structural net, the open porosity is only 0.58%, the relative density is 90.76%, and the water absorption is 0.09%.
Claims (8)
1. The large-scale structural ceramic formula comprises ceramic preparation raw materials and a reinforced structural net, and is characterized in that:
the reinforced structural net is a net-shaped supporting frame made of tungsten-titanium alloy, the net-shaped supporting frame is composed of a plurality of groups of pyramid-shaped supporting rods, 4 supporting rods forming a pyramid shape are arranged, a sphere is arranged at the top of the tower, a plurality of through holes are formed in the sphere, and the supporting rods are inserted into the through holes;
the ceramic preparation raw material uniformly covers the reinforced structural net in a smearing way and is shaped by firing;
the ceramic preparation raw materials comprise fly ash, caO, naOH solution and auxiliary agent, wherein the fly ash comprises lignite fly ash and high-alumina fly ash, and SiO in the lignite fly ash 2 With Al 2 O 3 The mass ratio of the addition is higher than 75%.
2. A large structural ceramic formulation according to claim 1, wherein: al in the high-alumina fly ash 2 O 3 The mass ratio of (2) is higher than 49%, and most preferably 53%.
3. A large structural ceramic formulation according to claim 1, wherein: the CaO gives a Ca/(Al+Si) molar ratio of 1 in the raw material mixture.
4. A large structural ceramic formulation according to claim 1, wherein: the concentration of the NaOH solution is 50g/L and 100 g/L.
5. A large structural ceramic formulation according to claim 1, wherein: the auxiliary agent comprises an antioxidant and a fluxing agent.
6. A large structural ceramic formulation according to claim 1, wherein: the fluxing agent is rare metal oxide Y 2 O 3 、V 2 O 5 、La 2 O 3 And CeO 2 One or more of the following.
7. A large structural ceramic formulation according to claim 1, wherein: the antioxidant comprises titanate and silicon nitride.
8. The method according to claim 1, wherein: siO in the lignite fly ash 2 With Al 2 O 3 The mass ratio of the addition is optimally 92%.
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