CN109133934A - The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste - Google Patents

The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste Download PDF

Info

Publication number
CN109133934A
CN109133934A CN201811099168.7A CN201811099168A CN109133934A CN 109133934 A CN109133934 A CN 109133934A CN 201811099168 A CN201811099168 A CN 201811099168A CN 109133934 A CN109133934 A CN 109133934A
Authority
CN
China
Prior art keywords
solid waste
silicon substrate
silicon carbide
porous ceramics
based porous
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811099168.7A
Other languages
Chinese (zh)
Inventor
马北越
张亚然
高陟
于敬雨
任鑫明
苏畅
吴桦
于景坤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Northeastern University China
Original Assignee
Northeastern University China
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Northeastern University China filed Critical Northeastern University China
Priority to CN201811099168.7A priority Critical patent/CN109133934A/en
Publication of CN109133934A publication Critical patent/CN109133934A/en
Priority to PCT/CN2019/080543 priority patent/WO2020057093A1/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/515—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
    • C04B35/573—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 obtained by reaction sintering or recrystallisation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063—Preparing or treating the raw materials individually or as batches
    • C04B38/0635—Compounding ingredients
    • C04B38/0645—Burnable, meltable, sublimable materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063—Preparing or treating the raw materials individually or as batches
    • C04B38/0635—Compounding ingredients
    • C04B38/0645—Burnable, meltable, sublimable materials
    • C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/424—Carbon black
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/425—Graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • C04B2235/762—Cubic symmetry, e.g. beta-SiC
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention belongs to secondary resource high-efficiency comprehensive utilization and porous ceramic film material preparation technical fields, and in particular to the method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste.Technical solution of the present invention: firstly, oxidation silicon substrate solid waste is pre-processed, removing impurity, secondly, mixing reducing agent according to oxidation silicon substrate solid waste component proportion；Then, using pretreated oxidation silicon substrate solid waste as raw material, binder and pore creating material is added, material is mixed；Finally, silicon carbide-based porous ceramics are made in high temperature sintering under protective atmosphere through dry-pressing formed.The method achieve the high value added utilizations of oxidation silicon substrate solid waste, reduce its pollution on the environment, advantageously reduce production cost, and operation is simple for this method, is convenient for industrialized production.

