CN103553647B - Method for preparation of silicon nitride bonded silicon carbide refractory material by using silicon cutting waste mortar - Google Patents
Method for preparation of silicon nitride bonded silicon carbide refractory material by using silicon cutting waste mortar Download PDFInfo
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Abstract
The invention discloses a method for preparation of silicon nitride bonded silicon carbide refractory material by using silicon cutting waste mortar, and the method comprises the following steps: (1), preparing raw materials, wherein the raw materials including, by weight, 5%-20% of the silicon cutting waste mortar, 50%-80% of silicon carbide, 2%-20% of silicon nitride and 1%-10% of alumina; (2), adding the raw materials into absolute ethanol for wet ball milling; (3), drying the raw materials treated by the wet ball milling; (4), adding PVA (polyvinyl acetate) to the dried raw materials for granulation to prepare blank, wherein the mass of the added PVA being 3%-8% of the mass of the raw materials; and (5), sintering the blank in air atmosphere into the silicon nitride bonded silicon carbide refractory material. The method can realize full utilization of the silicon cutting waste mortar, has no secondary pollution, also does not need the protection of nitrogen, and only needs an electric furnace for heating in the air atmosphere to prepare the low-volume-density and high-flexure-strength silicon nitride bonded silicon carbide refractory material, and can reduce environment pressure, turn waste into treasure, reduce the production cost and realize industrialized production.
Description
Technical field
The present invention relates to a kind of silicon cutting waste mortar recoverying and utilizing method, particularly relate to a kind of method utilizing silicon cutting waste mortar to prepare refractory materials.
Background technology
Along with a large amount of consumption of Nonrenewable energy resources utilize, global energy growing tension, sun power then becomes the most important new forms of energy of the mankind gradually as the permanent energy, and solar photovoltaic industry is developed rapidly in the whole world.When preparing solar cell, need elemental silicon body to cut into satisfactory silicon chip, current crystal silicon mainly adopts multi-wire saw technology to complete.Generally, the cutting waste slurry that cutting machine produces every year is up to ton up to a hundred, and along with China's solar photovoltaic industry fast development, the cutting waste material of generation is also increasing sharply, and brings immense pressure not only to enterprise and environment, also result in the significant wastage of resource.For this reason, the recycling of silicon cutting waste mortar is just being subject to increasing attention.
The main component of silicon cutting waste mortar is silicon carbide micro-powder, crystalline silicon and polyoxyethylene glycol, mainly takes solid-liquid separation to obtain solid silicon carbide/silicon mixture and liquid polyethylene glycol at present.The recycling of polyoxyethylene glycol achieves industrialization.And solid mixt silicon carbide/silicon due to physics, chemical property comparatively close, not easily separated, existing method is difficult to the separation realizing silica flour.Method conventional at present removes the pure silicon in silicon cutting waste material by pickling alkali cleaning and reclaims silicon carbide micro-powder again as the prepared using of Linear cut, not only cost recovery is high but also waste the higher HIGH-PURITY SILICON resource of economic worth for this, and whole removal process can produce collodial silica sodium sewage new in a large number, causes secondary pollution.
Silicon nitride combined with silicon carbide refractory material is for the silicon carbide high grade refractory in conjunction with phase with silicon nitride, many excellent properties of silicon nitride and carbofrax material are acted on, there is a series of premium propertiess such as the strong and high temperature abrasion resistance of the solution erosional competencyes such as hot strength is high, thermal conductivity is large, linear expansivity is little, good thermal shock, alkali attack are good, good in oxidation resistance, anti-zinc-aluminium copper-lead is good, produce at ferrous metallurgy, obtain widespread use in aluminium cell and the production of pottery kiln refractory slab etc.
