CN116199503B - Al is added 2 O 3 -Si 3 N 4 Composite powder sliding plate brick, composite sliding plate brick and preparation method thereof - Google Patents
Al is added 2 O 3 -Si 3 N 4 Composite powder sliding plate brick, composite sliding plate brick and preparation method thereof Download PDFInfo
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- CN116199503B CN116199503B CN202310109189.7A CN202310109189A CN116199503B CN 116199503 B CN116199503 B CN 116199503B CN 202310109189 A CN202310109189 A CN 202310109189A CN 116199503 B CN116199503 B CN 116199503B
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- sliding plate
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- 239000000843 powder Substances 0.000 title claims abstract description 111
- 239000011449 brick Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 44
- 238000000465 moulding Methods 0.000 claims abstract description 37
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 238000000227 grinding Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000007731 hot pressing Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 38
- 238000001035 drying Methods 0.000 claims description 35
- 229910052751 metal Inorganic materials 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 32
- 229910052593 corundum Inorganic materials 0.000 claims description 27
- 239000010431 corundum Substances 0.000 claims description 27
- 229910001570 bauxite Inorganic materials 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 16
- 239000011863 silicon-based powder Substances 0.000 claims description 16
- 239000007767 bonding agent Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 13
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000005011 phenolic resin Substances 0.000 claims description 11
- 229920001568 phenolic resin Polymers 0.000 claims description 11
- 230000002829 reductive effect Effects 0.000 claims description 11
- 229920001187 thermosetting polymer Polymers 0.000 claims description 11
- 239000006229 carbon black Substances 0.000 claims description 9
- 229910052580 B4C Inorganic materials 0.000 claims description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 241000276425 Xiphophorus maculatus Species 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 4
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- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 230000003064 anti-oxidating effect Effects 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- 238000012858 packaging process Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 11
- 238000007254 oxidation reaction Methods 0.000 abstract description 11
- 230000035939 shock Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000011819 refractory material Substances 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 17
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- 239000010410 layer Substances 0.000 description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 7
- 229910003564 SiAlON Inorganic materials 0.000 description 6
- 239000002274 desiccant Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000007580 dry-mixing Methods 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
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- 238000005265 energy consumption Methods 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 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
- 230000000670 limiting effect Effects 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
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- 229910052710 silicon Inorganic materials 0.000 description 2
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical group [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- -1 SiC Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
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- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- XUIMIQQOPSSXEZ-AKLPVKDBSA-N silicon-31 atom Chemical compound [31Si] XUIMIQQOPSSXEZ-AKLPVKDBSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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- 238000005507 spraying Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D41/00—Casting melt-holding vessels, e.g. ladles, tundishes, cups or the like
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- B22D41/32—Manufacturing or repairing thereof characterised by the materials used therefor
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- C21C5/28—Manufacture of steel in the converter
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Abstract
The invention discloses an Al-added alloy 2 O 3 ‑Si 3 N 4 Composite powder sliding plate brick, composite sliding plate brick and their preparation process belong to the field of refractory material technology. The synthetic sliding plate brick comprises a molding body I and a molding body II, wherein the molding body II is sleeved outside the molding body I. The molding body I is added with Al 2 O 3 ‑Si 3 N 4 The composite powder sliding plate brick is prepared from granular aggregate and co-grinding powder, wherein the co-grinding powder comprises 8% -15% of Al 2 O 3 ‑Si 3 N 4 And (5) compounding powder. The Al is 2 O 3 ‑Si 3 N 4 The composite powder is prepared from Al 2 O 3 And Si (Si) 3 N 4 The composite powder obtained by hot-pressing sintering in air is used as a raw material, and the prepared sliding plate brick has high sintering strength and density, high fracture toughness, thermal shock resistance and oxidation resistance.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and in particular relates to an additive Al 2 O 3 -Si 3 N 4 Composite powder sliding plate brick, composite sliding plate brick and their preparation process.
Background
At present, most of sliding plate bricks used for converters and steel ladles in the market are formed in one step, all materials adopted for sliding plates with long service life are high in material cost, and most of sliding plates are low in strength and density at the positions of a parent station in the forming process, so that reaming and erosion speeds of the sliding plates are too high in the using process, quality stability and service life of sliding plate products are affected, and in addition, requirements on product strength and compactness at cast holes and slide rail positions, particularly cast holes and anti-slip areas, are high.
