CN116283341A - Closed-cell foamed ceramic foamed at low temperature by utilizing SiC and preparation method thereof - Google Patents
Closed-cell foamed ceramic foamed at low temperature by utilizing SiC and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 94
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 66
- 238000005245 sintering Methods 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000006004 Quartz sand Substances 0.000 claims abstract description 23
- 229910021538 borax Inorganic materials 0.000 claims abstract description 23
- 238000005187 foaming Methods 0.000 claims abstract description 23
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 23
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 23
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052656 albite Inorganic materials 0.000 claims abstract description 17
- 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 abstract description 16
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 229910001863 barium hydroxide Inorganic materials 0.000 claims abstract description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 11
- 239000001038 titanium pigment Substances 0.000 claims abstract description 5
- 239000006260 foam Substances 0.000 claims description 45
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 11
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 239000004088 foaming agent Substances 0.000 description 8
- 239000011148 porous material Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
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- 238000007254 oxidation reaction Methods 0.000 description 3
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- 230000000694 effects Effects 0.000 description 2
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- 238000004321 preservation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
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- 239000010433 feldspar Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000010438 granite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000007800 oxidant agent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
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- 208000008864 scrapie Diseases 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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Abstract
The invention belongs to the technical field of ceramic materials, and particularly relates to a closed-cell foamed ceramic using SiC low-temperature foaming and a preparation method thereof, wherein the closed-cell foamed ceramic comprises the following raw materials: quartz sand, borax, talcum powder, albite, potassium feldspar, titanium white, barium hydroxide and Fe 2 O 3 SiC; the talcum powder, the albite, the potassium feldspar, the titanium pigment and the barium hydroxide form a mixture I, and the weight ratio of the talcum powder to the albite is 10:3 to 5:4 to 6:5 to 7: 8-10; the Fe is 2 O 3 With SiC to form a mixture II, fe 2 O 3 The weight ratio of the silicon carbide to the SiC is 12-14: 1, a step of; the quartz sand, the borax, the mixture I and the mixture II form a mixture III, and the weight ratio of the quartz sand to the borax to the mixture I to the mixture II is 100: 6-10: 9 to 11:5 to 7. The invention has the remarkable advantages of simple process and low sintering temperature.
Description
Technical Field
The invention relates to a closed-cell foamed ceramic using SiC low-temperature foaming and a preparation method thereof, belonging to the technical field of ceramic materials.
Background
The foamed ceramic is divided into 2 kinds of open cell type and closed cell type, the existing preparation method of the open cell foamed ceramic is many, the preparation process is mature, the product performance is stable, and the foamed ceramic is widely used in many traditional fields. The cells of the closed-cell foamed ceramic are independent and closed, so that the closed-cell foamed ceramic has excellent waterproof, dampproof, heat-insulating and heat-insulating properties and has wide application prospects in some high-end fields. Compared with the open-cell foam ceramic, the preparation process of the closed-cell foam ceramic has a great room for improvement, and the preparation of the closed-cell foam ceramic with high closed-cell rate, good mechanical property and uniform microstructure is still a difficult problem, which severely limits the application of the closed-cell foam ceramic.
High temperature foaming is the best method for preparing closed cell foam ceramics in the prior art, and most of the prior closed cell foam ceramics are prepared by adopting a high temperature foaming method. Summarizing research reports of preparing foamed ceramics by a high-temperature foaming method, common foaming agents are SiC and Si 3 N 4 、CaSO 4 、CaCO 3 、Na 2 CO 3 Etc. The existing foam ceramics are prepared by foaming agents with defects, such as CaSO 4 As a foaming agent, a large amount of harmful gas is generated, and the environment is seriously polluted; by CaCO 3 And Na (Na) 2 CO 3 As a foaming agent, the sintering temperature of the foamed ceramic is lower, generally in the range of 800-1000 ℃, but the strength of the product is lower; with SiC and Si 3 N 4 When used as a foaming agent, the foamed ceramic has better comprehensive performance, however, the sintering temperature is generally above 1000 ℃, and the manufacturing cost is higher.
