CN109111232A - 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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- CN109111232A CN109111232A CN201710485752.5A CN201710485752A CN109111232A CN 109111232 A CN109111232 A CN 109111232A CN 201710485752 A CN201710485752 A CN 201710485752A CN 109111232 A CN109111232 A CN 109111232A
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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
- C04B35/565—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 silicon carbide
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- 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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Abstract
The invention discloses a kind of Spray granulation method 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 it is suitable for manufacturing the high performance silicon carbide ceramics of high-compactness that the uniformity and compactness for obtaining biscuit, which improve,.The present invention is achieved by following scheme: weighing 40~60wt% silicon carbide micro-powder, 7~13wt% sintering aid, 1~5wt% binder, 0.1~0.5wt% dispersant A, 0.5~2.5wt% disperses B, a certain amount of deionized water is added by the way of ball milling, controls suitable ball milling parameter and obtains the stable dispersion slurry that solid content is 40~60%.Above-mentioned resulting slurry is injected directly into sponging granulator, obtains being granulated powder by technological parameters such as control mist projection granulating import/export temperature, centrifugal atomizer revolving speed, slurry feed rates.
Description
Technical field
This patent is related to a kind of Spray granulation method of silicon carbide powder.
Background technique
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, petroleum, 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 optimizes material structure to improve material property, 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 reduces agglomerating plant requirement and sintering cost, and improves sintering character.In liquid-phase sintering, how to guarantee sintering aid
It is evenly dispersed be very important link, while improve the uniformity of biscuit and consistency be the key that high-performance ceramic preparation
Technology.Therefore it is required that powder has extraordinary processing performance, comprising: mobility, filling property, compactness and mouldability etc., and
Each ingredient can be evenly dispersed.
Spray granulation is to start to be applied to advanced ceramics production field with the raising for requiring powder processing performance.
To ceramic slurry be 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 not only can be improved, be conducive to the density, uniformity and the agglutinating property that improve biscuit
Energy.
Ceramic industry traditionally uses organic solvent system to be spray-dried, but there are problems, such as: organic solvent valence
Lattice are higher, recycling is cumbersome and explosion accident is easy to happen in high-temperature drying procedures.In special cermacis field, water base body
It is slurry spray drying technology is still a kind of newer dry technology, the application in silicon carbide ceramics needs further development
With it is perfect.
Summary of the invention
This patent carries out mist projection granulating to silicon carbide aqueous compound slurry using centrifugal spray granulation technology, provides one kind
The Spray granulation method high, at low cost with yield, powder processing performance is good.Carborundum powder liquid flowability is significantly after mist projection granulating
It improves, processability is good, and the uniformity and compactness for obtaining biscuit improve, and is suitable for manufacturing the high performance silicon carbide pottery of high-compactness
Porcelain.
The technical solution adopted by the present invention: a kind of Spray granulation method of silicon carbide powder, specifically includes the following steps:
1) ingredient: silicon carbide powder, sintering aid, binder, dispersant A, B are weighed according to following weight ratio:
40~60wt% of silicon carbide micro-powder, sintering aid 7~13%: 1~5wt% of binder, 0.1~0.5wt% of dispersant A, dispersion
B0.5~2.5wt%.The suspension that deionized water is made into 40~60wt% of solid content is added.
2) ball milling slurrying: raw materials various in step 1) are put in polytetrafluoroethylene (PTFE) ball grinder, and ball milling ball is added and is 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: the resulting slurry of 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 binder of the present invention is polyvinyl alcohol (PVA), and PVA has very strong polarity.Test PVA alcoholysis degree used
88%, average molecular weight 1700 or so.
The above-mentioned dispersing agent of the present invention is tetramethylammonium hydroxide (TMAH) and polyethylene glycol (PEG).TMAH be alkalinity most
Strong organic matter is the preferable dispersing agent 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 an aqueous medium
It is fully extended, forms steric hindrance layer, hinder the Collision coagulation and gravitational settling of particle, PEG and TMAH are added jointly can increase ζ electricity
Position, is conducive to SiC ceramic powder by electrostatic stabilization mechanism and reaches stable dispersion.