Description

The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste
Technical field:
The invention belongs to secondary resource high-efficiency comprehensive utilization and porous ceramic film material preparation technical fields, relate to the use of oxidation The method that silicon substrate solid waste prepares silicon carbide-based porous ceramics.
Background technique:
With the continuous development of science and technology being constantly progressive with social economy, industry in recent years has obtained rapid hair Exhibition, however, the solid waste generated in industrial processes is also increasing, has caused serious storage and environmental pollution Problem.Therefore, rationally using the solid waste resource generated in industrial processes, turning waste into wealth seems outstanding to the development of global economy It is important.
At the same time, the fast development of ceramic production industry, the demand to ceramic raw material are also increasing, Production of Ceramics Primary raw material clay face the predicament of resource exhaustion thus.For this purpose, the ceramic raw material for finding alternative clay is china industry Important research direction.
Wherein, silicon carbide-based porous ceramics, can be applied to multiple fields, such as: metallurgy, chemical industry, environment, the energy.With Aoxidizing silicon substrate solid waste replaces clay as ceramic raw material, can both reduce the cost of ceramic raw material, prepare high-performance Silicon carbide-based porous ceramics, but can scale efficiently using a large amount of oxidation silicon substrate solid waste, solve its and stack and occupy The problem of soil and pollution environment.
Currently, the preparation method of silicon carbide-based porous ceramics mainly have particle packing sintering process, direct foaming method and Polymeric sponge method etc., but its higher to ingredient requirement and limitation product shape, and add pore creating material method and can effectively avoid This defect prepares air outlet hole structure multiplicity, complex-shaped silicon carbide-based porous ceramics.
Summary of the invention:
The purpose of the present invention is overcoming above-mentioned the shortcomings of the prior art, provides and utilize oxidation silicon substrate solid waste system The method of standby silicon carbide-based porous ceramics.The method achieve the high-efficiency comprehensive utilizations of oxidation silicon substrate solid waste；And have There is the advantages that operation is simple, is convenient for industrialized production.
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: feedstock processing
By oxidation silicon substrate solid waste through high-temperature calcination and the processing that pulverizes and sieves, silicon substrate clinker is made；
Step 2: dry-pressing formed
(1) according to the ratio, silicon substrate clinker: reducing agent: binder: pore creating material=100:(5~60): (5~40): (5~60), Material is uniformly mixed, ball milling must mix material；
(2) it is dry-pressing formed that material will be mixed, and dry；
Step 3: high temperature sintering
Material after drying is placed in high-temperature sintering apparatus, carbon is made in sintering and held for some time under protective atmosphere SiClx base porous ceramics, and correlated performance test is carried out to silicon carbide-based porous ceramics.
In the step 1, the oxidation silicon substrate solid waste is flyash, gangue, iron ore tailings or rice One or more of shell ash, main component are SiO2And Al2O3。
In the step 1, the impurity handled for going in silicon base solid waste is calcined and pulverized and sieved.
In the step 1, the calcining furnace is box resistance wire furnace, the Elema used under unprotect atmosphere One of furnace, Si-Mo rod furnace or tunnel oven.
In the step 1, the described treatment process that pulverizes and sieves are as follows: use jaw crusher pulverization process, powder warp After 200 meshes, silicon substrate clinker is made.
In the step 2 (1), the carbon powder of reducing agent is one of carbon black, fat coal or active carbon or a variety of.
In the step 2 (1), the reducing agent dosage is higher than SiO in oxidation silicon substrate solid waste2With reducing agent React the 5%~20% of consumption.
In the step 2 (1), the binder is in polyvinyl alcohol, phenolic resin, waterglass or aluminium dihydrogen phosphate It is one or more.
In the step 2 (1), the pore creating material be one of starch, graphite powder, ammonium hydrogen carbonate or ammonium chloride or It is a variety of.
In the step 2 (1), the material mixing equipment is high energy ball mill, and revolving speed is 200~600r min-1, runing time is 1~10h.
In the step 2 (2), the briquetting pressure is 50~300MPa, and the dwell time is 3~5min.
In the step 2 (2), the drying temperature of the drying process is 120 DEG C, drying time is 12~for 24 hours, it does Dry equipment is drying box or tunnel drying kiln.
In the step 3, the protection gas is the Ar gas of high-purity.
In the step 3, high-temperature sintering apparatus is chamber type electric resistance furnace, tube type resistance furnace, the vacuum high-temperature of ventable atmosphere One of furnace or tunnel oven.
In the step 3, sintering temperature is 1400~1800 DEG C, and the sintered heat insulating time is 2~10h.
In the step 3, the main object of silicon carbide-based porous ceramics obtained is mutually β-SiC or α-Al2O3, apparent pore Rate is 30%~70%, and room temperature compression strength is 4~15MPa, even aperture distribution.
The present invention is the method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, with prior art phase Than, the beneficial effect is that:
1. the method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste of the invention realizes oxidation The high-efficiency comprehensive utilization of silicon substrate solid waste is not only conducive to that high performance silicon carbide-based porous ceramics are made, it is right also to reduce its The pollution that environment generates has preferable economic benefit and environmental benefit.
2. the method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste of the invention is easy to operate easily Row, is convenient for industrialized production.
3. the method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste of the invention, is natural minerals Resource finds replaceable raw material, and its is cheap, pollution-free, has achieved the purpose that turn waste into wealth.
Detailed description of the invention:
Fig. 1 is process flow chart of the invention.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail.
The coherent detection includes object phase composition, apparent porosity and room temperature compression strength；Wherein, silicon carbide-based porous is made pottery The object phase composition of porcelain is analyzed and identified using X-ray diffractometer (XRD), and test condition is Cu-Ka ray as light source, tube voltage 30kV, tube current 30mA, scanning form are step-scan, and step-length is 0.02 °, and scanning speed is 9 DEG C/min, and scanning range is 5 ° ~90 °；Apparent porosity is measured according to GB/T 1997-2000, and room temperature compression strength is resistance to according to GB/T 1964-1996 porous ceramics Pressure test method(s) is tested.
Embodiment 1
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: pretreatment of raw material
(1) flyash is placed in box resistance wire furnace, 5h is calcined at 1000 DEG C, then crush through jaw crusher, powder 200 meshes are crossed, the clinker being had good stability；
(2) according to SiO in flyash2Composition and ratio, match preparing active carbon；
Step 2: dry-pressing formed
(1) choosing phenolic resin is binder, and ammonium hydrogen carbonate is pore creating material, by flyash: active carbon: phenolic resin: carbon The quality proportioning of sour hydrogen ammonia=100:30:5:10 weighs raw material, and by its high-energy ball milling 1h；
(2) material will be mixed and is placed in dry-pressing formed in press machine, pressure maintaining 5min under 100MPa is placed in 120 in drying box It is kept the temperature for 24 hours at DEG C；
Step 3: high temperature sintering
Material after drying is placed in 1400 DEG C of high-temperature vacuum furnace, is sintered 2h under Ar atmosphere, is cooled to room to high temperature furnace Temperature obtains silicon carbide-based porous ceramics, and carries out correlated performance test to silicon carbide-based porous ceramics；
Through detecting, the main object of gained silicon carbide-based porous ceramics is mutually β-SiC and α-Al2O3, apparent porosity 37%, Room temperature compression strength is 8.2MPa, even aperture distribution.
Embodiment 2
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: pretreatment of raw material
(1) rice hull ash is placed in box resistance wire furnace, 5h is calcined at 1000 DEG C, then crush through jaw crusher, powder 200 meshes are crossed, the clinker being had good stability；
(2) according to SiO in rice hull ash2Composition and ratio, prepare carbon black；
Step 2: dry-pressing formed
(1) choosing phenolic resin is binder, and ammonium hydrogen carbonate is pore creating material, by rice hull ash: carbon black: phenolic resin: carbonic acid Hydrogen ammonia=100:60:30:10 quality proportioning weighs raw material, and by its high-energy ball milling 1h；
(2) material will be mixed and is placed in dry-pressing formed in press machine, pressure maintaining 5min under 100MPa is placed in 120 in drying box It is kept the temperature for 24 hours at DEG C；
Step 3: high temperature sintering
Material after drying is placed in 1400 DEG C of high-temperature vacuum furnace, is sintered 2h under Ar atmosphere, is cooled to room to high temperature furnace Temperature obtains silicon carbide-based porous ceramics, and carries out correlated performance test to silicon carbide-based porous ceramics；
Through detecting, the main object of gained silicon carbide-based porous ceramics is mutually β-SiC, apparent porosity 42%, room temperature resistance to compression Intensity is 7.8MPa.
Embodiment 3
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: pretreatment of raw material
(1) gangue is placed in box resistance wire furnace, 5h is calcined at 1000 DEG C, then crush through jaw crusher, powder 200 meshes are crossed, the clinker being had good stability；
(2) according to SiO in gangue2Composition and ratio, prepare carbon black；
Step 2: dry-pressing formed
(1) choosing phenolic resin is binder, and ammonium hydrogen carbonate is pore creating material, by gangue: carbon black: phenolic resin: carbonic acid Hydrogen ammonia=100:45:40:10 quality proportioning weighs raw material, and by its high-energy ball milling 3h；
(2) material will be mixed and is placed in dry-pressing formed in press machine, pressure maintaining 5min under 100MPa is placed in 120 in drying box It is kept the temperature for 24 hours at DEG C；
Step 3: high temperature sintering
Material after drying is placed in 1600 DEG C of high-temperature vacuum furnace, is sintered 4h under Ar atmosphere, is cooled to room to high temperature furnace Temperature obtains silicon carbide-based porous ceramics, and carries out correlated performance test to silicon carbide-based porous ceramics；