SiC and Si 3 N 4 The foaming mechanism is the same, i.e. the gas generated by the oxidation reaction of both at high temperature is used to "blow up" a molten matrix of suitable viscosity and fluidity. According to the thermogravimetric curve of FIG. 1, si 3 N 4 Oxidation starts at 1000 c and SiC starts at 800 c. Because of the low initial oxidation temperature of SiC and moderate gas production rate in a wide temperature range of about 1000 ℃, and because the melting point of many material systems is just near 1000 ℃, compared with Si 3 N 4 The SiC serving as the foaming agent has the remarkable advantage of strong designability of a material system, and more reports are related.
Further, when the sintering temperature is lower than 950 ℃, the foamed ceramic prepared by SiC foaming generally has the problems of low foaming volume, low closed pore rate, uneven pore structure, poor mechanical property, unstable product performance and the like. Therefore, although lower sintering temperatures are advantageous for reducing manufacturing costs, in order to achieve the overall performance of the foamed ceramic, sintering temperatures of 1000 ℃ or higher are still common for the preparation of foamed ceramics by SiC foaming.
Disclosure of Invention
Aiming at the defects of higher high-temperature sintering cost and poor low-temperature sintering performance in the existing closed-cell foamed ceramic preparation process, the invention provides a closed-cell foamed ceramic foamed by utilizing SiC at a low temperature and a preparation method thereof.
The technical scheme for solving the technical problems is as follows:
a closed-cell foamed ceramic foamed by SiC at low temperature comprises the following raw materials:
quartz sand, borax, talcum powder, albite, potassium feldspar, titanium white, barium hydroxide and Fe 2 O 3 、SiC；
The talcum powder, the albite, the potassium feldspar, the titanium pigment and the barium hydroxide form a mixture I, wherein the weight ratio of the talcum powder, the albite, the potassium feldspar, the titanium pigment and the barium hydroxide in the mixture I is 10:3 to 5:4 to 6:5 to 7: 8-10;
the Fe is 2 O 3 And SiC, wherein in the mixture II, fe is contained in the mixture II 2 O 3 The weight ratio of the silicon carbide to the SiC is 12-14: 1, a step of;
the quartz sand, the borax, the mixture I and the mixture II form a mixture III, and in the mixture III, the weight ratio of the quartz sand to the borax to the mixture I to the mixture II is 100: 6-10: 9 to 11:5 to 7.
In the raw materials of the invention, quartz sand is a main material, borax is a fluxing agent, talcum powder, albite, potassium feldspar, titanium dioxide and barium hydroxide are viscosity regulators, and Fe 2 O 3 Is an oxidizing agent, and SiC is a foaming agent. The main functions of the raw materials are as follows: borax is added to reduce the melting temperature of the blankA degree; the contents of talcum powder, albite, potassium feldspar, titanium white and barium hydroxide are regulated, so that the blank body has proper melt viscosity at different temperatures to promote the molten matrix to form a uniform pore structure; regulating Fe 2 O 3 And the SiC content can adjust the foaming rate of the molten matrix and ultimately change the foaming volume of the ceramic foam.
Based on the technical scheme, the invention can also make the following improvements:
further, the sintering temperature is 830-940 ℃.
Further, the weight ratio of each raw material in the mixture II and the sintering temperature have the following corresponding relation:
fe in the mixture II when the sintering temperature is 880 ℃ to be less than or equal to 940 DEG C 2 O 3 The weight ratio of the silicon carbide to the SiC is 12-13: 1, a step of;
fe in mixture II at a sintering temperature of 880 DEG C 2 O 3 The optimal weight ratio to SiC is 13:1, a step of;
when the sintering temperature is more than or equal to 830 ℃ and less than 880 ℃, fe in the mixture II 2 O 3 The weight ratio of the silicon carbide to the SiC is 13-14: 1.
further, the weight ratio of each raw material in the mixture III and the sintering temperature have the following corresponding relation:
when the sintering temperature is 880 ℃ and is less than or equal to 940 ℃, the weight ratio of quartz sand, borax, mixture I and mixture II in the mixture III is 100: 6-8: 9-10: 5 to 6;
when the sintering temperature is 880 ℃, the optimal weight ratio of quartz sand, borax, mixture I and mixture II in the mixture III is 100:8:10:6, preparing a base material;
when the sintering temperature is more than or equal to 830 ℃ and less than 880 ℃, the weight ratio of quartz sand, borax, mixture I and mixture II in the mixture III is 100: 8-10: 10 to 11:6 to 7.
