CN108997003B - Ceramic slurry, ceramic device and preparation method thereof - Google Patents
Ceramic slurry, ceramic device and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a ceramic slurry, a ceramic device and a preparation method thereof, wherein the ceramic slurry comprises a main material, a gel and a dispersing agent, the main material comprises two kinds of fine fused quartz powder and coarse fused quartz powder, the median particle size of the fine fused quartz powder is 3-15 mu m, the median particle size of the coarse fused quartz powder is 0.2-3 mm, the mass of the gel is 1-5% of the mass of the main material, and the mass of the dispersing agent is 0.1-0.5% of the mass of the main material. The ceramic slurry can ensure the mechanical strength of the manufactured ceramic device, and can reduce the contractibility during subsequent drying and sintering, thereby effectively preventing the ceramic device from cracking during subsequent drying and sintering and effectively improving the yield of products. The ceramic slurry can be suitable for low-toxicity gels such as N, N-dimethylacrylamide, N-methylenebisacrylamide, hydroxymethyl acrylamide and amylopectin, is green and environment-friendly, and is suitable for industrial large-scale popularization.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic materials, in particular to ceramic slurry, a ceramic device and a preparation method thereof.
Background
With the exacerbation of the fossil energy crisis, new sustainable energy industries have received global attention and have gained rapid development. Solar energy is a clean and inexhaustible energy, the solar industry develops rapidly in recent years, the solar industry in China also develops rapidly in recent years, and the newly increased installed capacity of a solar power station and the output of a solar battery pack are at the top of the world in the current year. Crystalline silicon is one of the core materials of solar cells, and the productivity thereof is continuously improved with the development of the solar industry. The fused quartz ceramic crucible is an irreplaceable key consumable material in the production of polycrystalline silicon ingots due to the excellent properties of extremely low linear expansion coefficient, high thermal shock resistance, acid and alkali corrosion resistance, low dielectric constant and the like.
At present, the preparation of the fused quartz ceramic crucible in the industrial field mainly adopts a slip casting method and a gel casting molding process. The grouting method is limited by the process principle, and has the defects of long forming period, poor uniformity of biscuit structure, low strength, small applicable mold range and the like, so that the production period is long, the yield is low, and the production cost is high. The gel injection molding process has the advantages of simple process, low investment cost, compact structure of the molded blank, and the like. However, only a few enterprises in China master the gel injection molding process technology of the fused quartz ceramic crucible at present, and the gel injection molding process technology mainly faces the problems that the gel is usually acrylamide which is a gel monomer with neurotoxicity and is unfavorable for human health and environmental protection after long-term contact, and a ceramic biscuit body prepared by adopting a low-toxicity gel is easy to crack, so that the product yield is reduced.
Disclosure of Invention
Accordingly, there is a need for a ceramic slurry, a ceramic device and a method for manufacturing the same that can improve yield and can be applied to low-toxicity or non-toxicity gelling agents.
The ceramic slurry comprises a main body material, a gel and a dispersing agent, wherein the main body material comprises fine fused quartz powder and coarse fused quartz powder, the median particle size of the fine fused quartz powder is 3-15 mu m, the median particle size of the coarse fused quartz powder is 0.2-3 mm, the mass of the gel is 1-5% of that of the main body material, and the mass of the dispersing agent is 0.1-0.5% of that of the main body material.
The ceramic slurry adopts two kinds of fused quartz powder with large particle size difference, the particle size of the fused quartz powder is controlled within the range, and the component distribution ratio is combined, the two kinds of fused quartz powder of the ceramic slurry interact with each other and each component has synergistic effect, so that the mechanical strength of the prepared ceramic green body can be ensured, the contractility during subsequent drying and sintering can be reduced, the cracking of a ceramic device during subsequent drying and sintering can be effectively prevented, and the product yield is effectively improved.
The ceramic slurry can be suitable for low-toxicity gels such as N, N-dimethylacrylamide, N-methylenebisacrylamide, hydroxymethyl acrylamide and amylopectin, and the prepared ceramic green bodies have high mechanical strength and less cracking, so that the problem that the acrylamide used as the gel harms human health and environmental protection can be effectively avoided, and the ceramic slurry is green and environment-friendly and is suitable for industrial large-scale popularization.
