CN108218433A - A kind of Spray granulation method of silicon carbide powder - Google Patents
A kind of Spray granulation method of silicon carbide powder Download PDFInfo
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Abstract
The invention discloses a kind of Spray granulation methods of silicon carbide powder, have the characteristics that yield is high, at low cost, powder processing performance is good.Carborundum powder liquid flowability greatly improves after mist projection granulating, and processability is good, and the uniformity and compactness for obtaining biscuit improve, suitable for manufacturing the high performance silicon carbide ceramics of high-compactness.The present invention is achieved by following scheme：Weigh 40~60wt% silicon carbide micro-powders, 7~13wt% sintering aids, 1~5wt% binding agents, 0.1~0.5wt% dispersant As, 0.5~2.5wt% disperses B, a certain amount of deionized water is added in by the way of ball milling, suitable ball milling parameter is controlled to obtain the stable dispersion slurry that solid content is 40~60%.The slurry of above-mentioned gained is injected directly into sponging granulator, by the way that the technological parameters such as mist projection granulating import/export temperature, centrifugal atomizer rotating speed, slurry feed rate is controlled to obtain being granulated powder.
Description
Technical field
This patent is related to a kind of Spray granulation method of silicon carbide powder.
Background technology
Silicon carbide ceramics is a kind of high-temperature structural material, has high rigidity, high intensity, high high-temp stability, wear-resistant, resistance to
The advantages that acid and alkali corrosion, low-expansion coefficient, high thermal conductivity, good thermal shock, creep resistant and antioxygenic property are good, in machine
The fields such as the industrial circles such as tool, electronics, oil, chemical industry, metallurgy and national defense industry are widely used.
With silicon carbide industrial expansion, people are very fast to the research of silicon carbide and its composite diphase material and application development
Speed in order to improve material property, optimizes material structure, especially from material fracture toughness consideration is improved, both at home and abroad to silicon carbide
The research focus of ceramics concentrates on normal atmosphere sintering method -- in liquid-phase sintering.Normal pressure liquid-phase sintering is with a certain number of polynary low
Congruent melting oxide is sintering aid, and sintering aid forms congruent melting liquid phase at high temperature, and acceleration of sintering process reduces sintering temperature
Degree makes agglomerating plant requirement and sintering cost reduction, and improves sintering character.In liquid-phase sintering, how to ensure sintering aid
Homodisperse be very important link, while improve the uniformity of biscuit and consistency is the key that prepared by high-performance ceramic
Technology.Therefore it is required that powder has extraordinary processing performance, including：Mobility, filling property, compactness and mouldability etc., and
Each ingredient can uniformly disperse.
Spray granulation is as the raising required powder processing performance starts to be applied to advanced ceramics production field.
Ceramic slurry is spray-dried not only can to avoid each component reunite again and sedimentation separation, maintain slurry it is original
Even property；Slurry atomization is uniform simultaneously, obtains regular shape, even particle size distribution, good fluidity and is suitble to continuous automatic moulding
Pelletizing.Production efficiency and product stability can be not only improved, is conducive to improve density, uniformity and the agglutinating property of biscuit
Energy.
Ceramic industry is traditionally spray-dried using organic solvent system, but there are problems, such as：Organic solvent valency
Lattice are higher, recycling is cumbersome and explosion accident easily occurs in high-temperature drying procedures.In special cermacis field, water base body
Be slurry spray drying technology it is still a kind of newer dry technology, the application in silicon carbide ceramics needs further development
With it is perfect.
Invention content
This patent carries out mist projection granulating using centrifugal spray granulation technology to silicon carbide aqueous compound slurry, provides one kind
With high, at low cost, powder processing performance the is good Spray granulation method of yield.Carborundum powder liquid flowability is significantly after mist projection granulating
It improves, processability is good, and the uniformity and compactness for obtaining biscuit improve, suitable for the high performance silicon carbide pottery of manufacture high-compactness
Porcelain.