The invention also provides a preparation method of the closed-cell foamed ceramic using SiC low-temperature foaming, which comprises the following steps:
(1) Preparing mixed powder: sequentially mixing the raw materials, and grinding into mixed powder;
(2) Molding the mixed powder: molding the mixed powder obtained in the step (1) into a green body;
(3) Heating the blank obtained in the step (2) at a speed of 10-20 ℃/min, preserving heat for 30-60 min at 830-940 ℃, and then cooling to room temperature along with a furnace to obtain the closed-cell foamed ceramic.
Further, in the step (1), the prepared raw material is poured into a zirconia ball mill pot, and is milled by using a planetary ball mill.
Further, in the step (1), 20 to 25 zirconia balls with the diameter of 10 to 15mm are added per 100g of raw material.
Further, in the step (1), the particle size of the ground powder is less than 5 microns.
Further, in the step (2), the molding pressure is 4-6 MPa and the dwell time is 10-20 s.
The invention has the beneficial effects that:
(1) The preparation method has the remarkable advantages of simple process and low sintering temperature, and the manufacturing cost is far lower than that of the prior art because the sintering temperature is remarkably lower than that of the prior preparation process;
(2) The pores in the closed-pore foamed ceramic prepared by the invention are independent and not communicated with each other, and the surface is smooth and compact, so that the foamed ceramic has excellent heat preservation, sound insulation, water resistance and moisture resistance;
(3) The closed-cell foamed ceramic prepared by the invention has higher total porosity, closed-cell rate and compressive strength and excellent comprehensive performance.
Drawings
FIG. 1 is SiC and Si 3 N 4 A thermogravimetric plot in air;
FIG. 2 is a flow chart of the preparation of a closed cell foam ceramic using SiC low temperature foaming in accordance with the present invention;
FIG. 3 is a macroscopic photograph of a closed cell foam ceramic of example 1 of the present invention;
FIG. 4 is a photograph of a cross-section of a closed cell foam ceramic of example 1 of the present invention;
FIG. 5 is a photograph of the microstructure of the closed cell foam of example 1 of the present invention.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
In the specific embodiment, the raw materials used are all common commercial chemical reagents, and the specific conditions are as follows:
quartz sand: is selected from mountain-east Yantaixin mountain quartz sand factory, particle diameter is 1mm, silicon dioxide content is more than 98%, and impurities are mainly oxides of calcium, potassium, sodium and aluminum.
Borax: is selected from Henan Minmaite New Material technology Co., ltd, has a particle size of 20 μm and is industrially pure.
Talc powder: selected from Shandong KappaHonda Talcum powder, inc., 30 μm particle size, commercially pure.
Albite: is selected from Xingdong potassium sodium ore powder plant with particle size of 30 μm and industrial purity.
Potassium feldspar: is selected from Fuhua nanometer New materials limited company, the grain diameter is 50 mu m, and the industrial purity is realized.
Titanium white powder: selected from the company of Miou chemical reagent, inc. of Tianjin, the particle size of which is 30 μm, and is industrially pure.
Barium hydroxide: selected from the company of Miou chemical reagent, inc. of Tianjin, the particle size of which is 20 μm and analytically pure.
Fe 2 O 3 Powder: selected from the company of Miou chemical reagent, inc. of Tianjin, the particle size of which is 20 μm and analytically pure.
SiC powder: selected from Shandong Hua Yi Ind nano materials Co., ltd., particle size of 5 μm, analytical grade.
