CN109467448A - A kind of Al4SiC4Refractory material and preparation method - Google Patents
A kind of Al4SiC4Refractory material and preparation method Download PDFInfo
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- CN109467448A CN109467448A CN201811287829.9A CN201811287829A CN109467448A CN 109467448 A CN109467448 A CN 109467448A CN 201811287829 A CN201811287829 A CN 201811287829A CN 109467448 A CN109467448 A CN 109467448A
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- 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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/402—Aluminium
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/428—Silicon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
Abstract
The present invention relates to a kind of Al4SiC4Refractory material and preparation method thereof.Its technical solution is: metallic aluminium, elemental silicon and alusil alloy being added into thermosetting phenolic resin, control Al, Si and C molar ratio is 4:1:4~4:1:5, is stirred evenly to get premix;Above-mentioned premix is toasted again 24~30 hours under the conditions of 120~250 DEG C, is then handled by induction furnace up to Al4SiC4Refractory material.The present invention prepares Al4SiC4Refractory material has the characteristics that synthesis rate is fast, the uniform vapour resistant corrosivity of product component is strong.
Description
Technical field
The invention belongs to technical field of refractory materials, and in particular to a kind of Al4SiC4Refractory material and preparation method thereof.
Background technique
Double carbide Al4SiC4With high-melting-point (2037 DEG C), high intensity, good chemical stability, in high temperature oxygen
The stable mullite of Surface Creation and corundum protective film under the conditions of change have good antioxygenic property and resistance to vapor corrosion
Can, have broad application prospect in special refractories field.Generally use solid state reaction kinetics Al both at home and abroad at present4SiC4,
For Wang Gang using Al, Si and carbon black/graphite as raw material, 20~40h of mechanical ball mill is prepared for Al4SiC4[CN 101423215A];Chen
Using Al, Si and carbon black as raw material, is handled under an ar atmosphere by 1800 DEG C × 3h, obtain the Al of high-purity4SiC4[Chen J H,
Zhang Z H,Mi W J,et al.Fabrication and oxidation behavior of
Al4SiC4powders.J.Am.Ceram.S℃.,2017,100(7):3145-3154.].As it can be seen that current solid state reaction kinetics
Al4SiC4Have the shortcomings that reaction temperature is higher, soaking time is long.
Summary of the invention
To solve the deficiencies in the prior art, the present invention provides a kind of Al4SiC4Refractory material and preparation method thereof.
Technical solution provided by the present invention is as follows:
A kind of Al4SiC4The preparation method of refractory material, comprising the following steps: by thermosetting phenolic resin, metallic aluminium, list
Matter silicon and alusil alloy are mixed into premix, then toast the premix 24~30 hours under the conditions of 120~250 DEG C,
Sensed stove heating is reacted and is kept the temperature to get Al under protective atmosphere again4SiC4Refractory material, wherein Al in the premix,
Si and C molar ratio is 4:1:4~4:1:5.
In above-mentioned technical proposal, thermosetting phenolic resin is the common bonding agent of refractory material, and the present invention is to thermosetting property phenol
Metallic aluminium, elemental silicon and alusil alloy are added in urea formaldehyde, melts under high temperature and forms Al-Si metal bath, while phenolic resin
Pyrolysis forms the agraphitic carbon of high activity, reacts at a lower temperature with Al-Si metal bath and generates Al4SiC4。
In addition, the present invention heats raw material using induction furnace, induction furnace is produced by applying alternating current to induction coil
Alternating magnetic field is given birth to, conductive material generates induced electromotive force under action of alternating magnetic field in furnace, and conductive material is in faradic work
With generation Joule heat (eddy current effect), heated material;Under action of alternating magnetic field, conductive Al-Si metal bath is by long-range navigation
The hereby comprehensive function of power and gravity, periodically variable Lorentz force generate function composite by electromagnetic stirring in metal bath.In electromagnetism
In whipping process, Al-Si metal bath reacts the Al being precipitated with C4SiC4Crystal is during exercise since mutual fricting shearing is easy to disconnected
Destruction is split, dissociate the Al destroyed4SiC4Crystal becomes new nucleus, and electromagnetic agitation makes melt that convection current occur, and accelerates mass transfer and passes
Heat generates the crystallization of large area, accelerates Al4SiC4Formation.
Specifically, being increased to 1000~1600 DEG C with the rate of 3~20 DEG C/min carries out heating reaction.
Based on the above-mentioned technical proposal, the present invention is realized with lower reaction temperature, realizes Al4SiC4Generation.
Specifically, keeping the temperature 0.5~4h at 1000~1600 DEG C after heating reaction.
Based on the above-mentioned technical proposal, the present invention is realized with lower reaction temperature and shorter soaking time, is realized
Al4SiC4The growth of crystal.
Specifically, the Residual carbon of thermosetting phenolic resin is more than or equal to 45wt% after heating reaction and heat preservation, and be less than etc.
In 60wt%.
Specifically, Al content >=99wt% of metallic aluminium;Partial size≤38 μm of metallic aluminium.
Specifically, Si content >=99wt% of elemental silicon;Partial size≤38 μm of elemental silicon.