The technical solution adopted by the present invention：A kind of Spray granulation method of silicon carbide powder, specifically includes following steps：
1) dispensing：Silicon carbide powder, sintering aid, binding agent, dispersant A, B are weighed according to following weight ratio：
40~60wt% of silicon carbide micro-powder, sintering aid 7~13%：1~5wt% of binding agent, 0.1~0.5wt% of dispersant A, dispersion
B0.5~2.5wt%.Add in the suspension that deionized water is made into 40~60wt% of solid content.
2) ball milling slurrying：Raw materials various in step 1) are put in polytetrafluoroethylene (PTFE) ball grinder, add in ball milling ball and be placed in row
On celestial body grinding machine, ball mill mixing is carried out.Suitable milling parameters are determined, to obtain the slurry of stable dispersion.Wherein：Ball milling
Ball uses silicon carbide material, and big ball bulb diameter is about 9mm, and bead bulb diameter is about 4mm, and big ball pellet quality ratio is 3:2, ball material
Weight ratio than being medium ball and powder is (1~3):1, the ball mill mixing time is 1~10h, and rotational speed of ball-mill is 120~480r/
min。
3) mist projection granulating：Slurry obtained by step 2) is injected directly into sponging granulator, by controlling mist projection granulating work
Skill parameter obtains being granulated powder.
The D50 of the above-mentioned silicon carbide micro-powder of the present invention is 0.6 μm.
The above-mentioned sintering aid of the present invention is aluminium oxide and yttrium oxide (AL2O3:Y2O3=3:2).
The above-mentioned binding agent of the present invention is polyvinyl alcohol (PVA), and PVA has very strong polarity.PVA alcoholysis degrees used in experiment
88%, average molecular weight 1700 or so.
The above-mentioned dispersant of the present invention is tetramethylammonium hydroxide (TMAH) and polyethylene glycol (PEG).TMAH for alkalinity most
Strong organic matter is the preferable dispersant of effect in SiC aqueous slurries.Nonionic surface active agent PEG is as polymer height
Molecule is worked by steric hindrance type dispersal mechanism, and one end is adsorbed on the surface of solid particle, and the other end can be in aqueous medium
It is fully extended, forms steric hindrance layer, hinder the Collision coagulation and gravitational settling of particle, PEG and TMAH is added in jointly can increase ζ electricity
Position, is conducive to SiC ceramic powder and reaches stable dispersion by electrostatic stabilization mechanism.
The slurry of gained disperses slurry for low-viscosity stable in step 2) of the present invention, in suitable binding agent, dispersant ratio
Under example, obtain powder zeta potential and reach peak 46mV.
Slurry is spray-dried using centrifugal spray dryer in step 3) of the present invention, inlet temperature 300~350
DEG C, control outlet temperature is 90~110 DEG C, centrifugal atomizer 8000~24000r/min of rotating speed, and slurry feed rate is 5kg/
h。
Technique effect
Gained mist projection granulating mealiness can be as follows, Electronic Speculum observation：Powder is spherical in rule, pelletizing surface is regular, it is smooth and
Texture is uniform.Size distribution is in Unimodal Distribution, and particle diameter distribution is narrow, and under different technology conditions, median is substantially in 10~100 μ
m.Granulation powder pine 0.83~0.91g/cm3 of packed density, 22~29 ° of angle of repose.Compared with SiC original micro mist performances, pine fills close
Degree improves more than 50%, and angle of repose first mate reduces.By pelletizing after 40~160Mpa is dry-pressing formed, the relative density of biscuit is most
Up to 58%.
In summary, by mist projection granulating processing powder processing performance be improved significantly, obtain biscuit density height, fit
Preferably prepare the high performance silicon carbide ceramics of high-compactness.
Specific embodiment
The present invention is described below by specific embodiment, but the present invention is not limited only to following embodiment.