Example 1
1. Preparing closed-cell foamed ceramics foamed by SiC at low temperature:
the preparation flow of the closed-cell foamed ceramic foamed by SiC at low temperature in the embodiment is shown in fig. 2, and the preparation method comprises the following steps:
(1) Talcum powder, albite, potassium feldspar, titanium white powder and barium hydroxide are mixed according to the following ratio of 10:4:5:6:9, mixing the materials in a weight ratio to obtain a mixture I;
(2) Fe is added to 2 O 3 And SiC according to 13:1 to obtain a mixture II;
(3) Quartz sand, borax, mixture I and mixture II were mixed according to a ratio of 100:8:10:6, mixing in a weight ratio to obtain a mixture III;
(4) Pouring the mixture III into a zirconia ball milling tank, and grinding by using a planetary ball mill to obtain the mixture III with the particle size smaller than 5 microns;
(5) Pressing the ball-milled mixture III in the step (4) into a cylindrical blank with the diameter of 39mm and the height of 15mm, wherein the mould pressing pressure is 5MPa, and the pressure maintaining time is 15s;
(6) Heating the pressed green body to 880 ℃ at a speed of 15 ℃/min, preserving heat for 45min, and then cooling to room temperature along with a furnace to obtain the closed-cell foamed ceramic.
In the present invention, the dimensions of the green body pressed are merely used to exemplify the effects of the present invention, and are not intended to limit the scope of the present invention
2. The closed cell ceramic foam prepared above was subjected to performance testing.
Because the fully closed cell foam ceramic prepared by the invention cannot sink into water, the density and the porosity of the fully closed cell foam ceramic cannot be directly tested by adopting an Archimedes drainage method. The density and porosity of the present invention were tested using the indirect method in the paper "xenoming Li, mengyao Zheng, rui Li, guojian Yuan, guangyou Zhou, xenoao Zhu, guilna Ren, preparation, microstructure, properties and foaming mechanism of a foamed Ceramics with high closed porosity, ceramics international.2019,45 (5): 11982-11988.
First, a copper wire is wound around the sample so that the sample can be immersed in water, and the bulk density of the sample and the copper wire is calculated according to formula (1).
Wherein w is 1 And w 2 The weight of the sample and the weight of the copper wire can be directly measured; w (w) 1 ' and w 2 ' sample and copper wire saturated with water respectively in airThe weight of (2) can be directly measured; w (w) 1 "the float weight of the water-saturated sample in water can be directly measured; w (w) 2 "is the floating weight of copper wire in water, can directly measure; v 1 Unknown for the volume of the sample; v 2 The volume of the copper wire can be directly measured; calculating v according to formula (1) 1 And then calculating according to the formula (2) to obtain the density of the sample.
The overall open cell content of the sample and copper wire can be measured by calculation according to formula (3):
since the opening ratio of the copper wire is 0%, the opening ratio of the sample is further calculated according to the formula (4) on the basis of the formula (3).
Finally, the sample is ground into powder, and the volume v of the powder is measured by a measuring cylinder 3 After that, the total porosity of the sample was calculated according to formula (5).
The closed cell rate of the sample was calculated according to equation (6).
P c ＝P t -P o (6)
In the density and porosity testing process, the tested sample is placed in a beaker filled with water and boiled for 20 minutes to obtain a water-saturated sample.
In the compressive strength test, the test piece was processed into a cylindrical test piece having a height of 30mm and a diameter of 15mm, and the compressive strength test was performed by a uniaxial compression method.
The total porosity of the fully closed porous foam ceramic prepared in this example was 84%, the closed porosity was 81% and the density was 0.39g/cm, as measured in a room temperature environment 3 The compressive strength was 7.5MPa.
Example 2
1. Preparing closed-cell foamed ceramics foamed by SiC at low temperature:
the preparation flow of the closed-cell foamed ceramic foamed by SiC at low temperature in the embodiment is shown in fig. 2, and the preparation method comprises the following steps:
(1) Talcum powder, albite, potassium feldspar, titanium white powder and barium hydroxide are mixed according to the following ratio of 10:3:6:5:10 to obtain a mixture I;
(2) Fe is added to 2 O 3 And SiC according to 12:1 to obtain a mixture II;
(3) Quartz sand, borax, mixture I and mixture II were mixed according to a ratio of 100:6:9:5, mixing in a weight ratio to obtain a mixture III;
(4) Pouring the mixture III into a zirconia ball milling tank, and grinding by using a planetary ball mill to obtain the mixture III with the particle size smaller than 5 microns;
(5) Pressing the ball-milled mixture III in the step (4) into a cylindrical blank with the diameter of 39mm and the height of 15mm, wherein the mould pressing pressure is 5MPa, and the pressure maintaining time is 15s;
(6) Heating the pressed green body to 940 ℃ at the speed of 20 ℃/min, preserving heat for 30min, and then cooling to room temperature along with a furnace to obtain the closed-cell foamed ceramic.
