CN109704773A - SiC/B is prepared in situ in a kind of addition silicon powder4The method of C composite ceramic - Google Patents
SiC/B is prepared in situ in a kind of addition silicon powder4The method of C composite ceramic Download PDFInfo
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Abstract
The present invention proposes that SiC/B is prepared in situ in a kind of addition silicon powder4The method of C composite ceramic.Specific step is as follows: (1) carbonaceous reducing agent being first broken into powder；(2) the carbonaceous reducing agent powder that will be crushed, boric acid powder and silicon powder carry out compounding, mixing by certain proportion and are pressed into pelletizing, then pelletizing is dried；(3) it puts the green body into progress pyrolytic semlting in induction furnace and prepares boron carbide composite ceramic coarse powder；(4) obtained coarse powder is crushed and carries out classification removal of impurities；(5) obtained ground-slag is subjected to recycling and reusing, fine powder is for making boron carbide composite ceramic raw materials for sintering.The present invention not only increases the utilization rate of raw material, reduces production cost and energy consumption also significantly；Directly in preparation B4Silicon powder being added in the raw material of C, carbonization boryl composite ceramic being prepared in situ, then sintering prepares composite ceramics.Compared to mechanical mixture, there are apparent advantages；Improve the mechanical property of boron carbide base composite ceramic significantly；Environmental pollution can also be reduced simultaneously, reduce high-temperature gas discharge.
Description
Technical field
The invention belongs to the preparation field of boron carbide base composite ceramic, it is related to a kind of addition silicon powder and SiC/ is prepared in situ
B4The method of C 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, therefore and be concerned, be widely used in mechanical lapping,
The different fields such as refractory material, engineering ceramics, nuclear industry and military affairs.
There are many defects for traditional electric arc furnace smelting boron carbide material, and such as arc area temperature height, smelting temperature is unevenly, no
Controllably；Boric acid volatilization loss is serious；Boron oxide viscosity is high, hinders the timely discharge of gas, is unfavorable for the generation of boron carbide, together
When increase the complexity and processing difficulty of the working of a furnace.In view of the presence of these shortcomings improved, boric acid and carbonaceous also
It is incorporated a certain amount of silicon powder in former agent as sintering aid, carbonization boron carbide composite ceramic powder is prepared in situ, is passed to improve
Controlling for composite ceramics sintering process.
Si and C, B performance are close, in the positioned adjacent of the periodic table of elements.Inferred according to similar compatibility principle, is contained with addition
Si elemental substance is bound to promote B as sintering aid4The sintering densification of C.Silicon carbide has various excellent performances, such as
Superhard wear, high heat conductance and mechanical strength, low thermal coefficient of expansion, resistant to chemical etching, high-temperature stability are (until 2500 DEG C of point
Solve temperature), useful resistance characteristic etc..SiC/B4C composite diphase material should be the combination of ideal mechanical property and thermal property
Body is mutually tied the high intensity of silicon carbide, inoxidizability and thermal shock resistance and the low-density, high rigidity and wearability of boron carbide
It closes.
The present invention directly adds silicon powder in the raw material for preparing boron carbide, prepares SiC/B by reaction in-situ4C is compound
Ceramic powder, then sintering prepares boron carbide base composite ceramic.SiC/B is prepared with tradition4Method (the B of C composite ceramics4C powder, SiC
The simple and mechanical mixing of powder) it compares, grain morphology is more regular, and crystal grain is fuller.B4C is combined on a microscopic scale with SiC
It is closer, there is higher reactivity, be more conducive to ceramic sintered compact.
Summary of the invention
For conventional arc furnace smelt existing defect, composite material inherent advantages, Si system additive itself it is excellent
Performance with reaction in-situ compare mechanical mixture existing for advantage.The invention proposes a kind of addition silicon powders, and SiC/ is prepared in situ
B4The method of C composite ceramic.
