CN102515511B - Preparation method for quartz slurry for casting - Google Patents
Preparation method for quartz slurry for casting Download PDFInfo
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- CN102515511B CN102515511B CN201110460905.3A CN201110460905A CN102515511B CN 102515511 B CN102515511 B CN 102515511B CN 201110460905 A CN201110460905 A CN 201110460905A CN 102515511 B CN102515511 B CN 102515511B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention discloses a preparation method for quartz slurry for casting. The preparation method comprises the steps of primary slurry preparation, homogenization, material mixing, vacuum stirring and defoaming, and the like. The primary slurry preparation relates to preparation of primary slurry with different particle diameters by ball-milling fused quartz raw material, wherein the primary slurry is classified into primary slurry with the particle diameters below 10 Mum, primary slurry with the particle diameters ranging from 10 to 30 Mum and primary slurry with the particle diameters ranging from 30 to 700 Mum; a dispersant is added in the ball-milling process; and the primary slurry with the different particle diameters are homogenized respectively, then subject to graduation mixing, and finally subject to vacuum stirring and defoaming. Through the adoption of the slurry-slurry graduation mixing mode, the material mixing time is effectively shortened; besides, as the dispersant is added in the preparation process of the primary slurry, the dispersivity of the slurry is improved.
Description
[technical field]
The present invention relates to injection forming technical field, particularly relate to a kind of preparation method of quartz slurry for casting.
[background technology]
The preparation technology of quartz crucible for casting polycrystalline silicon ingot has injection forming and notes two kinds of solidification formings.Wherein, injection forming can be divided into two kinds of one side slip casting and two-sided slip castings, and the preparation method of quartzy slurry is injection forming, prepares the core technology of quartz crucible for casting polycrystalline silicon ingot.
The quartzy blank preparation technics that tradition injection forming is prepared quartz crucible for casting polycrystalline silicon ingot is: first quartzy powder wet ball grinding is obtained to magma, by old 4～96 hours of magma, by the magma batch mixing after old.Batch mixing adopts different grain size scope powder is carried out to grating mixing, and grating particle size range 5～10 μ m (Ma Erwen 2000 detects D50) are one-level, and 10～30 μ m are one-level, and 30 μ m are one-level above.During mixing, add a certain amount of binding agent, mixing time is 2～192 hours, then the slurry mixing is carried out to vacuum stirring and eliminates bubble, thereby make, meets the slurry that cast requires.
Tradition preparation technology's main drawback is: magma is mixed with powder, and efficiency is low; Slurry easily produces sedimentation.
[summary of the invention]
Based on this, be necessary to provide a kind of preparation method that can improve the quartz slurry for casting of batch mixing efficiency and slurry dispersiveness.
For this reason, propose a kind of preparation method of quartz slurry for casting, it is characterized in that, step is as follows:
(1) prepare magma
Utilize fused quartz raw material ball to grind standby magma a, b and c, after ball milling, the water-content of magma a, b and c (mass ratio) is 9%～25%, wherein the size distribution of magma a is > 0 and < 10 μ m, the size distribution of magma b is 10～30 μ m, the size distribution of magma c be > 30 and≤700 μ m;
In mechanical milling process, add dispersion agent respectively in magma a, b and c, adding proportion 5-100ppm, wherein adds current potential dispersion agent in magma a, adds current potential dispersion agent and/or organic dispersing agent in magma b, adds organic dispersing agent in magma c;
(2) homogenizing
By magma a, b and c difference homogenizing, the homogenizing time is 10～150 hours;
(3) batch mixing
Magma a, b and c are mixed according to following mass ratio, and mixing time is 0.5～10 hour;
Magma a:10%～70%, magma b:5%～40%, magma c:15%～50%;
(4) vacuum stirring de-bubble
The magma mixing is stirred to de-bubble under-100 to-10KPa vacuum condition, and churning time is 1～10 hour.
In a preferred embodiment, described organic dispersing agent is macrogol hard fatty acids fat.
In a preferred embodiment, described current potential dispersion agent is polyacrylamide.
In a preferred embodiment, in the process of batch mixing, according to mass ratio 0.001%～1.5%, add binding agent.
In a preferred embodiment, described all turn to old.
In a preferred embodiment, described vacuum stirring is carried out in vacuum stirring device.