2. The closed cell ceramic foam prepared above was subjected to performance testing.
The test method was the same as in example 1.
The total porosity of the fully closed porous foam ceramic prepared in this example was 85%, the closed porosity was 82% and the density was 0.38g/cm, as measured in a room temperature environment 3 The compressive strength was 7.2MPa.
Example 3
1. Preparing closed-cell foamed ceramics foamed by SiC at low temperature:
the preparation flow of the closed-cell foamed ceramic foamed by SiC at low temperature in the embodiment is shown in fig. 2, and the preparation method comprises the following steps:
(1) Talcum powder, albite, potassium feldspar, titanium white powder and barium hydroxide are mixed according to the following ratio of 10:5:4:7:8, mixing the materials in a weight ratio to obtain a mixture I;
(2) Fe is added to 2 O 3 And SiC according to 14:1 to obtain a mixture II;
(3) Quartz sand, borax, mixture I and mixture II were mixed according to a ratio of 100:10:11:7, mixing the materials in a weight ratio to obtain a mixture III;
(4) Pouring the mixture III into a zirconia ball milling tank, and grinding by using a planetary ball mill to obtain the mixture III with the particle size smaller than 5 microns;
(5) Pressing the ball-milled mixture III in the step (4) into a cylindrical blank with the diameter of 39mm and the height of 15mm, wherein the mould pressing pressure is 5MPa, and the pressure maintaining time is 15s;
(6) Heating the pressed green body to 830 ℃ at the speed of 10 ℃/min, preserving heat for 60min, and then cooling to room temperature along with a furnace to obtain the closed-cell foamed ceramic.
2. The closed cell ceramic foam prepared above was subjected to performance testing.
The test method was the same as in example 1.
The total porosity of the fully closed porous foam ceramic prepared in this example was 81%, the closed porosity was 79% and the density was 0.42g/cm, as measured in a room temperature environment 3 The compressive strength was 7.4MPa.
Example 4
1. Preparing closed-cell foamed ceramics foamed by SiC at low temperature:
the preparation flow of the closed-cell foamed ceramic foamed by SiC at low temperature in the embodiment is shown in fig. 2, and the preparation method comprises the following steps:
(1) Talcum powder, albite, potassium feldspar, titanium white powder and barium hydroxide are mixed according to the following ratio of 10:3:4:7:10 to obtain a mixture I;
(2) Fe is added to 2 O 3 And SiC according to 12.5:1 to obtain a mixture II;
(3) Quartz sand, borax, mixture I and mixture II were mixed according to a ratio of 100:7:9.5:5, mixing in a weight ratio to obtain a mixture III;
(4) Pouring the mixture III into a zirconia ball milling tank, and grinding by using a planetary ball mill to obtain the mixture III with the particle size smaller than 5 microns;
(5) Pressing the ball-milled mixture III in the step (4) into a cylindrical blank with the diameter of 39mm and the height of 15mm, wherein the mould pressing pressure is 5MPa, and the pressure maintaining time is 15s;
(6) Heating the pressed green body to 910 ℃ at a speed of 15 ℃/min, preserving heat for 45min, and then cooling to room temperature along with a furnace to obtain the closed-cell foamed ceramic.
2. The closed cell ceramic foam prepared above was subjected to performance testing.
The test method was the same as in example 1.
The total porosity of the fully closed porous foam ceramic prepared in this example was 81%, the closed porosity was 78% and the density was 0.43g/cm, as measured in a room temperature environment 3 The compressive strength was 7.6MPa.