In one embodiment, the mass ratio of the fine fused silica powder to the coarse fused silica powder is (0.33-2): 1.
In one embodiment, the gelling agent is at least one of N, N-dimethylacrylamide, N-methylenebisacrylamide, methylolacrylamide, and pullulan;
and when the gel agent contains at least one of N, N-dimethylacrylamide, N-methylenebisacrylamide and hydroxymethyl acrylamide, the ceramic slurry also comprises an initiator, and the mass of the initiator is 0.2-3% of that of the gel agent.
In one embodiment, the gelling agent is a mixture of N, N-dimethylacrylamide and N, N-methylenebisacrylamide, or the gelling agent is a mixture of methylolacrylamide and N, N-methylenebisacrylamide.
In one embodiment, the initiator is at least one of azobisisobutyronitrile, ammonium persulfate, potassium persulfate, and sodium persulfate.
The preparation method of the ceramic slurry comprises the following steps:
providing raw materials, wherein the raw materials comprise a main material, a gelling agent, a dispersing agent and water, the main material comprises fine fused quartz powder and coarse fused quartz powder, the median particle size of the fine fused quartz powder is 3-15 mu m, the median particle size of the coarse fused quartz powder is 0.2-3 mm, the mass of the gelling agent is 1-5% of the mass of the main material, and the mass of the dispersing agent is 0.1-0.5% of the mass of the main material;
mixing and ball-milling the fine fused quartz powder, the dispersing agent, the gel and water, adding the coarse fused quartz powder, and continuing ball-milling to obtain the ceramic slurry;
when the raw materials further comprise an initiator, the initiator is added after the coarse fused quartz powder is added and ball milling is continued to be completed.
In one embodiment, the rotation speed of the mixing and ball milling of the fine fused quartz powder, the dispersing agent, the gel and water is 160rpm-250rpm, and the time is 2 h-6 h; the rotating speed of the added coarse fused quartz powder for continuous ball milling is 60-120 rpm, and the time is 10-30 min.
A ceramic device is mainly prepared from the ceramic slurry.
In one embodiment, the ceramic device is a fused silica ceramic crucible.
A method for preparing a ceramic device, comprising the steps of:
defoaming the ceramic slurry, injecting the ceramic slurry into a mold, and heating and curing to obtain a ceramic blank;
and demolding, drying and sintering the ceramic blank to obtain the ceramic device.
Drawings
FIG. 1 is a SEM photograph of a ceramic body obtained in example 2;
FIG. 2 is a scanning electron micrograph of the surface of a fused silica ceramic crucible obtained in example 2;
FIG. 3 is an optical photograph of a fused silica ceramic crucible obtained in example 2;
FIG. 4 is a scanning electron micrograph of the fused silica ceramic obtained in comparative example 1.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The embodiment of the invention provides ceramic slurry and a preparation method thereof.
The ceramic slurry comprises a main body material, a gelling agent, a dispersing agent and the like.
The main material comprises two kinds of fine fused quartz powder and coarse fused quartz powder, wherein the median particle size of the fine fused quartz powder is 3-15 mu m, and the median particle size of the coarse fused quartz powder is 0.2-3 mm. The fine fused silica powder and the coarse fused silica powder preferably have a purity of 99% to 99.99% (mass percentage content).
The mass of the gel is 1-5% of the mass of the main material.
The mass of the dispersing agent is 0.1-0.5% of the mass of the main material.
The ceramic slurry adopts two kinds of fused quartz powder with large particle size difference, the particle size of the fused quartz powder is controlled within the range, and the component distribution ratio is combined, the two kinds of fused quartz powder of the ceramic slurry interact with each other and each component has synergistic effect, so that the mechanical strength of the prepared ceramic green body can be ensured, the contractility during subsequent drying and sintering can be reduced, the cracking of a ceramic device during subsequent drying and sintering can be effectively prevented, and the product yield is effectively improved.
The ceramic slurry can be suitable for low-toxicity or non-toxicity gels such as N, N-dimethylacrylamide, N-methylenebisacrylamide, hydroxymethyl acrylamide and amylopectin, and the prepared ceramic device has high mechanical strength and less cracking, so that the problem that the human health and the environment are harmed by adopting acrylamide as the gel can be effectively avoided, and the ceramic slurry is green and environment-friendly and is suitable for industrial large-scale popularization.