The method of a kind of microwave technology Fast Sintering silicon nitride combined with silicon carbide refractory material disclosed in No. 200410009794.4th, Chinese patent application, it utilizes microwave to the rapid and uniform heating principle of material and microwave field to the facilitation effect of nitrogenizing reaction, the silicon carbide mixed is become blank with a small amount of organic binder bond by pressure forming with silica flour, through drying and pre-skimming treatment, in a nitrogen atmosphere, utilize frequency be 900 ~ 3000 megahertzes industrial microwave source produce microwave blank is heated to 1100 ~ 1500 DEG C at carry out nitrogenizing reaction and sintering densification.But the technique disclosed in this patent application mixes silica flour in sic raw material, burnt till by high-temperature ammonolysis reaction after shaping.Due to desired raw material as silicon carbide and silica flour price higher, and due to silicon nitride and silicon carbide be all high temperature resistant compound, and be the oxidizable compound of covalent linkage and high temperature, need to carry out burning till preparation under high temperature nitrogen atmosphere, the requirement of this technique to nitrogenize equipment and control climate is stricter, thus, cause holding at high price of silicon nitride combined with silicon carbide refractory material, and be difficult to realize scale operation.
A kind of high-strength light silicon nitride combined with silicon carbide refractory material and for example disclosed in No. 201210287828.0th, Chinese patent application and preparation method thereof, this material mainly with silicon carbide and silica flour for raw material is made, the weight ratio of silicon carbide and silica flour is 65 ~ 85:15 ~ 30; Wherein, silicon carbide particle diameter D50=0.1 μm ~ 150 μm, silica flour particle diameter D50=0.1 μm ~ 1 μm; Carry out ball milling by after the mixing of whole raw material, Ball-milling Time is 8 ~ 12 hours, ball milling post-drying, add raw material heavy 8 ~ 12% PVA granulation, cross 40 ~ 80 mesh sieves, room temperature places more than 24 hours, dry-pressing formed, and forming pressure is 40 ~ 80MPa, and binder removal is nitridation sintered.Equally, also there is the problem of No. 200410009794.4th, Chinese patent application in the method disclosed in this patent application.
For another example a kind of crystalline silicon processing waste mortar disclosed in No. 201310024132.3rd, Chinese patent application reclaims the entrained-flow reactor that beta-silicon nitride powder prepared by silica flour, its with crystalline silicon processing waste mortar reclaim silica flour and nitrogen for raw material, using nitrogen as silica flour and heat delivery carrier, under air-flow condition, nitrogenizing reaction generates silicon nitride powder; Due to reclaim silica flour particle diameter≤8um, Reactive Synthesis time≤15s, synthesis crystal grain is not free grows up, and can generate nano-grade silicon nitride micro mist.But the method disclosed in this patent application is still confined to prepare silicon nitride under nitrogen atmosphere, meanwhile, this patent application does not disclose or advises utilizing crystalline silicon processing waste mortar to prepare silicon nitride combined with silicon carbide refractory material.
Therefore, a kind of silicon cutting waste mortar that utilizes is provided to become urgent problem in the industry to the method preparing low cost silicon nitride combined with silicon carbide refractory material.
Summary of the invention
The object of this invention is to provide the method that a kind of silicon cutting waste mortar prepares silicon nitride combined with silicon carbide refractory material, the method can realize the recycling completely of silicon cutting waste mortar, effectively reduces the production cost of silicon nitride combined with silicon carbide refractory material simultaneously.
According to the solution of the present invention, a kind of silicon cutting waste mortar is provided to prepare the method for silicon nitride combined with silicon carbide refractory material, comprise: (1), preparation raw material, raw material comprise weight percent be respectively 5% ~ 20% silicon cutting waste mortar, the silicon carbide of 50% ~ 80%, the silicon nitride of 2% ~ 20% and 1% ~ 10% aluminum oxide; (2), raw material is added dehydrated alcohol and carry out wet ball grinding; (3) raw material after wet ball grinding, is dried; (4), in the raw material after drying add PVA and carry out granulation, obtained biscuit, the quality of wherein added PVA is 3% ~ 8% of raw materials quality; And (5), sinter biscuit into silicon nitride combined with silicon carbide refractory material in air atmosphere.
Wherein, silicon cutting waste mortar is the silicon cutting waste mortar after chemical settling, press filtration process.
