CN109942300A - The method that carbonization boron-carbon SiClx composite ceramics are prepared in situ as raw material using mortar cutting waste material - Google Patents
The method that carbonization boron-carbon SiClx composite ceramics are prepared in situ as raw material using mortar cutting waste material Download PDFInfo
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Abstract
A method of carbonization boron-carbon SiClx composite ceramics being prepared in situ by raw material of mortar cutting waste material, sequentially include the following steps: (1) for after the crushing of mortar cutting waste material, acidleach removal of impurities obtains removal of impurities waste material；(2) waste material that will clean is levigate to partial size≤60 μm, and removal of impurities powder is made；(3) carbonaceous reducing agent is levigate to partial size≤60 μm, carbonaceous reducing agent powder is made；(4) carbonaceous reducing agent powder, removal of impurities powder and boron carbide powder are uniformly mixed, water and binder is added, suppress squarely agglomerate with ball press；(5) drying obtains green compact under the conditions of 50~120 DEG C of temperature；(6) it is put into vacuum sintering funace.Method of the invention significantly improves the uniformity of silicon carbide, improves the bonding state of boron carbide and silicon carbide interface in material, and the boron carbide-carbide composite ceramic for preparing sintering has more excellent performance.
Description
Technical field
It is the invention belongs to composite ceramic material technical field, in particular to a kind of to be made in situ using mortar cutting waste material as raw material
The method of standby boron carbide-carbide composite ceramic.
Background technique
Boron carbide molecular formula B4C is dark gray powder, is most hard one of manufactured abrasive；Boron carbide have hardness it is 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 it is concerned, be widely used in mechanical lapping,
The different fields such as refractory material, engineering ceramics, nuclear industry and military affairs.
The defects of that there are fracture toughnesses is low for boron carbide ceramics, and covalent linkage content high fever knot densification is difficult；It then passes through and draws
The form for entering second phase particles prepares boron carbide base composite ceramic, defect existing for Lai Gaishan single boron carbide ceramics；Si and C,
B performance is close, in the positioned adjacent of the periodic table of elements, is inferred according to similar compatibility principle, using add elemental substance containing Si as
Sintering aid is bound to promote B4The sintering densification of C；SiC/B4C composite diphase material should be ideal mechanical property and calorifics
Can combination, i.e., by the low-density of the high intensity of silicon carbide, inoxidizability and thermal shock resistance and boron carbide, high rigidity and wear-resisting
Property combines.
Ingot casting, evolution, slice, cleaning, assembling etc. need to be passed through from solar level silicon materials to solar cell module is prepared
Working procedures；It is wherein had in slicing process and generates a large amount of waste material；Mortar cutting is exactly the sand mouth by silicon ingot both sides, will
Slurries (mostly using silicon carbide slurries) containing abrasive material are transported to silicon ingot cutting region, cut silicon by the abrasive action of abrasive material
Ingot；With the high speed development of global photovoltaic industry, crystalline silicon mortar cutting waste material is also in that blowout increases, comprehensive reutilization
Have very important significance to reducing environmental pollution, improving resource utilization tool.
Summary of the invention
The object of the present invention is to provide one kind to be prepared in situ carbonization boron-carbon SiClx composite ceramic by raw material of mortar cutting waste material
The method of porcelain, for defect existing for boron carbide ceramics, composite material inherent advantages, Si system additive itself Optimality
Can, by in-situ preparation second phase particles compared to advantage existing for mechanical mixture, the good boron carbide-silicon carbide of processability is multiple
Close ceramic material.
Method of the invention sequentially includes the following steps:
1, after crushing mortar cutting waste material, impurity is removed with inorganic Ore Leaching, then filters out leached mud, then be washed to
Washing lotion is neutrality, and moisture removal is removed in drying, obtains removal of impurities waste material；
2, the waste material that will clean is levigate to partial size≤60 μm, and removal of impurities powder is made；
3, carbonaceous reducing agent is levigate to partial size≤60 μm, carbonaceous reducing agent powder is made；
4, carbonaceous reducing agent powder, removal of impurities powder and boron carbide powder are uniformly mixed, obtain mixed material；To mixed material
Then middle addition water and binder suppress squarely agglomerate with ball press；
5, rectangular agglomerate is dried to 20~40h under the conditions of 50~120 DEG C of temperature, obtains green compact；
6, vacuum sintering funace is put the green body into, boron carbide-silicon carbide composite ceramic materials are made in sintering.
Above-mentioned inorganic acid be mass concentration 20~30% hydrochloric acid or mass concentration 20~30% sulfuric acid solution, or
The mixed acid of the two.
48~52mm of length of above-mentioned rectangular agglomerate, 3~7mm of width, 5~10mm of height.
