CN101007429A - Preparation method of ceramic slurry capable of high solid content and good fluidity - Google Patents
Preparation method of ceramic slurry capable of high solid content and good fluidity Download PDFInfo
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- CN101007429A CN101007429A CNA2007100195546A CN200710019554A CN101007429A CN 101007429 A CN101007429 A CN 101007429A CN A2007100195546 A CNA2007100195546 A CN A2007100195546A CN 200710019554 A CN200710019554 A CN 200710019554A CN 101007429 A CN101007429 A CN 101007429A
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Abstract
The invention discloses a preparation method of ceramic slurry with high solid content and good mobility. First weighing certain quality alumina powder and putting in boiling flask with temperature control and stirring device; then weighing polyacrylic acid dispersant according 0.8 to 1.8% of dry powder quality, weighing deionized water according to the solid-phase volume percentage of actual needed prepared slurry and preparing dispersant water solution, adjusting the pH to 2.5~6.5, heating to 60 ~ 95 degree C; finally, mixing the dispersant water solution and the powder body, putting it in ultrasonic instrument 5 ~ 10 mins at constant temperature 60-95DEG C, adsorbing 2~12 hours in the constant temperature stirring status after ultrasound action then preparing the slurry product. The invention reduces the structural water of solid particles surface of slurry through heating, increases the free water amount in slurry, reduces the slurry viscosity, increases the chain segment density of dispersant through temperature, increases the repelling force position energy between particles to making the slurry keep uniform and stable performance while the flowability is increased.
Description
Technical field
The present invention relates to the wet processing technology of sending out of high-performance ceramics material, be specifically related to a kind of preparation method with high solids content and good fluidity ceramic size.
Background technology
Wet moulding is a high-performance ceramics material forming method commonly used.But wet moulding is subjected to material supplier author's great attention with biscuit density height, pore multiple superiority such as ceramic component little, pore size narrowly distributing dead size forming shape complexity.A wet moulding process mainly comprises three aspects to the requirement of ceramic slurry: the one, and high solid volume fraction φ＞50%, it is high solids content, biscuit density after the high more moulding of solid volume fraction is big more, and the shrinkage factor behind the biscuit sintering is more little, and the effect of dead size moulding is unreasonable to be thought; The 2nd, good flowability, the flowability that slurry is good, promptly having lower viscosity characteristics is the wet important prerequisite of sending out the complicated and accurate ceramic material of moulding different shape; The 3rd, slurry must have good homogeneous stability, and the uniform and stable performance impact of slurry the pore size and the Size Distribution of the biscuit after the moulding, thereby the quality of final ceramic material goods is had fundamental influence.High solid volume fraction and good flowability are that low viscosity is a pair of paradox, and solid volume fraction is high more, and the flowability of slurry is more little usually.For common powder, traditional wet therapy forming process can satisfy the requirement of general ceramic material wet therapy forming process to ceramic slurry to a certain extent by the method for adding dispersant, but for being for the wet moulding of high-performance ceramics material of base-material with sub-micron and nano-powder, because the superfine powder grain diameter is little, specific surface energy is big, the surface-active height, in aqueous medium, highly active powder granule and hydrone effect, a large amount of Free water are converted into constitution water, be difficult to make slurry when having high solid volume fraction, to keep good flowability again, and when the solid volume fraction of slurry is very high, intergranular distance is little, and interparticle active force is strong, and particle is easy to reunite and loses the original special performance of ultra-fine grain.The surface modification of superfine powder is the major technique approach that present people address this problem, but because the processing technology for surface modification complexity, technical difficulty is big, thereby has restricted the extensive use of superfine powder in high-performance ceramics material field.
Summary of the invention
The objective of the invention is to: a kind of preparation method with high solids content and good fluidity ceramic size is provided, the ceramic size that this method is produced has high solid volume, has good flowability simultaneously, for dead size moulding high-performance ceramics material provides desirable slurry.