Preferably, silicon cutting waste mortar is the silicon carbide/silicon mixture after removing liquid polyethylene glycol and macrobead silicon carbide, and its particle diameter is less than or equal to 100 μm, such as about 10 μm, 30 μm,
50 μm, 80 μm or its arbitrary combination.
Selectively, silicon cutting waste mortar iron-holder is higher, and impact is recycled, sulfuric acid first can be adopted to soak molten method deironing is carried out to it, such as: the mass ratio 1:3 ~ 1:5 of silicon cutting waste mortar and sulfuric acid, sulfuric acid concentration 15 ~ 25%, soaking temperature 60 ~ 90 DEG C, soak time 60 ~ 120 minutes.
Wherein, silicon nitride particle diameter may be selected to be 5 μm ~ 100 μm, such as about 10 μm, 30 μm, 50 μm, 80 μm or its arbitrary combination.
Wherein, alumina particle may be selected to be 5 μm ~ 100 μm, such as about 10 μm, 30 μm, 50 μm, 80 μm or its arbitrary combination.
Preferably, raw material comprise weight percent be respectively 5% ~ 15% silicon cutting waste mortar, the silicon carbide of 65% ~ 75%, the silicon nitride of 10% ~ 15% and 5% ~ 10% aluminum oxide.
Selectively, the silicon carbide micro-powder particle diameter in raw material is set as 1 μm ~ 500 μm, such as about 10 μm, 100 μm, 200 μm, 300 μm, 400 μm or its arbitrary combination.
Preferably, silicon carbide micro-powder in raw material comprises coarse particles silicon carbide micro-powder and fine particle silicon carbide micro-powder, the particle diameter of coarse particles silicon carbide micro-powder is set as 100 μm ~ 450 μm, the particle diameter of fine particle silicon carbide micro-powder is set as 1 μm ~ 19 μm, the quality of coarse particles silicon carbide micro-powder and fine particle silicon carbide micro-powder is 1.5:1 ~ 5:1 than scope, such as approximately 2:1,3:1,4:1 etc.
Preferably, silicon carbide micro-powder in raw material comprises coarse particles silicon carbide micro-powder, middle grained silicon carbide micro mist and fine particle silicon carbide micro-powder, the particle diameter of coarse particles silicon carbide micro-powder is set as 100 μm ~ 450 μm, the particle diameter of middle grained silicon carbide micro mist is set as 20 μm ~ 99 μm, the particle diameter of fine particle silicon carbide micro-powder is set as 1 μm ~ 19 μm, wherein, the quality of coarse particles silicon carbide micro-powder and middle grained silicon carbide micro mist is 10:1 ~ 30:1 than scope, such as about 15:1, 20:1, 25:1 etc., the quality of coarse particles silicon carbide micro-powder and fine particle silicon carbide micro-powder is 10:1 ~ 15:1 than scope, such as about 12:1, 13:1, 14:1 etc.
More preferably, the particle diameter of coarse particles silicon carbide micro-powder is set as 400 μm ~ 450 μm, and the particle diameter of middle grained silicon carbide micro mist is set as 30 μm ~ 40 μm, and the particle diameter of fine particle silicon carbide micro-powder is set as 1 μm ~ 10 μm.
Selectively, in step (2), the quality of raw material and ball milling ball is 1:2 ~ 2:1 than range set, such as approximately 1:1.5,1:1,1.5:1 etc.; The quality of raw material and dehydrated alcohol is 1:2 ~ 2:1 than range set, such as approximately 1:1.5,1:1,1.5:1 etc., and Ball-milling Time is set as 0.5 ~ 4 hour, such as about 1 hour, 2 hours, 3 hours etc.
Selectively, in step (3), bake out temperature is set as 60 ~ 80 DEG C, such as about 65 DEG C, 70 DEG C, 75 DEG C etc.
Selectively, in step (4), also comprise room temperature after granulation place at least 24 hours, such as about 30 hours, 36 hours, 48 hours etc.Dry-pressing formed again, forming pressure is 10 ~ 40MPa, such as about 15MPa, 20MPa, 30MPa etc.Thus obtained biscuit.
