CN107739203B - Preparation method of ceramic slurry and ceramic slurry - Google Patents
Preparation method of ceramic slurry and ceramic slurry Download PDFInfo
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Abstract
The invention relates to a preparation method of ceramic slurry and the ceramic slurry. A preparation method of ceramic slurry comprises the following steps: according to the mass parts, 30 to 45 parts of recycled ceramics, 2 to 8 parts of ceramic powder, 0.05 to 0.25 part of dispersant, 45 to 80 parts of solvent and 0.03 to 0.15 part of defoamer are mixed to obtain mixed slurry; and carrying out magnetic separation treatment on the mixed slurry to obtain the ceramic slurry. According to the preparation method of the ceramic slurry, the recycled ceramics are doped with the ceramic powder, so that the resin content ratio in the recycled ceramics can be reduced, the effect of reducing the density of the diaphragm can be achieved when the ceramic diaphragm is prepared, and the occurrence of laminated foaming is reduced; and a dispersant, a solvent and a defoaming agent in a certain ratio are mixed in the separation of the recovered ceramic slurry, so that the recovered ceramic has better dispersibility to obtain uniformly dispersed ceramic slurry, and a ceramic membrane with good appearance is obtained.
Description
Technical Field
The invention relates to the technical field of ceramic material recovery, in particular to a preparation method of ceramic slurry and the ceramic slurry.
Background
At present, the development of the electronic industry is rapid, strict requirements on the miniaturization, high capacity, low cost, high reliability and the like of a chip multilayer ceramic capacitor (MLCC) are provided, at present, slurry for manufacturing the MLCC is made into a membrane with certain viscosity and strength through tape casting, an inner electrode is printed on the membrane, and when the MLCC is laminated, the membrane is cut, so that a large amount of unusable rim charge is generated in the process, the production cost is high, and finally the competitiveness in the market is insufficient. By recycling the rim charge, the cost of the MLCC production process can be reduced, so that the cost of manufacturing the MLCC is reduced, and remarkable benefits can be obtained. However, the slurry made of the recycled edge material still has the problems of poor appearance of a subsequent processing product, high electric breakdown rate of a membrane and easy occurrence of laminated bubbles.
Disclosure of Invention
Therefore, it is necessary to provide a method for preparing ceramic slurry and ceramic slurry, which aim at the problems that slurry prepared from recycled edge material still has poor appearance of subsequent processed products, high electrical breakdown rate of membranes and easy occurrence of laminated bubbles.
A preparation method of ceramic slurry comprises the following steps:
according to the mass parts, 30 to 45 parts of recycled ceramics, 2 to 8 parts of ceramic powder, 0.05 to 0.25 part of dispersant, 45 to 80 parts of solvent and 0.03 to 0.15 part of defoamer are mixed to obtain mixed slurry; and
and carrying out magnetic separation treatment on the mixed slurry to obtain the ceramic slurry.
In one embodiment, the recycled ceramic is a non-magnetic recycled ceramic and the ceramic powder is a non-magnetic ceramic powder; the mass ratio of the ceramic powder to the recovered ceramic is 1: 20-1: 5.
In one embodiment, the recycled ceramic is at least one of a barium titanate ceramic and an alumina ceramic;
and/or the ceramic powder is at least one of barium titanate ceramic powder and aluminum oxide ceramic powder.
In one embodiment, the solvent is selected from at least one of toluene, xylene, methyl ethyl ketone, methyl isobutyl ketone, ethanol, isopropanol, ethylene glycol, ethyl acetate, and n-butanol.
In one embodiment, the solvent is selected from a mixed solution of toluene and ethanol, and the mass ratio of the toluene to the ethanol is 0.5: 1-2: 1.
In one embodiment, the defoamer is selected from at least one of polyether modified silicone oil defoamer, mineral oil defoamer, mixed silicone oil defoamer, phenyl silicone oil defoamer, dimethyl silicone oil defoamer.