Specifically, Al content >=80wt% of alusil alloy, Si content >=18wt%;Partial size≤38 of the alusil alloy
μm。
Based on the above-mentioned technical proposal, metallic aluminium, elemental silicon and alusil alloy particle are easier to the fast reaction in induction furnace.
The present invention also provides according to above-mentioned Al4SiC4The Al that the preparation method of refractory material is prepared4SiC4Fire proofed wood
Material.
The Al that the present invention obtains4SiC4Refractory material, by 1000 DEG C of vapor corrosion 100h (vapor and volume of air
Than for 1:4, stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain is 1.5~4.0%.
The present invention has following good effect compared with prior art:
The present invention prepares Al4SiC4The uniform vapour resistant of fast, product component is rotten with synthesis rate for the method for refractory material
The strong feature of corrosion.Compared with method provided by the prior art, reaction time and soaking time further reduced.
Detailed description of the invention
Fig. 1 is the Al of preparation of the embodiment of the present invention4SiC4The XRD diagram of refractory material, it can be seen that synthesizing in
Al4SiC4Purity with higher.
Specific embodiment
The principles and features of the present invention are described below, and illustrated embodiment is served only for explaining the present invention, is not intended to
It limits the scope of the invention.
Embodiment 1
The present embodiment prepares Al4SiC4The method of refractory material is:
Metallic aluminium, elemental silicon and alusil alloy are added into thermosetting phenolic resin, control Al, Si and C molar ratio is 4:
1:4 stirs evenly to get premix;Above-mentioned premix is toasted 27 hours under the conditions of 200 DEG C again, then at sensed furnace
Reason, sensed stove heating reaction and heat preservation, are added wherein being increased to 1000 DEG C with the rate of 10 DEG C/min under protective atmosphere
Thermal response keeps the temperature 0.5h at 1000 DEG C to get Al after heating reaction4SiC4Refractory material.
Al manufactured in the present embodiment4SiC4Refractory material, purity >=80%, by 1000 DEG C of vapor corrosion 100h, (water steams
Gas and volume of air ratio are 1:4, and stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain 3.75%.
Embodiment 2
The present embodiment prepares Al4SiC4The method of refractory material is:
Metallic aluminium, elemental silicon and alusil alloy are added into thermosetting phenolic resin, control Al, Si and C molar ratio is 4:
1:4.2 stirs evenly to get premix;Above-mentioned premix is toasted 24~30 hours under the conditions of 200 DEG C again, is then passed through
Induction furnace processing, sensed stove heating reaction and heat preservation under protective atmosphere, wherein being increased to 1200 with the rate of 11 DEG C/min
Heating reaction DEG C is carried out, 0.5h is kept the temperature after heating reaction at 1200 DEG C to get Al4SiC4Refractory material.
Al manufactured in the present embodiment4SiC4Refractory material, purity >=83%, by 1000 DEG C of vapor corrosion 100h, (water steams
Gas and volume of air ratio are 1:4, and stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain 3.35%.
Embodiment 3
The present embodiment prepares Al4SiC4The method of refractory material is:
Metallic aluminium, elemental silicon and alusil alloy are added into thermosetting phenolic resin, control Al, Si and C molar ratio is 4:
1:4.4 stirs evenly to get premix;Above-mentioned premix is toasted 24~30 hours under the conditions of 200 DEG C again, is then passed through
Induction furnace processing, sensed stove heating reaction and heat preservation under protective atmosphere, wherein being increased to 1300 with the rate of 12 DEG C/min
Heating reaction DEG C is carried out, 0.5h is kept the temperature after heating reaction at 1300 DEG C to get Al4SiC4Refractory material.
Al manufactured in the present embodiment4SiC4Refractory material, purity >=85%, by 1000 DEG C of vapor corrosion 100h, (water steams
Gas and volume of air ratio are 1:4, and stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain 2.95%.
Embodiment 4
The present embodiment prepares Al4SiC4The method of refractory material is:
Metallic aluminium, elemental silicon and alusil alloy are added into thermosetting phenolic resin, control Al, Si and C molar ratio is 4:
1:4.6 stirs evenly to get premix;Above-mentioned premix is toasted 24~30 hours under the conditions of 200 DEG C again, is then passed through
Induction furnace processing, sensed stove heating reaction and heat preservation under protective atmosphere, wherein being increased to 1400 with the rate of 20 DEG C/min
Heating reaction DEG C is carried out, 2h is kept the temperature after heating reaction at 1400 DEG C to get Al4SiC4Refractory material.
Al manufactured in the present embodiment4SiC4Refractory material, purity >=89%, by 1000 DEG C of vapor corrosion 100h, (water steams
Gas and volume of air ratio are 1:4, and stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain 2.55%.