Preferably, in step (5), firing condition is: be first incubated 1 ~ 3 hour (such as 1.5 hours or 2 hours) with the ramp of 5 ~ 10 DEG C/min (such as 8 DEG C/min) to 1000-1150 DEG C, next 1 ~ 3 hour is incubated (such as 1.5 hours or 2 hours) with ramp to 1300 ~ 1350 of 1 ~ 5 DEG C/min (such as 3 DEG C/min) DEG C, be incubated 1 ~ 3 hour (such as 1.5 hours or 2 hours) with ramp to 1400 ~ 1450 of 1 ~ 5 DEG C/min (such as 2 DEG C/min) DEG C again, then room temperature is naturally cooled to.
The invention has the beneficial effects as follows: (1) present method achieves the utilization completely of silicon cutting waste mortar, reduces environmental pollution, turns waste into wealth; (2) and present method do not need nitrogen protection, can prepare on the electric furnace of air atmosphere, firing time is short, can effectively reduce energy consumption and cost, improve the competitiveness of product in market; (3) the present invention adopts step heat preservation method, can effectively avoid flowing silicon; (4) silicon carbide micro-powder of the present invention comprises coarse particles silicon carbide micro-powder, middle grained silicon carbide micro mist and fine particle silicon carbide micro-powder, and in thick, fine particle proportioning is suitable, can improve the physicals of product; (5) utilize method of the present invention, the silicon nitride combined with silicon carbide refractory material obtained, its unit weight is 1.6 ~ 1.9g/cm
3, folding strength is greater than 30MPa, and void content is less than 15%, can meet general service requirements, have cost advantage.
Embodiment
The present invention is described in detail referring to non-limiting embodiment.
The invention provides the method that a kind of silicon cutting waste mortar prepares low cost silicon nitride combined with silicon carbide refractory material, comprise following steps:
(1) raw material choose following component and weight percent:
Wherein silicon carbide micro-powder particle diameter is 1 μm ~ 500 μm, and preferably, in silicon carbide micro-powder, to be silicon carbide and the particle diameter of 1 μm ~ 50 μm be particle diameter that the silicon carbide quality of 50 μm ~ 450 μm is 1:7 ~ 7:1 than scope.
(2) above-mentioned whole raw material is added appropriate dehydrated alcohol and carry out wet ball grinding, wherein, the quality of raw material and ball milling ball is 1:2 ~ 2:1 than scope; The quality of raw material and dehydrated alcohol is 1:2 ~ 2:1 than scope, and Ball-milling Time is 0.5 ~ 4 hour, ball milling post-drying, and selected bake out temperature is preferably 60 ~ 80 DEG C.
(3) compound after above-mentioned oven dry is added PVA (polyvinyl alcohol) granulation that mass percent is 5%, room temperature places more than 24 hours, dry-pressing formed, and forming pressure is 10 ~ 40MPa, obtained biscuit.
(4) biscuit is burnt till in air atmosphere, firing condition is 1400 ~ 1450 DEG C, burn till the ramp to 1000 DEG C that Elevated Temperature Conditions is 5 ~ 10 DEG C/min, 1000-1150 DEG C of insulation 1 ~ 3 hour, again with ramp to 1300 ~ 1350 of 1 ~ 5 DEG C/min DEG C insulation 1 ~ 3 hour, again with ramp to 1400 ~ 1450 of 1 ~ 5 DEG C/min DEG C insulation 1 ~ 3 hour, then naturally cool to room temperature, the silicon nitride combined with silicon carbide refractory material of good mechanical properties can be obtained.
