CN114014674A - Technological method for preparing SiC-C plate by adopting hot press molding process - Google Patents
Technological method for preparing SiC-C plate by adopting hot press molding process Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000465 moulding Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007767 bonding agent Substances 0.000 claims abstract description 12
- 238000007731 hot pressing Methods 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000032683 aging Effects 0.000 claims abstract description 4
- 239000012467 final product Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000011819 refractory material Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000010720 hydraulic oil Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 230000003628 erosive effect Effects 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 230000035939 shock Effects 0.000 claims description 4
- 230000002411 adverse Effects 0.000 claims description 2
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 2
- 239000008157 edible vegetable oil Substances 0.000 claims description 2
- 239000010687 lubricating oil Substances 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000005245 sintering Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000000748 compression moulding Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910016384 Al4C3 Inorganic materials 0.000 description 1
- 240000008415 Lactuca sativa Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 235000012045 salad Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/74—Ceramic products containing macroscopic reinforcing agents containing shaped metallic materials
- C04B35/76—Fibres, filaments, whiskers, platelets, or the like
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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Abstract
The invention relates to a preparation method of a SiC-C refractory plate. The disclosed technological method for preparing SiC-C plate by adopting hot press molding process, the SiC-C plate takes silicon carbide and carbon as main raw materials; fixing the basic shape and the basic structure of the material by adopting a normal-temperature temporary bonding agent; aluminum-based fibers are also added into the raw materials of the SiC-C plate; the process method comprises the steps of fully and uniformly mixing the raw materials in an edge runner mill and ageing the mixture; molding at normal temperature in a hot-press molding machine at the molding pressure of 30-80 MPa; then the hot-pressing equipment enters an Ar atmosphere protection and temperature rise control program; controlling the temperature when the temperature of the hot-pressing equipment rises to 650-750 ℃; then secondary pressure molding is carried out, and the molding pressure is 5-30 MPa; finally, cooling together with hot-pressing equipment to obtain a final product; the process overcomes the defects of the traditional high-temperature sintering process, eliminates the energy consumption procedure of high-temperature sintering and greatly reduces the production cost.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a process method for preparing a SiC-C plate by adopting a hot press molding process.
Background
The SiC-C plate has various excellent performances of high temperature resistance, erosion resistance, good thermal shock resistance and the like, and can be used in various high-temperature smelting furnaces and thermal equipment; the prefabricated part is usually made by adopting a casting process, but because the porosity is relatively high, a friction press or hydraulic equipment is more adopted, the prefabricated part is pressed into a fixed shape under a certain pressure condition, and a final product is obtained after high-temperature heat treatment; in the preparation process, each treatment program is independent; the improvement of the material performance after pressing completely depends on the thermal firing system to influence the material performance; in order to improve the high-temperature performance of the SiC-C refractory material, a certain protective atmosphere is required to prevent the oxidation of SiC and C raw materials during heat treatment, and the bonding strength of the material can be improved only by sintering at a higher temperature (generally more than 1400 ℃) for a long time.
In order to overcome the defects of the current preparation process, the high-temperature performance of the refractory material is improved, the heat treatment and the forming process are combined to realize the medium-low temperature hot pressing preparation of the SiC-C plate, so that various performances and using effects of the refractory material can be guaranteed, the high-temperature sintering process can be omitted, and the production cost of the refractory material is greatly reduced.
Disclosure of Invention
Aiming at the technical problems, the invention overcomes the defects of the prior art and provides a process method for preparing a SiC-C plate by adopting a hot press molding process.
The invention adopts the following technical scheme for achieving the purpose:
a technological method for preparing SiC-C board by adopting a hot-press forming process, the SiC-C board takes silicon carbide and carbon as main raw materials, and the material is ensured to have higher refractoriness, wear resistance, erosion resistance and thermal shock resistance; the basic shape and the basic structure of the material are fixed by the normal-temperature temporary bonding agent, and the components of the normal-temperature temporary bonding agent can be almost burnt at a low temperature of not more than 300 ℃, so that the high-temperature performance of the refractory material cannot be adversely affected; the raw material of the SiC-C plate is also added with aluminum-based fiber; the preparation method comprises mixing the raw materials in an edge runner mill, and ageing; molding at normal temperature in a hot-press molding machine at the molding pressure of 30-80 MPa; then the hot-pressing equipment enters an Ar atmosphere protection and temperature rise control program; when the temperature of the hot-pressing equipment rises to 650-750 ℃, controlling the temperature, wherein the heat preservation time is not less than 30 min; then secondary pressure molding is carried out, and the molding pressure is 5-30 MPa; finally, cooling together with hot-pressing equipment to obtain a final product; the aluminum-based fiber is in a molten or semi-molten state within the range of 650-750 ℃ by means of low-melting-point aluminum element, and has good metal plasticity; under the pressure condition of hot-pressing equipment, the liquid phase or semi-liquid phase enters the interior of the refractory material, so that the function of filling air holes can be achieved, the porosity of the material is reduced, surrounding materials can be more tightly linked together, and the direct bonding force of the material is increased.
