CN108821772A - A method of addition alumina powder prepares Boral system composite ceramic - Google Patents
A method of addition alumina powder prepares Boral system composite ceramic Download PDFInfo
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- CN108821772A CN108821772A CN201810800412.1A CN201810800412A CN108821772A CN 108821772 A CN108821772 A CN 108821772A CN 201810800412 A CN201810800412 A CN 201810800412A CN 108821772 A CN108821772 A CN 108821772A
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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
- C04B35/56—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
- C04B35/563—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 boron carbide
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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
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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
- 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
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Abstract
The invention discloses a kind of methods that addition alumina powder prepares Boral system composite ceramic.Steps are as follows：(1) carbonaceous reducing agent is first broken into powder；(2) the carbonaceous reducing agent powder that will be crushed, boric acid powder and Al2O3Powder carries out compounding, mixing by certain proportion and is pressed into pelletizing, then pelletizing is dried；(3) pelletizing is put into progress pyrolytic semlting in heating furnace and prepares boron carbide composite ceramic coarse powder；(4) obtained coarse powder is crushed and carries out classification removal of impurities；(5) ground-slag obtained carries out recycling and reusing, and boron carbide composite ceramic fine powder is for making boron carbide composite ceramic raw materials for sintering.The present invention improves the utilization rate of raw material, significantly reduces production cost and energy consumption compared with conventional arc furnace is smelted；Directly Al is added in the raw material of configuration2O3Compared to in-situ preparation Al in the reaction2O3There are apparent advantages；Significantly improve the fracture toughness of boron carbide composite ceramic；This technique can reduce environmental pollution, reduce high-temperature gas discharge.
Description
Technical field
The invention belongs to the preparation field of boron carbide composite ceramic, it is related to a kind of addition alumina powder and prepares Boral system
The method of composite ceramic.
Background technique
Boron carbide, molecular formula B4C is dark gray powder, is most hard one of manufactured abrasive.Boron carbide has hardness high
(Mohs' hardness 9.36), wearability be good, the small (2.52g/cm of density3), fusing point high (2450 DEG C), low (the room temperature 140s/ of thermoelectricity capability
M), the excellent characteristics such as resistance to acid and alkali is strong and neutron absorption capability is strong are widely used in mechanical lapping, refractory material, engineering pottery
The different fields such as porcelain, nuclear industry and military affairs.
Composite material usually has the good comprehensive performance that different materials are mutually learnt from other's strong points to offset one's weaknesses.There are two types of composite material has both
Or the characteristics of two or more materials, the performance of homogenous material can be improved, intensity is such as improved, increase toughness, shock resistance fatigue resistance
Can and improve chemical stability, dielectric properties etc..As the ceramic composite of high-temperature structural material, it is mainly used for aerospace,
The departments such as military project.In addition, various ceramic composites are also widely used in fields such as machinery, chemical industry, electronic technology.
There are many shortcomings for traditional electric arc furnace smelting boron carbide material, and such as arc area temperature height, smelting temperature is uneven
It is even, it is uncontrollable；Boric acid volatilization loss is serious；Gas emissions are high；Boron oxide viscosity is high, hinders the timely discharge of gas, no
Conducive to the generation of boron carbide, while increasing the complexity and processing difficulty of the working of a furnace.In view of the presence of these shortcomings carry out
Improve, a small amount of additive Al is added directly into raw materials for metallurgy2O3Powder realizes the purpose for improving traditional smelting process.
Aluminium oxide inherently has many excellent physical and chemical performances, is a kind of comparatively ideal additive.Aluminium oxide is
A kind of compound of high rigidity, fusing point are 2054 DEG C, and boiling point is 2980 DEG C, and fusing point is high, hardness height and resourceful, preparation process
Simply, low in cost.With the increase of aluminium oxide, the hardness presentation of composite material first increases the changing rule reduced afterwards, bending resistance
The changing rule for first reducing and increasing afterwards is presented in intensity and fracture toughness.Addition aluminium oxide makes B4The density of C sintered body is mentioned
Height, this is B4C sintered body difficulty densification problem provides solution.The aluminium oxide of addition different content not only reduces B4C
Sintering range, and consistency is made to be improved.Al based additive also has preferable toughness, therefore burns as additive
The toughness for the composite material formed can also have significant improvement.
The present invention uses adds alumina sintering into B directly in the boron carbide raw material of generation4C-Al2O3Composite ceramic,
B is prepared with tradition4C-Al2O3Raw material (the B of composite ceramics4C powder, Al2O3Powder) it is simple and mechanical mixing compare, B4C and Al2O3?