Nitrogenizing reaction due to Si is strong exothermal reaction, and the nitrogenization speed of exothermic heat of reaction on Si has larger impact, and therefore conservative control reaction process is the key determining nitriding rate.Si and N
2from 1100 just reaction, but speed of reaction is lower, and when 1200 DEG C ~ 1420 DEG C, reaction is acutely carried out, and releases a large amount of reaction heat simultaneously.Therefore the temperature of base substrate inside may exceed about 40 DEG C than furnace temperature, if effectively can not control reaction process, reaction heat can make the temperature of base substrate exceed the fusing point (1420 DEG C) of metal Si, and unreacted Si will melt; The molten group of less silicon can because of cannot nitrogenize and the most free silica remain in base substrate, worsen the mechanical behavior under high temperature of material; And the molten group of larger silicon even from billet surface benefit, can make base substrate spalling, melts and collapse, namely cause serious " stream silicon " phenomenon, thus goods are scrapped.Control reaction process to realize mainly through controlling temperature rise rate.
The process that method according to the present invention prepares example product 1-5 is specifically described hereinafter with reference to table 1.
The composition of raw materials that table 1 product 1-5 adopts and performance comparison table
Wherein, the particle diameter of coarse particles silicon carbide micro-powder is set as 100 μm ~ 450 μm, can select the arbitrary combination of about 350 μm, 400 μm, 420 μm, 450 μm or these particle diameters; The particle diameter of middle grained silicon carbide micro mist is set as 20 μm ~ 99 μm, can select the arbitrary combination of about 30 μm, 35 μm, 45 μm, 60 μm or these particle diameters; The particle diameter of fine particle silicon carbide micro-powder is set as 1 μm ~ 19 μm, can select the arbitrary combination of about 3 μm, 5 μm, 10 μm, 15 μm or these particle diameters.
The preparation method of product 1 is:
Ball milling is carried out by after whole raw material mixing, take dehydrated alcohol as ball-milling medium, ball milling (mass ratio of raw material, ball and dehydrated alcohol is 1:2:1.3) in planetary mills, Ball-milling Time is 1 hour, and the slurry after ball milling is dried under 60 DEG C of conditions, with the PVA granulation of concentration 5%, room temperature places 24 hours, get the powder after appropriate granulation in mould, dry-pressing formed, forming pressure is 10 ~ 15MPa.Under air atmosphere, high temperature burns till, firing condition: first with the ramp to 1100 DEG C of 5 DEG C/min, then with the ramp to 1300 DEG C of 2 DEG C/min, at 1300 DEG C of insulation 1h, again with the ramp to 1400 DEG C of 1.5 DEG C/min, under temperature 1400 DEG C of conditions, be incubated 3h.Last with the ramp to 1450 DEG C of 1 DEG C/min, under temperature 1450 DEG C of conditions, be incubated 3h, obtaining bending strength is 32MPa, unit weight 1.64g/cm3, the silicon nitride combined silicon carbide material that thermal shock resistance is good.
The preparation method of product 2 is:
Ball milling is carried out by after whole raw material mixing, take dehydrated alcohol as ball-milling medium, ball milling (mass ratio of raw material, ball and dehydrated alcohol is 1:1.5:1.5) in planetary mills, Ball-milling Time is 0.5 hour, and the slurry after ball milling is dried under 70 DEG C of conditions, with the PVA granulation of concentration 8%, room temperature places 36 hours, get the powder after appropriate granulation in mould, dry-pressing formed, forming pressure is 15 ~ 20MPa.Under air atmosphere, high temperature burns till, firing condition: first with the ramp to 1100 DEG C of 3 DEG C/min, at 1100 DEG C of insulation 2h, then with the ramp to 1300 DEG C of 2 DEG C/min,
At 1300 DEG C of insulation 0.5h, then with the ramp to 1400 DEG C of 1.5 DEG C/min, under temperature 1400 DEG C of conditions, be incubated 1h.Last with the ramp to 1450 DEG C of 1 DEG C/min, under temperature 1450 DEG C of conditions, be incubated 2.5h, obtain the silicon nitride combined silicon carbide material of good mechanical properties.