The SiC-C plate comprises the following raw materials in percentage by weight: 1-10% of 3-1mm silicon carbide; 35-45% of 1-0mm silicon carbide; 200-40% of 325-mesh silicon carbide; silicon carbide of more than 800 meshes, 5-10%; 1-5% of graphite and 10-20% of aluminum-based fiber; the total weight of all the raw materials is 100 percent, and 3 to 5 percent of normal temperature temporary bonding agent is additionally added.
The silicon carbide comprises silicon carbide particles and silicon carbide fine powder; the silicon carbide particles and the silicon carbide fine powder are any one of industrial or natural silicon carbide, and the SiC content is more than 90 percent.
The graphite is any one of natural graphite or artificial graphite, the granularity of the graphite is less than 100 meshes, and the C content is more than 90%.
The aluminum-based fiber is any one of metal aluminum-based fibers with the Al content of more than 95%.
The normal-temperature temporary bonding agent is any one of hydraulic oil, lubricating oil or edible oil.
The invention provides a process method for preparing a SiC-C plate by adopting a hot press molding process; silicon carbide and carbon are used as main raw materials, so that the material is guaranteed to have high refractoriness, wear resistance, erosion resistance and thermal shock resistance; hydraulic oil and the like are used as a normal-temperature temporary bonding agent to fix the basic shape and the basic structure of the material, and the components of the material can be almost completely burnt at a lower temperature (generally not more than 300 ℃), so that the high-temperature performance of the refractory material cannot be affected.
The aluminum-based fiber is added in the invention, the low melting point (660 ℃) aluminum element is in a molten or semi-molten state within the range of 650-750 ℃, and the aluminum-based fiber has better metal plasticity; under a certain pressure condition, the liquid phase or the semi-liquid phase enters the interior of the refractory material, so that the function of filling gas holes can be achieved, and the porosity of the material is reduced; more importantly, surrounding materials can be linked together more closely, and the direct bonding force of the materials is increased. Meanwhile, the metal fibers have small granularity (the transverse size is in the micron order), high toughness and easy dispersion in refractory materials, are beneficial to improving the uniformity of the materials and increasing the fracture toughness of the refractory materials. Meanwhile, part of the aluminum-based liquid can also react with graphitic carbon to form microcrystalline aluminum carbide Al4C3The bonding strength of the material is further improved, and the effect of optimizing the structure and the performance of the material is achieved.
In summary, the invention has the following advantages:
(1) the invention adopts the hot press molding process to prepare the SiC-C plate, eliminates the energy consumption procedure that the traditional silicon carbide refractory material needs to be sintered at high temperature, and has simple manufacturing flow and greatly reduced production cost.
(2) The invention realizes the secondary compression molding of the material by utilizing the plastic state of the aluminum-based element at a certain temperature, not only does not damage the compression shape and the material structure at normal temperature, but also further strengthens the tissue structure of the material by utilizing the filling performance, increases the density of the material and improves the bonding strength of the material.
(3) The invention adopts secondary forming, can reduce the process control requirement of primary forming, reduce the time length of material trapping and further simplify the manufacturing process of materials.
(4) The raw materials and the temporary bonding agent adopted by the invention belong to environment-friendly raw materials, and almost no polluting gas is formed in the preparation process, so that the preparation method conforms to the national environmental protection policy and industry regulations.
Detailed Description
The invention is illustrated by the examples given, but is not to be construed as being in any way limited thereto. The aggregate is firstly put into an edge runner mill and is mixed and ground for 5 min, and then the bonding agent of about 1/3 is slowly added along a certain direction and is mixed and ground for 3-5 min. And then, adding all the base materials premixed by the powerful stirrer into an edge runner mill, mixing and grinding for 8-10 min, finally slowly adding the rest of the binding agent, continuously mixing and grinding for about 20 min, and discharging. The ageing mixture can be treated after 6 hours.
Example 1: 95 silicon carbide is used as particles and fine powder, wherein the addition proportion of the particles is 5 percent, 40 percent, 32 percent and 10 percent in turn for 3-1mm, 1-0mm, 200 meshes and 325 meshes and 800 meshes; 3% of graphite and 10% of aluminum fiber; +3.5% of hydraulic oil (added). The molding pressure at normal temperature is 50MPa, the heat preservation time is 0.5h after the temperature is raised to 670 ℃, and then the compression molding is carried out at 15 MPa.
