CN116730731A - Silicon carbide-based ceramic heat accumulator and preparation method thereof - Google Patents
Silicon carbide-based ceramic heat accumulator and preparation method thereof Download PDFInfo
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- CN116730731A CN116730731A CN202310513313.6A CN202310513313A CN116730731A CN 116730731 A CN116730731 A CN 116730731A CN 202310513313 A CN202310513313 A CN 202310513313A CN 116730731 A CN116730731 A CN 116730731A
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- silicon carbide
- carbide particles
- based ceramic
- heat accumulator
- ceramic heat
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 163
- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 104
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000000967 suction filtration Methods 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 29
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 17
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 13
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 230000035939 shock Effects 0.000 abstract description 19
- 238000005338 heat storage Methods 0.000 abstract description 12
- 238000007598 dipping method Methods 0.000 abstract 1
- 229910052839 forsterite Inorganic materials 0.000 description 12
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 238000011065 in-situ storage Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000011449 brick Substances 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 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
- 239000000463 material Substances 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- -1 machinery Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012782 phase change material Substances 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D20/00—Heat storage plants or apparatus in general; Regenerative heat-exchange apparatus not covered by groups F28D17/00 or F28D19/00
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Abstract
The invention relates to a silicon carbide-based ceramic heat accumulator and a preparation method thereof. The technical proposal is as follows: mixing silicon carbide particles A, silicon carbide particles B and silicon carbide particles C, placing the mixed silicon carbide particles in silica sol, and dipping under vacuum; drying the impregnated silicon carbide particles, performing heat treatment, mixing the nano silicon dioxide coated silicon carbide particles obtained after the heat treatment with magnesium chloride, sequentially adding deionized water and an ammonia water solution, stirring, and performing suction filtration; the product after suction filtration is placed in a rotary evaporator to rotate, dried and heat treated to obtain magnesia-silica coated silicon carbide particles; mixing magnesia-silica coated silicon carbide particles, silicon carbide fine powder and light burned magnesium powder, adding a polyvinyl alcohol solution, and mixing; pressing and forming, and performing heat treatment at 800-1000 ℃ for 2-4 h and 1400-1500 ℃ for 2-4 h to obtain the silicon carbide-based ceramic heat accumulator. The product prepared by the invention has high heat conductivity, high heat storage capacity, high thermal shock stability and high compressive strength.
Description
Technical Field
The invention belongs to the technical field of refractory materials. In particular to a silicon carbide-based ceramic heat accumulator and a preparation method thereof.
Technical Field
The heat accumulating combustion technology is one of the most potential energy saving and environment protecting technology in 21 st century, and through the reversing device, the technology uses the heat accumulating chamber of the heat accumulator to preheat fuel for supporting combustion and to recover heat in high temperature fume to the maximum, so as to realize the aim of saving energy and reducing emission, and is widely used in various heating furnaces in the industries of steel, machinery, building materials, nonferrous metal smelting and the like.
The heat accumulator is a key part of the heat accumulator, and the performance of the heat accumulator is directly related to the combustion efficiency and energy-saving level of heat accumulating kiln equipment. The selection of the heat accumulator mainly considers the following aspects: heat storage capacity, heat exchange efficiency, thermal shock stability, oxidation resistance, erosion resistance, economy, etc., which are being studied by those skilled in the art:
a silicon carbide large-sized ceramic heat accumulator and a preparation process (CN 201610426165.4) thereof are disclosed, and the silicon carbide heat accumulator prepared by the technology has good wear resistance and corrosion resistance, but has small heat accumulating capacity, so that the energy utilization rate is reduced. The technology adopts silicon carbide coated alumina and a preset hole on complex phase ceramic to fill phase change material, which improves the heat storage capacity of the heat storage body, but reduces the heat conduction performance of the heat storage body by the thermal resistance of the two-phase interface. The patent technology of a silicon carbide-corundum composite honeycomb heat accumulator (CN 201010103068.4) adopts a honeycomb heat accumulator prepared by an extrusion molding method, and has the problems of large heat exchange area, high heat accumulation efficiency, low compressive strength and poor thermal shock stability. The technology of the silicon carbide mullite heat accumulator composite material and the preparation method thereof (CN 2010102553792A) adopts a method of compounding silicon carbide and mullite two phases, and although the corrosion resistance of the heat accumulator is improved, the heat conduction performance of the heat accumulator is lower, and the high conductivity of the silicon carbide is not fully exerted by simple compounding. The patent technology of a magnesium silicon carbide brick and a production mode (CN201810982571.8A) thereof introduces silicon carbide fine powder into a magnesium oxide heat storage brick, although the erosion resistance of the magnesium silicon carbide brick is improved, the dispersibility of silicon carbide particles in the magnesium brick is not ideal, and the particles are aggregated or agglomerated, so that the uniformity and the performance of the material are reduced, and the thermal shock stability of the material is further improved.
