CN106854081A - 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
A kind of Spray granulation method of silicon carbide powder of the present invention, the features such as it has yield high, low cost, good powder processing performance.Carborundum powder liquid flowability is greatly improved after mist projection granulating, and processability is good, and the uniformity and compactness for obtaining biscuit are improved, and suitably manufacture 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 by the way of ball milling, controls suitable ball milling parameter to obtain the stable dispersion slurry that solid content is 40~60%.The slurry of above-mentioned gained is injected directly into sponging granulator, obtains granulating powder by controlling the technological parameters such as mist projection granulating import/export temperature, centrifugal atomizer rotating speed, slurry feed rate.
Description
Technical field
The invention belongs to ceramic technology field, it 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, with high rigidity, high intensity, high high-temp stability,
Wear-resistant, acid-alkali-corrosive-resisting, low-expansion coefficient, high thermal conductivity, good thermal shock, creep resistant and
The advantages of antioxygenic property is good, in the industrial circles such as machinery, electronics, oil, chemical industry, metallurgy and national defence
The fields such as industry are widely used.
With carborundum industrial expansion, people to the research of carborundum and its phase material and application development very
Rapidly, in order to improve material property, optimize material structure, especially consider from raising material fracture toughness,
The research focus to silicon carbide ceramics concentrate on normal atmosphere sintering method both at home and abroad -- in liquid-phase sintering.Normal pressure liquid phase
Sintering is that, with a number of polynary eutectic oxide as sintering aid, sintering aid is formed altogether at high temperature
Liquation phase, acceleration of sintering process, reduces sintering temperature, makes agglomerating plant requirement and sintering cost reduction,
And improve sintering character.In liquid-phase sintering, how to ensure that the dispersed of sintering aid is very important
Link, while the uniformity and consistency that improve biscuit are key technologies prepared by high-performance ceramic.Therefore
Seeking powder has extraordinary processing performance, including：Mobility, filling property, compactness and mouldability etc.,
And each composition can be with dispersed.
Spray granulation is produced with starting to be applied to advanced ceramics to the raising that powder processing performance is required
Field.Ceramic slurry is spray-dried can not only avoid reuniting again and sedimentation separation for each component, protect
The original uniformity of slurry is held；Slurry atomization is uniform simultaneously, obtain regular shape, even particle size distribution,
The pelletizing of good fluidity and suitable continuous automatic moulding.Not only can with improve production efficiency and product stability,
Be conducive to improving density, uniformity and the sintering character of biscuit.
Ceramic industry is traditionally spray-dried using organic solvent system, but there are problems, such as：Have
Machine solvent price is higher, it is cumbersome to recycle and explosion accident is susceptible in high-temperature drying procedures.
Special cermacis field, aqueous based systems slurry spray drying technology is still a kind of newer dry technology, in carbon
Application in SiClx ceramics needs further to develop and perfect.
The content of the invention
The present invention carries out mist projection granulating using centrifugal spray granulation technology to silicon carbide aqueous compound slurry, there is provided
It is a kind of with yield is high, the good Spray granulation method of low cost, powder processing performance.Carbon after mist projection granulating
SiClx powder fluidity is greatly improved, and processability is good, and the uniformity and compactness for obtaining biscuit are improved, and are fitted
Preferably manufacture the high performance silicon carbide ceramics of high-compactness.
A kind of Spray granulation method of silicon carbide powder of the present invention, it is comprised the following steps：
1) dispensing：By silicon carbide powder, sintering aid, binding agent, dispersant A, B according to following weight ratio
Weighed：40~60wt% of silicon carbide micro-powder, sintering aid 7~13%：1~5wt% of binding agent, dispersant
A0.1~0.5wt%, disperses B0.5~2.5wt%.Deionized water is added to be made into the suspension of 40~60wt% of solid content
Liquid.
2) ball milling slurrying：By step 1) in various raw materials, be put in polytetrafluoroethylene (PTFE) ball grinder, add ball
Abrading-ball is placed on planetary ball mill, carries out ball mill mixing.It is determined that suitable milling parameters, steady to obtain
Fixed scattered slurry.Wherein：Ball milling ball uses silicon carbide material, big ball bulb diameter to be about 9mm, and bead ball is straight
Footpath is about 4mm, and big ball pellet quality ratio is 3:2, ratio of grinding media to material be medium ball with the weight ratio of powder for (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：By step 2) obtained by slurry be injected directly into sponging granulator, by control spray
Mist granulation process parameters obtain granulating powder.