Above-mentioned mortar cutting waste material is crystalline silicon mortar cutting waste material, and ingredient contains SiO by mass percentage239~
40%；Si 24~25%；SiC 24~25%；Surplus is Fe and inevitable impurity.
Above-mentioned carbonaceous reducing agent is the mixture of one or more of graphite, petroleum coke and carbon black.
Partial size≤20 μm of above-mentioned boron carbide powder.
In above-mentioned mixed material by mass percentage are as follows: boron carbide powder accounts for 60~80%, and carbonaceous reducing agent powder accounts for 10
~20%, removal of impurities powder accounts for 5~20%.
In above-mentioned step 3, water accounts for the 5~10% of mixed material gross mass, and binder accounts for the 0.5 of mixed material gross mass
~3%.
Above-mentioned binder is cellulose binder.
In above-mentioned step 4, the 10~40Mpa of pressure, 40~120s of dwell time when squarely agglomerate are suppressed.
It is dried in a vacuum drying oven in above-mentioned step 5.
In above-mentioned step 6,1800~2200 DEG C of sintering temperature, 30~150min of time.
Above-mentioned 3.3~5.3MPam1/2 of boron carbide-silicon carbide composite ceramic materials fracture toughness；Bending strength
200~385MPa.
Compared with existing smelting technique, the invention has the advantages that
1, raw material is first ground to the powder that granularity is≤60 μm, both ensure that the dispersibility and uniformity of raw material, simultaneously
The specific surface area of raw material is also increased, the reactivity of raw material is improved；
2, raw material is mixed to and is pressed into pelletizing, is then dried, its contact area and gas permeability are increased, in smelting process
In significantly reduce raw material fugitive dust loss, for guarantee and realize raw material proportioning outside furnace and furnace in accuracy established base
Plinth；
3, raw material innovation is realized using mortar cutting waste material as additive, can not only be reduced the pollution of environment, can also
Boron carbide-the carbide composite ceramic for producing function admirable, brings considerable economic benefit；
4, the silicon in mortar cutting waste material and silica are reacted with carbon generates second phase particles silicon carbide, while in waste material
The silicon carbide contained can also serve as the effect of crystal seed.By the way of in-situ preparation second phase particles silicon carbide, can significantly it mention
The uniformity of high silicon carbide distribution improves the bonding state of boron carbide and silicon carbide interface in material, and sintering processability is more
Excellent boron carbide-carbide composite ceramic；
5, using vacuum sintering funace, accurate temperature control and temperature can be increased to 2300 DEG C, these are all processabilities
Excellent boron carbide ceramics material is essential.
Contain silicon, silica, silicon carbide and a small amount of impurity in mortar cutting waste material；Impurity elimination is removed using the method for pickling
After matter, it can be added to sintering in boron carbide raw material using mortar cutting waste material as additive and prepare boron carbide-silicon carbide compound pottery
Porcelain；Silicon, silica in high-temperature smelting process in waste material can be reacted with the carbon in raw material generates silicon carbide, while in waste material
Silicon carbide can also serve as the effect of crystal seed, realize the original intention that second phase particles are prepared in situ, significantly improve silicon carbide distribution
Uniformity, improve material in boron carbide and silicon carbide interface bonding state, and then improve to a certain extent boron carbide pottery
The defects of porcelain fracture toughness is low, and sintering densification is difficult；It is not only realized waste material as the raw material for preparing boron carbide composite ceramic
The secondary use of resource, protects environment, and huge economic benefit is also brought while save the cost.
The raw material proportioning that method of the invention uses is more reasonable, realizes the synthetical recovery of mortar cutting waste material, reduces environment
Pollution, while reducing production cost；And it provides one kind and carbonization boron-carbon is prepared in situ by raw material of mortar cutting waste material
The method of Si composite ceramic material, turns waste into wealth, and realizes the secondary use of resource.It is carbonized using in-situ preparation second phase particles
The method of silicon can significantly improve the uniformity of silicon carbide, improve the bonding state of boron carbide and silicon carbide interface in material, make
Boron carbide-carbide composite ceramic of sintering preparation has more excellent performance, meets market to boron carbide base composite ceramic
Demand.
Detailed description of the invention
Fig. 1 is the method for the invention that carbonization boron-carbon SiClx composite ceramics are prepared in situ by raw material of mortar cutting waste material
Flow diagram.
Specific embodiment
The vacuum sintering funace used in the embodiment of the present invention is the ZRY55B of Jinzhou Hangxing Vacuum Equipment Co., Ltd.
Type vacuum sintering funace.
The water used in the embodiment of the present invention is distilled water.