In summary, the conventional silicon carbide ceramic heat accumulator has the following technical defects: the heat storage capacity is small, the heat conductivity is low, the compressive strength is low, and the thermal shock stability is poor.
Disclosure of Invention
The invention aims to overcome the technical defects existing in the prior art, and aims to provide a preparation method of a silicon carbide-based ceramic heat accumulator, which has the advantages of high heat accumulating capacity, high heat conductivity, high compressive strength and high thermal shock stability.
In order to achieve the above purpose, the technical scheme adopted by the invention comprises the following specific steps:
firstly, mixing 45-55wt% of silicon carbide particles A with the granularity of 1-1.5 mm, 5-15wt% of silicon carbide particles B with the granularity of 0.5-1 mm and 35-45wt% of silicon carbide particles C with the granularity of 0.1-0.5 mm to obtain silicon carbide particles; placing the silicon carbide particles into silica sol, and soaking for 20-40 min under the vacuum degree of-0.08 to-0.10 MPa to obtain soaked silicon carbide particles; and (3) drying the impregnated silicon carbide particles for 8-10 hours at the temperature of 90-110 ℃, and performing heat treatment for 2-4 hours at the temperature of 900-1000 ℃ to obtain the nano silicon dioxide coated silicon carbide particles.
Step two, mixing 80 to 90 weight percent of nano silicon dioxide coated silicon carbide particles and 10 to 20 weight percent of magnesium chloride to obtain a first mixture; adding deionized water accounting for 150-200 wt% of the first mixture into the first mixture, and stirring for 5-10 min; adding ammonia water solution accounting for 10-15 wt% of the first mixture into the first mixture, stirring for 20-30 min, pouring into a sand core suction filtration device, and performing suction filtration for 10-20 min; placing the product obtained after suction filtration in a rotary evaporator, and rotating for 2-3 h under the conditions that the water temperature is 60-80 ℃ and the rotating speed is 50-70 rad/min; finally, drying for 8-10 h at 100-110 ℃, and heat-treating for 1-3 h at 700-800 ℃ to obtain the magnesia-silica coated silicon carbide particles.
Thirdly, mixing 85-90 wt% of magnesia-silica coated silicon carbide particles, 3-5 wt% of silicon carbide fine powder and 7-10 wt% of light burned magnesium powder to obtain a second mixture, adding a polyvinyl alcohol solution accounting for 5-10 wt% of the second mixture into the second mixture, and uniformly mixing; and then pressing and forming under the condition of 80-100 MPa, and performing heat treatment on the pressed and formed green body for 2-4 hours at 800-1000 ℃ and heat treatment on the pressed and formed green body for 2-4 hours at 1400-1500 ℃ to obtain the silicon carbide-based ceramic heat accumulator.
The SiC content of the silicon carbide particles A, B and C is more than 97wt%, fe 2 O 3 The content of (C) is less than 0.50wt%.
The silica sol: siO (SiO) 2 More than 25.50wt%, na 2 The content of O is less than 0.35wt%, the pH is 8.5-9.5, and the average particle size of the colloidal particles is 8-25 nm.