The D50 of silicon carbide micro-powder of the present invention is 0.6 μm, and sintering aid is aluminum oxide and yittrium oxide
(AL2O3:Y2O3=3:2), binding agent is polyvinyl alcohol (PVA), and PVA has very strong polarity, and experiment is used
PVA alcoholysis degrees 88%, mean molecule quantity 1700 or so, dispersant is TMAH (TMAH) and gathers
Ethylene glycol (PEG).TMAH is the most strong organic matter of alkalescence, is the preferable dispersant of effect in SiC aqueous slurries.
Nonionic surface active agent PEG is worked as polymeric by steric hindrance type dispersal mechanism, and one
On the surface of solid particle, the other end can be fully extended in aqueous medium for end absorption, form steric hindrance layer, resistance
Hinder the Collision coagulation and gravitational settling of particle, PEG and TMAH is added jointly can increase zeta potential, be conducive to SiC
Ceramic powder reaches stable dispersion by electrostatic stabilization mechanism.
Step 2 of the present invention) in gained slurry for low-viscosity stable disperse slurry, suitable binding agent, point
Under powder ratio, obtain powder current potential and reach peak 46mV.
Step 3 of the present invention) in slurry is spray-dried using centrifugal spray dryer, inlet temperature
300~350 DEG C, it is 90~110 DEG C to control outlet temperature, centrifugal atomizer 8000~24000r/min of rotating speed,
Slurry feed rate is 5kg/h.
Technique effect
Gained mist projection granulating mealiness can be, electron microscopic 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, under different technology conditions, middle position
Particle diameter is substantially at 10~100 μm.Granulation powder pine 0.83~0.91g/cm3 of packed density, 22~29 ° of angle of repose.
Compared with SiC original micro mist performances, apparent density improves more than 50%, and angle of repose first mate reduces.Pelletizing is existed
After 40~160Mpa is dry-pressing formed, the relative density of biscuit is up to 58%.
In sum, by mist projection granulating treatment powder processing performance be improved significantly, obtain biscuit close
Degree is high, suitably prepares the high performance silicon carbide ceramics of high-compactness.
Specific embodiment
The present invention is described in further detail below by specific embodiment, but the present invention be not limited only to
Lower embodiment.
Embodiment 1：
Weigh 1000g silicon carbide powders, 80g sintering aids, 20g binding agents, 2g dispersant As, 5g dispersant Bs
Weigh in proportion, add deionized water to be made into the suspension that solid content is 50%.This solution is placed on ball mill,
2000g ball milling balls are added, the ball milling 4h under conditions of 480r/min obtains the slurry of stable dispersion, by gained
Slurry is injected directly into sponging granulator, and inlet temperature is 300 DEG C, and control outlet temperature is in 90 DEG C, atomizer
Rotating speed 12000r/min, obtains mist projection granulating powder.
Test analysis are as follows, and the viscosity of gained slurry is 60mPa ﹒ s.Mist projection granulating powder electron microscopic observation：Powder
Spherical in rule, pelletizing surface is regular, smooth and texture is uniform.Size distribution is in Unimodal Distribution, particle diameter
Narrowly distributing, it will be seen that large-size diameter is between 50~70 μm.Granulation powder pine packed density 0.9g/cm3, not
22 ° of angle till, by pelletizing after 160Mpa is dry-pressing formed, the density of biscuit is 1.89g/cm3, relative density
Reach 58%.
Embodiment 2：
Weigh 1000g silicon carbide powders, 80g sintering aids, 20g binding agents, 2g dispersant Bs, 5g dispersing agent Cs
Weigh in proportion, add deionized water to be made into the suspension that solid content is 50%.This solution is placed on ball mill,
2000g ball milling balls are added, the ball milling 4h under conditions of 480r/min obtains the slurry of stable dispersion, by gained
Slurry is injected directly into sponging granulator, controls inlet temperature for 300 DEG C, and outlet temperature is in 90 DEG C, atomizer
Rotating speed 24000r/min, obtains mist projection granulating powder.