On micro-scale combine it is closer, have higher reactivity, be more conducive to sintering densification.
Summary of the invention
Conventional arc furnace smelts Shortcomings aiming at the problem that, for the advantages of composite ceramics, Al based additive itself
Excellent performance, additive is directly added in the feed, and than smelting product that reaction in-situ generates, there are advantages.
The technical scheme is that proposing a kind of side for adding alumina powder and preparing Boral system composite ceramic
Method.Include the following steps：
(1) carbonaceous reducing agent is broken into powder；
(2) by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder is according to weight ratio：Boric acid powder 45~85%, Al2O3Powder 5~
30%, remaining carries out ingredient for the ratio of carbonaceous reducing agent powder, and a small amount of water is added to carry out mixing, is then pressed on ball press
Agglomerate；
(3) the agglomerate wet feed suppressed is dried；
(4) agglomerate dried is put into heating furnace and carries out pyrolytic semlting into boron carbide composite ceramic coarse powder；It is described to add
Hot stove is one of induction furnace, electric arc furnaces, mineral hot furnace or resistance furnace；
(5) boron carbide composite ceramic coarse powder is crushed, and carry out classification and removal of impurities obtain boron carbide composite ceramic essence
Powder；
(6) ground-slag is subjected to recycling and reusing.
Further, above-mentioned carbonaceous reducing agent powder is one or more of petroleum coke, graphite, charcoal, active carbon, is accounted for
The weight percent of raw material is petroleum coke 0~35%, graphite 0~25%, charcoal 0~30%, active carbon 0~35%.
Further, the broken granularity of carbonaceous reducing agent described in above-mentioned steps (1) is not more than 1cm.
Further, the pressure of pressed pellet described in above-mentioned steps (2) is 5~40Mpa, 10~60s of dwell time, group
The diameter of block is 5~35mm.
Further, at 50~120 DEG C, drying time is 5~15h for the temperature control of drying described in above-mentioned steps (3).
Further, the heating rate of heating furnace described in above-mentioned steps (4) is adjustable, and temperature controls in high-temperature smelting process
At 1000~2500 DEG C, the duration of heat is controlled in 10~120min.
Compared with existing smelting technique, it is an advantage of the invention that：
(1) raw material is first broken into the granularity no more than 1cm, it is dispersed and uniform after both having ensure that feed proportioning mixing
Property, while the specific surface area of raw material is also increased, improve the reactivity of raw material；
(2) agglomerating by suppressing mixture, and dried, the area that contacts with each other of raw material is increased, is substantially reduced
The vaporization at high temperature loss of the fugitive dust loss of raw material and boric acid in stove, to realize and guaranteeing feed proportioning ratio outside furnace and furnace
Interior accurately controlling is laid a good foundation；
(3) it uses different stoves to be smelted, hence it is evident that improve the uniformity of different zones temperature in furnace, these are all
Produce the necessary condition of high-quality boron carbide composite ceramic powder.
(4) method for directly adding aluminium oxide in the feed is used, the deficiency of traditional reaction in-situ can be improved.
In production method of the invention, not only raw material availability is high, and production cost is low, has saved the energy, and produce
Boron carbide composite ceramic powder purity it is high, hardness is high, fracture toughness is good, consistency is high, can satisfy boron carbide composite ceramic completely
The raw materials requirement of porcelain sintering greatly reduces dust pollution in addition, volatility of raw material is less, improves workshop condition.
Detailed description of the invention
Fig. 1 is a kind of product Boral system composite ceramics for preparing addition alumina powder preparation of the embodiment of the present invention 5
Powder XRD diagram.
Fig. 2 is product Boral system composite ceramic SEM prepared by a kind of addition alumina powder of the embodiment of the present invention 5
Figure.
Fig. 3 is the Novel smelting of product Boral system composite ceramic prepared by a kind of addition alumina powder of the invention
The flow chart of technique.
Specific embodiment
Purity >=99.0% of boric acid raw material is used in the embodiment of the present invention.
From the graph as can be seen that the product smelted is mainly boron carbide and aluminium oxide, while also containing a small amount of boric acid
Aluminium.So that boron carbide and aluminium oxide in smelting product is effectively bonded together by this method, improves ceramic powder
Sintering activity, and then Boral system composite ceramics are prepared convenient for follow-up sintering.