MgCl in the magnesium chloride 2 ·6H 2 The purity of O is more than 98wt%.
NH in the ammonia water solution 3 ·H 2 The concentration of O is 25-28 wt%.
The content of SiC in the silicon carbide fine powder is more than 97wt percent, and Fe 2 O 3 The content of (2) is less than 0.50wt%; the granularity of the silicon carbide fine powder is less than 0.088mm.
The MgO content in the light-burned magnesium powder is more than 97wt%, and the granularity of the light-burned magnesium powder is less than 0.088mm.
The concentration of the polyvinyl alcohol solution is 5-10wt%.
The suction filtration is reduced pressure suction filtration, and the vacuum degree of the suction filtration is-0.09 to-0.10 MPa.
By adopting the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) The invention fully utilizes the characteristic of high heat capacity of forsterite, and combines high-temperature heat treatment to generate forsterite in situ by coating silicon dioxide and magnesium oxide on the surfaces of silicon carbide particles, so that the product has high heat storage capacity, and the silicon carbide-based ceramic heat accumulator prepared by the invention has the characteristic of high heat storage capacity.
(2) The invention combines the high heat conductivity of silicon carbide with the excellent oxidation resistance and erosion resistance of forsterite, and the oxidation of the silicon carbide in the high-temperature use process is avoided and the high heat conductivity of the silicon carbide is maintained by forming the forsterite around the silicon carbide particles and the fine powder in situ, so that the silicon carbide-based ceramic heat accumulator prepared by the invention has excellent heat conductivity.
(3) On the basis of strictly limiting the grain composition of the raw materials, the invention realizes that the forsterite is formed in situ on the surfaces of the silicon carbide particles and is also formed in situ between the silicon carbide fine powder and the light burned magnesia powder by limiting the preparation process and the characteristics of the raw materials, thereby forming stable forsterite combination between the raw material particles; and the characteristic of high thermal shock stability of the silicon carbide is fully utilized, so that the prepared silicon carbide-based ceramic heat accumulator has higher compressive strength and thermal shock stability.
The silicon carbide-based ceramic heat accumulator prepared by the invention is detected by the following steps: the volume density is more than or equal to 3.00g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The heat conductivity is more than or equal to 60W/(m.K); the specific heat capacity is more than or equal to 1.4J/(g.K); the thermal shock stability is more than or equal to 20 times (1100 ℃ C., air cooling); the compressive strength is 80-100 MPa; the thermal expansion coefficient (20-1000 ℃) is (4.5-5). Times.10 -6 /℃。
Therefore, the silicon carbide-based ceramic heat accumulator prepared by the invention has high heat conductivity, high heat accumulation capacity, high thermal shock stability and high compressive strength.
Detailed Description
The invention is further described in connection with the following detailed description, which is not intended to limit the scope of the invention.
A silicon carbide-based ceramic heat accumulator and a preparation method thereof. The preparation method of the specific embodiment comprises the following steps:
firstly, mixing 45-55wt% of silicon carbide particles A with the granularity of 1-1.5 mm, 5-15wt% of silicon carbide particles B with the granularity of 0.5-1 mm and 35-45wt% of silicon carbide particles C with the granularity of 0.1-0.5 mm to obtain silicon carbide particles; placing the silicon carbide particles into silica sol, and soaking for 20-40 min under the vacuum degree of-0.08 to-0.10 MPa to obtain soaked silicon carbide particles; and (3) drying the impregnated silicon carbide particles for 8-10 hours at the temperature of 90-110 ℃, and performing heat treatment for 2-4 hours at the temperature of 900-1000 ℃ to obtain the nano silicon dioxide coated silicon carbide particles.