By searching, sialon is a solid solution formed by Si source and Al source in the prior art, and is often applied to ceramic products for improving fracture toughness, for example, patent CN113149663A discloses a Sialon ceramic with high fracture toughness, a preparation method and application thereof, and a main crystal phase of the Sialon ceramic is alpha-Sialon or a composite phase of alpha-Sialon and beta-Sialon. The preparation method comprises the following steps: mixing isopropanol, polyethylene glycol and powder, stirring, ball milling, spraying and granulating to obtain Sialon-Ti granulating balls; heating the Sialon-Ti granulating ball to 550-650 ℃ under vacuum condition for degreasing, and briquetting to obtain a green body; placing the green blanks in a pressureless furnace under the nitrogen atmosphere to presintered at 1200 ℃ to fully nitridize the green blanks, and then cooling the green blanks along with the furnace; the obtained presintered body is sintered and insulated in nitrogen atmosphere, and the sintering mode is air pressure sintering and furnace cooling to obtain Sialon ceramic. However, the ceramic material has low sintering temperature, low volume density and high porosity, and thus has low oxidation resistance and slag erosion resistance. Patent CN102718496A discloses an Al with beta-Sialon as a transition layer 2 O 3 -Si 3 N 4 A preparation method of gradient material. By beta-Sialon powder and Al 2 O 3 Powder, si 3 N 4 Powder and Y 2 O 3 Preparing mixed powder of each monolayer by taking powder as a raw material, grinding each monolayer mixed powder in an agate mortar respectively, stacking the ground powder layer by layer in a mould to form an original gradient stack body of 10-20 layers by using a powder stacking method, pressing and forming by using 15-25 MPa pressure, and then preserving heat for 3-5 hours in a pneumatic sintering furnace under the conditions of 4-6 MPa nitrogen pressure and 1600-1800 ℃ sintering temperature to obtain the Al taking beta-Sialon as a transition layer 2 O 3 -Si 3 N 4 A gradient material; the purity of the beta-Sialon powder is Z=3 and is more than 97%, al 2 O 3 Powder, si 3 N 4 Powder and Y 2 O 3 The powder has the purity of more than chemical purity and the granularity of 800 nm-1000 nm. The method has the defects that the nitriding sintering temperature is too low, covalent compounds are difficult to sinter together, and in addition, the nitriding sintering needs to be carried out in a nitriding furnace, so that the production cost is high.
In addition, yan Chaofan [ beta-Sialon combined with structural optimization and reinforcement mechanism of aluminum-carbon refractory, yan Chaofan, university of martial arts, doctor's treatise on science and technology, 2020 ] utilizes metallic Al powder and elemental Si powder to study the generation of beta-Sialon in aluminum-carbon refractory and its influence on material properties, and explores the growth factors of beta-Sialon in aluminum-carbon refractory including (calcination temperature, nitrogen partial pressure, holding time, silicon to aluminum ratio) and its effect on mechanical properties of aluminum-carbon refractory. However, it uses metallic Al powder and elemental Si powder as raw materials, and the above reaction needs to be carried out under nitrogen atmosphere and is easily affected by sintering temperature, and in addition, if hot press sintering is not adopted, it is difficult to sinter covalent compounds together, affecting the sintering property of the material.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems that the existing sliding plate is too fast in reaming and erosion speed due to low strength and density of the sliding plate, and the quality stability and the service life of the sliding plate product are affected, the invention provides an Al-added sliding plate 2 O 3 -Si 3 N 4 Composite powder sliding plate brick and sliding plate made of sameThe brick has high sintering strength and density.
The invention further aims to provide the synthetic sliding plate brick comprising the sliding plate brick and a preparation method thereof, and the prepared synthetic sliding plate brick has high product quality stability and long service life.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the invention is as follows:
al is added 2 O 3 -Si 3 N 4 The utility model provides a composite powder's slide brick, includes cover shell, shaping body I and shaping body II, shaping body II cover is established in shaping body I outside, shaping body II is the cavity form, and it is equipped with the through-hole that is used for the cover to establish shaping body I, and shaping body I is inlayed by the binder and is formed integrated into one piece in shaping body II, the cover shell cover is established in shaping body II outsides.
The addition of Al 2 O 3 -Si 3 N 4 The sliding plate brick of the composite powder, the said shaping body I is shaped on 1500 tons of presses, have improved volume density and intensity of the cast hole department; the molding body II is molded on a 1500 ton press, a non-burning process is adopted, the production process and the energy consumption are reduced, and the molding body II and the energy consumption are bonded by an adhesive to form an integral sliding plate after being inspected to be qualified, so that the density and the strength of a cast hole are enhanced. And the forming body I and the forming body II are filled in the gap by an adhesive for bonding. Preferably, the adhesive is chrome corundum fire clay taking solid water glass as a bonding agent.
Wherein the raw materials of the forming body I comprise plate-shaped corundum particles, silicon carbide and co-milled powder, and the raw materials are as follows in percentage by weight: 47-65% of plate-shaped corundum particles, 3-5% of silicon carbide, 31-48% of co-milled powder, and 100% of total percentage; 4 to 5.5 percent of thermosetting phenolic resin binder is added. Wherein the co-grinding powder consists of 8 to 15 percent of Al 2 O 3 -Si 3 N 4 Composite powder, 5-13% of platy corundum micropowder and 8-12% of alpha-Al 2 O 3 Mixing the micro powder, 2 to 4 percent of metal aluminum powder, 1 to 3 percent of boron carbide fine powder, 1 to 3 percent of carbon black and 1 to 3 percent of metal silicon powderIs prepared by the method; the forming body II comprises, by weight, a granular aggregate and a co-grinding powder, wherein the granular aggregate comprises 30% of 80D bauxite particles with the weight of 5-3 mm, 17% of 80D bauxite particles with the weight of 3-1 mm and 18% of 80D bauxite particles with the weight of 1-0 mm, the co-grinding powder comprises 32% of 80D bauxite fine powder with the weight of less than or equal to 0.075mm, 1% of 325-mesh metal aluminum powder, 2% of 325-mesh metal silicon powder, 100% of total weight, and 4% -5% of an additional bonding agent, and the bonding agent is a thermosetting phenolic resin bonding agent.