Thus, preferably, the gelling agent may be at least one of N, N-dimethylacrylamide, N-methylenebisacrylamide, methylolacrylamide, and pullulan.
The amylopectin has a dendritic branch structure, and the molten quartz powder can be bonded by water absorption and gelatinization at a higher temperature, so that the ceramic blank has higher mechanical strength.
When the gel agent contains at least one of N, N-dimethylacrylamide, N-methylenebisacrylamide and hydroxymethyl acrylamide, the ceramic slurry also comprises an initiator, and the mass of the initiator is 0.2-3% of that of the gel agent. Thus, the gelling agent is polymerized to form a two-dimensional structure or a three-dimensional network structure under the action of the initiator, so that the ceramic slurry is solidified in situ, and the green body has higher mechanical strength.
Further preferably, the gelling agent is a mixture of N, N-dimethylacrylamide and N, N-methylenebisacrylamide, or the gelling agent is a mixture of methylolacrylamide and N, N-methylenebisacrylamide. Thus, N-dimethylacrylamide or methylolacrylamide and N, N-methylene-bisacrylamide are polymerized to form a three-dimensional network structure under the action of an initiator, so that the ceramic green body has higher mechanical strength.
When the gelling agent is a mixture of N, N-dimethylacrylamide and N, N-methylene bisacrylamide, the mass ratio of the N, N-dimethylacrylamide to the N, N-methylene bisacrylamide is 20: 1-5: 1, preferably 10:1, and the gelling agent can obtain a sufficient network structure under the action of an initiator at the preferable ratio, so that the gelling agent is beneficial to the mechanical strength of the ceramic green body. When the gelling agent is a mixture of hydroxymethyl acrylamide and N, N-methylene bisacrylamide, the mass ratio of the hydroxymethyl acrylamide to the N, N-methylene bisacrylamide is 20: 1-5: 1, and is preferably 10: 1.
The initiator may be at least one of azobisisobutyronitrile, ammonium persulfate, potassium persulfate, and sodium persulfate. In one specific example, the initiator is preferably ammonium persulfate.
The dispersant may be at least one of acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer, polyvinylpyrrolidone, and naphthalenesulfonic acid-formaldehyde condensate. In a specific example, the dispersant is preferably an acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer.
Through further research, the effect of preventing cracking of the ceramic device during subsequent drying and sintering can be further improved by controlling the mass ratio of the fine fused quartz powder to the coarse fused quartz powder to be (0.33-2): 1.
It is understood that the raw material of the ceramic slurry further includes water. Furthermore, the mass ratio of water to the main body material is 1 (4-10), and the ceramic green body prepared in the range has high mechanical strength and low cracking rate.
The preparation method of the ceramic slurry comprises the following steps:
providing the above raw materials of the ceramic slurry;
mixing and ball-milling the fine fused quartz powder, the dispersing agent, the gel and water, adding the coarse fused quartz powder, and continuing ball-milling to obtain the ceramic slurry.
When the raw materials of the ceramic slurry also comprise an initiator, the initiator is added after the coarse fused quartz powder is added and the ball milling is continued to be completed. The initiator is added after other components are fully mixed, so that the phenomenon that the uniformity of component mixing is influenced by adding the initiator too early is avoided.
Adding fine fused quartz powder, a dispersing agent, a gelling agent, water and the like into a ball mill and grinding for a period of time; and adding the coarse fused quartz powder into the slurry, and continuously grinding for a period of time to obtain the ceramic slurry. Thus, the ceramic device blank with good uniformity and difficult cracking can be formed.
Specifically, the rotation speed of the fine fused quartz powder, the dispersing agent, the gelling agent and the water are mixed and ball-milled at 160rpm-250rpm, preferably 220rpm, for 2 h-6 h. Adding the coarse fused quartz powder, and continuously ball-milling at the rotation speed of 60-120 rpm, preferably 80rpm for 10-30 min.
Correspondingly, the embodiment of the invention also provides a ceramic device and a preparation method thereof.