Step two, mixing 80 to 90 weight percent of nano silicon dioxide coated silicon carbide particles and 10 to 20 weight percent of magnesium chloride to obtain a first mixture; adding deionized water accounting for 150-200 wt% of the first mixture into the first mixture, and stirring for 5-10 min; adding ammonia water solution accounting for 10-15 wt% of the first mixture into the first mixture, stirring for 20-30 min, pouring into a sand core suction filtration device, and performing suction filtration for 10-20 min; placing the product obtained after suction filtration in a rotary evaporator, and rotating for 2-3 h under the conditions that the water temperature is 60-80 ℃ and the rotating speed is 50-70 rad/min; finally, drying for 8-10 h at 100-110 ℃, and heat-treating for 1-3 h at 700-800 ℃ to obtain the magnesia-silica coated silicon carbide particles.
Thirdly, mixing 85-90 wt% of magnesia-silica coated silicon carbide particles, 3-5 wt% of silicon carbide fine powder and 7-10 wt% of light burned magnesium powder to obtain a second mixture, adding a polyvinyl alcohol solution accounting for 5-10 wt% of the second mixture into the second mixture, and uniformly mixing; and then pressing and forming under the condition of 80-100 MPa, and performing heat treatment on the pressed and formed green body for 2-4 hours at 800-1000 ℃ and heat treatment on the pressed and formed green body for 2-4 hours at 1400-1500 ℃ to obtain the silicon carbide-based ceramic heat accumulator.
NH in the ammonia water solution 3 ·H 2 The concentration of O is 25-28 wt%;
the concentration of the polyvinyl alcohol solution is 5-10wt%;
the suction filtration is reduced pressure suction filtration, and the vacuum degree of the suction filtration is-0.09 to-0.10 MPa.
In this embodiment:
the SiC content of the silicon carbide particles A, B and C is more than 97wt%, fe 2 O 3 The content of (2) is less than 0.50wt%;
the silica sol: siO (SiO) 2 More than 25.50wt%, na 2 The content of O is less than 0.35 weight percent, and the pH value is 8.5-9.5; the average particle size of colloidal particles of the silica sol is 8-25 nm;
MgCl in the magnesium chloride 2 ·6H 2 O purity greater than 98wt%;
the content of SiC in the silicon carbide fine powder is more than 97wt percent, and Fe 2 O 3 The content of (2) is less than 0.50wt%; the granularity of the silicon carbide fine powder is less than 0.088mm;
the MgO content in the light-burned magnesium powder is more than 97wt%, and the granularity of the light-burned magnesium powder is less than 0.088mm.
The embodiments are not described in detail.
Example 1
A silicon carbide-based ceramic heat accumulator and a preparation method thereof. The preparation method of the embodiment is as follows:
firstly, mixing 45wt% of silicon carbide particles A with the granularity of 1-1.5 mm, 15wt% of silicon carbide particles B with the granularity of 0.5-1 mm and 40wt% of silicon carbide particles C with the granularity of 0.1-0.5 mm to obtain silicon carbide particles; placing the silicon carbide particles into silica sol, and soaking for 20min under the condition that the vacuum degree is-0.08 MPa to obtain soaked silicon carbide particles; and drying the impregnated silicon carbide particles for 8 hours at 90 ℃, and performing heat treatment for 2 hours at 900 ℃ to obtain the nano silicon dioxide coated silicon carbide particles.
Secondly, mixing 80wt% of nano silicon dioxide coated silicon carbide particles with 20wt% of magnesium chloride to obtain a first mixture; adding deionized water accounting for 150wt% of the first mixture into the first mixture, and stirring for 5min; adding ammonia water solution accounting for 10wt% of the first mixture into the first mixture, stirring for 20min, pouring into a sand core suction filtration device, and suction-filtering for 10min; placing the product obtained after suction filtration in a rotary evaporator, and rotating for 2 hours under the conditions that the water temperature is 60 ℃ and the rotating speed is 50 rad/min; and finally, drying for 8 hours at the temperature of 100 ℃, and carrying out heat treatment for 1 hour at the temperature of 700 ℃ to obtain the magnesia-silica coated silicon carbide particles.