In a preferred embodiment,
(1) described magma a makes by mode below:
With 0～60mm piece material 1t, 4-20 order particle 2t and water 0.42t, be milled to D50:8.3 μ m, water-content (mass ratio) 14%, adds polyethylene of dispersing agent glycol hard fatty acids fat, and addition is 40ppm;
(2) described magma b makes by mode below:
With 0～60mm piece material 1t, 4-20 order particle 2t, water 0.3t, be milled to D50:15 μ m, water-content (mass ratio) 10%, adds polyethylene of dispersing agent glycol hard fatty acids fat, and addition is 20ppm;
(3) described magma c makes by mode below:
With 0～60mm piece material 1t, 4-20 order particle 2t, water 0.3t, be milled to D50:40 μ m, water-content (mass ratio) 10%, adds dispersion agent polyacrylamide, and addition is 100ppm;
In a preferred embodiment, described magma a, b and c are in homogenizing case old 6 days respectively.
In a preferred embodiment, described magma a, b and c mix according to mass ratio at 4: 2: 4, and wherein the quality of magma a, b and c is respectively 400kg, 200kg and 400kg; Mix the CMC solution 4kg that adds 1.5% (mass ratio) after 2 hours, and then mix 1 hour.
In a preferred embodiment, the slurry mixing is put into vacuum stirring device and vacuumize stirring, vacuum tightness is-50KPa.
The preparation method of above-mentioned quartz slurry for casting, adopts slurry to carry out with slurry the mode that grating is mixed, and can effectively shorten mixing time, by add dispersion agent in preparation magma process, has effectively improved slurry dispersed in addition.
[embodiment]
The preparation method of the quartz slurry for casting of present embodiment, comprises the steps such as preparation magma, homogenizing, batch mixing and vacuum stirring de-bubble.
1, preparation magma:
Ball milling, first grinds slurry with fused quartz raw material ball.
Ball milling particle diameter, the particle diameter different according to grating ball milling, 10 μ m (micron) are with next stage, 10～30 μ m one-levels, 30～700 μ m one-levels, make magma a, b and c thus, and after ball milling, the moisture mass ratio of magma a, b and c is 9%～25%.
In mechanical milling process, add dispersion agent, adding proportion 5-100ppm (parts permillion, PPM); Wherein the magma a below particle diameter 10 μ m adds current potential dispersion agent, in the magma b of particle diameter 10～30 μ m, add current potential and/or organic dispersing agent, in the magma c of particle diameter 30～700 μ m, add organic dispersing agent, wherein current potential dispersion agent is macrogol hard fatty acids fat, organic dispersing agent is polyacrylamide, magma b can add current potential dispersion agent and organic dispersing agent simultaneously, also can only add wherein a kind of.
2, homogenizing:
Magma a, the b and the c that ball milling are obtained to different-grain diameter put into respectively homogenizing case homogenizing, and the homogenizing time is 10～150 hours.
3, batch mixing:
Magma a, b and c that homogenizing is good mix according to following mass ratio, magma a:10%～70%, magma b:5%～40%, magma c:15%～50%;
Mix after for some time, in mixed slurry, add appropriate binding agent to increase moulding green compact plasticity again, the binding agent of interpolation and the mass ratio of mixed slurry are 0.001%～1.5%, and mixing total time is 0.5～10 hour.
4, vacuum stirring de-bubble:
The slurry mixing is stirred and is vacuumized in vacuum tank, vacuum tightness-100 to-10KPa (kPa), churning time 1～10 hour.
In an application case, preparation method's step of the quartz slurry for casting of present embodiment is as follows:
The first step, preparation magma
(1) magma a makes by mode below:
With 0～60mm (millimeter) piece material 1t (ton), 4-20 order particle 2t and water 0.42t, be milled to D50:8.3 μ m, water-content (mass ratio) 14%, adds polyethylene of dispersing agent glycol hard fatty acids fat, and addition is 40ppm;
(2) magma b makes by mode below:
With 0～60mm piece material 1t, 4-20 order particle 2t, water 0.3t, be milled to D50:15 μ m, water-content (mass ratio) 10%, adds polyethylene of dispersing agent glycol hard fatty acids fat, and addition is 20ppm;
(3) magma c makes by mode below:
With 0～60mm piece material 1t, 4-20 order particle 2t, water 0.3t, be milled to D50:40 μ m, water-content (mass ratio) 10%, adds dispersion agent polyacrylamide, and addition is 100ppm.