Technical solution of the present invention is that this method may further comprise the steps: the powder that at first takes by weighing certain mass places the flask of band temperature control agitating device; Then according to actual needs the preparation the slurry solid volume fraction, be the volume of powder: the volume sum of the volume of powder and solvent is measured the deionized water of certain volume, press 0.8～1.8% weighing polyacrylic dispersant of superfine powder dry powder quality, dispersant and water are mixed and made into aqueous dispersant, regulate pH value to 2.5～6.5, be heated to 60～95 ℃; At last aqueous dispersant is mixed with powder, is placed in the ultrasonoscope through stirring, ultrasonic 5～10min under constant temperature 60-95 ℃ condition, after ultrasonication, under the constant temperature stirring, adsorb 2～12h get final product the finished product slurry.
Mechanism of the present invention: the superfine powder specific grain surface is long-pending big, and the surface exists a large amount of unsaturated dangling bonds.Be in the dispersion of decentralized photo with water, the interaction between ultrafine particle and hydrone makes large quantity of moisture become constitution water, and in the dispersion of high solid volume fraction, the formation of this a large amount of constitution waters descends the flowability of slurry.Temperature has very big influence to the performance of slurry, and on the one hand, temperature raises, and the effect between powder granule surface and hydrone is weakened, and the quantity of constitution water molecule reduces, and the free moisture quantum count increases, and helps the improvement of slurry fluidity; On the other hand, the minimizing of constitution water makes the hydration shell thickness attenuation of particle surface, is unfavorable for stability of slurry.But for be dispersant with polyacrylic acid (PAA), polypropylene ammonium salt or sodium salt and PAA/PEOA copolymer, with α-Al
2O
3Or α-Al
2O
3-ZrO
2Be the slurry system of powder as dispersate, because temperature raises, dispersant is at α-Al
2O
3The adsorbance of particle surface improves with temperature and increases, utilize this relation, improve the segment density of ceramic grain surface dispersant, increase intergranular space steric effect, Yin Wendu improves with compensation, hydration effect weakens and makes the negative effect that particle agglomeration is inclined to be increased, thereby makes high solid volume fraction slurry both keep higher dispersion stabilization, has desirable flowability simultaneously again
The invention has the beneficial effects as follows: significantly reduce the viscosity of high solid volume fraction φ＞50%vol slurry, improve its flowability; Simultaneously slurry prepares under a certain definite temperature, has overcome conventional method and has caused difference on the different batches slurry performance because of variation of ambient temperature, thereby improved the repeatability of finished product ceramic material final performance.
The specific embodiment
The present invention is described further below in conjunction with some specific embodiments.
Example 1:
Be averaged α-Al that particle diameter is 0.51 μ m
2O
3Powder 160g places flask at the bottom of the garden; Taking by weighing molecular weight by the mass ratio 1.5% of aluminium oxide dry powder is 9000～1000 ammonium polyacrylate (PAA-NH
4) dispersant 2.40g, the deionized water of dispersant and 30ml mixes, and is heated to 85 ℃ after the HCl adjusting pH value to 4.5 with 0.5M; Aqueous dispersant is poured in the powder, mixed, ultrasonic 5min in 85 ℃ water bath with thermostatic control continues absorption 12h and gets slurry under 85 ℃ and stirring.This slurry solid content is that solid volume fraction is 57%vol, and with its flowability of rotary viscosity instrumentation, recording its apparent viscosity is 0.35Pa.s; This slurry with 20 ℃ down the slurry of the identical solid volume fractions of preparation compare, its apparent viscosity drop to 16% (20 ℃, η=0.42Pa.s).
