CN106892666A - A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders - Google Patents
A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders Download PDFInfo
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- CN106892666A CN106892666A CN201710161697.4A CN201710161697A CN106892666A CN 106892666 A CN106892666 A CN 106892666A CN 201710161697 A CN201710161697 A CN 201710161697A CN 106892666 A CN106892666 A CN 106892666A
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- sialon
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- 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
- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/597—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon oxynitride, e.g. SIALONS
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
Abstract
A kind of method of coal gangue combustion synthesis β SIALON based composite powders is with colliery powder as raw material, with aluminium powder and β Si3N4Powder is additive, and raw material and additive are ground mixing, ground and mixed material is contained in graphite material boat is again put into combustion synthesis reaction kettle, nitrogen is filled with after being vacuumized to reactor, detonator is lighted using local electric heat ignition mode, the combustion synthesis reaction of initiation reaction material, after completion of the reaction by product milled processed, obtains β SIALON based composite powders.With gangue as raw material, using combustion synthesis method, low cost is prepared for β SIALON based composite powders to the present invention.Its process is simple is convenient, building-up process saving power and preventing pollution dye, is conducive to environmental protection, and for developing gangue Application way, the added value for increasing gangue is significant.
Description
Technical field
High performance material technical field is prepared the invention belongs to mineral products comprehensive utilization, more particularly to burning synthesis for preparing β-
The method of SIALON based composite powders.
Background technology
SIALON is a kind of solid solution that eighties of last century the seventies find, is by silicon (Si), aluminium (Al), oxygen (O), nitrogen
(N) compound of composition.SIALON structures are with the Si of hexagonal3N4As its architecture basics, A1 and O atom collective effect shape
Into chemical bond, replace Si3N4Si-N keys in crystal structure, ultimately form SIALON.SIALON have fabulous thermal shock resistance,
Inoxidizability, corrosion resistance and high temperature creep resistance, are a kind of excellent refractory materials, with the continuous progressive of science and technology with
Demand, the material property that β-SIALON are protruded meets it in fields such as hot industry, building materials, automobile, space flight, metallurgy, petrochemical industry
Application, be for example made the materials such as mould, refractory material, engine, bearing, cutting element, nozzle.Therefore, SIALON materials
Preparation method has obtained worldwide universal research and discovery.
The method of synthesis SIALON materials mainly has following three kinds at present：
Direct synthesis technique is with pure material Si3N4、Al2O3, AlN and SiO2It is raw material, with N2It is anti-through high temperature chemical combination as protective atmosphere
SIALON should be synthesized.When a certain amount of metal oxide is added in Si-Al-O-N systems, not jljl phase composition can be obtained
α-SIALON, β-SIALON and multiphase composite S IALON.SIALON materials such as patent of invention " is produced using direct synthesis technique
The method for planting fabricated in situ magnesium A Long/β-composite ceramics material "（Patent No. CN200910076060.0）, mainly with purifying
It is reducing agent reduction nitridation synthesis magnesium A Long/β-composite ceramics material to learn raw silicon, aluminium, with can synthesize single phase magnesium Ah
The advantage of grand material or β-sialon material, but this method preparation cost is big compared with high, energy consumption, it is high to equipment requirement, it is unsuitable for big
Large-scale production.
CRN method adds aluminum oxide and silicon, aluminum feedstock etc. in the feed with carbon as reducing agent, is arrived at 1350 DEG C
Sintered under 1650 DEG C of atmospheric flow nitrogen, prepare SIALON materials, referred to as CRN method.Such as a kind of patent of invention " profit
With coal ash for manufacturing for β-SiAlON composite diphase materials method "（Patent No. CN201410102599.X）Using flyash with carbon heat
Reduction nitridation prepares β-SIALON composite diphase materials, and 1450~1550 DEG C of sintering produce β-SIALON in 4~6 hours in a nitrogen atmosphere
Composite diphase material.It is raw material that the advantage of this kind of method is the use of cheap cheap flyash, has also produced out β-SiAlON complex phases
Material, but the CRN method that the method is used needs lasting thermal source to heat with the energy of the system of supplementing, its energy consumption phase
To higher.For another example a kind of title " synthetic method of the bar-shaped β-Sialon of sub-micron " of patent No. CN201210164383.7, is somebody's turn to do
Invention adds catalyst Fe with carbon black, Ludox, aluminium hydroxide, ammonium chloride as raw material2O3Presoma is made, presoma one
Carbothermal reduction-nitridation prepares β-Sialon powders in determining nitrogen stream.Reaction temperature is at 1350 ~ 1500 DEG C, and soaking time 2 ~ 6 is small
When this kind of method advantage be to use pure chemicals more pure with β-Sialon powders that carbothermal reduction-nitridation synthesizes, but
Building-up process is complex, and needs continuous heat source to supply, and is also possible to that thermograde can be produced in course of reaction.
Conbustion synthesis（Combustion Synthesis）It is the new technology that material is prepared using the self-heat generation that chemically reacts.