In one embodiment, the mixing process specifically includes:
according to the mass parts, stirring 30 to 45 parts of recycled ceramics, 2 to 8 parts of ceramic powder, 0.05 to 0.25 part of dispersant, 45 to 80 parts of solvent and 0.03 to 0.15 part of defoamer at the rotating speed of 300 to 1000rpm for 10 to 60 min;
standing for 10-60 min; and
and then stirring at the rotating speed of 300-1000 rpm for 10-60 min.
In one embodiment, the step of performing magnetic separation treatment on the mixed slurry to obtain ceramic slurry further comprises the following steps: and carrying out ball milling treatment on the ceramic slurry.
In one embodiment, the ceramic slurry is ball milled using zirconia balls; the diameter of the zirconia ball is 2.0 mm-7.5 mm; the rotating speed of the ball milling treatment is 30-50 rpm.
The ceramic slurry is prepared by adopting the preparation method of the ceramic slurry.
According to the preparation method of the ceramic slurry, the ceramic powder is doped in the recovered ceramic, the ceramic slurry is prepared under the action of the dispersing agent, the defoaming agent and the solvent, and the magnetic metals such as nickel and the like in the slurry are removed through magnetic separation treatment, so that the electrical breakdown rate of the diaphragm is reduced while the appearance of the product is improved; the content ratio of resin in the recycled ceramics can be reduced by doping the ceramic powder in the recycled ceramics, and the effect of reducing the density of the membrane can be achieved when the ceramic membrane is prepared, so that the occurrence of laminated foaming is reduced; and a dispersant, a solvent and a defoaming agent in a certain ratio are mixed in the separation of the recovered ceramic slurry, so that the recovered ceramic has better dispersibility to obtain uniformly dispersed ceramic slurry, and a ceramic membrane with good appearance is obtained.
Drawings
Fig. 1 is a flowchart of a method of preparing a ceramic slurry according to an embodiment.
Detailed Description
The method for preparing the ceramic slurry and the ceramic slurry will be described in further detail with reference to the following embodiments and accompanying drawings.
A method of preparing a ceramic slurry according to an embodiment includes the steps of:
s110, mixing 30-45 parts of recycled ceramics, 2-8 parts of ceramic powder, 0.05-0.25 part of dispersant, 45-80 parts of solvent and 0.03-0.15 part of defoamer according to parts by mass to obtain mixed slurry.
In one embodiment, the recycled ceramic is a large amount of unusable scrap resulting from trimming the film sheets during the preparation of the MLCC. The rim charge contains magnetic materials such as nickel and other nonferrous metals.
In one embodiment, the recycled ceramic is a non-magnetic recycled ceramic. The recycled ceramic is at least one of barium titanate ceramic and alumina ceramic. Barium titanate ceramics are typically used in capacitor systems and alumina ceramics are typically used in resistor systems.
In one embodiment, the ceramic powder is a non-magnetic ceramic powder. Preferably, the mass ratio of the ceramic powder to the recovered ceramic is 1: 20-1: 5. More preferably, the mass ratio of the ceramic powder to the recovered ceramic is 1: 10.
In one embodiment, the ceramic powder is at least one of barium titanate ceramic powder and alumina ceramic powder. Further, the ceramic powder is preferably the same as the material of the reclaimed ceramic, that is, when the reclaimed ceramic is barium titanate ceramic, the ceramic powder is barium titanate ceramic powder, and when the reclaimed ceramic is alumina ceramic, the ceramic powder is alumina ceramic powder.
In one embodiment, the dispersant is selected from at least one of G700 from Nippon oil, AKM-0531 from Nippon oil, RE-610 from Nippon oil, NK-1 from Hydrocarbon, NK-3 from Hydrocarbon, NK01 from Hydrocarbon, and GTO from Hydrocarbon.
In one embodiment, the mass ratio of the dispersant to the reclaimed ceramic is 0.1% to 1%. Preferably, the mass ratio of the dispersant to the reclaimed ceramic is 0.25%.
In one embodiment, the solvent is selected from at least one of toluene, xylene, methyl ethyl ketone, methyl isobutyl ketone, ethanol, isopropanol, ethylene glycol, ethyl acetate, and n-butanol.