Embodiment 5
The present embodiment prepares Al4SiC4The method of refractory material is:
Metallic aluminium, elemental silicon and alusil alloy are added into thermosetting phenolic resin, control Al, Si and C molar ratio is 4:
1:4.8 stirs evenly to get premix;Above-mentioned premix is toasted 24~30 hours under the conditions of 200 DEG C again, is then passed through
Induction furnace processing, sensed stove heating reaction and heat preservation under protective atmosphere, wherein being increased to 1500 DEG C with the rate of 5 DEG C/min
Heating reaction is carried out, 2h is kept the temperature after heating reaction at 1500 DEG C to get Al4SiC4Refractory material.
Al manufactured in the present embodiment4SiC4Refractory material, purity >=92%, by 1000 DEG C of vapor corrosion 100h, (water steams
Gas and volume of air ratio are 1:4, and stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain 2.15%.
Embodiment 6
The present embodiment prepares Al4SiC4The method of refractory material is:
Metallic aluminium, elemental silicon and alusil alloy are added into thermosetting phenolic resin, control Al, Si and C molar ratio is 4:
1:5 stirs evenly to get premix;Above-mentioned premix is toasted under the conditions of 200 DEG C again 24~30 hours, then by sense
Furnace is answered to handle, sensed stove heating reaction and heat preservation under protective atmosphere, wherein being increased to 1600 DEG C with the rate of 12 DEG C/min
Heating reaction is carried out, 1h is kept the temperature after heating reaction at 1600 DEG C to get Al4SiC4Refractory material.
Al manufactured in the present embodiment4SiC4Refractory material, purity >=96%, by 1000 DEG C of vapor corrosion 100h, (water steams
Gas and volume of air ratio are 1:4, and stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain 1.75%.
To the Al of each embodiment preparation4SiC4Refractory material, by 1000 DEG C of vapor corrosion 100h (vapor and air
Volume ratio is 1:4, and stagnation pressure is 1 standard atmospheric pressure), rate of body weight gain is 1.5~4.0%.
Therefore, Al provided by the present invention4SiC4The preparation method of refractory material is fast with synthesis rate, product component is equal
Even feature, obtained Al4SiC4Refractory material has the characteristics that vapour resistant corrosivity is strong.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of Al4SiC4The preparation method of refractory material, which comprises the following steps: by thermosetting phenolic resin,
Metallic aluminium, elemental silicon and alusil alloy are mixed into premix, and the premix is then toasted 24 under the conditions of 120~250 DEG C
~30 hours, then sensed stove heating is reacted and is kept the temperature to get Al under protective atmosphere4SiC4Refractory material, wherein described pre-
Al, Si and C molar ratio are 4:1:4~4:1:5 in mixing.
2. Al according to claim 14SiC4The preparation method of refractory material, it is characterised in that: with 3~20 DEG C/min's
Rate is increased to 1000~1600 DEG C and carries out heating reaction.
3. Al according to claim 24SiC4The preparation method of refractory material, it is characterised in that: 1000 after heating reaction
0.5~4h is kept the temperature at~1600 DEG C.
4. Al according to any one of claims 1 to 34SiC4The preparation method of refractory material, it is characterised in that: heating reaction
After heat preservation, the Residual carbon of thermosetting phenolic resin is more than or equal to 45wt%, and is less than or equal to 60wt%.
5. Al according to any one of claims 1 to 34SiC4The preparation method of refractory material, it is characterised in that: metallic aluminium
Al content >=99wt%;Partial size≤38 μm of metallic aluminium.
6. Al according to any one of claims 1 to 34SiC4The preparation method of refractory material, it is characterised in that: elemental silicon
Si content >=99wt%;Partial size≤38 μm of elemental silicon.
7. Al according to any one of claims 1 to 34SiC4The preparation method of refractory material, it is characterised in that: alusil alloy
Al content >=80wt%, Si content >=18wt%;Partial size≤38 μm of the alusil alloy.
8. a kind of Al according to any one of claims 1 to 74SiC4The Al that the preparation method of refractory material is prepared4SiC4
Refractory material.
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Citations (5)
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JP2014156366A (en) * | 2013-02-14 | 2014-08-28 | Nippon Steel & Sumitomo Metal | METHOD FOR MANUFACTURING AN Al4SiC4 POWDER, METHOD FOR MANUFACTURING AN MgO-C BRICK, AND MgO-C BRICK |
CN105836718A (en) * | 2016-04-27 | 2016-08-10 | 北京科技大学 | Sol-gel method for preparing submicron-order titanium nitride powdery material |
CN106747446A (en) * | 2016-06-25 | 2017-05-31 | 河南工业大学 | A kind of Microwave Hybrid Heating synthesizes Al4SiC4The new method of powder |
CN106747447A (en) * | 2016-06-25 | 2017-05-31 | 河南工业大学 | One kind synthesis Al4SiC4The new method of powder body material |
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2018
- 2018-10-31 CN CN201811287829.9A patent/CN109467448A/en active Pending
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CN105836718A (en) * | 2016-04-27 | 2016-08-10 | 北京科技大学 | Sol-gel method for preparing submicron-order titanium nitride powdery material |
CN106747446A (en) * | 2016-06-25 | 2017-05-31 | 河南工业大学 | A kind of Microwave Hybrid Heating synthesizes Al4SiC4The new method of powder |
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Application publication date: 20190315 |