Wherein the Al is 2 O 3 -Si 3 N 4 The composite powder is prepared from Al 2 O 3 (. Ltoreq.45 μm) and Si 3 N 4 (. Ltoreq.75 μm) as raw material, hot-pressing sintering in air to obtain composite powder, al 2 O 3 And Si (Si) 3 N 4 The mass ratio of (55-65): (35 to 45), preferably 60:40, al is mixed with 2 O 3 And Si (Si) 3 N 4 Hot-pressing and sintering for 3-5 h in air at the temperature of between 1650 and 1750 ℃ under the pressure of 30MPa to form Al 2 O 3 -Si 3 N 4 The particle size of the composite powder is 500 meshes; preferably, the Al 2 O 3 -Si 3 N 4 In the composite powder: al (Al) 2 O 3 The content of Si is more than or equal to 66.69 percent 3 N 4 The content of (2) is more than or equal to 32.13 percent. To improve sintering performance, sintering aids such as rare earth oxides such as Y may also be added 2 O 3 、Re 2 O 3 The addition amount of the sintering aid is 2-6%. During sintering, a part of Si 3 N 4 And Al 2 O 3 The SiAlON phase is generated by the reaction, and the generated SiAlON small particles are dispersed and distributed in Al 2 O 3 The grain boundary of the particles generates a nanocrystallization effect, and meanwhile, the fracture of the material is changed from the crystal fracture to the crystal-penetrating fracture, so that the mechanical property of the material is greatly improved; part of Si 3 N 4 First of all oxidized SiO 2 Protective film for preventing O 2 When the oxygen partial pressure in the sample is reduced to meet the active oxidation condition, si 3 N 4 Oxidation to form SiO, and SiO diffusion to the surface layer to re-oxidize to form SiO 2 ，SiO 2 Further reaction of corundum and silicon nitride in Al 2 O 3 The mullite and X phase are generated on the surface to form a compact layer, so that the thermal shock stability and oxidation resistance of the material are improved; in addition, a part of Si remains 3 N 4 Remain at Al 2 O 3 And the surface is continuously oxidized in the subsequent use, so that the oxidation resistance of the material is improved. Thus, in reasonable Al 2 O 3 And Si (Si) 3 N 4 Under the proportion of (2), the improvement of the material performance is realized.
In addition, the invention uses Al 2 O 3 And Si (Si) 3 N 4 The hexagonal columnar beta-SiAlON matrix is generated as a raw material, and the hexagonal columnar beta-SiAlON matrix and the strip corundum phase form a cross-woven structure, so that the corrosion resistance and the thermal shock stability of the product are improved, the slag blocking performance and the service life of the sliding plate are improved, and the average temperature is improved to 26 furnaces.
The addition of Al 2 O 3 -Si 3 N 4 In the composite powder sliding plate brick, the particle size of the plate-shaped corundum particles is (2-1, 1-0.5 and 0.5-0) mm, the particle size of the plate-shaped corundum micro powder is 325 meshes, and the weight percentages of the particle sizes are as follows: 20-28% of plate-shaped corundum particles with the particle size of 2-1 mm, 13-18% of plate-shaped corundum particles with the particle size of 1-0.5 mm, 14-19% of plate-shaped corundum particles with the particle size of 0.5-0 mm and 5-13% of plate-shaped corundum micro powder with the particle size of 325 mm; the chemical components and the contents of the plate-shaped corundum particles and the plate-shaped corundum micro powder are as follows: al (Al) 2 O 3 Is 99.07% of NaO 2 The content of (3) is 0.31%, the content of CaO is 0.08%, fe 2 O 3 The content of (2) is 0.06%, the content of MgO is 0.18%, siO 2 The content of (2) was 0.1%.
Preferably, the alpha-Al 2 O 3 The grain diameter of the micro powder is 0-2 mu m, and the alpha-Al 2 O 3 The micro powder comprises the following components: al (Al) 2 O 3 The content of SiO is more than or equal to 99.0 percent 2 The content of Fe is less than or equal to 0.1 percent 2 O 3 The content of Na is less than or equal to 0.08 percent 2 O+K 2 The content of O is less than or equal to 0.3 percent.
Preferably, the particle size of the metal aluminum powder is 0-0.075 mm, and the weight percentage of the particle size is 2% -4%; the metal aluminum powder comprises the following components: 99.5% of Al, 0.18% of Fe, 0.2% of Si and 0.1% of Cu.
Preferably, in the carbon black: the fixed carbon content is more than or equal to 99%, the volatile content is less than or equal to 0.5%, the ash content is less than or equal to 0.5%, the moisture content is less than or equal to 0.5%, and the average particle size of the carbon black is 20nm.
Preferably, the boron carbide particle size is 325 mesh.
The forming body II comprises the following raw materials in percentage by weight: 30% of 80D high bauxite particles with the diameter of 5-3 mm, 17% of 80D high bauxite particles with the diameter of 3-1 mm, 18% of 80D high bauxite particles with the diameter of 1-0 mm, 32% of 80D high bauxite fine powder with the diameter of less than or equal to 0.075mm, 1% of 325-mesh metal aluminum powder and 2% of 325-mesh metal silicon powder.