Mortar cutting waste material is crushed to partial size≤0.5mm in the embodiment of the present invention.
Boron carbide-silicon carbide composite ceramic materials consistency 94~97% in the embodiment of the present invention.
Graphite, petroleum coke, carbon black, boron carbide powder and the cellulose binder used in the embodiment of the present invention is commercially available production
Product.
48~52mm of length of rectangular agglomerate in the embodiment of the present invention, 3~7mm of width, 5~10mm of height.
Mortar cutting waste material in the embodiment of the present invention is crystalline silicon mortar cutting waste material, and ingredient contains by mass percentage
SiO239~40%；Si 24~25%；SiC 24~25%；Surplus is Fe and inevitable impurity.
It is dried in a vacuum drying oven in the embodiment of the present invention.
Embodiment 1
Process is as shown in Figure 1；
After mortar cutting waste material is crushed, impurity is removed with inorganic Ore Leaching, then filters out leached mud, then be washed to and wash
Liquid is neutrality, and moisture removal is removed in drying, obtains removal of impurities waste material；Inorganic acid is the hydrochloric acid of mass concentration 20%；
The waste material that will clean is levigate to partial size≤60 μm, and removal of impurities powder is made；
Carbonaceous reducing agent is levigate to partial size≤60 μm, carbonaceous reducing agent powder is made；Graphite, petroleum in carbonaceous reducing agent
Burnt and carbon black mass ratio is 9:5:3；
Carbonaceous reducing agent powder, removal of impurities powder and boron carbide powder are uniformly mixed, mixed material is obtained；It is pressed in mixed material
Mass percent are as follows: boron carbide powder accounts for 80%, and carbonaceous reducing agent powder accounts for 10%, and removal of impurities powder accounts for 10%；Into mixed material
Water and binder is added, then suppresses squarely agglomerate with ball press；Partial size≤20 μm of boron carbide powder；It is total that water accounts for mixed material
The 5% of quality, binder account for the 0.5% of mixed material gross mass；Binder is cellulose binder；When suppressing squarely agglomerate
Pressure 10Mpa, dwell time 40s；
Rectangular agglomerate is dried into 40h under the conditions of temperature 50 C, obtains green compact；
Vacuum sintering funace is put the green body into, 1800 DEG C of sintering temperature, time 150min, carbonization boron-carbon is made in sintering
SiClx composite ceramic material, fracture toughness 5.3MPam1/2；Bending strength 200MPa, consistency 94%.
Embodiment 2
With embodiment 1, difference is method:
(1) inorganic acid leached is the sulfuric acid solution of mass concentration 20%；
(2) it is 2:1 that carbonaceous reducing agent, which is the mass ratio of petroleum coke and carbon black,；
(3) in mixed material by mass percentage are as follows: boron carbide powder accounts for 60%, and carbonaceous reducing agent powder accounts for 20%, removal of impurities
Powder accounts for 20%；Water accounts for the 6% of mixed material gross mass, and binder accounts for the 1% of mixed material gross mass；
(4) the pressure 20Mpa, dwell time 60s when squarely agglomerate are suppressed；
(5) rectangular agglomerate is dried into 35h under the conditions of temperature 60 C；
(6) 1900 DEG C of sintering temperature, time 120min；Boron carbide-silicon carbide composite ceramic materials fracture toughness
3.3MPa·m1/2；Bending strength 385MPa, consistency 95%.
Embodiment 3
With embodiment 1, difference is method:
(1) inorganic acid leached is the hydrochloric acid of mass concentration 30%；
(2) it is 3:2 that carbonaceous reducing agent, which is the mass ratio of petroleum coke and graphite,；
(3) in mixed material by mass percentage are as follows: boron carbide powder accounts for 70%, and carbonaceous reducing agent powder accounts for 15%, removal of impurities
Powder accounts for 15%；Water accounts for the 8% of mixed material gross mass, and binder accounts for the 1.5% of mixed material gross mass；
(4) the pressure 30Mpa, dwell time 90s when squarely agglomerate are suppressed；
(5) rectangular agglomerate is dried into 30h under the conditions of 90 DEG C of temperature；
(6) 2000 DEG C of sintering temperature, time 120min；Boron carbide-silicon carbide composite ceramic materials fracture toughness
4.1MPa·m1/2；Bending strength 295MPa, consistency 96%.