Second step, homogenizing:
Good magma a, the b of ball milling and c are placed in respectively in homogenizing case old 6 days.
The 3rd step, batch mixing:
Batch mixing in mechanical mixer, slurry blending ratios at different levels are a: b: c=4: 2: 4, wherein magma a:400kg (kilogram), magma b:200kg, magma c:400kg.Mixing time is added CMC (Carboxyl methyl Cellulose, Xylo-Mucine) the solution 4kg of 1.5% (mass ratio) as binding agent after 2 hours, the mass ratio of binding agent and magma a, b and c is 0.4%, and then mixes 1 hour.
The 4th step, vacuum stirring de-bubble:
Three kinds of slurries that mix are put into vacuum stirring device and vacuumize stirring 1 hour, vacuum tightness is-50KPa.
In concrete application case, can see, the total time that magma a, b and c mix is only 3 hours, and compared with 2～192 hours of conventional art, the method for present embodiment effectively shortened mixing time, raises the efficiency, and reduces costs.
The effect system of dispersion agent verifies by slurry sedimentation, conventional art, and 24 hourly average sedimentations are 18.18mm; And the mode that the different-grain diameter that adopts present embodiment adds dispersion agent, 24 hourly average sedimentations are 8.8mm, and slurry dispersing property improves clearly, can not produce size particles demixing phenomenon, makes green density even, and performance is better.
The mode that the preparation method of the quartz slurry for casting of present embodiment adopts slurry+slurry+slurry to carry out grating mixing, the grating hybrid mode compared with the slurry+powder+powder of conventional art, has improved mixing efficiency.In addition, by add dispersion agent in preparation magma process, effectively improved slurry dispersed.
The slurry viscosity that utilizes the preparation method of the quartz slurry for casting of embodiment to prepare is moderate, good fluidity, and the crucible crackle of cast is few, can effectively improve the crucible rate that manufactures a finished product, and reaches the object that reduces costs and increase efficiency.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. a preparation method for quartz slurry for casting, is characterized in that, step is as follows:
(1) prepare magma
Utilize fused quartz raw material ball to grind standby magma a, b and c, after ball milling, the water-content of magma a, b and c (mass ratio) is 9%～25%, wherein the size distribution of magma a is >0 and <10 μ m, the size distribution of magma b is 10～30 μ m, the size distribution of magma c be >30 and≤700 μ m;
In mechanical milling process, in magma a, b and c, add dispersion agent respectively, adding proportion 5-100ppm, the dispersion agent adding in described magma a is macrogol hard fatty acids fat, the dispersion agent adding in magma b is macrogol hard fatty acids fat and/or polyacrylamide, and the dispersion agent adding in magma c is polyacrylamide;
(2) homogenizing
By magma a, b and c difference homogenizing, the homogenizing time is 10～150 hours;
(3) batch mixing
Magma a, b and c are mixed according to following mass ratio, and mixing time is 0.5～10 hour;
Magma a:10%～70%, magma b:5%～40%, magma c:15%～50%;
(4) vacuum stirring de-bubble
The magma mixing is stirred to de-bubble under-100 to-10KPa vacuum condition, and churning time is 1～10 hour.
2. the preparation method of quartz slurry for casting according to claim 1, is characterized in that, in the process of batch mixing, according to mass ratio 0.001%～1.5%, adds binding agent.
3. the preparation method of quartz slurry for casting according to claim 1, is characterized in that, described all turn to old.
4. the preparation method of quartz slurry for casting according to claim 1, is characterized in that, described vacuum stirring is carried out in vacuum stirring device.
5. the preparation method of quartz slurry for casting according to claim 1, is characterized in that,
(1) described magma a makes by mode below:
With 0.42 ton, 1 ton, 0～60mm piece material, 2 tons of 4-20 order particles and water, be milled to D50:8.3 μ m, water-content (mass ratio) 14%, adds polyethylene of dispersing agent glycol hard fatty acids fat, and addition is 40ppm;
(2) described magma b makes by mode below:
With 1 ton, 0～60mm piece material, 2 tons of 4-20 order particles, 0.3 ton, water, be milled to D50:15 μ m, water-content (mass ratio) 10%, adds polyethylene of dispersing agent glycol hard fatty acids fat, and addition is 20ppm;
(3) described magma c makes by mode below:
With 1 ton, 0～60mm piece material, 2 tons of 4-20 order particles, 0.3 ton, water, be milled to D50:40 μ m, water-content (mass ratio) 10%, adds dispersion agent polyacrylamide, and addition is 100ppm;
6. the preparation method of quartz slurry for casting according to claim 5, is characterized in that, described magma a, b and c in homogenizing case old 6 days respectively.