Another object of the present invention is to provide a method of adding Al 2 O 3 -Si 3 N 4 The preparation method of the composite powder sliding plate brick comprises the following steps:
step S1, preparing a molded body I
S1.1, proportioning: the material is prepared according to the weight percentage of the raw materials of the molding body I: 47% -65% of plate-shaped corundum particles, 3% -5% of 97 silicon carbide, 31% -48% of co-milled powder, and the total percentage is 100%; 4 to 5.5 percent of external binding agent, wherein the co-grinding powder comprises 8 to 15 percent of Al 2 O 3 -Si 3 N 4 Composite powder, 5-13% of platy corundum micropowder and 8-12% of alpha-Al 2 O 3 The powder comprises, by weight, 2% -4% of metal aluminum powder, 1% -3% of boron carbide fine powder, 1% -3% of carbon black and 1% -3% of metal silicon powder, wherein the bonding agent is a thermosetting phenolic resin bonding agent;
s1.2, premixing and co-grinding: 8 to 15 percent of Al is mixed by a V-shaped mixer 2 O 3 -Si 3 N 4 Composite powder, 5-13% of platy corundum micropowder and 8-12% of alpha-Al 2 O 3 Premixing the micro powder, 2-4% of metal aluminum powder, 1-3% of boron carbide fine powder, 1-3% of carbon black and 1-3% of metal silicon powder for at least 30min;
s1.3, mixing and grinding: dry-mixing 60% -71% of plate-shaped corundum particles and 3% -5% of silicon carbide for 3-5 minutes by a wet mill, then slowly adding a thermosetting phenolic resin binder, finally adding co-milled powder, and mixing for 35-40 minutes to obtain a mixture;
s1.4, mechanically pressing and forming: pressing and molding the mixture on a 1500t electric spiral brick press to obtain a molded body I;
s1.5, drying: naturally airing the green body for 8 hours, putting the green body into a tunnel natural gas drying kiln, drying according to a set curve, wherein the initial kiln feeding temperature is 30 ℃, raising the temperature from 30 ℃ to 80 ℃ within 4 hours, and preserving heat for 1 hour; raising the temperature from 80 ℃ to 120 ℃ within 4 hours, and preserving the heat for 1 hour; raising the temperature from 120 ℃ to 150 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 150 ℃ to 180 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 180 ℃ to 210 ℃ within 3 hours, and preserving the heat for 16 hours; the total drying time was 37 hours; checking the products after kiln discharge, and selecting the products with qualified sizes and appearances to enter the next working procedure;
s1.6, medium temperature treatment: and (3) kiln-loading the dried qualified products, wherein the green bricks are laterally loaded in a built sagger, sealed by a stainless steel cover, and after kiln car loading, the green bricks are fed into a medium-temperature tunnel kiln for sintering, wherein the sintering atmosphere is an oxidizing atmosphere, the sintering maximum temperature is 600 ℃, and the specific sintering process curve is as follows: heating from room temperature to 200 ℃ within 9 hours; heating from 200deg.C to 300deg.C within 12 hours, heating from 300deg.C to 400deg.C within 12 hours, heating from 600deg.C within 10 hours, and maintaining at 600deg.C for 15 hours; stopping fire and airing the kiln; the kiln temperature is reduced to 300 ℃, and the kiln door handle is loosened; the kiln temperature is reduced to 200 ℃, and a kiln door is opened for natural cooling; cooling the kiln to 100 ℃ and discharging the kiln car; when the kiln is taken out, the kiln is taken out and put down lightly, and the qualified products after inspection can enter the next working procedure.
S1.7, checking to obtain a product molding body I;
step S2: preparation of shaped body II
S2.1, batching: the raw materials of the forming body II are prepared according to the weight percentage: 30% of 80D high bauxite with the thickness of 5-3 mm, 17% of 80D high bauxite with the thickness of 3-1 mm, 18% of 80D high bauxite with the thickness of 1-0 mm, 32% of 80D high bauxite fine powder with the thickness of less than or equal to 0.075mm, 1% of 325-mesh metal aluminum powder and 2% of 325-mesh metal silicon powder;
s2.2, premixing powder: premixing powder, which comprises 32% of 80D high bauxite fine powder less than or equal to 0.075mm, 1% of 325 mesh metal aluminum powder and 2% of 325 mesh metal silicon powder, by a mixer mill for not less than 30min;
s2.3, mixing and grinding: dry-mixing the granular aggregate for 3-5 minutes by a wet mill, slowly adding the thermosetting phenolic resin binder, finally adding the co-milled powder, and mixing for 35-40 minutes to obtain a mixture;
s2.4, mechanically pressing and forming: pressing and molding the mixture on a 1500t electric spiral brick press to obtain a molded body II;
s2.5, drying: naturally airing the green body for 8 hours, putting the green body into a tunnel natural gas drying kiln, drying according to a set curve, wherein the initial kiln feeding temperature is 30 ℃, raising the temperature from 30 ℃ to 80 ℃ within 4 hours, and preserving heat for 1 hour; raising the temperature from 80 ℃ to 120 ℃ within 4 hours, and preserving the heat for 1 hour; raising the temperature from 120 ℃ to 150 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 150 ℃ to 180 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 180 ℃ to 210 ℃ within 3 hours, and preserving the heat for 16 hours; the total drying time was 37 hours; checking the products after kiln discharge, and selecting the products with qualified sizes and appearances to enter the next working procedure;
s2.6, checking to obtain a molded body II;
step S3, mosaic: embedding the molding body I into the molding body II by using an adhesive, and airing for more than 24 hours;