Example 5
1. Preparing closed-cell foamed ceramics foamed by SiC at low temperature:
the preparation flow of the closed-cell foamed ceramic foamed by SiC at low temperature in the embodiment is shown in fig. 2, and the preparation method comprises the following steps:
(1) Talcum powder, albite, potassium feldspar, titanium white powder and barium hydroxide are mixed according to the following ratio of 10:5:6:5:8, mixing the materials in a weight ratio to obtain a mixture I;
(2) Fe is added to 2 O 3 And SiC according to 13.5:1 to obtain a mixture II;
(3) Quartz sand, borax, mixture I and mixture II were mixed according to a ratio of 100:9:10.5:6, mixing in a weight ratio to obtain a mixture III;
(4) Pouring the mixture III into a zirconia ball milling tank, and grinding by using a planetary ball mill to obtain the mixture III with the particle size smaller than 5 microns;
(5) Pressing the ball-milled mixture III in the step (4) into a cylindrical blank with the diameter of 39mm and the height of 15mm, wherein the mould pressing pressure is 5MPa, and the pressure maintaining time is 15s;
(6) Heating the pressed green body to 860 ℃ at a speed of 20 ℃/min, preserving heat for 60min, and then cooling to room temperature along with a furnace to obtain the closed-cell foamed ceramic.
2. The closed cell ceramic foam prepared above was subjected to performance testing.
The test method was the same as in example 1.
The total porosity of the fully closed porous foam ceramic prepared in this example was 82%, the closed porosity was 80% and the density was 0.40g/cm, as measured in a room temperature environment 3 The compressive strength was 7.1MPa.
FIG. 3 is a macroscopic photograph of the closed cell foam obtained in example 1. As shown in FIG. 3, the closed cell foam ceramic of example 1 had a smooth and dense shell, resembling an egg shell, with few defects.
FIG. 4 is a photograph of a cross-section of a closed cell foam obtained in example 1. As shown in fig. 4, the inside of the ceramic foam prepared in example 1 had a foam porous structure, and the sizes of the foam pores were uniform.
FIG. 5 is a photograph of the microstructure of the closed cell foam obtained in example 1. As shown in FIG. 5, the foam ceramic prepared in example 1 has independent and non-interconnected inner cells and excellent sealing performance.
According to the integral structure shown in fig. 3, 4 and 5, the closed-cell foamed ceramic prepared by the invention has the advantages of light weight, heat preservation and sound insulation, and simultaneously has excellent waterproof and moistureproof performances.
Table 1 shows the comparison of the sintering temperatures and performance parameters obtained by testing the performance of the ceramic foams prepared in examples 1 to 5 and those prepared by the prior art.
TABLE 1 sintering temperatures and Properties of the foam ceramics of examples 1 to 5 and the prior art
The prior art in table 1 is specifically derived from the following documents:
document 1: jiang Congcong, huang Shift, li Guozhong, et al Formation of closed-pore foam ceramic from granite scrapies International,2018,44:3469-3471.
Document 2: xia Fan, cui Shicai, pu Xipeng, performance study of foam ceramics prepared by direct foaming method using red mud and K-feldspar washed waste, ceramics International,2022,48:5197-5203.
Document 3: liang Jian, tang Zijuan, jiang Weihui, et al Effects of magnesite addition on the properties and structure of foam ceramics International 2021,47:18584-18591.
Document 4: liang Bin, zhang Mingxing, li Hao, et al, preparation of ceramic foams from ceramictile polishing waste and fly ash without added foaming agent.
Compared with the techniques described in documents 1 to 4, the preparation method of the present invention has the remarkable advantage of low sintering temperature, which can be as low as 830 ℃. In the aspect of comprehensive performance, the closed-cell rate of the closed-cell foamed ceramic prepared by the method is only 2-3% lower than the total porosity, and the closed-cell foamed ceramic still has relatively high compressive strength under the condition of higher total porosity.
The closed-cell ceramic foam prepared by the present invention has a total porosity and a closed-cell ratio comparable to those of the closed-cell ceramic foam described in document 1, but the closed-cell ceramic foam of the present invention has a higher compressive strength and a lower sintering temperature.
The closed cell ceramic foam of the present invention has compressive strength comparable to that of the closed cell ceramic foam described in document 4, but the closed cell ceramic foam of the present invention has a higher closed cell rate and a lower sintering temperature.