Thirdly, mixing 85wt% of magnesia-silica coated silicon carbide particles, 5wt% of silicon carbide fine powder and 10wt% of light burned magnesium powder to obtain a second mixture, adding a polyvinyl alcohol solution accounting for 5wt% of the second mixture into the second mixture, and uniformly mixing; and then pressing and forming under the condition of 80MPa, and carrying out heat treatment on the pressed and formed green body for 2h at 800 ℃ and 2h at 1400 ℃ to obtain the silicon carbide-based ceramic heat accumulator.
In this embodiment:
NH in the ammonia water solution 3 ·H 2 The concentration of O is 25wt%;
the concentration of the polyvinyl alcohol solution is 10wt%;
the suction filtration is reduced pressure suction filtration, and the vacuum degree of the suction filtration is-0.09 MPa.
The silicon carbide-based ceramic heat accumulator prepared in the embodiment is detected by the following steps: bulk density of 3.06g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The thermal conductivity was 62.2W/(mK); the specific heat capacity is 1.56J/(g.K); the thermal shock stability is 22 times (1100 ℃ C., air cooling); the compressive strength is 98MPa; average thermal expansion coefficient (20-1000 ℃) of 4.8X10 -6 /℃。
Example 2
A silicon carbide-based ceramic heat accumulator and a preparation method thereof. The preparation method of the embodiment is as follows:
firstly, 48wt% of silicon carbide particles A with the granularity of 1-1.5 mm, 14wt% of silicon carbide particles B with the granularity of 0.5-1 mm and 38wt% of silicon carbide particles C with the granularity of 0.1-0.5 mm are mixed to obtain silicon carbide particles; placing the silicon carbide particles in silica sol, and soaking for 25min under the condition that the vacuum degree is-0.09 MPa to obtain soaked silicon carbide particles; and (3) drying the impregnated silicon carbide particles for 9 hours at the temperature of 100 ℃, and performing heat treatment for 3 hours at the temperature of 950 ℃ to obtain the nano silicon dioxide coated silicon carbide particles.
Secondly, mixing 84wt% of nano silicon dioxide coated silicon carbide particles and 16wt% of magnesium chloride to obtain a first mixture; adding 160wt% of deionized water to the first mixture, and stirring for 7min; adding ammonia water solution accounting for 12wt% of the first mixture into the first mixture, stirring for 25min, pouring into a sand core suction filtration device, and suction-filtering for 15min; placing the product obtained after suction filtration in a rotary evaporator, and rotating for 2 hours under the conditions that the water temperature is 65 ℃ and the rotating speed is 55 rad/min; and finally, drying for 9 hours at 105 ℃, and performing heat treatment for 2 hours at 750 ℃ to obtain the magnesia-silica coated silicon carbide particles.
Thirdly, mixing 87wt% of magnesia-silica coated silicon carbide particles, 4wt% of silicon carbide fine powder and 9wt% of light burned magnesium powder to obtain a second mixture, adding a polyvinyl alcohol solution accounting for 7wt% of the second mixture into the second mixture, and uniformly mixing; and then pressing and forming under the condition of 85MPa, and carrying out heat treatment on the pressed and formed green body at 900 ℃ for 3h and 1400 ℃ for 3h to obtain the silicon carbide-based ceramic heat accumulator.
In this embodiment:
NH in the ammonia water solution 3 ·H 2 The concentration of O is 26wt%;
the concentration of the polyvinyl alcohol solution is 9wt%;
the suction filtration is reduced pressure suction filtration, and the vacuum degree of the suction filtration is-0.09 MPa.