Example 2:
Get α-Al
2O
3-ZrO
2Composite granule 200g, wherein α-Al
2O
3Content is 80%, α-Al
2O
3And ZrO
2Average grain diameter is respectively 0.51 μ m and 0.43 μ m; Measure dried up 38ml and molecular weight and be 12000～14000 PAA/PEO copolymer dispersant 3.6g and mix, regulate pH value to 3.5, be heated to 95 ℃; Aqueous dispersant is poured powder into and is mixed, and ultrasonic 10min in 95 ℃ water bath with thermostatic control continues absorption 10h and gets slurry under 95 ℃ and stirring.This slurry solid content is that solid volume fraction is 53%vol, and with its flowability of rotary viscosity instrumentation, recording its apparent viscosity is 0.39Pa.s; This slurry with 20 ℃ down the slurry of the identical solid volume fractions of preparation compare, its apparent viscosity descend and be about 22% (20 ℃, η=0.50Pa.s).
Example 3:
Take by weighing α-Al that average grain diameter is 0.68 μ m
2O
3Powder 200g places flask at the bottom of the garden; Taking by weighing and accounting for alumina dry grain weight 1.8% molecular weight is 12000～14000 PAA/PEO dispersant 3.0g, and dispersant is mixed with the deionized water of 32ml, with regulating pH value to 5.0, is heated to 90 ℃; Aqueous dispersant is poured in the powder, fully stirs, and ultrasonic 6min in 90 ℃ the water bath with thermostatic control, absorption 8h gets slurry under 90 ℃ and stirring.This slurry solid content is that solid volume fraction is 61%vol, with its flowability of rotary viscosity instrumentation, recording its apparent viscosity is 0.78Pa.s, and this slurry is compared with the slurry of 20 ℃ of identical solid volume fractions that prepare down, its apparent viscosity descend and be about 12% (20 ℃, η=0.89Pa.s).
Example 4
Get α-Al
2O
3-ZrO
2Composite granule 180g, wherein α-Al
2O
3Content is 80%, α-Al
2O
3And ZrO
2Average grain diameter is respectively 0.51 μ m and 0.43 μ m; Measure water 31ml and molecular weight and be 8000～9000 polyacrylic acid (PAA) dispersant 2.8g and mix, be heated to 80 ℃; Aqueous dispersant and powder mix, and ultrasonic 8min in 80 ℃ water bath with thermostatic control continues absorption 6h and gets slurry under 80 ℃ and stirring.This slurry solid content is that solid volume fraction is 57%vol, and with this slurry its flowability of rotary viscosity instrumentation, recording its apparent viscosity is 0.62Pa.s; This slurry with 20 ℃ down the slurry of the identical solid volume fractions of preparation compare, its apparent viscosity descend and be about 16% (20 ℃, η=0.74Pa.s).
Example 5:
Be averaged α-Al that particle diameter is 0.51 μ m
20
3Powder 160g places flask at the bottom of the garden, and taking by weighing molecular weight by the mass ratio 0.8% of aluminium oxide dry powder is 9000～1000 ammonium polyacrylate (PAA-NH
4) dispersant 1.3g, the deionized water of dispersant and 40ml mixes, and is heated to 60 ℃ after the HCl adjusting pH value to 2.5 with 0.5M; Aqueous dispersant is poured in the powder, mixed, ultrasonic 5min in 60 ℃ water bath with thermostatic control continues absorption 2h and gets slurry under 60 ℃ and stirring.This slurry solid content is that solid volume fraction is 50%vol, and with its flowability of rotary viscosity instrumentation, recording its apparent viscosity is 0.22Pa.s; This slurry with 20 ℃ down the slurry of the identical solid volume fractions of preparation compare, its apparent viscosity descend and be about 12% (20 ℃, η=0.25Pa.s).