Compared with the closed-cell foamed ceramics disclosed in the documents 2 and 3, the closed-cell foamed ceramics prepared by the invention has more obvious advantages, has the technical advantage of low sintering temperature, and has the performance advantages of high total porosity, closed-cell rate and compressive strength.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (9)
1. The closed-cell foamed ceramic foamed by SiC at low temperature is characterized by being prepared from the following raw materials:
quartz sand, borax, talcum powder, albite, potassium feldspar, titanium white, barium hydroxide and Fe 2 O 3 、SiC；
The talcum powder, the albite, the potassium feldspar, the titanium pigment and the barium hydroxide form a mixture I, wherein the weight ratio of the talcum powder, the albite, the potassium feldspar, the titanium pigment and the barium hydroxide in the mixture I is 10:3 to 5:4 to 6:5 to 7: 8-10;
the Fe is 2 O 3 And SiC, wherein in the mixture II, fe is contained in the mixture II 2 O 3 The weight ratio of the silicon carbide to the SiC is 12-14: 1, a step of;
the quartz sand, the borax, the mixture I and the mixture I I form a mixture II, wherein the weight ratio of the quartz sand to the borax to the mixture II in the mixture II is 100: 6-10: 9 to 11:5 to 7.
2. The closed-cell foamed ceramic using SiC low-temperature foaming according to claim 1, characterized in that the sintering temperature thereof is 830 to 940 ℃.
3. The closed-cell foamed ceramic using SiC low-temperature foaming according to claim 2, wherein the weight ratio of each raw material in the mixture I I has the following correspondence with the sintering temperature:
fe in the mixture II when the sintering temperature is 880 ℃ to be less than or equal to 940 DEG C 2 O 3 The weight ratio of the silicon carbide to the SiC is 12-13: 1, a step of;
fe in mixture II at a sintering temperature of 880 DEG C 2 O 3 The weight ratio of the silicon carbide to SiC is 13:1, a step of;
when the sintering temperature is more than or equal to 830 ℃ and less than 880 ℃, fe in the mixture II 2 O 3 The weight ratio of the silicon carbide to the SiC is 13-14:1。
4. the closed-cell foamed ceramic using SiC low-temperature foaming according to claim 2, wherein the weight ratio of each raw material in the mixture ii has the following correspondence with the sintering temperature:
when the sintering temperature is 880 ℃ and is less than or equal to 940 ℃, the weight ratio of quartz sand, borax, mixture I and mixture II in the mixture III is 100: 6-8: 9-10: 5 to 6;
when the sintering temperature is 880 ℃, the weight ratio of quartz sand, borax, mixture I and mixture II in the mixture III is 100:8:10:6, preparing a base material;
when the sintering temperature is more than or equal to 830 ℃ and less than 880 ℃, the weight ratio of quartz sand, borax, mixture I and mixture II in the mixture III is 100: 8-10: 10 to 11:6 to 7.
5. A method for producing a closed-cell foamed ceramic using SiC low-temperature foaming according to any one of claims 1 to 4, comprising the steps of:
(1) Preparing mixed powder: sequentially mixing the raw materials, and grinding into mixed powder;
(2) Molding the mixed powder: molding the mixed powder obtained in the step (1) into a green body;
(3) Heating the blank obtained in the step (2) at a speed of 10-20 ℃/min, preserving heat for 30-60 min at 830-940 ℃, and then cooling to room temperature along with a furnace to obtain the closed-cell foamed ceramic.
6. The method for producing a closed-cell foam ceramic using SiC low-temperature foaming according to claim 5, wherein in said step (1), the prepared raw material is poured into a zirconia ball mill pot and milled using a planetary ball mill.
7. The method for producing a closed-cell foamed ceramic using SiC low-temperature foaming according to claim 5, wherein in said step (1), 20 to 25 zirconia balls having a diameter of 10 to 15mm are added per 100g of raw material.
8. The method for producing a closed-cell foamed ceramic using SiC low-temperature foaming according to claim 7, wherein in said step (1), the particle size of the ground powder is less than 5 μm.
9. The method for producing a closed-cell foamed ceramic using SiC low-temperature foaming according to claim 5, wherein in said step (2), the molding pressure is 4 to 6MPa and the dwell time is 10 to 20s.
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