The ceramic device is mainly prepared from the ceramic slurry. In a specific example, the ceramic device is a fused silica ceramic crucible which can be used for the ingot production of polycrystalline silicon.
The preparation method of the ceramic device comprises the following steps:
defoaming the ceramic slurry, injecting the ceramic slurry into a mold, and heating and curing to obtain a ceramic blank; and demolding, drying and sintering the ceramic blank to obtain the ceramic device.
Wherein the heating and curing adopts water bath heating and curing, the temperature of the water bath is 65-90 ℃, and the time of the water bath is 0.5-1.5 h.
Wherein the sintering condition is that the temperature is kept for 1 to 6 hours at 1100 to 1300 ℃.
When the fused silica ceramic crucible is required to be manufactured, a mold corresponding to the crucible can be adopted, such as a square shape or a cylindrical shape.
The preparation method of the ceramic device adopts a gel injection molding technology, has simple process and low cost, the prepared ceramic blank has high mechanical strength and less cracking, the product yield is effectively improved, and the preparation method can be suitable for low-toxicity, green and environment-friendly gels, is green and environment-friendly and is suitable for industrial large-scale popularization.
The following are specific examples.
Example 1:
adding 1 part by mass of water, 2.6 parts by mass of fine fused quartz powder, a dispersing agent, a gelling agent and the like into a ball mill, carrying out ball milling for 4 hours at the rotating speed of 160rpm to prepare initial fused quartz slurry, adding 1.4 parts by mass of coarse fused quartz powder into the slurry, continuing ball milling for 15 minutes at the rotating speed of 120rpm, and adding ammonium persulfate (prepared into a 10% aqueous solution by mass concentration) accounting for 2% of the mass of the gelling agent into the ball-milled slurry to obtain the required ceramic slurry. And then, carrying out vacuum defoaming on the ceramic slurry, injecting the defoamed ceramic slurry into a crucible mold, placing the mold in a water bath environment at 70 ℃ for 1h, then demolding to obtain a fused quartz crucible blank, carrying out temperature control and humidity control drying on the blank, and then carrying out heat preservation at 1150 ℃ for 5h in a kiln to obtain the fused quartz ceramic crucible. The median particle size of the fine fused silica powder used in this example was 4 μm, and the median particle size of the coarse fused silica powder used was 0.3 mm; the dispersant is acrylic acid-diacrylamide-dimethyl propanesulfonic acid copolymer, and the dosage of the dispersant is 0.5 percent of the total mass of the fused quartz powder; the gel is N, N-dimethylacrylamide and N, N-methylene bisacrylamide, the mass ratio of the N, N-dimethylacrylamide to the N, N-methylene bisacrylamide is 10:1, and the total dosage of the gel is 2% of the total mass of the fused quartz powder.
Example 2:
adding 1 part by mass of water, 3.3 parts by mass of fine fused quartz powder, a dispersing agent, a gelling agent and the like into a ball mill, carrying out ball milling for 5 hours at the rotating speed of 220rpm to prepare initial fused quartz slurry, adding 3.3 parts by mass of coarse fused quartz powder into the slurry, continuing ball milling for 25 minutes at the rotating speed of 80rpm, and adding ammonium persulfate (prepared into a 10% aqueous solution by mass concentration) accounting for 2% of the mass of the gelling agent into the ball-milled slurry to obtain the required ceramic slurry. And then, carrying out vacuum defoaming on the ceramic slurry, injecting the defoamed ceramic slurry into a crucible mold, placing the mold in a water bath environment at 75 ℃ for 1h, then demolding to obtain a fused quartz crucible blank, carrying out temperature control and humidity control drying on the blank, and then carrying out heat preservation at 1200 ℃ for 3h in a kiln to obtain the fused quartz ceramic crucible. The median particle size of the fine fused silica powder used in this example was 8 μm, and the median particle size of the coarse fused silica powder used was 1 mm; the dispersant is acrylic acid-diacrylamide-dimethyl propanesulfonic acid copolymer, and the dosage of the dispersant is 0.3 percent of the total mass of the fused quartz powder; the gel is N, N-dimethylacrylamide and N, N-methylene bisacrylamide, the mass ratio of the N, N-dimethylacrylamide to the N, N-methylene bisacrylamide is 10:1, and the total dosage of the gel is 1.5% of the total mass of the fused quartz powder.