The silicon carbide-based ceramic heat accumulator prepared in the embodiment is detected by the following steps: bulk density of 3.13g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The thermal conductivity was 64.6W/(mK); the specific heat capacity was 1.51J/(g.K); the thermal shock stability is 23 times (1100 ℃ C., air cooling); the compressive strength is 94MPa; average thermal expansion coefficient (20-1000 ℃) of 4.7X10 -6 /℃。
Example 3
A silicon carbide-based ceramic heat accumulator and a preparation method thereof. The preparation method of the embodiment is as follows:
firstly, 50wt% of silicon carbide particles A with the granularity of 1-1.5 mm, 5wt% of silicon carbide particles B with the granularity of 0.5-1 mm and 45wt% of silicon carbide particles C with the granularity of 0.1-0.5 mm are mixed to obtain silicon carbide particles; placing the silicon carbide particles into silica sol, and soaking for 30min under the condition that the vacuum degree is-0.10 MPa to obtain soaked silicon carbide particles; and (3) drying the impregnated silicon carbide particles for 9 hours at the temperature of 110 ℃, and performing heat treatment for 4 hours at the temperature of 950 ℃ to obtain the nano silicon dioxide coated silicon carbide particles.
Secondly, mixing 86 weight percent of nano silicon dioxide coated silicon carbide particles with 14 weight percent of magnesium chloride to obtain a first mixture; adding deionized water accounting for 180wt% of the first mixture into the first mixture, and stirring for 9min; adding ammonia water solution accounting for 14wt% of the first mixture into the first mixture, stirring for 25min, pouring into a sand core suction filtration device, and performing suction filtration for 20min; placing the product obtained after suction filtration in a rotary evaporator, and rotating for 2 hours under the conditions that the water temperature is 70 ℃ and the rotating speed is 60 rad/min; and finally, drying for 9 hours at 105 ℃, and performing heat treatment for 2 hours at 800 ℃ to obtain the magnesia-silica coated silicon carbide particles.
Thirdly, mixing 88wt% of magnesia-silica coated silicon carbide particles, 4wt% of silicon carbide fine powder and 8wt% of light burned magnesium powder to obtain a second mixture, adding a polyvinyl alcohol solution accounting for 8wt% of the second mixture into the second mixture, and uniformly mixing; and then pressing and forming under the condition of 90MPa, and carrying out heat treatment on the pressed and formed green body at 1000 ℃ for 3h and 1500 ℃ for 3h to obtain the silicon carbide-based ceramic heat accumulator.
In this embodiment:
NH in the ammonia water solution 3 ·H 2 The concentration of O is 27wt%;
the concentration of the polyvinyl alcohol solution is 7wt%;
the suction filtration is reduced pressure suction filtration, and the vacuum degree of the suction filtration is-0.10 MPa.
The silicon carbide-based ceramic heat accumulator prepared in the embodiment is detected by the following steps: bulk density of 3.21g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The thermal conductivity was 66.1W/(mK); the specific heat capacity was 1.49J/(g.K); the thermal shock stability is 23 times (1100 ℃ C., air cooling); the compressive strength is 89MPa; average thermal expansion coefficient (20-1000 ℃) of 4.9X10 -6 /℃。
Example 4
A silicon carbide-based ceramic heat accumulator and a preparation method thereof. The preparation method of the embodiment is as follows:
firstly, 55wt% of silicon carbide particles A with the granularity of 1-1.5 mm, 10wt% of silicon carbide particles B with the granularity of 0.5-1 mm and 35wt% of silicon carbide particles C with the granularity of 0.1-0.5 mm are mixed to obtain silicon carbide particles; placing the silicon carbide particles into silica sol, and soaking for 40min under the condition that the vacuum degree is-0.10 MPa to obtain soaked silicon carbide particles; and (3) drying the impregnated silicon carbide particles for 10 hours at the temperature of 110 ℃, and performing heat treatment for 4 hours at the temperature of 1000 ℃ to obtain the nano silicon dioxide coated silicon carbide particles.
Secondly, mixing 90wt% of nano silicon dioxide coated silicon carbide particles with 10wt% of magnesium chloride to obtain a first mixture; adding deionized water accounting for 200wt% of the first mixture into the first mixture, and stirring for 10min; adding ammonia water solution accounting for 15wt% of the first mixture into the first mixture, stirring for 30min, pouring into a sand core suction filtration device, and suction-filtering for 20min; placing the product obtained after suction filtration in a rotary evaporator, and rotating for 3 hours under the conditions that the water temperature is 80 ℃ and the rotating speed is 70 rad/min; and finally, drying for 10 hours at 110 ℃, and performing heat treatment for 3 hours at 800 ℃ to obtain the magnesia-silica coated silicon carbide particles.