Its feature is using the self-heat generation that chemically reacts, completely（Or part）External heat source is not needed, is propagated by fast automatic combustion wave
Automatic holding reaction obtain the product of required composition and structure.
Combustion synthesis process ensures that reaction is persistently carried out by the heat release of itself between reactant, and whole process is almost not required to
Any energy extraneous to be provided, and reaction was completed in tens seconds, thus be a kind of method of the synthesis powder for receiving much attention.
Some SIALON powders are synthesized using this technique, such as portion of China Metallurgical Industry Iron and Steel Research Geueral Inst Korea Spro celebrates human hair joyously
Bright " a kind of preparation method of ceramic powder (CN1055279C) " is aluminium powder and silica or aluminum oxide to be added in silica flour or is added
Plus aluminium nitride and aluminum oxide, β-SIALON powders are synthesized using SHS technology, but profit is not directed in the patent
With mine solid waste thing gangue etc. SIALON powders are produced as reaction primary raw material.
The present invention obtains SIALON base complex phase powder with Mine Solid Wastes gangue as raw material using combustion synthesis process
Body material.The present invention can not only overcome the waste energy shortcoming of traditional carbon thermal reduction synthetic method, and be discarded using mine
Thing coal gangue combustion synthesizes SIALON powder body materials, not only reduces its cost, it is also possible to for efficient utilization of gangue is opened up newly
Technology path.The present invention has that production efficiency is high, energy saving, equipment are simple, with low cost, it is easily operated the features such as.
The content of the invention
It is an object of the invention to provide a kind of method that coal gangue combustion synthesizes β-SIALON based composite powders, particular technique
Scheme is as follows：
A kind of coal gangue combustion synthesizes the method for β-SIALON based composite powders, and methods described is by colliery powder：Aluminium powder：β-
Si3N4The mass ratio of powder is 55~85：0~25：0~45 weighs raw material, and raw material is placed in ground and mixed is carried out on milling apparatus
Treatment 1~2 hour, then ground and mixed material is contained in graphite material boat is put into combustion synthesis reaction kettle, reactor is taken out
Nitrogen is filled with after vacuum, nitrogen pressure is controlled in 5~10MPa, and detonator is lighted using local electric heat ignition mode, triggers anti-
Answer the combustion synthesis reaction of material；After completion of the reaction by product milled processed, obtain the β of hexagonal crystal shape or column pattern-
SIALON based composite powders.
Further technical scheme is as follows：
The average grain diameter of the colliery powder is 1~100 μm.
The purity of the aluminium powder is more than 95%, and average grain diameter is 1~100 μm.
β-the Si3N4The purity of powder is more than 80%, and average grain diameter is 0.5~100 μm.
The nitrogen gas purity is more than 99.9%.
The milling apparatus are the one kind in planetary ball mill, horizontal rotor-grinding machine and oscillating mill.
The present invention is reacted by implementing conbustion synthesis in high pressure nitrogen using the nitridation system of colliery powder and additive
A large amount of heat energy are discharged, the stabilization for realizing conbustion synthesis system continues propagating combustion reaction, and by Optimizing Process Parameters,
Reasonable Regulation And Control combustion reaction feature, the product of generation is that the β-SIALON bases of the preferable hexagonal crystal shape of development or column pattern are combined
Powder.
Compared with the prior art, this method uses the Coal Refuse in mine as main raw material(s), and conventional
Use chemical reagent be raw material compared to low cost, while the environmental pollution that can largely solve mine gangue is asked
Topic.
Principal phase material β-SIALON are more than 85% in the β-SIALON based composite powders of this method synthesis.
This method process is simple, it is with short production cycle, realize building-up process by reaction self-heat generation, a large amount of save energies,
Reduces cost.
The whole building-up process of this method expects and obtains synthetic product from reaction cloth, produces the time less than 3 minutes, and whole closes
It is pollution-free into process, the efficient utilization from raw material to product can be realized, it is adapted to large-scale production.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of the β-SIALON based composite powders of preparation in embodiment of the present invention l.
Fig. 2 is the ESEM microphoto of the β-SIALON based composite powders of preparation in the embodiment of the present invention 1.
Specific embodiment
Specific embodiment of the invention is further illustrated below.
Embodiment 1
Colliery powder, the aluminium powder of 5 μm of average grain diameter that 3 μm of average grain diameter（Purity is higher than 95%）, 5 μm of average grain diameter silicon nitride
Powder（Purity is higher than 80%）, in mass ratio 60：23：17 weigh raw material and mix, and are then placed in the stainless steel of liner SiC wearing layers
Pre-processed within 1 hour with vibrator ground and mixed in ball grinder.Mixed material after pretreatment is uniformly contained in
In semi-cylindrical graphite material boat, apparent density is 0.6g/cm3.In graphite material boat, using appropriate titanium valve as detonator, vacuum
After pumping vacuum, high pure nitrogen to 5 MPa is filled with.Local igniting induces conbustion synthesis.Reaction terminate to obtain it is powdered or
Loose block product.X-ray diffraction and SEM scanning electron microscope analysis results show that the powder is hexagonal crystal shape or column
Homogeneous β-SIALON the based composite powders of pattern.