step S4, hooping: polishing and flattening the welding seam of the iron hoop, wherein the position of the hoop is positioned in the middle of the sliding plate, the welding seam of the iron hoop is not more than 1mm, and the gap between the iron hoop and the semi-finished sliding plate is not more than 1mm;
step S5, a shell is arranged: sleeving the shell on the outer side of the molding body II, and then putting the molding body II into a drying kiln for drying, wherein the total drying time is not less than 24 hours;
step S6, grinding: grinding on a numerical control vertical shaft round table plane grinding machine, controlling the cutter feeding amount to be 2mm/min and controlling the multiplying power to be 60-80%; the flatness of the working surface of the polished slide plate is less than or equal to 0.05mm, and the parallelism is less than or equal to 0.5mm; immediately drying in a continuous infrared drying kiln after grinding, wherein the drying temperature is 220 ℃, and entering a coating and packaging procedure after inspection;
step S7, coating: coating an oxidation-resistant coating on the dried sliding plate working surface, wherein the coating is uniform and smooth; wherein the antioxidation coating can be an emulsion coating containing carbon-containing compounds, such as SiC, B 4 C。
Step S8, packaging: naturally airing the coated brick body for 24 hours, inspecting and packing after the temperature of the brick body is reduced to room temperature, enlarging a plastic bag at the bottom of the box, placing a drying agent in the box, putting a layer of drying agent after each layer of drying agent is packed, and fastening the large plastic bag by a tying rope after the filling is finished.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) The sliding plate brick of the invention is based on the existing aluminum carbon sliding plate brick, and Al is added in 2 O 3 -Si 3 N 4 The composite powder is matched with reasonable proportion, si is added in the sintering process 3 N 4 With Al 2 O 3 The SiAlON phase is generated by the reaction, so that the sintering and the density improvement of the material are promoted, and the bending strength and the fracture toughness are improved; si (Si) 3 N 4 Oxidation to form SiO 2 ，SiO 2 Further reaction of corundum and silicon nitride in Al 2 O 3 Surface-grown mullite and X-phase (Si 12 Al 18 O 39 N 8 ) A compact layer is formed, so that the thermal shock stability and oxidation resistance of the material are improved; remainder of Si 3 N 4 Remain at Al 2 O 3 The surface of the material is improved in oxidation resistance, and the prepared sliding plate brick is high in quality stability and long in service life;
(2) The sliding plate brick of the invention is added with Al 2 O 3 -Si 3 N 4 The composite powder body generates the beta-SiAlON matrix which exists in a hexagonal column shape and forms a cross knitting structure with the strip corundum phase, thereby being beneficial to improving the erosion resistance and the thermal shock stability of the product, improving the slag blocking performance and the service life of the sliding plate and averagely improving the slag blocking performance to 26 furnaces;
(3) The invention adopts a split molding mode to independently mold the molding body I contacted with molten steel, thereby playing a role in strengthening the density and strength of the molding body I, and in addition, the molding body II is not directly contacted with molten steel and is manufactured by adopting a low-grade material and a non-burning process, thereby reducing the production steps and energy consumption and greatly reducing the production cost.
Drawings
The technical solution of the present invention will be described in further detail below with reference to the accompanying drawings and examples, but it should be understood that these drawings are designed for the purpose of illustration only and thus are not limiting the scope of the present invention. Moreover, unless specifically indicated otherwise, the drawings are intended to conceptually illustrate the structural configurations described herein and are not necessarily drawn to scale.
FIG. 1 is a view of the Al of the present invention 2 O 3 -Si 3 N 4 A cross-sectional view of the composite powder sliding plate brick;
FIG. 2 is a drawing showing the microstructure of a sliding plate brick according to example 1 of the present invention;
in the figure: 1. forming a body I; 2. forming a body II; 3. the casing.
Detailed Description
The following detailed description of exemplary embodiments of the invention refers to the accompanying drawings, which form a part hereof, and in which are shown by way of illustration exemplary embodiments in which the invention may be practiced. While these exemplary embodiments are described in sufficient detail to enable those skilled in the art to practice the invention, it is to be understood that other embodiments may be realized and that various changes to the invention may be made without departing from the spirit and scope of the invention. The following more detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely illustrative and not limiting of the invention's features and characteristics in order to set forth the best mode of carrying out the invention and to sufficiently enable those skilled in the art to practice the invention. Accordingly, the scope of the invention is limited only by the attached claims.
The following detailed description and example embodiments of the invention may be better understood when read in conjunction with the accompanying drawings, in which elements and features of the invention are identified by reference numerals.