Example 3:
adding 1 part by mass of water, 2.8 parts by mass of fine fused quartz powder, a dispersing agent, a gelling agent and the like into a ball mill, carrying out ball milling for 3 hours at the rotating speed of 220rpm to prepare initial fused quartz slurry, adding 6 parts by mass of coarse fused quartz powder into the slurry, continuing ball milling for 30 minutes at the rotating speed of 80rpm, and adding ammonium persulfate (prepared into a 10% aqueous solution by mass concentration) accounting for 2% of the mass of the gelling agent into the ball-milled slurry to obtain the required ceramic slurry. And then, carrying out vacuum defoaming on the ceramic slurry, injecting the defoamed ceramic slurry into a crucible mold, placing the mold in a water bath environment at 80 ℃ for 1h, then demolding to obtain a fused quartz crucible blank, carrying out temperature control and humidity control drying on the blank, and then carrying out heat preservation at 1220 ℃ for 2h in a kiln to obtain the fused quartz ceramic crucible. The median particle size of the fine fused silica powder used in this example was 12 μm, and the median particle size of the coarse fused silica powder used was 1.8 mm; the dispersant is acrylic acid-diacrylamide-dimethyl propanesulfonic acid copolymer, and the dosage of the dispersant is 0.2 percent of the total mass of the fused quartz powder; the gel is N, N-dimethylacrylamide and N, N-methylene bisacrylamide, the mass ratio of the N, N-dimethylacrylamide to the N, N-methylene bisacrylamide is 10:1, and the total dosage of the gel is 1.5% of the total mass of the fused quartz powder.
Example 4:
adding 1 part by mass of water, 2.5 parts by mass of fine fused quartz powder, a dispersing agent, a gelling agent and the like into a ball mill, carrying out ball milling for 2 hours at the rotating speed of 250rpm to prepare initial fused quartz slurry, adding 7.5 parts by mass of coarse fused quartz powder into the slurry, continuing ball milling for 30 minutes at the rotating speed of 80rpm, and adding ammonium persulfate (prepared into a 10% aqueous solution by mass concentration) accounting for 2% of the mass of the gelling agent into the ball-milled slurry to obtain the required ceramic slurry. And then, carrying out vacuum defoaming on the ceramic slurry, injecting the defoamed ceramic slurry into a crucible mold, placing the mold in a water bath environment at 85 ℃ for 1h, then demolding to obtain a fused quartz crucible blank, and firing the fused quartz crucible blank in a kiln at 1250 ℃ for 1h after temperature control, humidity control and drying to obtain the fused quartz ceramic crucible. The median particle size of the fine fused silica powder used in this example was 15 μm, and the median particle size of the coarse fused silica powder used was 2.5 mm; the dispersant is acrylic acid-diacrylamide-dimethyl propanesulfonic acid copolymer, and the dosage of the dispersant is 0.1 percent of the total mass of the fused quartz powder; the gel is hydroxymethyl acrylamide and N, N-methylene diacryloyl, the mass ratio of the hydroxymethyl acrylamide to the N, N-methylene diacryloyl is 10:1, and the total dosage of the gel is 1.8% of the total mass of the fused quartz powder.
Example 5:
adding 1 part by mass of water, 3 parts by mass of fine fused quartz powder, a dispersing agent, a gelling agent and the like into a ball mill, carrying out ball milling for 4 hours at the rotating speed of 250rpm to prepare initial fused quartz slurry, adding 3.6 parts by mass of coarse fused quartz powder into the slurry, and continuing ball milling for 25 minutes at the rotating speed of 60rpm to obtain the required ceramic slurry. And then, defoaming the ceramic slurry in vacuum, injecting the ceramic slurry into a crucible mold, placing the mold in a water bath environment at 80 ℃ for 1h, demolding to obtain a fused quartz crucible blank, drying the blank under controlled temperature and humidity, and then keeping the temperature of 1200 ℃ for 3h in a kiln to obtain the fused quartz ceramic crucible. The median particle size of the fine fused silica powder used in this example was 8 μm, and the median particle size of the coarse fused silica powder used was 1.5 mm; the dispersant is acrylic acid-diacrylamide-dimethyl propanesulfonic acid copolymer, and the dosage of the dispersant is 0.3 percent of the total mass of the fused quartz powder; the used gelling agent is amylopectin, and the total dosage of the gelling agent is 3 percent of the total mass of the fused quartz powder.