Embodiment 1：
1, carbonaceous reducing agent is ground, is sieved；
2, by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder carries out ingredient according to certain weight ratio：Boric acid 77%, graphite
5%, petroleum coke 5%, charcoal 3%, active carbon 5%, then in the raw material prepared be added 5% Al2O3。
3, mixed material is pressed into the agglomerate of 10mm thickness on high-pressure ball press；
4, the agglomerate wet feed suppressed is dried, drying temperature is 60 DEG C, drying time 8h；
5, the agglomerate dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1300 DEG C, and the duration of heat is
100min is prepared into boron carbide composite ceramic coarse powder；
6, boron carbide composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide composite ceramic essence
Powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 2：
1, carbonaceous reducing agent is ground, is sieved；
2, by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder carries out ingredient according to certain weight ratio：Boric acid 60%, graphite
8%, petroleum coke 8%, charcoal 5%, active carbon 9%, then in the raw material prepared be added 10% Al2O3。
3, mixed material is pressed into the agglomerate of 15mm thickness on high-pressure ball press；
4, the agglomerate wet feed suppressed is dried, drying temperature is 80 DEG C, drying time 11h；
5, the agglomerate dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1600 DEG C, and the duration of heat is
80min is prepared into boron carbide composite ceramic coarse powder；
6, boron carbide composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide composite ceramic essence
Powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 3：
1, carbonaceous reducing agent is ground, is sieved；
2, by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder carries out ingredient according to certain weight ratio：Boric acid 45%, graphite
5%, petroleum coke 5%, charcoal 10%, active carbon 20%, then in the raw material prepared be added 15% Al2O3。
3, mixed material is pressed into the agglomerate of 25mm thickness on high-pressure ball press；
4, the agglomerate wet feed suppressed is dried, drying temperature is 100 DEG C, drying time 6h；
5, the agglomerate dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 2300 DEG C, and the duration of heat is
30min is prepared into boron carbide composite ceramic coarse powder；
6, boron carbide composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide composite ceramic essence
Powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 4：
1, carbonaceous reducing agent is ground, is sieved；
2, by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder carries out ingredient according to certain weight ratio：Boric acid 45%, graphite
8%, then 30% Al is added in petroleum coke 17% in the raw material prepared2O3。
3, mixed material is pressed into the agglomerate of 20mm thickness on ball press；
4, the agglomerate wet feed suppressed is dried, drying temperature is 120 DEG C, drying time 9h；
5, the agglomerate dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1500 DEG C, and the duration of heat is
50min is prepared into boron carbide composite ceramic coarse powder；
6, boron carbide composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide composite ceramic essence
Powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 5：
1, carbonaceous reducing agent is ground, is sieved；
2, by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder carries out ingredient according to certain weight ratio：Boric acid 80%, petroleum
Then 10% Al is added in coke 10% in the raw material prepared2O3。
3, mixed material is pressed into the agglomerate of 20mm thickness on high-pressure ball press；
4, the agglomerate wet feed suppressed is dried, drying temperature is 120 DEG C, drying time 6h；
5, the agglomerate dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 2000 DEG C, and the duration of heat is
40min is prepared into boron carbide composite ceramic coarse powder；
6, boron carbide composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide composite ceramic essence
Powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 6：
1, carbonaceous reducing agent is ground, is sieved；
2, by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder carries out ingredient according to certain weight ratio：Boric acid 60%, graphite
3%, then 25% Al is added in petroleum coke 7%, charcoal 5% in the raw material prepared2O3。
3, mixed material is pressed into the agglomerate of 20mm thickness on ball press；
4, the agglomerate wet feed suppressed is dried, drying temperature is 110 DEG C, drying time 6h；
5, the agglomerate dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 2400 DEG C, and the duration of heat is
30min is prepared into boron carbide composite ceramic coarse powder；
6, boron carbide composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide composite ceramic essence
Powder；
7, ground-slag is subjected to recycling and reusing.
Claims (10)
1. a kind of addition alumina powder method for preparing Boral system composite ceramic, which is characterized in that according to the following steps into
Row：
(1) carbonaceous reducing agent is broken into powder；
(2) by boric acid powder, carbonaceous reducing agent powder, Al2O3Powder is according to weight ratio：Boric acid powder 45~85%, Al2O3Powder 5~30%,
Remaining carries out ingredient for the ratio of carbonaceous reducing agent powder, and a small amount of water is added to carry out mixing, and agglomerate is then pressed on ball press；
(3) the agglomerate wet feed suppressed is dried；
(4) agglomerate dried is put into heating furnace and carries out pyrolytic semlting into boron carbide composite ceramic coarse powder；The heating furnace
For one of induction furnace, electric arc furnaces, mineral hot furnace or resistance furnace；
(5) boron carbide composite ceramic coarse powder is crushed, and carry out classification and removal of impurities obtain boron carbide composite ceramic fine powder；
(6) ground-slag is subjected to recycling and reusing.