As shown in FIG. 1, the present invention adds Al 2 O 3 -Si 3 N 4 The utility model provides a composite powder's slide brick, includes cover shell 3, shaping body I1 and is hollow form shaping body II 2, shaping body I1 is inlayed by solid sodium silicate binder and is formed integrated into one piece structure in shaping body II 2, and the cover shell suit is in shaping body II 2 outsides, and wherein the raw materials of shaping body I1 are as follows according to the weight percent ratio: 47% -65% of plate-shaped corundum particles, 3% -5% of 97 silicon carbide, 31% -48% of co-milled powder, and the total percentage is 100%; 4 to 5.5 percent of thermosetting phenolic resin binder is added. Wherein the co-grinding powder consists of 8 to 15 percent of Al 2 O 3 -Si 3 N 4 Composite powder, 5-13% of platy corundum micropowder and 8-12% of alpha-Al 2 O 3 The powder is prepared by mixing micro powder, 2 to 4 percent of metal aluminum powder, 1 to 3 percent of boron carbide fine powder, 1 to 3 percent of carbon black and 1 to 3 percent of metal silicon powder; the raw materials of the forming body II 2 are as follows in percentage by weight: 30% of 80D high bauxite with the thickness of 5-3 mm, 17% of 80D high bauxite with the thickness of 3-1 mm, 18% of 80D high bauxite with the thickness of 1-0 mm, 32% of 80D high bauxite fine powder with the thickness of less than or equal to 0.075mm, 1% of 325-mesh metal aluminum powder and 2% of 325-mesh metal silicon powder.
Wherein Table 1 shows the Al of each embodiment of the present invention 2 O 3 -Si 3 N 4 The preparation process parameters of the composite powder are shown in Table 2, and the raw material compositions (wt%) of the molded body I in each example of the present invention are shown.
TABLE 1 inventive examples Al 2 O 3 -Si 3 N 4 Preparation process parameters of composite powder
TABLE 2 composition of raw materials (wt%) for molded body I according to each example of the present invention
Example 1
Example 1 provides a method for preparing a synthetic sliding plate brick, which comprises the following steps:
step S1, preparing a molded body I1
S1.1, proportioning: the material is prepared according to the weight percentage of the raw materials of the molding body I1: 70% of plate-shaped corundum particles, 4% of 97 silicon carbide and 31% of co-milled powder, wherein the total percentage is 100%; 4 to 5.5 percent of thermosetting phenolic resin binder is added. Wherein the co-milled powder consists of 10% Al 2 O 3 -Si 3 N 4 Composite powder, 5% plate-shaped corundum micropowder and 8% alpha-Al 2 O 3 Micropowder, 3% of metal aluminum powder, 1% of boron carbide fine powder, 2% of carbon black and 2% of metal silicon powder;
s1.2, premixing powder: 10% of Al was mixed with a V-shaped mixer 2 O 3 -Si 3 N 4 Composite powder, 5% plate-shaped corundum micropowder and 8% alpha-Al 2 O 3 Premixing the micro powder, 3% of metal aluminum powder, 1% of boron carbide fine powder, 2% of carbon black and 2% of metal silicon powder for at least 30min;
s1.3, mixing and grinding: dry-mixing the granular aggregate for 3-5 minutes by a wet mill, slowly adding the thermosetting phenolic resin binder, finally adding the co-milled powder, and mixing for 35-40 minutes to obtain a mixture;
s1.4, mechanically pressing and forming: pressing and molding the mixture on a 1500t electric spiral brick press to obtain a molded body I1;
s1.5, drying: naturally airing the green body for 8 hours, putting the green body into a tunnel natural gas drying kiln, drying according to a set curve, wherein the initial kiln feeding temperature is 30 ℃, raising the temperature from 30 ℃ to 80 ℃ within 4 hours, and preserving heat for 1 hour; raising the temperature from 80 ℃ to 120 ℃ within 4 hours, and preserving the heat for 1 hour; raising the temperature from 120 ℃ to 150 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 150 ℃ to 180 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 180 ℃ to 210 ℃ within 3 hours, and preserving the heat for 16 hours; the total drying time was 37 hours; checking the products after kiln discharge, and selecting the products with qualified sizes and appearances to enter the next working procedure;
s1.6, medium temperature treatment: and (3) kiln-loading the dried qualified products, wherein the green bricks are laterally loaded in a built sagger, sealed by a stainless steel cover, and after kiln car loading, the green bricks are fed into a medium-temperature tunnel kiln for sintering, wherein the sintering atmosphere is an oxidizing atmosphere, the sintering maximum temperature is 600 ℃, and the specific sintering process curve is as follows: heating from room temperature to 200 ℃ in 9 hours, heating from 200 ℃ to 300 ℃ in 12 hours, heating from 300 ℃ to 400 ℃ in 12 hours, heating from 400 ℃ to 600 ℃ in 10 hours, and preserving heat for 15 hours at 600 ℃ and the total firing time is 58 hours; stopping fire and airing the kiln; the kiln temperature is reduced to 300 ℃, and the kiln door handle is loosened; the kiln temperature is reduced to 200 ℃, and a kiln door is opened for natural cooling; cooling the kiln to 100 ℃ and discharging the kiln car; when the kiln is taken out, the kiln is taken out and put down lightly, and the inspected qualified product can enter the next working procedure;
s1.7, checking to obtain a molded body I1;
step S2, preparing a molded body II 2
S2.1, batching: the raw materials of the forming body II 2 are prepared according to the weight percentage: 30% of 80D high bauxite with the thickness of 5-3 mm, 17% of 80D high bauxite with the thickness of 3-1 mm, 18% of 80D high bauxite with the thickness of 1-0 mm, 32% of 80D high bauxite fine powder with the thickness of less than or equal to 0.075mm, 1% of 325-mesh metal aluminum powder and 2% of 325-mesh metal silicon powder;