Realize that the present invention follows the steps below:
(1) carbonaceous reducing agent is broken into powder；
(2) according to mass ratio by boric acid powder 45~80%, silicon powder 5~30%, remaining mix for carbonaceous reducing agent powder it is equal
It is even, and water is added to carry out mixing, pelletizing is then pressed on ball press；
(3) pelletizing suppressed is dried；
(4) green compact dried are put into progress pyrolytic semlting in induction furnace and obtain boron carbide base composite ceramic coarse powder；
(5) boron carbide base composite ceramic coarse powder is crushed, and carry out classification and removal of impurities obtain boron carbide-based composite ceramic
Porcelain fine powder；
(6) ground-slag is subjected to recycling and reusing.
Carbonaceous reducing agent described in the step (1) be one or both of graphite, petroleum coke, charcoal or active carbon with
On mixture.
The particle size range control of carbonaceous reducing agent described in the step (1) is no more than 100 μm.
Carbonaceous reducing agent powder additive amount described in the step (2) are as follows: petroleum coke 0~35%, graphite 0~25%, charcoal 0
~30% or active carbon 0~35%.
The pressure of high pressure pressed pellet described in the step (2) is 10~40Mpa, 10~60s of dwell time, green compact matter
Measure 5~10g, diameter 10mm, a height of 5~35mm.
At 50~120 DEG C, drying time is 5~15h for the temperature control of drying described in the step (3).
Induction furnace described in the step (4) can be adjustable with fast heating ramp rate, and temperature control exists in high-temperature smelting process
1600~2000 DEG C, the duration of heat controls in 30~120min.
Compared with existing smelting technique, the invention has the advantages that
(1) raw material is first broken into the powder that granularity is not more than 100 μm, both ensure that the dispersibility and uniformity of raw material,
The specific surface area of raw material is also increased simultaneously, improves the reactivity of raw material；
(2) raw material is mixed to and is pressed into pelletizing, is then dried, the contact area between reactant is increased and is breathed freely
Property, the vaporization at high temperature loss of the fugitive dust loss and boric acid of raw material in furnace is significantly reduced in smelting process, for guarantee and in fact
Accuracy of the existing raw material proportioning outside furnace and in furnace is laid a good foundation；
(3) boric acid and carbonaceous reducing agent generate boron carbide, and silicon powder and carbonaceous reducing agent generate silicon carbide.Matrix and addition
Agent can be grown during preparing in situ by nucleating center of carbonaceous reducing agent, reach micron order fusion；
(4) using in preparation B4Silicon powder is added in C raw material, reaction in-situ obtains SiC/B4The method of C composite ceramic,
Tradition preparation B can be obviously improved4The defect of C base composite ceramic.
In production method of the invention, not only raw material availability is high, but also the boron carbide base composite ceramic powder produced is pure
Degree is high, crystal form is good, crystal grain is full.It can satisfy the raw materials requirement of boron carbide base composite ceramic sintering completely.In addition, boron in raw material
Acid volatilization is reduced, and is greatly reduced dust pollution, is improved workshop condition.
Detailed description of the invention
Fig. 1 is that SiC/B is prepared in situ in a kind of addition silicon powder of the embodiment of the present invention 14The method of C composite ceramic
XRD diagram.
Fig. 2 is that SiC/B is prepared in situ in a kind of addition silicon powder of the embodiment of the present invention 14The method of C composite ceramic
SEM figure.
Fig. 3 is that SiC/B is prepared in situ in a kind of addition silicon powder of the invention4The Novel smelting of the method for C composite ceramic
The flow chart of technique.
Specific embodiment
Purity >=99.0% of boric acid raw material is used in the embodiment of the present invention.
Embodiment 1:
1, carbonaceous reducing agent is ground, is sieved；
2, boric acid powder, carbonaceous reducing agent powder, silicon powder are subjected to ingredient: boric acid 77%, graphite according to certain mass ratio
5%, petroleum coke 9%, charcoal 2%, active carbon 2%, then in the raw material prepared be added 5% silicon powder；
3, it weighs the mixed raw material of 5g and is pressed into the pelletizing that diameter is 10mm on ball press；
4, the pelletizing suppressed is dried, drying temperature is 60 DEG C, drying time 8h；
5, the pelletizing dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1600 DEG C, and the duration of heat is
100min is prepared into boron carbide base composite ceramic coarse powder；
6, boron carbide base composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide-based composite ceramic
Porcelain fine powder；
7, ground-slag is subjected to recycling and reusing.