Through detecting, the main object of gained silicon carbide-based porous ceramics is mutually β-SiC and α-Al2O3, apparent porosity 48%, Room temperature compression strength is 6.7MPa.
Embodiment 4
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: pretreatment of raw material
(1) iron ore tailings are placed in box resistance wire furnace, 5h are calcined at 1000 DEG C, then crush through jaw crusher, Powder crosses 200 meshes, the clinker being had good stability；
(2) according to SiO in iron ore tailings2Composition and ratio, prepare carbon black；
Step 2: dry-pressing formed
(1) choosing aluminium dihydrogen phosphate is binder, and graphite powder is pore creating material, by iron ore tailings: carbon black: biphosphate Aluminium: graphite powder=100:5:20:20 quality proportioning weighs raw material, and by its high-energy ball milling 5h；
(2) material will be mixed and is placed in dry-pressing formed in press machine, pressure maintaining 5min under 100MPa is placed in 120 in drying box It is kept the temperature for 24 hours at DEG C；
Step 3: high temperature sintering
Material after drying is placed in 1700 DEG C of high-temperature vacuum furnace, is sintered 6h under Ar atmosphere, is cooled to room to high temperature furnace Temperature obtains silicon carbide-based porous ceramics, and carries out correlated performance test to silicon carbide-based porous ceramics；
Through detecting, the main object of gained silicon carbide-based porous ceramics is mutually β-SiC and α-Al2O3, apparent porosity 55%, Room temperature compression strength is 4.5MPa.
Embodiment 5
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: pretreatment of raw material
(1) flyash is placed in box resistance wire furnace, 5h is calcined at 1000 DEG C, then crush through jaw crusher, powder 200 meshes are crossed, the clinker being had good stability；
(2) according to SiO in flyash2Composition and ratio, match preparing active carbon；
Step 2: dry-pressing formed
(1) choosing phenolic resin is binder, and ammonium hydrogen carbonate is pore creating material, by flyash: active carbon: phenolic resin: carbon The quality proportioning of sour hydrogen ammonia=100:60:15:60 weighs raw material, and by its high-energy ball milling 1h；
(2) material will be mixed and is placed in dry-pressing formed in press machine, pressure maintaining 5min under 100MPa is placed in 120 in drying box It is kept the temperature for 24 hours at DEG C；
Step 3: high temperature sintering
Material after drying is placed in 1400 DEG C of high-temperature vacuum furnace, is sintered 2h under Ar atmosphere, is cooled to room to high temperature furnace Temperature obtains silicon carbide-based porous ceramics, and carries out correlated performance test to silicon carbide-based porous ceramics；
Through detecting, the main object of gained silicon carbide-based porous ceramics is mutually β-SiC and α-Al2O3, apparent porosity 65%, Room temperature compression strength is 5.6MPa, even aperture distribution.
Embodiment 6
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: pretreatment of raw material
(1) flyash is placed in box resistance wire furnace, 5h is calcined at 1000 DEG C, then crush through jaw crusher, powder 200 meshes are crossed, the clinker being had good stability；
(2) according to SiO in flyash2Composition and ratio, match preparing active carbon；
Step 2: dry-pressing formed
(1) choosing phenolic resin is binder, and ammonium hydrogen carbonate is pore creating material, by flyash: active carbon: phenolic resin: carbon The quality proportioning of sour hydrogen ammonia=100:30:25:60 weighs raw material, and by its high-energy ball milling 1h；
(2) material will be mixed and is placed in dry-pressing formed in press machine, pressure maintaining 5min under 300MPa is placed in 120 in drying box It is kept the temperature for 24 hours at DEG C；
Step 3: high temperature sintering
Material after drying is placed in 1400 DEG C of high-temperature vacuum furnace, is sintered 2h under Ar atmosphere, is cooled to room to high temperature furnace Temperature obtains silicon carbide-based porous ceramics, and carries out correlated performance test to silicon carbide-based porous ceramics；
Through detecting, the main object of gained silicon carbide-based porous ceramics is mutually β-SiC and α-Al2O3, apparent porosity 53%, Room temperature compression strength is 7.2MPa, even aperture distribution.
Embodiment 7
The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: pretreatment of raw material
(1) flyash is placed in box resistance wire furnace, 5h is calcined at 1000 DEG C, then crush through jaw crusher, powder 200 meshes are crossed, the clinker being had good stability；
(2) according to SiO in flyash2Composition and ratio, match preparing active carbon；
Step 2: dry-pressing formed
(1) choosing phenolic resin is binder, and ammonium hydrogen carbonate is pore creating material, by flyash: active carbon: phenolic resin: carbon The quality proportioning of sour hydrogen ammonia=100:30:5:10 weighs raw material, and by its high-energy ball milling 1h；
(2) material will be mixed and is placed in dry-pressing formed in press machine, pressure maintaining 5min under 100MPa is placed in 120 in drying box It is kept the temperature for 24 hours at DEG C；
Step 3: high temperature sintering
Material after drying is placed in 1800 DEG C of high-temperature vacuum furnace, is sintered 2h under Ar atmosphere, is cooled to room to high temperature furnace Temperature obtains silicon carbide-based porous ceramics, and carries out correlated performance test to silicon carbide-based porous ceramics；
Through detecting, the main object of gained silicon carbide-based porous ceramics is mutually β-SiC and α-Al2O3, apparent porosity 32%, Room temperature compression strength is 8.9MPa, even aperture distribution.