Thirdly, mixing 90wt% of magnesia-silica coated silicon carbide particles, 3wt% of silicon carbide fine powder and 7wt% of light burned magnesium powder to obtain a second mixture, adding 10wt% of polyvinyl alcohol solution in the second mixture, and uniformly mixing; and then pressing and forming under the condition of 100MPa, and carrying out heat treatment on the pressed and formed green body at 1000 ℃ for 4 hours and 1500 heat treatment for 4 hours to obtain the silicon carbide-based ceramic heat accumulator.
In this embodiment:
NH in the ammonia water solution 3 ·H 2 The concentration of O is 28wt%;
the concentration of the polyvinyl alcohol solution is 5wt%;
the suction filtration is reduced pressure suction filtration, and the vacuum degree of the suction filtration is-0.10 MPa.
The silicon carbide-based ceramic heat accumulator prepared in the embodiment is detected by the following steps: bulk density of 3.24g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The thermal conductivity was 67.9W/(mK); specific heat capacity of 1.46J/(g.K); the thermal shock stability is 25 times (1100 ℃ C., air cooling); the compressive strength is 87MPa; average thermal expansion coefficient (20-1000 ℃) of 4.5X10 -6 /℃。
Compared with the prior art, the specific embodiment has the following positive effects:
(1) The specific embodiment fully utilizes the characteristic of high heat capacity of the forsterite, and the silicon dioxide and the magnesium oxide are sequentially coated on the surfaces of the silicon carbide particles, and the forsterite is generated in situ by combining high-temperature heat treatment, so that the high heat storage capacity of the product is provided, and the silicon carbide-based ceramic heat storage body prepared by the specific embodiment has the characteristic of high heat storage capacity.
(2) The silicon carbide ceramic heat accumulator prepared by the specific embodiment has excellent heat conduction performance because the specific embodiment combines high heat conductivity of silicon carbide and excellent oxidation resistance and erosion resistance of forsterite, and the oxidation of the silicon carbide in the high-temperature use process is avoided by forming the forsterite around the silicon carbide particles and the fine powder in situ, so that the characteristic of high heat conductivity of the silicon carbide is maintained.
(3) On the basis of strictly limiting the grain composition of the raw materials, the preparation process and the limitation of the characteristics of the raw materials realize that the forsterite is formed in situ on the surfaces of the silicon carbide particles and is also formed in situ between the silicon carbide fine powder and the light burned magnesium powder, so that stable forsterite combination is formed between the raw material particles; and the characteristic of high thermal shock stability of the silicon carbide is fully utilized, so that the prepared silicon carbide-based ceramic heat accumulator has higher compressive strength and thermal shock stability.
The silicon carbide-based ceramic heat accumulator prepared by the specific embodiment is detected by: the volume density is more than or equal to 3.00g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The heat conductivity is more than or equal to 60W/(m.K); the specific heat capacity is more than or equal to 1.4J/(g.K); the thermal shock stability is more than or equal to 20 times (1100 ℃ C., air cooling); the compressive strength is 80-100 MPa; the thermal expansion coefficient (20-1000 ℃) is (4.5-5). Times.10 -6 /℃。
Test criteria for performance indicators according to the examples of this embodiment: bulk density is measured according to GB/T2999-2016; the thermal conductivity is measured according to the GB/T5990-2021 standard; specific heat capacity is measured according to GB/T5990-2021; the thermal shock stability is measured according to GB/T30873-2014; the compressive strength was measured according to GB/T5072-2008; the coefficient of thermal expansion was measured according to GB/T7320-2018.
Therefore, the silicon carbide-based ceramic heat accumulator prepared by the specific embodiment has high heat conductivity, high heat accumulation capacity, high thermal shock stability and high compressive strength.