7. the preparation method of quartz slurry for casting according to claim 6, is characterized in that, described magma a, b and c mix according to mass ratio 4:2:4, and wherein the quality of magma a, b and c is respectively 400kg, 200kg and 400kg; Mix and add 1.5%(mass ratio after 2 hours) CMC solution 4kg, and then mix 1 hour.
8. the preparation method of quartz slurry for casting according to claim 7, is characterized in that, the slurry mixing is put into vacuum stirring device and vacuumize stirring, and vacuum tightness is-50KPa.
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| CN201110460905.3A CN102515511B (en) | 2011-12-31 | 2011-12-31 | Preparation method for quartz slurry for casting |
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| CN201110460905.3A CN102515511B (en) | 2011-12-31 | 2011-12-31 | Preparation method for quartz slurry for casting |
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| CN102515511B true CN102515511B (en) | 2014-02-19 |
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| CN106966711B (en) * | 2016-01-14 | 2019-09-03 | 杭州大和江东新材料科技有限公司 | A method of improving quartz sand slurry suspension |
| CN116813318A (en) * | 2023-04-24 | 2023-09-29 | 江苏锡沂高新材料产业技术研究院有限公司 | Preparation method of dynamic gel injection molding fused quartz ceramic biscuit |
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| EP0492124A2 (en) * | 1990-12-24 | 1992-07-01 | Degussa Aktiengesellschaft | Precipitated silica paste |
| DE102006046619A1 (en) * | 2006-09-29 | 2008-04-03 | Heraeus Quarzglas Gmbh & Co. Kg | Coatable silicon dioxide slip used in the production of layered quartz glass contains a dispersion liquid and amorphous nano-particles with a specified particle size of less |
| CN102167500A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Preparation method of non-transparent quartz labware |
| CN102180596A (en) * | 2011-01-31 | 2011-09-14 | 圣戈班石英（锦州）有限公司 | Slurry for solar polycrystalline silicon ingot casting crucible and preparation method thereof |
| CN102225837A (en) * | 2011-05-08 | 2011-10-26 | 江苏润弛太阳能材料科技有限公司 | Manufacture method of spray-free fused quartz crucible used for polycrystalline silicon cast ingots |
| CN102260422A (en) * | 2010-05-25 | 2011-11-30 | 中国地质大学（北京） | Method for preparing TiO2/powdered quartz composite powder material |
| JP5024852B2 (en) * | 2005-11-04 | 2012-09-12 | 株式会社ソフイア | Game machine |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0524852A (en) * | 1991-07-18 | 1993-02-02 | Tosoh Corp | Production of quartz glass |
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- 2011-12-31 CN CN201110460905.3A patent/CN102515511B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0492124A2 (en) * | 1990-12-24 | 1992-07-01 | Degussa Aktiengesellschaft | Precipitated silica paste |
| JP5024852B2 (en) * | 2005-11-04 | 2012-09-12 | 株式会社ソフイア | Game machine |
| DE102006046619A1 (en) * | 2006-09-29 | 2008-04-03 | Heraeus Quarzglas Gmbh & Co. Kg | Coatable silicon dioxide slip used in the production of layered quartz glass contains a dispersion liquid and amorphous nano-particles with a specified particle size of less |
| CN102260422A (en) * | 2010-05-25 | 2011-11-30 | 中国地质大学（北京） | Method for preparing TiO2/powdered quartz composite powder material |
| CN102167500A (en) * | 2011-01-10 | 2011-08-31 | 圣戈班石英（锦州）有限公司 | Preparation method of non-transparent quartz labware |
| CN102180596A (en) * | 2011-01-31 | 2011-09-14 | 圣戈班石英（锦州）有限公司 | Slurry for solar polycrystalline silicon ingot casting crucible and preparation method thereof |
| CN102225837A (en) * | 2011-05-08 | 2011-10-26 | 江苏润弛太阳能材料科技有限公司 | Manufacture method of spray-free fused quartz crucible used for polycrystalline silicon cast ingots |
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