The preparation method of product 3,4,5 is:
Ball milling is carried out by after whole raw material mixing, take dehydrated alcohol as ball-milling medium, ball milling (mass ratio of raw material, ball and dehydrated alcohol is 1:1:1) in planetary mills, Ball-milling Time is 1.5 hours, and the slurry after ball milling is dried under 80 DEG C of conditions, with the PVA granulation of concentration 4%, room temperature places 48 hours, get the powder after appropriate granulation in mould, dry-pressing formed, forming pressure is 20 ~ 25MPa.Under air atmosphere, high temperature burns till, firing condition: first with the ramp to 1100 DEG C of 4 DEG C/min, at 1100 DEG C of insulation 2h, again with the ramp to 1300 DEG C of 2 DEG C/min, at 1300 DEG C of insulation 1h, then with the ramp to 1400 DEG C of 1.5 DEG C/min, under temperature 1400 DEG C of conditions, be incubated 1h.Last with the ramp to 1450 DEG C of 1 DEG C/min, under temperature 1450 DEG C of conditions, be incubated 3h, obtain the silicon nitride combined silicon carbide material of good mechanical properties.
Although describe the preferred embodiment of the present invention in detail at this, but should be understood that the present invention is not limited to the concrete structure described in detail and illustrate here, other modification and variant can be realized when not departing from the spirit and scope of the invention by those skilled in the art.Such as, the parameter such as proportioning, size, temperature and pressure suitably can be chosen in scope disclosed in this invention according to concrete application conditions.
Claims (10)
1. prepare a method for silicon nitride combined with silicon carbide refractory material with silicon cutting waste mortar, comprising:
(1), preparation raw material, described raw material comprise weight percent be respectively 5% ~ 20% silicon cutting waste mortar, the silicon carbide of 50% ~ 80%, the silicon nitride of 2% ~ 20% and 1% ~ 10% aluminum oxide;
(2), described raw material is added dehydrated alcohol and carry out wet ball grinding;
(3) the described raw material after wet ball grinding, is dried;
(4), in the described raw material after drying add PVA and carry out granulation, obtained biscuit, the quality of wherein added PVA is 3% ~ 8% of described raw materials quality; And
(5), described biscuit is sintered into silicon nitride combined with silicon carbide refractory material in air atmosphere.
2. the method for silicon nitride combined with silicon carbide refractory material is prepared as claimed in claim 1 with silicon cutting waste mortar, it is characterized in that, described raw material comprise weight percent be respectively 5% ~ 15% silicon cutting waste mortar, the silicon carbide of 65% ~ 75%, the silicon nitride of 10% ~ 15% and 5% ~ 10% aluminum oxide.
3. prepare the method for silicon nitride combined with silicon carbide refractory material as claimed in claim 1 with silicon cutting waste mortar, it is characterized in that, the silicon carbide micro-powder particle diameter in described raw material is set as 1 μm ~ 500 μm.
4. the method for silicon nitride combined with silicon carbide refractory material is prepared as claimed in claim 3 with silicon cutting waste mortar, it is characterized in that, silicon carbide micro-powder in described raw material comprises coarse particles silicon carbide micro-powder and fine particle silicon carbide micro-powder, the particle diameter of described coarse particles silicon carbide micro-powder is set as 100 μm ~ 450 μm, the particle diameter of described fine particle silicon carbide micro-powder is set as 1 μm ~ 19 μm, and the quality of described coarse particles silicon carbide micro-powder and described fine particle silicon carbide micro-powder is 1.5:1 ~ 5:1 than scope.
5. the method for silicon nitride combined with silicon carbide refractory material is prepared as claimed in claim 3 with silicon cutting waste mortar, it is characterized in that, silicon carbide micro-powder in described raw material comprises coarse particles silicon carbide micro-powder, middle grained silicon carbide micro mist and fine particle silicon carbide micro-powder, the particle diameter of described coarse particles silicon carbide micro-powder is set as 100 μm ~ 450 μm, the particle diameter of described middle grained silicon carbide micro mist is set as 20 μm ~ 99 μm, the particle diameter of described fine particle silicon carbide micro-powder is set as 1 μm ~ 19 μm, wherein, the quality of described coarse particles silicon carbide micro-powder and described middle grained silicon carbide micro mist is 10:1 ~ 30:1 than scope, the quality of described coarse particles silicon carbide micro-powder and described fine particle silicon carbide micro-powder is 10:1 ~ 15:1 than scope.