Embodiment 1：
1000g silicon carbide powders, 80g sintering aids, 20g binding agents, 2g dispersant As, 5g dispersant Bs is weighed in proportion to claim
Amount adds in deionized water and is made into the suspension that solid content is 50%.This solution is placed on ball mill, adds in 2000g ball milling balls,
The ball milling 4h under conditions of 480r/min obtains the slurry of stable dispersion, and gained slurry is injected directly into sponging granulator, is entered
Mouth temperature is 300 DEG C, and for control outlet temperature at 90 DEG C, atomizer rotating speed 12000r/min obtains mist projection granulating powder.
Test analysis is as follows, and the viscosity of gained slurry is 60mPa ﹒ s.Mist projection granulating powder Electronic Speculum is observed：Powder is in regular ball
Shape, pelletizing surface is regular, smooth and texture is uniform.Size distribution is in Unimodal Distribution, and particle diameter distribution is narrow, it will be seen that large-size is straight
Diameter is between 50~70 μm.Granulation powder pine packed density 0.9g/cm3,22 ° of angle of repose are dry-pressing formed in 160Mpa by pelletizing
Afterwards, the density of biscuit is 1.89g/cm3, and relative density reaches 58%.
Embodiment 2：
1000g silicon carbide powders, 80g sintering aids, 20g binding agents, 2g dispersant Bs, 5g dispersing agent Cs is weighed in proportion to claim
Amount adds in deionized water and is made into the suspension that solid content is 50%.This solution is placed on ball mill, adds in 2000g ball milling balls,
The ball milling 4h under conditions of 480r/min obtains the slurry of stable dispersion, and gained slurry is injected directly into sponging granulator, control
Inlet temperature processed is 300 DEG C, and outlet temperature obtains mist projection granulating powder in 90 DEG C, atomizer rotating speed 24000r/min.
Test analysis is as follows, and the viscosity of gained slurry is 60mPa ﹒ s.Mist projection granulating powder Electronic Speculum is observed：Powder is in regular ball
Shape, pelletizing surface is regular, smooth and texture is uniform.Size distribution is in Unimodal Distribution, and particle diameter distribution is narrow, and large-size diameter is situated between
In 50~60 μm.Granulation powder pine packed density 0.86g/cm3,29 ° of angle of repose.
Embodiment 3：
1000g silicon carbide powders, 80g sintering aids, 20g binding agents, 2g dispersant Bs, 5g dispersing agent Cs is weighed in proportion to claim
Amount adds in deionized water and is made into the suspension that solid content is 40%.This solution is placed on ball mill, adds in 2000g ball milling balls,
The ball milling 4h under conditions of 480r/min obtains the slurry of stable dispersion, and gained slurry is injected directly into sponging granulator, control
Inlet temperature processed is 300 DEG C, and outlet temperature obtains mist projection granulating powder in 90 DEG C, atomizer rotating speed 12000r/min.
Test analysis is as follows, and the viscosity of gained slurry is 30mPa ﹒ s.Mist projection granulating powder Electronic Speculum is observed：Powder is in regular ball
Shape, pelletizing surface are regular, smooth.Size distribution is in Unimodal Distribution, and large-size diameter is between 50~100 μm.Granulation powder
Loose packed density 0.83g/cm3,28 ° of angle of repose.
Claims (7)
1. a kind of Spray granulation method of silicon carbide powder, specifically includes following steps：
1) dispensing：Silicon carbide powder, sintering aid, binding agent, dispersant A, B are weighed according to following weight ratio：Carbonization
40~60wt% of silicon powder, sintering aid 7~13%：1~5wt% of binding agent, 0.1~0.5wt% of dispersant A disperse B0.5
~2.5wt%.Add in the suspension that deionized water is made into solid content 40~60%.