Test analysis are as follows, and the viscosity of gained slurry is 60mPa ﹒ s.Mist projection granulating powder electron microscopic observation：Powder
Spherical in rule, pelletizing surface is regular, smooth and texture is uniform.Size distribution is in Unimodal Distribution, particle diameter
Narrowly distributing, large-size diameter is between 50~60 μm.Granulation powder pine packed density 0.86g/cm3, angle of repose
29°。
Embodiment 3：
Weigh 1000g silicon carbide powders, 80g sintering aids, 20g binding agents, 2g dispersant Bs, 5g dispersing agent Cs
Weigh in proportion, add deionized water to be made into the suspension that solid content is 40%.This solution is placed on ball mill,
2000g ball milling balls are added, the ball milling 4h under conditions of 480r/min obtains the slurry of stable dispersion, by gained
Slurry is injected directly into sponging granulator, controls inlet temperature for 300 DEG C, and outlet temperature is in 90 DEG C, atomizer
Rotating speed 12000r/min, obtains mist projection granulating powder.
Test analysis are as follows, and the viscosity of gained slurry is 30mPa ﹒ s.Mist projection granulating powder electron microscopic observation：Powder
Spherical in rule, pelletizing surface is regular, smooth.Size distribution is in Unimodal Distribution, and large-size diameter is situated between
In 50~100 μm.Granulation powder pine packed density 0.83g/cm3,28 ° of angle of repose.
Claims (4)
1. a kind of Spray granulation method of silicon carbide powder, it is characterised in that comprise the following steps：
1) dispensing：By silicon carbide powder, sintering aid, binding agent, dispersant A, B according to following weight
Than being weighed：40~60wt% of silicon carbide micro-powder, sintering aid 7~13%：1~5wt% of binding agent, dispersion
Agent A0.1~0.5wt%, disperses B0.5~2.5wt%.Deionized water is added to be made into the outstanding of solid content 40~60%
Supernatant liquid.
2) ball milling slurrying：By step 1) in various raw materials, be put in polytetrafluoroethylene (PTFE) ball grinder, add ball
Abrading-ball is placed on planetary ball mill, carries out ball mill mixing.It is determined that suitable milling parameters, steady to obtain
Fixed scattered slurry.Wherein：Ball milling ball uses silicon carbide material, big ball bulb diameter to be about 9mm, and bead ball is straight
Footpath is about 4mm, and big ball pellet quality ratio is 3:2, ratio of grinding media to material be medium ball with the weight ratio of powder for (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：By step 2) obtained by slurry be injected directly into sponging granulator, by control spray
Mist granulation process parameters obtain granulating powder.
2. a kind of Spray granulation method of the silicon carbide powder according to right 1, it is characterised in that step
1) D50 of the silicon carbide micro-powder described in is 0.6 μm；Sintering aid is aluminum oxide and yittrium oxide
(AL2O3:Y2O3=3:2)；Binding agent is polyvinyl alcohol (PVA)；Dispersant is TMAH (TMAH)
With polyethylene glycol (PEG).
3. the Spray granulation method of a kind of silicon carbide powder according to right 1, it is characterised in that slurry is
Low-viscosity stable disperses slurry, under suitable binding agent, dispersive agent ratio, obtains powder current potential and reaches most
High level 46mV.
4. the Spray granulation method of a kind of silicon carbide powder according to right 1, it is characterised in that spraying is dry
Dry machine is centrifugal spray dryer, and 300~350 DEG C of inlet temperature controls outlet temperature for 90~110 DEG C,
Centrifugal atomizer 8000~24000r/min of rotating speed, slurry feed rate is 5kg/h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249928A (en) * | 2018-01-18 | 2018-07-06 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of solid-phase sintered silicon carbide ceramics wet moulding low viscosity high solids content water-based slurry |
| 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 |
-
2015
- 2015-12-08 CN CN201510902410.XA patent/CN106854081A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249928A (en) * | 2018-01-18 | 2018-07-06 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of solid-phase sintered silicon carbide ceramics wet moulding low viscosity high solids content water-based slurry |
| 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 |
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Application publication date: 20170616 |