Example 6:
adding 1 part by mass of water, 2.8 parts by mass of fine fused quartz powder, a dispersing agent, a gelling agent and the like into a ball mill, carrying out ball milling for 3 hours at the rotating speed of 220rpm to prepare fused quartz slurry, adding 6 parts by mass of coarse fused quartz powder into the slurry, and continuing ball milling for 30 minutes at the rotating speed of 80rpm to obtain the required ceramic slurry. And then, defoaming the ceramic slurry in vacuum, injecting the ceramic slurry into a crucible mold, placing the mold in a water bath environment at 75 ℃ for 1h, demolding to obtain a fused quartz crucible blank, drying the blank under controlled temperature and humidity, and then keeping the temperature of 1220 ℃ for 2h in a kiln to obtain the fused quartz ceramic crucible. The median particle size of the fine fused silica powder used in this example was 12 μm, and the median particle size of the coarse fused silica powder used was 1.8 mm; the dispersant is acrylic acid-diacrylamide-dimethyl propanesulfonic acid copolymer, and the dosage of the dispersant is 0.2 percent of the total mass of the fused quartz powder; the used gelling agent is amylopectin, and the total dosage of the gelling agent is 4.5 percent of the total mass of the fused quartz powder.
Comparative example 1
Comparative example 1 is substantially the same as example 2 except that the coarse fused silica powder was replaced with the equivalent amount of fine fused silica powder having a median particle diameter of 8 μm.
Comparative example 2
Comparative example 2 is substantially the same as example 2 except that the coarse fused silica powder having a median particle diameter of 1mm was replaced with the same amount of fused silica powder having a median particle diameter of 5 mm.
Comparative example 3
Comparative example 3 is substantially the same as example 2 except that the coarse fused silica powder having a median particle diameter of 1mm was replaced with the same amount of fused silica powder having a median particle diameter of 0.05 mm.
The fused silica ceramic crucibles prepared in examples 1 to 6 and the fused silica ceramic crucibles prepared in comparative examples 1 to 3 were subjected to yield statistics according to cracking conditions. The obtained product yield is shown in table 1 below.
TABLE 1
| Group of | Product yield |
| Example 1 | 45％ |
| Example 2 | 82％ |
| Example 3 | 80％ |
| Example 4 | 75％ |
| Example 5 | 60％ |
| Example 6 | 78％ |
| Comparative example 1 | 5％ |
| Comparative example 2 | 35％ |
| Comparative example 3 | 20％ |
The fracture of the ceramic green body obtained in example 2 and the surface of the fused silica ceramic crucible after sintering were subjected to scanning electron microscope tests, as shown in fig. 1 and 2, respectively. As can be seen from FIGS. 1 and 2, the fracture of the ceramic body which is not sintered and the surface of the fused silica ceramic crucible after sintering are very uniform, and no cracking occurs. The actual product of the fused silica ceramic crucible obtained in example 2, as shown in FIG. 3, comprised a square or cylindrical shape, was found to have a uniform color, a smooth surface, and no cracking. FIG. 4 is a scanning electron micrograph of the fused silica ceramic obtained in comparative example 1, and it can be seen from FIG. 4 that a significant cracking phenomenon occurred in the ceramic device.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The ceramic slurry is characterized by comprising a main material, a gelling agent and a dispersing agent, wherein the main material is composed of fine fused quartz powder and coarse fused quartz powder, and the mass ratio of the fine fused quartz powder to the coarse fused quartz powder is (0.33-2): 1; the median particle size of the fine fused quartz powder is 3-15 microns, the median particle size of the coarse fused quartz powder is 0.2-3 mm, the mass of the gelling agent is 1-5% of the mass of the main material, and the mass of the dispersing agent is 0.1-0.5% of the mass of the main material.