It can be seen that the mixture that institute's smelting product is mainly boron carbide and silicon carbide from Fig. 1-Fig. 2, while can also be remaining
A small amount of free carbon, sintering ceramics also need to clean before.Make institute by adding silicon powder in the raw material for preparing boron carbide
Together with boron carbide can be effectively combined with silicon carbide in smelting product, what is merged on micro-scale is even closer, improves
The sintering activity of ceramic powder, and then the SiC/B excellent convenient for sintering processability4C composite ceramics.
Embodiment 2
1, carbonaceous reducing agent is ground, is sieved；
2, boric acid powder, carbonaceous reducing agent powder, silicon powder are subjected to ingredient: boric acid 60%, graphite according to certain mass ratio
15%, petroleum coke 8%, charcoal 3%, active carbon 4%, then in the raw material prepared be added 10% silicon powder；
3, it weighs the mixed material of 6g and is pressed into the pelletizing that diameter is 10mm on ball press；
4, the pelletizing suppressed is dried, drying temperature is 80 DEG C, drying time 11h；
5, the pelletizing dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1700 DEG C, and the duration of heat is
80min is prepared into boron carbide base composite ceramic coarse powder；
6, boron carbide base composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide-based composite ceramic
Porcelain fine powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 3
1, carbonaceous reducing agent is ground, is sieved；
2, boric acid powder, carbonaceous reducing agent powder, silicon powder are subjected to ingredient: boric acid 55%, graphite according to certain mass ratio
12%, then 15% silicon powder is added in petroleum coke 15%, active carbon 3% in the raw material prepared；
3, it weighs the mixed material of 7g and is pressed into the pelletizing that diameter is 11mm on ball press；
4, the pelletizing suppressed is dried, drying temperature is 100 DEG C, drying time 6h；
5, the pelletizing dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1750 DEG C, and the duration of heat is
40min is prepared into boron carbide base composite ceramic coarse powder；
6, boron carbide base composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide-based composite ceramic
Porcelain fine powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 4
1, carbonaceous reducing agent is ground, is sieved；
2, boric acid powder, carbonaceous reducing agent powder, silicon powder are subjected to ingredient: boric acid 55%, graphite according to certain mass ratio
10%, then 20% silicon powder is added in petroleum coke 10%, charcoal 5% in the raw material prepared；
3, it weighs the mixed material of 8g and is pressed into the pelletizing that diameter is 11mm on ball press；
4, the pelletizing suppressed is dried, drying temperature is 100 DEG C, drying time 6h；
5, the pelletizing dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1800 DEG C, and the duration of heat is
30min is prepared into boron carbide base composite ceramic coarse powder；
6, boron carbide base composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide-based composite ceramic
Porcelain fine powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 5
1, carbonaceous reducing agent is ground, is sieved；
2, boric acid powder, carbonaceous reducing agent powder, silicon powder are subjected to ingredient: boric acid 65%, petroleum according to certain mass ratio
Then 25% silicon powder is added in coke 10% in the raw material prepared；
3, it weighs the mixed material of 9g and is pressed into the pelletizing that diameter is 12mm on ball press；
4, the pelletizing suppressed is dried, drying temperature is 120 DEG C, drying time 6h；
5, the pelletizing dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 1900 DEG C, and the duration of heat is
40min is prepared into boron carbide base composite ceramic coarse powder；
6, boron carbide base composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide-based composite ceramic
Porcelain fine powder；
7, ground-slag is subjected to recycling and reusing.