Claims (10)

1. the method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste, sequentially includes the following steps:
Step 1: feedstock processing
By oxidation silicon substrate solid waste through high-temperature calcination and the processing that pulverizes and sieves, silicon substrate clinker is made；
Step 2: dry-pressing formed
(1) according to the ratio, silicon substrate clinker: reducing agent: binder: pore creating material=100:(5~60): (5~40): (5~60), by object Material is uniformly mixed, and ball milling must mix material；
(2) it is dry-pressing formed that material will be mixed, and dry；
Step 3: high temperature sintering
Material after drying is placed in high-temperature sintering apparatus, silicon carbide is made in sintering and held for some time under protective atmosphere Base porous ceramics, and correlated performance test is carried out to silicon carbide-based porous ceramics.
2. the method according to claim 1, wherein in the step 1, the oxidation silicon substrate solid waste Object is one or more of flyash, gangue, iron ore tailings or rice hull ash, and main component is SiO2And Al2O3。
3. the method according to claim 1, wherein in the step 1, the calcining and place is pulverized and sieved Manage the impurity for going in silicon base solid waste；The calcining furnace is the box electricity used under unprotect atmosphere Hinder one of silk furnace, silicon carbide rod furnace, Si-Mo rod furnace or tunnel oven；The treatment process that pulverizes and sieves is using jaw crushing Machine pulverization process, powder is through 200 meshes.
4. the method according to claim 1, wherein the carbon powder of reducing agent is in the step 2 (1) One of carbon black, fat coal or active carbon are a variety of；The reducing agent dosage is higher than in oxidation silicon substrate solid waste SiO2The 5%~20% of consumption is reacted with reducing agent.
5. the method according to claim 1, wherein the binder is poly- second in the step 2 (1) One of enol, phenolic resin, waterglass or aluminium dihydrogen phosphate are a variety of.
6. the method according to claim 1, wherein in the step 2 (1), the pore creating material be starch, One of graphite powder, ammonium hydrogen carbonate or ammonium chloride are a variety of.
7. the method according to claim 1, wherein in the step 2 (1), the material mixing equipment For high energy ball mill, revolving speed is 200~600rmin-1, runing time is 1~10h.
8. the method according to claim 1, wherein the briquetting pressure is 50 in the step 2 (2) ~300MPa, dwell time are 3~5min；The drying temperature of the drying process be 120 DEG C, drying time be 12~for 24 hours, Drying equipment is drying box or tunnel drying kiln.
9. the method according to claim 1, wherein the protection gas is high-purity in the step 3 Ar gas.
10. the method according to claim 1, wherein in the step 3, the high-temperature sintering apparatus is One of chamber type electric resistance furnace, tube type resistance furnace, high-temperature vacuum furnace or tunnel oven of ventable atmosphere；Sintering temperature be 1400~ 1800 DEG C, the sintered heat insulating time is 2~10h.
CN201811099168.7A 2018-09-20 2018-09-20 The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste Pending CN109133934A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201811099168.7A CN109133934A (en) 2018-09-20 2018-09-20 The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste
PCT/CN2019/080543 WO2020057093A1 (en) 2018-09-20 2019-03-29 Method for preparing silicon carbide-based porous ceramic by using silicon oxide-based solid waste

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811099168.7A CN109133934A (en) 2018-09-20 2018-09-20 The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste

Publications (1)

Publication Number Publication Date
CN109133934A true CN109133934A (en) 2019-01-04

Family

ID=64815268

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811099168.7A Pending CN109133934A (en) 2018-09-20 2018-09-20 The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste

Country Status (2)

Country Link
CN (1) CN109133934A (en)
WO (1) WO2020057093A1 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109929560A (en) * 2019-04-26 2019-06-25 珠海三豫环保新材料科技有限公司 A method of magnetic bio-carrier is prepared using gangue
WO2020057093A1 (en) * 2018-09-20 2020-03-26 东北大学 Method for preparing silicon carbide-based porous ceramic by using silicon oxide-based solid waste
CN114149274A (en) * 2021-12-14 2022-03-08 中国建筑材料工业地质勘查中心宁夏总队 Method for preparing directional porous SiC ceramic by using coal slime as pore-forming agent
CN114516751A (en) * 2022-02-28 2022-05-20 肇庆学院 Method for preparing reticular porous ceramic material by utilizing solid waste