s2.2, premixing powder: premixing 32% of 80D high bauxite fine powder less than or equal to 0.075mm, 1% of 325 mesh metal aluminum powder and 2% of 325 mesh metal silicon powder by using a mixing mill for not less than 30min;
s2.3, mixing and grinding: dry-mixing the granular aggregate for 3-5 minutes by a wet mill, slowly adding the thermosetting phenolic resin binder, finally adding the co-milled powder, and mixing for 35-40 minutes to obtain a mixture;
s2.4, mechanically pressing and forming: pressing and molding the mixture on a 1500t electric spiral brick press to obtain a molded body II 2;
s2.5, drying: naturally airing the green body for 8 hours, putting the green body into a tunnel natural gas drying kiln, drying according to a set curve, wherein the initial kiln feeding temperature is 30 ℃, raising the temperature from 30 ℃ to 80 ℃ within 4 hours, and preserving heat for 1 hour; raising the temperature from 80 ℃ to 120 ℃ within 4 hours, and preserving the heat for 1 hour; raising the temperature from 120 ℃ to 150 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 150 ℃ to 180 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 180 ℃ to 210 ℃ within 3 hours, and preserving the heat for 16 hours; the total drying time was 37 hours; checking the products after kiln discharge, and selecting the products with qualified sizes and appearances to enter the next working procedure;
s2.6, checking to obtain a molded body II 2;
step S3, mosaic: embedding the molding body I1 into the molding body II 2 by using an adhesive, and airing for more than 24 hours;
step S4, hooping: polishing and flattening the welding seam of the iron hoop, wherein the position of the hoop is positioned in the middle of the sliding plate, the welding seam of the iron hoop is not more than 1mm, and the gap between the iron hoop and the semi-finished sliding plate is not more than 1mm;
step S5, a shell is arranged: sleeving the shell 3 on the outer side of the forming body II 2, and then putting the shell into a drying kiln for drying, wherein the total drying time is not less than 24 hours;
step S6, grinding: grinding on a numerical control vertical shaft round table plane grinding machine, controlling the cutter feeding amount to be 2mm/min and controlling the multiplying power to be 60-80%; the flatness of the working surface of the polished slide plate is less than or equal to 0.05mm, and the parallelism is less than or equal to 0.5mm; immediately drying in a continuous infrared drying kiln after grinding, wherein the drying temperature is 220 ℃, and entering a coating and packaging procedure after inspection;
step S7, coating: coating an oxidation-resistant coating on the dried sliding plate working surface, wherein the coating is uniform and smooth;
step S8, packaging: naturally airing the coated brick body for 24 hours, inspecting and packing after the temperature of the brick body is reduced to room temperature, enlarging a plastic bag at the bottom of the box, placing a drying agent in the box, putting a layer of drying agent after each layer of drying agent is packed, and fastening the large plastic bag by a tying rope after the filling is finished.
The surface of the obtained sliding plate brick is shown in figure 2, and the bending strength and the fracture toughness are high.
Example 2
The embodiment adds Al 2 O 3 -Si 3 N 4 The composition and weight percentage of the composite powder sliding plate brick and the composite sliding plate brick are as shown in the formula in table 1, and the preparation method is the same as that of example 1.
Example 3
The embodiment adds Al 2 O 3 -Si 3 N 4 The composition and weight percentage of the composite powder sliding plate brick and the composite sliding plate brick are as shown in the formula in table 1, and the preparation method is the same as that of example 1.
Example 4
The embodiment adds Al 2 O 3 -Si 3 N 4 The composition and weight percentage of the composite powder sliding plate brick and the composite sliding plate brick are as shown in the formula in table 1, and the preparation method is the same as that of example 1.
Claims (7)
1. Al is added 2 O 3 -Si 3 N 4 The composite powder sliding plate brick comprises 31-48% of granular aggregate and 100% of co-grinding powder, and is characterized in that the co-grinding powder comprises 8-15% of Al 2 O 3 -Si 3 N 4 Composite powder of Al 2 O 3 -Si 3 N 4 The composite powder is made of Al 2 O 3 And Si (Si) 3 N 4 Hot-press sintering in air under the condition of Al 2 O 3 And Si (Si) 3 N 4 Hot-pressing sintering for 3-5 h at the temperature of between 1650 and 1750 ℃ under the pressure of 30MPa, wherein the Al is 2 O 3 And Si (Si) 3 N 4 The ratio of (5-65): (35-45);
the co-grinding powder also comprises 5 to 13 percent of platy corundum micro powder and 8 to 12 percent of alpha-Al 2 O 3 Micro powder, 2-4% of metal aluminum powder, 1-3% of boron carbide fine powder, 1-3% of carbon black and 1-3% of metal silicon powder;
the particle aggregate comprises 47% -65% of plate-shaped corundum particles and 3% -5% of silicon carbide.
2. The added Al of claim 1 2 O 3 -Si 3 N 4 The composite powder sliding plate brick is characterized by further comprising a bonding agent, wherein the bonding agent is a thermosetting phenolic resin bonding agent, and the mass of the bonding agent is particle aggregate and particle aggregate4 to 5.5 percent of the total mass of the co-milled powder.