Claims (10)
1. A preparation method of a silicon carbide-based ceramic heat accumulator is characterized by comprising the following steps:
firstly, mixing 45-55wt% of silicon carbide particles A with the granularity of 1-1.5 mm, 5-15wt% of silicon carbide particles B with the granularity of 0.5-1 mm and 35-45wt% of silicon carbide particles C with the granularity of 0.1-0.5 mm to obtain silicon carbide particles; placing the silicon carbide particles into silica sol, and soaking for 20-40 min under the vacuum degree of-0.08 to-0.10 MPa to obtain soaked silicon carbide particles; drying the impregnated silicon carbide particles for 8-10 hours at the temperature of 90-110 ℃, and performing heat treatment for 2-4 hours at the temperature of 900-1000 ℃ to obtain nano silicon dioxide coated silicon carbide particles;
step two, mixing 80 to 90 weight percent of nano silicon dioxide coated silicon carbide particles and 10 to 20 weight percent of magnesium chloride to obtain a first mixture; adding deionized water accounting for 150-200 wt% of the first mixture into the first mixture, and stirring for 5-10 min; adding ammonia water solution accounting for 10-15 wt% of the first mixture into the first mixture, stirring for 20-30 min, pouring into a sand core suction filtration device, and performing suction filtration for 10-20 min; placing the product obtained after suction filtration in a rotary evaporator, and rotating for 2-3 h under the conditions that the water temperature is 60-80 ℃ and the rotating speed is 50-70 rad/min; finally, drying for 8-10 h at 100-110 ℃, and performing heat treatment for 1-3 h at 700-800 ℃ to obtain magnesia-silica coated silicon carbide particles;
thirdly, mixing 85-90 wt% of magnesia-silica coated silicon carbide particles, 3-5 wt% of silicon carbide fine powder and 7-10 wt% of light burned magnesium powder to obtain a second mixture, adding a polyvinyl alcohol solution accounting for 5-10 wt% of the second mixture into the second mixture, and uniformly mixing; and then pressing and forming under the condition of 80-100 MPa, and performing heat treatment on the pressed and formed green body for 2-4 hours at 800-1000 ℃ and heat treatment on the pressed and formed green body for 2-4 hours at 1400-1500 ℃ to obtain the silicon carbide-based ceramic heat accumulator.
2. The method for producing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that the SiC content of the silicon carbide particles A, B and C is more than 97% by weight, fe 2 O 3 The content of (C) is less than 0.50wt%.
3. The method for producing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that the silica sol: siO (SiO) 2 More than 25.50wt%, na 2 The content of O is less than 0.35wt%, the pH is 8.5-9.5, and the average particle size of the colloidal particles is 8-25 nm.
4. The method for preparing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that MgCl in the magnesium chloride 2 ·6H 2 The purity of O is more than 98wt%.
5. The method for producing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that NH in the aqueous ammonia solution 3 ·H 2 The concentration of O is 25-28 wt%.
6. The method for producing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that the content of SiC in the silicon carbide fine powder is more than 97wt%, fe 2 O 3 The content of (2) is less than 0.50wt%; the granularity of the silicon carbide fine powder is less than 0.088mm.
7. The method for preparing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that the MgO content in the light burned magnesium powder is more than 97wt%, and the granularity of the light burned magnesium powder is less than 0.088mm.
8. The method for producing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that the concentration of the polyvinyl alcohol solution is 5 to 10wt%.
9. The method for preparing a silicon carbide-based ceramic heat accumulator according to claim 1, characterized in that the suction filtration is reduced pressure suction filtration, and the vacuum degree of the suction filtration is-0.09 to-0.10 MPa.
10. A silicon carbide-based ceramic heat accumulator characterized in that the silicon carbide-based ceramic heat accumulator is a silicon carbide-based ceramic heat accumulator produced by the production method of the silicon carbide-based ceramic heat accumulator according to any one of claims 1 to 9.
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