2. a kind of method that addition alumina powder prepares Boral system composite ceramic according to claim 1, special
Sign is that the carbonaceous reducing agent powder is one or more of petroleum coke, graphite, charcoal, active carbon, accounts for the weight of raw material
Percentage is petroleum coke 0~35%, graphite 0~25%, charcoal 0~30%, active carbon 0~35%.
3. a kind of method that addition alumina powder prepares Boral system composite ceramic according to claim 1 or 2,
It is characterized in that, the broken granularity of carbonaceous reducing agent described in step (1) is not more than 1cm.
4. a kind of method that addition alumina powder prepares Boral system composite ceramic according to claim 1 or 2,
It is characterized in that, the pressure of pressed pellet described in step (2) is 5~40Mpa, 10~60s of dwell time, the diameter of agglomerate
For 5~35mm.
5. a kind of method that addition alumina powder prepares Boral system composite ceramic according to claim 3, special
Sign is that the pressure of pressed pellet described in step (2) is 5~40Mpa, and the diameter of 10~60s of dwell time, agglomerate are
5~35mm.
6. the side that a kind of addition alumina powder described according to claim 1 or 2 or 5 prepares Boral system composite ceramic
Method, which is characterized in that at 50~120 DEG C, drying time is 5~15h for the temperature control of drying described in step (3).
7. a kind of method that addition alumina powder prepares Boral system composite ceramic according to claim 3, special
Sign is that at 50~120 DEG C, drying time is 5~15h for the temperature control of drying described in step (3).
8. a kind of method that addition alumina powder prepares Boral system composite ceramic according to claim 4, special
Sign is that at 50~120 DEG C, drying time is 5~15h for the temperature control of drying described in step (3).
9. a kind of addition alumina powder described according to claim 1 or 2 or 5 or 7 or 8 prepares Boral system composite ceramic
Method, which is characterized in that the heating rate of heating furnace described in step (4) is adjustable, in high-temperature smelting process temperature control exists
1000~2500 DEG C, the duration of heat controls in 10~120min.
10. a kind of method that addition alumina powder prepares Boral system composite ceramic according to claim 3, special
Sign is that the heating rate of heating furnace described in step (4) is adjustable, and temperature control is 1000~2500 in high-temperature smelting process
DEG C, the duration of heat controls in 10~120min.
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Citations (5)
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|---|---|---|---|---|
| CN1155271A (en) * | 1994-08-12 | 1997-07-23 | 陶氏化学公司 | Boron carbide cermet structural materials with high flexure strength at elevated temp. |
| CN101337816A (en) * | 2008-08-29 | 2009-01-07 | 牡丹江金刚钻碳化硼有限公司 | Boron carbide-based composite material and preparation method thereof |
| CN105502404A (en) * | 2016-01-22 | 2016-04-20 | 东北大学 | Method for smelting preparation of high-quality boron carbide crystals |
| CN106702192A (en) * | 2016-09-13 | 2017-05-24 | 安泰核原新材料科技有限公司 | Boron carbide aluminum matrix composite material and preparation method thereof |
| CN106747452A (en) * | 2016-11-24 | 2017-05-31 | 东北大学 | A kind of method that resistance furnace produces boron carbide ingot |
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2018
- 2018-07-20 CN CN201810800412.1A patent/CN108821772B/en active Active
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|---|---|---|---|---|
| CN1155271A (en) * | 1994-08-12 | 1997-07-23 | 陶氏化学公司 | Boron carbide cermet structural materials with high flexure strength at elevated temp. |
| CN101337816A (en) * | 2008-08-29 | 2009-01-07 | 牡丹江金刚钻碳化硼有限公司 | Boron carbide-based composite material and preparation method thereof |
| CN105502404A (en) * | 2016-01-22 | 2016-04-20 | 东北大学 | Method for smelting preparation of high-quality boron carbide crystals |
| CN106702192A (en) * | 2016-09-13 | 2017-05-24 | 安泰核原新材料科技有限公司 | Boron carbide aluminum matrix composite material and preparation method thereof |
| CN106747452A (en) * | 2016-11-24 | 2017-05-31 | 东北大学 | A kind of method that resistance furnace produces boron carbide ingot |
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