6. the method for silicon nitride combined with silicon carbide refractory material is prepared as claimed in claim 5 with silicon cutting waste mortar, it is characterized in that, the particle diameter of described coarse particles silicon carbide micro-powder is set as 400 μm ~ 450 μm, the particle diameter of described middle grained silicon carbide micro mist is set as 30 μm ~ 40 μm, and the particle diameter of described fine particle silicon carbide micro-powder is set as 1 μm ~ 10 μm.
7. the method preparing silicon nitride combined with silicon carbide refractory material with silicon cutting waste mortar according to any one of claim 1 ~ 6, it is characterized in that, in described step (2), the quality of described raw material and ball milling ball is 1:2 ~ 2:1 than range set; The quality of described raw material and dehydrated alcohol is 1:2 ~ 2:1 than range set, and Ball-milling Time is set as 0.5 ~ 4 hour.
8. the method preparing silicon nitride combined with silicon carbide refractory material with silicon cutting waste mortar according to any one of claim 1 ~ 6, it is characterized in that, in described step (3), bake out temperature is set as 60 ~ 80 DEG C.
9. the method preparing silicon nitride combined with silicon carbide refractory material with silicon cutting waste mortar according to any one of claim 1 ~ 6, it is characterized in that, in described step (4), also comprise room temperature after granulation place at least 24 hours, dry-pressing formed again, forming pressure is 10 ~ 40MPa, thus obtained described biscuit.
10. the method preparing silicon nitride combined with silicon carbide refractory material with silicon cutting waste mortar according to any one of claim 1 ~ 6, it is characterized in that, in described step (5), firing condition is: be first incubated 1 ~ 3 hour with the ramp of 5 ~ 10 DEG C/min to 1000-1150 DEG C, next 1 ~ 3 hour is incubated with ramp to 1300 ~ 1350 of 1 ~ 5 DEG C/min DEG C, be incubated 1 ~ 3 hour with ramp to 1400 ~ 1450 of 1 ~ 5 DEG C/min DEG C again, then naturally cool to room temperature.
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| CN104045358B (en) * | 2014-03-06 | 2016-11-23 | 新疆众和股份有限公司 | A kind of composite refractory and preparation method thereof |
| CN104045357B (en) * | 2014-03-06 | 2016-05-25 | 新疆众和股份有限公司 | One is composite refractory and preparation method thereof cheaply |
| CN107445623A (en) * | 2017-08-23 | 2017-12-08 | 沈阳长信碳化硅微粉有限公司 | A kind of production method of the silicon carbide micro-powder of fine ceramics product |
| CN111892403A (en) * | 2020-08-03 | 2020-11-06 | 福赛特(唐山)新材料有限公司 | High-temperature anti-bending silicon nitride combined silicon carbide slab and preparation method thereof |
| CN113416042A (en) * | 2021-07-15 | 2021-09-21 | 龙南县彩艺装饰材料厂 | Dry-mixed thin layer masonry mortar |
| CN114956829B (en) * | 2022-06-18 | 2023-06-02 | 江苏诺明高温材料股份有限公司 | Silicon nitride combined silicon carbide brick for dry quenching chute and preparation method thereof |
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| CN102746013A (en) * | 2012-08-13 | 2012-10-24 | 南京工业大学 | Light high-strength silicon nitride bonded silicon carbide refractory and preparation method thereof |
| CN103183324A (en) * | 2013-01-23 | 2013-07-03 | 尹克胜 | Unit for preparing silicon nitride product by silica powder recovered from crystalline silicon processed waste mortar |
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| CN1657404A (en) * | 2004-02-18 | 2005-08-24 | 中国科学院理化技术研究所 | Method for synthesizing silicon nitride powder by atmospheric pressure combustion |
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| CN103183324A (en) * | 2013-01-23 | 2013-07-03 | 尹克胜 | Unit for preparing silicon nitride product by silica powder recovered from crystalline silicon processed waste mortar |
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