Embodiment 6
1, carbonaceous reducing agent is ground, is sieved；
2, boric acid powder, carbonaceous reducing agent powder, silicon powder are subjected to ingredient: boric acid 50%, graphite according to certain mass ratio
10%, then 30% silicon powder is added in petroleum coke 10% in the raw material prepared；
3, it weighs the mixed material of 10g and is pressed into the pelletizing that diameter is 10mm on ball press；
4, the pelletizing suppressed is dried, drying temperature is 80 DEG C, drying time 11h；
5, the pelletizing dried is put into induction furnace and carries out pyrolytic semlting, smelting temperature is 2000 DEG C, and the duration of heat is
80min is prepared into boron carbide base composite ceramic coarse powder；
6, boron carbide base composite ceramic coarse powder is crushed, and is classified and is cleaned, obtain boron carbide-based composite ceramic
Porcelain fine powder；
7, ground-slag is subjected to recycling and reusing.
Claims (7)
1. SiC/B is prepared in situ in a kind of addition silicon powder4The method of C composite ceramic, which comprises the following steps:
(1) carbonaceous reducing agent is broken into powder；
(2) according to mass ratio by boric acid powder 45~80%, silicon powder 5~30%, remaining be uniformly mixed for carbonaceous reducing agent powder, and
Add water to carry out mixing, pelletizing is then pressed on ball press；
(3) pelletizing suppressed is dried；
(4) green compact dried are put into progress pyrolytic semlting in induction furnace and obtain boron carbide base composite ceramic coarse powder；
(5) boron carbide base composite ceramic coarse powder is crushed, and carry out classification and removal of impurities obtain boron carbide base composite ceramic essence
Powder；
(6) ground-slag is subjected to recycling and reusing.
2. SiC/B is prepared in situ in addition silicon powder according to claim 14The method of C composite ceramic, which is characterized in that
Carbonaceous reducing agent described in step (1) is the mixture of one or more of graphite, petroleum coke, charcoal or active carbon.
3. SiC/B is prepared in situ in addition silicon powder according to claim 24The method of C composite ceramic, which is characterized in that
Carbonaceous reducing agent powder additive amount described in step (2) is petroleum coke 0~35%, graphite 0~25%, charcoal 0~30% or activity
Charcoal 0~35%.
4. SiC/B is prepared in situ in addition silicon powder according to claim 1 or 2 or 34The method of C composite ceramic, it is special
Sign is that the broken granularity control of carbonaceous reducing agent described in step (1) is no more than 100 μm.
5. SiC/B is prepared in situ in addition silicon powder according to claim 1 or 2 or 34The method of C composite ceramic, it is special
Sign is, the pressure of pressed pellet described in step (2) is 10~40Mpa, 10~60s of dwell time, green compact 5~10g of quality,
Green compact diameter is 10mm, is highly 5~35mm.
6. SiC/B is prepared in situ in addition silicon powder according to claim 1 or 2 or 34The method of C composite ceramic, it is special
Sign is that at 50~120 DEG C, drying time is 5~15h for the temperature control of drying described in step (3).
7. SiC/B is prepared in situ in addition silicon powder according to claim 1 or 2 or 34The method of C composite ceramic, it is special
Sign is that induction furnace fast heating ramp rate described in step (4) is adjustable, and temperature control is 1600~2000 in high-temperature smelting process
DEG C, the duration of heat controls in 30~120min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114920564A (en) * | 2022-05-07 | 2022-08-19 | 刘峻廷 | Preparation method of high-purity boron carbide tubular ceramic filtering membrane |
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| CN109400166A (en) * | 2019-01-12 | 2019-03-01 | 东北大学 | The method of crystalline silicon diamond wire cutting waste material preparation Boron carbide silicon carbide composite ceramic |
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| CN109081697A (en) * | 2018-08-28 | 2018-12-25 | 东北大学 | It is a kind of to prepare B4The method of C/SiC composite ceramic |
| CN109400166A (en) * | 2019-01-12 | 2019-03-01 | 东北大学 | The method of crystalline silicon diamond wire cutting waste material preparation Boron carbide silicon carbide composite ceramic |
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| CN114920564A (en) * | 2022-05-07 | 2022-08-19 | 刘峻廷 | Preparation method of high-purity boron carbide tubular ceramic filtering membrane |
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Application publication date: 20190503 |