Slurry obtained in step 2) of the present invention is that low-viscosity stable disperses slurry, in suitable binder, dispersing agent ratio
Under example, obtains 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 revolving speed, and slurry feed rate is 5kg/
h。
Technical effect
Gained mist projection granulating mealiness can be as follows, Electronic Speculum observation: powder in regular spherical, 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 performance, pine fills close
Degree improves 50% or more, 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 the processing performance of mist projection granulating processing powder be improved significantly, it is high to obtain biscuit density, fits
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 powder, 80g sintering aid, 20g binder, 2g dispersant A, 5g dispersant B is weighed to claim in proportion
Amount is added deionized water and is made into the suspension that solid content is 50%.This solution is placed on ball mill, 2000g ball milling ball is added,
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, controls 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 60mPas.The observation of mist projection granulating powder Electronic Speculum: 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 larger 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 powder, 80g sintering aid, 20g binder, 2g dispersant B, 5g dispersing agent C is weighed to claim in proportion
Amount is added deionized water and is made into the suspension that solid content is 50%.This solution is placed on ball mill, 2000g ball milling ball is added,
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 60mPas.The observation of mist projection granulating powder Electronic Speculum: 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 larger 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 powder, 80g sintering aid, 20g binder, 2g dispersant B, 5g dispersing agent C is weighed to claim in proportion
Amount is added deionized water and is made into the suspension that solid content is 40%.This solution is placed on ball mill, 2000g ball milling ball is added,
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 30mPas.The observation of mist projection granulating powder Electronic Speculum: powder is in regular ball
Shape, pelletizing surface are regular, smooth.Size distribution is in Unimodal Distribution, and larger 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 the following steps:
1) ingredient: silicon carbide powder, sintering aid, binder, dispersant A, B are weighed according to following weight ratio: carbonization
40~60wt% of silicon powder, sintering aid 7~13%: 1~5wt% of binder, 0.1~0.5wt% of dispersant A disperse B0.5
~2.5wt%.The suspension that deionized water is made into solid content 40~60% is added.
2) ball milling slurrying: raw materials various in step 1) are put in polytetrafluoroethylene (PTFE) ball grinder, and ball milling ball is added and is 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, and 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: the resulting slurry of step 2) is injected directly into sponging granulator, passes through control atomizing granulating technology ginseng
Number obtains being granulated powder.
2. a kind of Spray granulation method of silicon carbide powder according to right 1, it is characterised in that carbonization described in step 1)
The D50 of silicon powder is 0.6 μm.
3. a kind of Spray granulation method of silicon carbide powder according to right 1, it is characterised in that sintering described in step 1)
Auxiliary agent is aluminium oxide and yttrium oxide (AL2O3: Y203=3: 2).
4. a kind of Spray granulation method of silicon carbide powder according to right 1, it is characterised in that bonding described in step 1)
Agent is polyvinyl alcohol (PVA).
5. a kind of Spray granulation method of silicon carbide powder according to right 1, it is characterised in that dispersion described in step 1)
Agent is tetramethylammonium hydroxide (TMAH) and polyethylene glycol (PEG).
6. a kind of Spray granulation method of silicon carbide powder according to right 1, it is characterised in that slurry described in step 2)
Disperse slurry for low-viscosity stable, under suitable binder, dispersive agent ratio, obtains powder zeta potential and reach peak 46mV.
7. a kind of Spray granulation method of silicon carbide powder according to right 1, it is characterised in that be sprayed 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 revolving speed, slurry feed rate are 5kg/h.
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| CN201710485752.5A CN109111232A (en) | 2017-06-23 | 2017-06-23 | A kind of Spray granulation method of silicon carbide powder |
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Cited By (2)
| 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 |
| CN115925429A (en) * | 2022-03-22 | 2023-04-07 | 南通三责精密陶瓷有限公司 | Manufacturing method of ceramic composite material 3D printing wire |
-
2017
- 2017-06-23 CN CN201710485752.5A patent/CN109111232A/en active Pending
Cited By (2)
| 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 |
| CN115925429A (en) * | 2022-03-22 | 2023-04-07 | 南通三责精密陶瓷有限公司 | Manufacturing method of ceramic composite material 3D printing wire |
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