Embodiment 2
Colliery powder, the aluminium powder of 5 μm of average grain diameter that 8 μm of average grain diameter（Purity is higher than 95%）, in mass ratio 76：24 weigh original
Expect and mix, be then placed in being carried out within 0.5 hour with vibrator ground and mixed in the stainless steel jar mill of liner SiC wearing layers
Pretreatment.Mixed material after pretreatment is uniformly contained in cylindric graphite material boat, apparent density is about 0.8g/cm3。
Using appropriate titanium valve as detonator in graphite material boat.After vavuum pump is vacuumized, vacuum pump valve is closed, and is filled with nitrogen to 7 MPa.
Local igniting induces conbustion synthesis.Reaction terminates that powdered or loose block product can be obtained, and locates after levigate classification etc.
Homogeneous β-SIALON the based composite powders of hexagonal crystal shape or column pattern are obtained after science and engineering skill.
Embodiment 3
Colliery powder, the silicon nitride powder of 5 μm of average grain diameter that 10 μm of average grain diameter（Purity is higher than 80%）, in mass ratio 55：45 claim
Take raw material and mix, be then placed in being entered within 2 hours with vibrator ground and mixed in the stainless steel jar mill of liner SiC wearing layers
Row pretreatment.Mixed material after pretreatment is uniformly contained in cylindric graphite material boat, apparent density is about 1g/cm3。
After appropriate titanium valve is vacuumized as detonator vavuum pump in graphite material boat, high pure nitrogen to 10 MPa is filled with.Local igniting
Induce conbustion synthesis.Reaction terminates that powdered or loose block product can be obtained, after the aftertreatment technologys such as levigate classification
Obtain the homogeneous β-SIALON based composite powders of hexagonal crystal shape or column pattern.
The X-ray diffraction spectrogram of the β-SIALON based composite powders prepared in embodiment of the present invention l, SEM ESEMs show
Micro- photo is shown in accompanying drawing 1 and accompanying drawing 2.
Raw material colliery powder and additive aluminium powder and the mix proportion scheme of silicon nitride powder, are only of the invention in above-described embodiment
Preferably implement, any limitation not made to technical scheme, in colliery powder：Aluminium powder：β-Si3N4The quality of powder
Than being 55~85：0~25：Other ratios can reach similar product effect in the range of 0~45.Technology according to the present invention is implemented
Any trickle amendment, equivalent variations and modification that scheme is made to above example, still fall within the model of technical solution of the present invention
In enclosing.
Claims (7)
1. a kind of method that coal gangue combustion synthesizes β-SIALON based composite powders, methods described is by colliery powder：Aluminium powder：β-
Si3N4The mass ratio of powder is 55~85：0~25：0~45 weighs raw material, and raw material is placed in ground and mixed is carried out on milling apparatus
Treatment 1~2 hour, then ground and mixed material is contained in graphite material boat is put into combustion synthesis reaction kettle, reactor is taken out
Nitrogen is filled with after vacuum, nitrogen pressure is controlled in 5~10MPa, and detonator is lighted using local electric heat ignition mode, triggers anti-
Answer the combustion synthesis reaction of material；After completion of the reaction by product milled processed, obtain the β of hexagonal crystal shape or column pattern-
SIALON based composite powders.
2. method according to claim 1, methods described is by colliery powder：Aluminium powder：β-Si3N4The mass ratio of powder enters one
Walk is 60：23：17.
3. method according to claim 1, the average grain diameter of the colliery powder is 1~100 μm.
4. method according to claim 1, the purity of the aluminium powder is more than 95%, and average grain diameter is 1~100 μm.
5. method according to claim 1, the β-Si3N4The purity of powder is more than 80%, and average grain diameter is 0.5~100 μ
m。
6. method according to claim 1, the nitrogen gas purity is more than 99.9%.
7. method according to claim 1, the milling apparatus are planetary ball mill, horizontal rotor-grinding machine and vibration
One kind in grinder.
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| CN201710161697.4A CN106892666A (en) | 2017-03-17 | 2017-03-17 | A kind of coal gangue combustion synthesizes the method for β SIALON based composite powders |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110203894A (en) * | 2019-06-26 | 2019-09-06 | 西北农林科技大学 | A method of β-SiAlON is prepared using aluminium lime-ash |
| CN114772619A (en) * | 2022-04-19 | 2022-07-22 | 百色学院 | Method for recycling Bayer process red mud |
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| KR100232057B1 (en) * | 1997-04-21 | 1999-12-01 | 장기중 | Sialon synthesis from natural silicon and aluminium powder using microwave heating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110203894A (en) * | 2019-06-26 | 2019-09-06 | 西北农林科技大学 | A method of β-SiAlON is prepared using aluminium lime-ash |
| CN114772619A (en) * | 2022-04-19 | 2022-07-22 | 百色学院 | Method for recycling Bayer process red mud |
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