2) ball milling slurrying：Raw materials various in step 1) are put in polytetrafluoroethylene (PTFE) ball grinder, add in ball milling ball and be placed in planet ball
On grinding machine, ball mill mixing is carried out.Suitable milling parameters are determined, to obtain the slurry of stable dispersion.Wherein：Ball milling ball is adopted
With silicon carbide material, big ball bulb diameter is about 9mm, and bead bulb diameter is about 4mm, and big ball pellet quality ratio is 3:2, ratio of grinding media to material is
The weight ratio of medium ball and powder is (1~3):1, the ball mill mixing time is 1~10h, and rotational speed of ball-mill is 120~480r/min.
3) mist projection granulating：Slurry obtained by step 2) is injected directly into sponging granulator, by the way that atomizing granulating technology is controlled to join
Number obtains being granulated powder.
A kind of 2. Spray granulation method of silicon carbide powder according to right 1, it is characterised in that the carbonization described in step 1)
The D50 of silicon powder is 0.6 μm.
A kind of 3. Spray granulation method of silicon carbide powder according to right 1, it is characterised in that the sintering described in step 1)
Auxiliary agent is aluminium oxide and yttrium oxide (AL2O3:Y2O3=3:2).
A kind of 4. Spray granulation method of silicon carbide powder according to right 1, it is characterised in that the bonding described in step 1)
Agent is polyvinyl alcohol (PVA).
A kind of 5. Spray granulation method of silicon carbide powder according to right 1, it is characterised in that the dispersion described in step 1)
Agent is tetramethylammonium hydroxide (TMAH) and polyethylene glycol (PEG).
A kind of 6. Spray granulation method of silicon carbide powder according to right 1, it is characterised in that the slurry described in step 2)
Disperse slurry for low-viscosity stable, under suitable binding agent, dispersive agent ratio, obtain powder zeta potential and reach peak 46mV.
A kind of 7. Spray granulation method of silicon carbide powder according to right 1, it is characterised in that the spraying described in step 3)
Drying machine is centrifugal spray dryer, and 300~350 DEG C of inlet temperature, control outlet temperature is 90~110 DEG C, centrifugal atomizing
Device 8000~24000r/min of rotating speed, slurry feed rate are 5kg/h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368918A (en) * | 2019-08-15 | 2019-10-25 | 西南化工研究设计院有限公司 | A kind of Spray granulation method of boehmite powder |
| CN113372096A (en) * | 2020-03-09 | 2021-09-10 | 江苏省宜兴非金属化工机械厂有限公司 | Preparation method of low-temperature normal-pressure sintered silicon carbide composite ceramic, silicon carbide composite ceramic product prepared by preparation method and application of silicon carbide composite ceramic product |
| CN116352057A (en) * | 2023-03-27 | 2023-06-30 | 重庆罗曼新材料科技有限公司 | ZTA ceramic particle composite wear-resistant part and preparation method thereof |
-
2016
- 2016-12-13 CN CN201611146260.5A patent/CN108218433A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368918A (en) * | 2019-08-15 | 2019-10-25 | 西南化工研究设计院有限公司 | A kind of Spray granulation method of boehmite powder |
| CN113372096A (en) * | 2020-03-09 | 2021-09-10 | 江苏省宜兴非金属化工机械厂有限公司 | Preparation method of low-temperature normal-pressure sintered silicon carbide composite ceramic, silicon carbide composite ceramic product prepared by preparation method and application of silicon carbide composite ceramic product |
| CN113372096B (en) * | 2020-03-09 | 2022-08-02 | 江苏省宜兴非金属化工机械厂有限公司 | Preparation method of low-temperature normal-pressure sintered silicon carbide composite ceramic, silicon carbide composite ceramic product prepared by preparation method and application of silicon carbide composite ceramic product |
| CN116352057A (en) * | 2023-03-27 | 2023-06-30 | 重庆罗曼新材料科技有限公司 | ZTA ceramic particle composite wear-resistant part and preparation method thereof |
| CN116352057B (en) * | 2023-03-27 | 2024-06-18 | 重庆罗曼新材料科技有限公司 | ZTA ceramic particle composite wear-resistant part and preparation method thereof |
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