3. Comprising the additive Al according to any one of claims 1-2 2 O 3 -Si 3 N 4 The composite powder sliding plate brick is characterized by comprising a molding body I (1) and a molding body II (2), wherein the molding body II (2) is sleeved outside the molding body I (1) and fixedly connected with the molding body I (1), and the molding body I (1) is added with Al 2 O 3 -Si 3 N 4 Composite powder sliding plate brick.
4. The synthetic sliding plate brick according to claim 3, wherein the raw materials of the molding body II (2) comprise granular aggregate and a co-grinding powder, the granular aggregate comprises, by weight, 30% of 80D bauxite particles with the weight percentage of 5-3 mm, 17% of 80D bauxite particles with the weight percentage of 3-1 mm, 18% of 80D bauxite particles with the weight percentage of 1-0 mm, the co-grinding powder comprises 32% of 80D bauxite fine powder with the weight percentage of less than or equal to 0.075mm, 1% of 325 mesh metal aluminum powder, 2% of 325 mesh metal silicon powder, 100% of total, and 4% -5% of an additional bonding agent, and the bonding agent is a thermosetting phenolic resin bonding agent.
5. The composite sliding tile according to claim 4, further comprising a casing (3), the casing (3) being arranged outside the shaped body ii (2).
6. A method for preparing a synthetic sliding tile according to any one of claims 3 to 5, comprising the steps of:
step S1, preparing a molded body I (1)
S1.1, proportioning: proportioning according to the weight percentage of the raw materials of the molding body I (1);
s1.2, premixing and co-grinding: premixing the co-milled powder;
s1.3, mixing and grinding: uniformly mixing the granular aggregate, slowly adding a bonding agent, finally adding co-milled powder, and uniformly mixing to obtain a mixture;
s1.4, mechanically pressing and forming: pressing and molding the mixture to obtain a molded body I (1);
s1.5, drying: naturally airing the green body, and drying;
s1.6, medium temperature treatment: kiln filling the dried qualified products, and sintering in a medium-temperature tunnel kiln;
s1.7, checking: checking to obtain a molded body I (1);
step S2, preparing a molded body II (2)
S2.1, batching: the raw materials of the forming body II (2) are mixed according to the weight percentage;
s2.2, premixing powder: premixing the co-milled powder;
s2.3, mixing and grinding: uniformly mixing the granular aggregate, slowly adding a binding agent, finally adding co-milled powder, and uniformly mixing to obtain a mixture;
s2.4, mechanically pressing and forming: pressing and molding the mixture to obtain a molded body II (2);
s2.5, drying: naturally airing the green body, and drying;
s2.6, checking: obtaining a molded body II (2) after inspection;
step S3: and (3) mosaic: embedding the molding body I (1) into the molding body II (2) by using an adhesive, and airing;
step S4: hooping: polishing and flattening the welding seam of the iron hoop, wherein the hoop-polishing position is positioned in the middle of the sliding plate;
step S5: the shell is as follows: sleeving the shell on the outer side of the molding body II (2), and drying in a drying kiln;
step S6: grinding: grinding, drying in a continuous infrared drying kiln, and checking to be qualified to enter a coating and packaging process;
step S7: and (3) coating: coating an anti-oxidation coating on the dried sliding plate working surface;
step S8: and (3) packaging: naturally airing the coated bricks, and starting boxing after the temperature of the bricks is reduced to room temperature.
7. The method for producing synthetic sliding bricks according to claim 6, wherein,
in the step S1.5, the initial kiln feeding temperature is 30 ℃, the temperature is increased from 30 ℃ to 80 ℃ within 4 hours, and the temperature is kept for 1 hour; raising the temperature from 80 ℃ to 120 ℃ within 4 hours, and preserving the heat for 1 hour; raising the temperature from 120 ℃ to 150 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 150 ℃ to 180 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 180 ℃ to 210 ℃ within 3 hours, and preserving the heat for 16 hours; the total drying time was 37 hours; checking the products after kiln discharge, and selecting the products with qualified sizes and appearances to enter the next working procedure;
in the step S1.6, the sintering atmosphere is an oxidizing atmosphere, the sintering highest temperature is 600 ℃, and the specific sintering process curve is as follows: heating from room temperature to 200 ℃ in 9 hours, heating from 200 ℃ to 300 ℃ in 12 hours, heating from 300 ℃ to 400 ℃ in 12 hours, heating from 400 ℃ to 600 ℃ in 10 hours, and preserving heat for 15 hours at 600 ℃ and the total firing time is 58 hours; stopping fire and airing the kiln; the kiln temperature is reduced to 300 ℃, and the kiln door handle is loosened; the kiln temperature is reduced to 200 ℃, and a kiln door is opened for natural cooling; cooling the kiln to 100 ℃ and discharging the kiln car; the inspected qualified product can enter the next working procedure;
in the step S2.5, the initial kiln feeding temperature is 30 ℃, the temperature is increased from 30 ℃ to 80 ℃ within 4 hours, and the temperature is kept for 1 hour; raising the temperature from 80 ℃ to 120 ℃ within 4 hours, and preserving the heat for 1 hour; raising the temperature from 120 ℃ to 150 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 150 ℃ to 180 ℃ within 3 hours, and preserving the heat for 1 hour; raising the temperature from 180 ℃ to 210 ℃ within 3 hours, and preserving the heat for 16 hours; the total drying time was 37 hours; and after the kiln is taken out, checking the products, and selecting the products with qualified size and appearance to enter the next working procedure.
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