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107686369A (en) * 2017-08-22 2018-02-13 东北大学 A kind of method for preparing carborundum porous ceramics with the carborundum cutting waste material of crystalline silicon

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3192786B1 (en) * 2014-09-09 2019-04-17 Nanjing Tech University Preparation method of sic porous ceramic material
CN107399988B (en) * 2017-08-22 2020-10-16 东北大学 Method for preparing alumina-silicon carbide composite porous ceramic by using aluminum-silicon industrial waste residues
CN109133934A (en) * 2018-09-20 2019-01-04 东北大学 The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107686369A (en) * 2017-08-22 2018-02-13 东北大学 A kind of method for preparing carborundum porous ceramics with the carborundum cutting waste material of crystalline silicon

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020057093A1 (en) * 2018-09-20 2020-03-26 东北大学 Method for preparing silicon carbide-based porous ceramic by using silicon oxide-based solid waste
CN109929560A (en) * 2019-04-26 2019-06-25 珠海三豫环保新材料科技有限公司 A method of magnetic bio-carrier is prepared using gangue
CN114149274A (en) * 2021-12-14 2022-03-08 中国建筑材料工业地质勘查中心宁夏总队 Method for preparing directional porous SiC ceramic by using coal slime as pore-forming agent
CN114516751A (en) * 2022-02-28 2022-05-20 肇庆学院 Method for preparing reticular porous ceramic material by utilizing solid waste
CN114516751B (en) * 2022-02-28 2022-12-09 肇庆学院 Method for preparing reticular porous ceramic material by utilizing solid waste

Also Published As

Publication number Publication date
WO2020057093A1 (en) 2020-03-26

Similar Documents

Publication Publication Date Title
CN109133934A (en) The method for preparing silicon carbide-based porous ceramics using oxidation silicon substrate solid waste
CN104556022B (en) It is a kind of that the method for expanding microcrystalline graphite material is prepared with micro crystal graphite
WO2020057094A1 (en) Silicon carbide closed-cell ceramic prepared by using industrial silicon-based waste residue and preparation method therefor
CN107686369A (en) A kind of method for preparing carborundum porous ceramics with the carborundum cutting waste material of crystalline silicon
Ren et al. Green synthesis of porous SiC ceramics using silicon kerf waste in different sintering atmospheres and pore structure optimization
Kariya et al. Reaction performance of calcium hydroxide and expanded graphite composites for chemical heat storage applications
CN105197952A (en) Preparation of nano single crystal lanthanum hexaboride and application of nano single crystal lanthanum hexaboride in electron microscope filament preparation
CN102826851A (en) Preparation method of zirconium boride-silicon carbide complex phase high temperature resistance powder material
CN101428808B (en) Method for synthesizing dichroite with solid castoff
CN106631033A (en) Method for preparing ZrB2 powder
CN109279615A (en) A kind of preparation method of the high whiteness calcination of talc of low cost
CN103833406A (en) Foam ceramic warming plate, and preparation method thereof
CN104843727B (en) Multi-component rare earth boride (LaxCe1-x)B6 solid solution polycrystalline cathode material and preparation method thereof
CN109912309B (en) Novel mixing process for preparing aluminum nitride powder
CN104150911B (en) A kind of method of microwave-assisted quickly synthesis in low temperature nano-silicon nitride-silicon carbide composite powder body
CN100361895C (en) Method for preparing SiC complex-phase material utilizing iron ore tailings
CN103922744A (en) Preparation method for high-toughness nanometer black porcelain material
CN109650753A (en) A method of high density magnesia is prepared using magnesite discharge plasma sintering
CN103086704A (en) Preparation method of high-porosity mineral-based ceramic membrane support
CN113213498A (en) Cement-based material carbonization recycling method and calcium carbonate whisker material
CN100532327C (en) Method of synthesizing AlN-SiC composite material while controlling content of carbon and nitrogen
CN101186506B (en) Method for preparing boron nitride/sialon ceramic composite material by using boron-rich slag
Zhihe et al. Research on preparation optimization of nano CeB6 powder and its high temperature stability
CN102731109B (en) AlON material synthetic method
CN105330183A (en) Calcium aluminate cement preparing method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190104