2. The ceramic slurry of claim 1, wherein the gelling agent is at least one of N, N-dimethylacrylamide, N-methylenebisacrylamide, methylolacrylamide, and pullulan;
and when the gel agent contains at least one of N, N-dimethylacrylamide, N-methylenebisacrylamide and hydroxymethyl acrylamide, the ceramic slurry also comprises an initiator, and the mass of the initiator is 0.2-3% of that of the gel agent.
3. The ceramic slurry of claim 2, wherein the gelling agent is a mixture of N, N-dimethylacrylamide and N, N-methylenebisacrylamide.
4. The ceramic slurry of claim 2, wherein the gelling agent is a mixture of methylolacrylamide and N, N-methylene bisacrylamide.
5. The ceramic slurry of claim 2, 3 or 4, wherein the initiator is at least one of azobisisobutyronitrile, ammonium persulfate, potassium persulfate and sodium persulfate.
6. The preparation method of the ceramic slurry is characterized by comprising the following steps of:
providing a raw material, wherein the raw material comprises a main body material, a gelling agent, a dispersing agent and water, the main body material comprises fine fused quartz powder and coarse fused quartz powder, and the mass ratio of the fine fused quartz powder to the coarse fused quartz powder is (0.33-2): 1; the median particle size of the fine fused quartz powder is 3-15 microns, the median particle size of the coarse fused quartz powder is 0.2-3 mm, the mass of the gelling agent is 1-5% of the mass of the main material, and the mass of the dispersing agent is 0.1-0.5% of the mass of the main material;
mixing and ball-milling the fine fused quartz powder, the dispersing agent, the gel and water, adding the coarse fused quartz powder, and continuing ball-milling to obtain the ceramic slurry;
when the raw materials further comprise an initiator, the initiator is added after the coarse fused quartz powder is added and ball milling is continued to be completed.
7. The method for preparing ceramic slurry according to claim 6, wherein the rotation speed of the fine fused quartz powder, the dispersing agent, the gelling agent and the water mixing and ball milling is 160rpm to 250rpm, and the time is 2h to 6 h; the rotating speed of the added coarse fused quartz powder for continuous ball milling is 60-120 rpm, and the time is 10-30 min.
8. A ceramic device prepared mainly from the ceramic slurry according to any one of claims 1 to 5.
9. The ceramic device of claim 8, wherein the ceramic device is a fused silica ceramic crucible.
10. A method for manufacturing a ceramic device, comprising the steps of:
defoaming the ceramic slurry according to any one of claims 1 to 5, injecting the ceramic slurry into a mold, and heating and curing to obtain a ceramic blank;
and demolding, drying and sintering the ceramic blank to obtain the ceramic device.
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| KR20030057134A (en) * | 2001-12-28 | 2003-07-04 | 한국기계연구원 | Slip for making ceramic core and its making method |
| CN101580339A (en) * | 2009-06-18 | 2009-11-18 | 王迎奎 | Method for manufacturing composite multi-stage fused quartz powder ceramic crucible |
| CN101880166A (en) * | 2010-06-13 | 2010-11-10 | 洛阳北苑特种陶瓷有限公司 | Preparation method of large quartz ceramic crucible |
| CN103030382A (en) * | 2012-12-12 | 2013-04-10 | 南京工业大学 | Method for forming fused quartz ceramic by low-toxicity gel system gel injection |
| CN105060867A (en) * | 2015-08-10 | 2015-11-18 | 南京工业大学 | Gel injection molding method of high-strength fused quartz ceramic |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030057134A (en) * | 2001-12-28 | 2003-07-04 | 한국기계연구원 | Slip for making ceramic core and its making method |
| CN101580339A (en) * | 2009-06-18 | 2009-11-18 | 王迎奎 | Method for manufacturing composite multi-stage fused quartz powder ceramic crucible |
| CN101880166A (en) * | 2010-06-13 | 2010-11-10 | 洛阳北苑特种陶瓷有限公司 | Preparation method of large quartz ceramic crucible |
| CN103030382A (en) * | 2012-12-12 | 2013-04-10 | 南京工业大学 | Method for forming fused quartz ceramic by low-toxicity gel system gel injection |
| CN105060867A (en) * | 2015-08-10 | 2015-11-18 | 南京工业大学 | Gel injection molding method of high-strength fused quartz ceramic |
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