Example 6:
Be averaged α-Al that particle diameter is 0.51 μ m
2O
3Powder 160g places flask at the bottom of the garden; Taking by weighing molecular weight by the mass ratio 1.0% of aluminium oxide dry powder is 9500～1100 Sodium Polyacrylate (PAA-Na) dispersant 1.6g, and the deionized water of dispersant and 30ml mixes, and is heated to 70 ℃ after regulating pH value to 5.5 with the HCl of 0.5M; Aqueous dispersant is poured in the powder, mixed, ultrasonic 10min in 70 ℃ water bath with thermostatic control continues absorption 4h and gets slurry under stirring.This slurry solid content is that solid volume fraction is 57%vol, and with its flowability of rotary viscosity instrumentation, recording its apparent viscosity is 0.41Pa.s; This slurry with 20 ℃ down the slurry of the identical solid volume fractions of preparation compare, its apparent viscosity descend and be about 10% (20 ℃, η=0.46Pa.s).
Claims (2)
1. preparation method with high solids content and good fluidity ceramic size, this method may further comprise the steps: the ultra-fine alumina powder body that at first takes by weighing certain mass places the flask of band temperature control agitating device; Press 0.8～1.8% weighing polyacrylic dispersant of superfine powder dry powder quality then, Zhi Bei slurry solid volume fraction is measured deionized water and is mixed with aqueous dispersant according to actual needs, regulates pH value to 2.5～6.5, is heated to 60～95 ℃; At last aqueous dispersant is mixed with powder, constant temperature 60-95 ℃ of ultrasonic 5～10min after ultrasonication, adsorbs 2～12h and gets slurry under the constant temperature stirring in ultrasonoscope.
2. a kind of preparation method with high solids content and good fluidity ceramic size according to claim 1, it is characterized in that: dispersant is ammonium polyacrylate PAA-NH
4, PAA-PEO copolymer, polyacrylic acid PAA or PAA-Na.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100195546A CN101007429A (en) | 2007-01-13 | 2007-01-13 | Preparation method of ceramic slurry capable of high solid content and good fluidity |
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|---|---|---|---|
| CNA2007100195546A CN101007429A (en) | 2007-01-13 | 2007-01-13 | Preparation method of ceramic slurry capable of high solid content and good fluidity |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102522557A (en) * | 2011-10-24 | 2012-06-27 | 连云港连连化学有限公司 | Preparation method for high-purity ultrathin easily-dispersible aluminum oxide for lithium ion battery |
| CN103121835A (en) * | 2012-12-12 | 2013-05-29 | 上海电气钠硫储能技术有限公司 | Na precursor powdery sizing agent for synthesizing beta''-aluminum oxide ceramics and preparation method of Li precursor powdery sizing agent |
| CN107129283A (en) * | 2017-05-12 | 2017-09-05 | 南京工业大学 | A kind of photocuring 3D printing high solid loading ceramic slurry and its preparation technology |
| CN113954234A (en) * | 2021-10-21 | 2022-01-21 | 东莞市景泰机电设备有限公司 | Ceramic production slurry treatment method |
| CN114605157A (en) * | 2022-03-21 | 2022-06-10 | 广东工业大学 | Photocuring aluminum nitride ceramic slurry and preparation method thereof |
-
2007
- 2007-01-13 CN CNA2007100195546A patent/CN101007429A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102522557A (en) * | 2011-10-24 | 2012-06-27 | 连云港连连化学有限公司 | Preparation method for high-purity ultrathin easily-dispersible aluminum oxide for lithium ion battery |
| CN103121835A (en) * | 2012-12-12 | 2013-05-29 | 上海电气钠硫储能技术有限公司 | Na precursor powdery sizing agent for synthesizing beta''-aluminum oxide ceramics and preparation method of Li precursor powdery sizing agent |
| CN107129283A (en) * | 2017-05-12 | 2017-09-05 | 南京工业大学 | A kind of photocuring 3D printing high solid loading ceramic slurry and its preparation technology |
| CN113954234A (en) * | 2021-10-21 | 2022-01-21 | 东莞市景泰机电设备有限公司 | Ceramic production slurry treatment method |
| CN114605157A (en) * | 2022-03-21 | 2022-06-10 | 广东工业大学 | Photocuring aluminum nitride ceramic slurry and preparation method thereof |
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Open date: 20070801 |