The performance indexes are as follows: the volume weight is 2.63-2.65 g/cm 3; the compressive strength is 50-55 MPa.
Example 2: 90 silicon carbide is taken as particles and fine powder, wherein the addition proportion of the particles is 10 percent, 35 percent, 30 percent and 5 percent in turn for 3-1mm, 1-0mm, 200 meshes and 325 meshes and 1000 meshes; graphite, 1%, aluminum fiber, 20%; plus 5% of hydraulic oil (additionally added). The molding pressure at normal temperature is 40MPa, the heat preservation time is 1h after the temperature is raised to 670 ℃, and then the compression molding is carried out at 20 MPa.
The performance indexes are as follows: 3 with the bulk density of 2.60-2.63 g/cm; the compressive strength is 45-50 MPa.
Example 3: 95 silicon carbide is used as particles and fine powder, wherein the addition proportion of the particles is 2 percent, 42 percent, 34 percent and 6 percent in turn for 3-1mm, 1-0mm, 200 meshes and 325 meshes and 800 meshes; 4% of graphite, 12% of aluminum fiber; salad oil (additional) + 4%. The molding pressure at normal temperature is 60MPa, the heat preservation time is 0.5h after the temperature is raised to 700 ℃, and then the compression molding is carried out at 10 MPa.
The performance indexes are as follows: the bulk density is 2.65-2.67 g/cm 3; the compressive strength is 55-60 MPa.
Claims (6)
1. A technological method for preparing a SiC-C plate by adopting a hot press molding process is characterized by comprising the following steps: the SiC-C plate takes silicon carbide and carbon as main raw materials, so that the material is guaranteed to have high refractoriness, wear resistance, erosion resistance and thermal shock resistance; the basic shape and the basic structure of the material are fixed by the normal-temperature temporary bonding agent, and the components of the normal-temperature temporary bonding agent can be almost burnt at a low temperature of not more than 300 ℃, so that the high-temperature performance of the refractory material cannot be adversely affected; the raw material of the SiC-C plate is also added with aluminum-based fiber; the process method comprises the steps of fully and uniformly mixing the raw materials in an edge runner mill and ageing the mixture; molding at normal temperature in a hot-press molding machine at the molding pressure of 30-80 MPa; then the hot-pressing equipment enters an Ar atmosphere protection and temperature rise control program; when the temperature of the hot-pressing equipment rises to 650-750 ℃, controlling the temperature, wherein the heat preservation time is not less than 30 min; then secondary pressure molding is carried out, and the molding pressure is 5-30 MPa; finally, cooling together with hot-pressing equipment to obtain a final product; the aluminum-based fiber is in a molten or semi-molten state within the range of 650-750 ℃ by means of low-melting-point aluminum element, and has good metal plasticity; under the pressure condition of hot-pressing equipment, the liquid phase or semi-liquid phase enters the interior of the refractory material, so that the function of filling air holes can be achieved, the porosity of the material is reduced, surrounding materials can be more tightly linked together, and the direct bonding force of the material is increased.
2. The process for preparing a SiC-C plate by the hot press forming process according to claim 1, wherein: the SiC-C plate comprises the following raw materials in percentage by weight: 1-10% of 3-1mm silicon carbide; 35-45% of 1-0mm silicon carbide; 200-40% of 325-mesh silicon carbide; silicon carbide of more than 800 meshes, 5-10%; 1-5% of graphite and 10-20% of aluminum-based fiber; the total weight of all the raw materials is 100 percent, and 3 to 5 percent of normal temperature temporary bonding agent is additionally added.
3. The process for preparing a SiC-C plate by the hot press forming process according to claim 1, wherein: the silicon carbide comprises silicon carbide particles and silicon carbide fine powder; the silicon carbide particles and the silicon carbide fine powder are any one of industrial or natural silicon carbide, and the SiC content is more than 90 percent.
4. The process for preparing a SiC-C plate by the hot press forming process according to claim 1, wherein: the graphite is any one of natural graphite or artificial graphite, the granularity of the graphite is less than 100 meshes, and the C content is more than 90%.
5. The process for preparing a SiC-C plate by the hot press forming process according to claim 1, wherein: the aluminum-based fiber is any one of metal aluminum-based fibers with the Al content of more than 95%.
6. The process for preparing a SiC-C plate by the hot press forming process according to claim 1, wherein: the normal temperature temporary bonding agent is any one of hydraulic oil, lubricating oil or edible oil.
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