Embodiment 4
With embodiment 1, difference is method:
(1) inorganic acid leached is the sulfuric acid solution of mass concentration 30%；
(2) carbonaceous reducing agent is carbon black；
(3) in mixed material by mass percentage are as follows: boron carbide powder accounts for 75%, and carbonaceous reducing agent powder accounts for 20%, removal of impurities
Powder accounts for 5%；Water accounts for the 9% of mixed material gross mass, and binder accounts for the 2% of mixed material gross mass；
(4) the pressure 35Mpa, dwell time 100s when squarely agglomerate are suppressed；
(5) rectangular agglomerate is dried into 25h under the conditions of 100 DEG C of temperature；
(6) 2100 DEG C of sintering temperature, time 60min；Boron carbide-silicon carbide composite ceramic materials fracture toughness
3.9MPa·m1/2；Bending strength 305MPa, consistency 96%.
Embodiment 5
With embodiment 1, difference is method:
(1) inorganic acid leached be the hydrochloric acid of mass concentration 25% and the sulfuric acid solution of mass concentration 25% etc. quality it is mixed
Close acid；
(2) carbonaceous reducing agent is petroleum coke；
(3) in mixed material by mass percentage are as follows: boron carbide powder accounts for 72%, and carbonaceous reducing agent powder accounts for 16%, removal of impurities
Powder accounts for 12%；Water accounts for the 10% of mixed material gross mass, and binder accounts for the 3% of mixed material gross mass；
(4) the pressure 40Mpa, dwell time 120s when squarely agglomerate are suppressed；
(5) rectangular agglomerate is dried into 20h under the conditions of 120 DEG C of temperature；
(6), 2200 DEG C of sintering temperature, time 30min；Boron carbide-silicon carbide composite ceramic materials fracture toughness
5.0MPa·m1/2；Bending strength 265MPa, consistency 97%.
Claims (10)
1. a method of carbonization boron-carbon SiClx composite ceramics are prepared in situ by raw material of mortar cutting waste material, it is characterised in that
It sequentially includes the following steps:
(1) after crushing mortar cutting waste material, impurity is removed with inorganic Ore Leaching, then filters out leached mud, then be washed to and wash
Liquid is neutrality, and moisture removal is removed in drying, obtains removal of impurities waste material；
(2) waste material that will clean is levigate to partial size≤60 μm, and removal of impurities powder is made；
(3) carbonaceous reducing agent is levigate to partial size≤60 μm, carbonaceous reducing agent powder is made；
(4) carbonaceous reducing agent powder, removal of impurities powder and boron carbide powder are uniformly mixed, obtain mixed material；Into mixed material
Water and binder is added, then suppresses squarely agglomerate with ball press；
(5) rectangular agglomerate is dried to 20~40h under the conditions of 50~120 DEG C of temperature, obtains green compact；
(6) vacuum sintering funace is put the green body into, boron carbide-silicon carbide composite ceramic materials are made in sintering.
2. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that the inorganic acid is the hydrochloric acid or mass concentration 20~30% of mass concentration 20~30%
Sulfuric acid solution, or both mixed acid.
3. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that the mortar cutting waste material is crystalline silicon mortar cutting waste material, and ingredient is by mass percentage
Containing SiO239~40%；Si24~25%；SiC24~25%；Surplus is Fe and inevitable impurity.
4. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that the carbonaceous reducing agent is the mixed of one or more of graphite, petroleum coke and carbon black
Close object.
5. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that the 3.3~5.3MPam1/ of boron carbide-silicon carbide composite ceramic materials fracture toughness
2；200~385MPa of bending strength.
6. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that in step (6), 1800~2200 DEG C of sintering temperature, 30~150min of time.
7. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that in step (4), suppress squarely agglomerate when 10~40Mpa of pressure, the dwell time 40~
120s。
8. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that the binder is cellulose binder.
9. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that in step (3), water accounts for the 5~10% of mixed material gross mass, and binder accounts for the total matter of mixed material
The 0.5~3% of amount.
10. carbonization boron-carbon SiClx composite ceramic is prepared in situ by raw material of mortar cutting waste material in one kind according to claim 1
The method of porcelain, it is characterised in that in the mixed material by mass percentage are as follows: boron carbide powder accounts for 60~80%, carbonaceous reduction
Agent powder accounts for 10~20%, and removal of impurities powder accounts for 5~20%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113024256A (en) * | 2021-03-19 | 2021-06-25 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Production method for preparing boron carbide-silicon carbide composite ceramic by using silicon carbide crystal grinding waste liquid |
| CN114918382A (en) * | 2022-07-20 | 2022-08-19 | 昆明理工大学 | Method for recycling and recycling ceramic particle reinforced steel-based composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024256A (en) * | 2021-03-19 | 2021-06-25 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Production method for preparing boron carbide-silicon carbide composite ceramic by using silicon carbide crystal grinding waste liquid |
| CN114918382A (en) * | 2022-07-20 | 2022-08-19 | 昆明理工大学 | Method for recycling and recycling ceramic particle reinforced steel-based composite material |
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