Further, the solvent is a mixed solution of toluene and ethanol. The mixed solution of toluene and ethanol can provide the dissolving effect of the ceramic material, further improve the grinding effect, improve the separation effect of magnetic separation, ensure better nickel removal effect and reduce the electric breakdown rate of the membrane. The mass ratio of the toluene to the ethanol is 0.5: 1-2: 1. Further, the mass ratio of toluene to ethanol was 0.5:1, 1:1, 1.5:1, and 2: 1. Furthermore, the mass ratio of toluene to ethanol was 1.5: 1.
In another embodiment, the solvent is a mixed solution of toluene, ethanol, methyl ethyl ketone, and isopropanol. Wherein the mass ratio of the toluene to the ethanol to the butanone to the isopropanol is 0.8-1.5: 1: 0.1-0.5: 0.01-0.05. Preferably, the mass ratio of toluene, ethanol, butanone and isopropanol is 1.1:1:0.1: 0.02.
In one embodiment, the defoamer is selected from at least one of polyether modified silicone oil type defoamers, mineral oil type defoamers, mixed silicone oil type defoamers, phenyl silicone oil type defoamers, and dimethyl silicone oil type defoamers. Further, the defoaming agent is dimethyl silicone oil defoaming agent.
In one embodiment, the step of performing the mixing process specifically includes:
s111, according to the mass parts, stirring 30-45 parts of recycled ceramics, 2-8 parts of ceramic powder, 0.05-0.25 part of dispersant, 45-80 parts of solvent and 0.03-0.15 part of defoamer at the rotating speed of 300-1000 rpm for 10-60 min.
In one embodiment, the agitation treatment may be performed in a blender. Of course, the stirring process may be manual stirring or other methods.
And S112, standing for 10-60 min.
S113, stirring at the rotating speed of 300-1000 rpm for 10-60 min.
And S120, performing magnetic separation treatment on the mixed slurry to obtain ceramic slurry.
In one embodiment, the mixed slurry is subjected to a magnetic separation process using a magnetic separator.
And S130, performing ball milling treatment on the ceramic slurry.
In one embodiment, the ceramic slurry is ball milled using zirconia balls. Furthermore, the diameter of the zirconia ball is 2.0 mm-7.5 mm. Further, the zirconia balls have a diameter of 2.0mm, 3.0mm, 6.5mm, or 7.5 mm.
In one embodiment, the ball milling process is performed at a speed of 30rpm to 50 rpm.
In one embodiment, the ball milling is performed for 120min to 360 min.
According to the preparation method of the ceramic slurry, the ceramic powder is doped in the recovered ceramic, the ceramic slurry is prepared under the action of the dispersing agent, the defoaming agent and the solvent, and the magnetic metals such as nickel and the like in the slurry are removed through magnetic separation treatment, so that the electrical breakdown rate of the diaphragm is reduced while the appearance of the product is improved; the content ratio of resin in the recycled ceramics can be reduced by doping the ceramic powder in the recycled ceramics, and the effect of reducing the density of the membrane can be achieved when the ceramic membrane is prepared, so that the occurrence of laminated foaming is reduced; and a dispersant, a solvent and a defoaming agent in a certain ratio are mixed in the separation of the recovered ceramic slurry, so that the recovered ceramic has better dispersibility to obtain uniformly dispersed ceramic slurry, and a ceramic membrane with good appearance is obtained.
Meanwhile, the preparation method of the ceramic slurry can effectively separate the magnetic metal in the recovered ceramic, reduce the electric breakdown rate of the product and improve the qualification rate of the product.
In other embodiments, step S130 may be omitted.
An embodiment of a ceramic slurry includes, in parts by mass:
the ceramic slurry is obtained after being processed by the preparation method of the ceramic slurry.
According to the ceramic slurry, a large amount of recovered ceramic is used as a raw material, so that the manufacturing cost of the ceramic slurry is remarkably reduced, and the ceramic slurry has good appearance and film forming property when used for preparing a ceramic membrane.
The following is a description of specific embodiments.
Example 1
44Kg of recovered ceramic, 4Kg of ceramic powder, 0.1Kg of dispersant, 31Kg of toluene, 15.5Kg of absolute ethanol and 0.06Kg of defoamer were stirred at 600rpm for 30min, and then left to stand for 30min, and then stirred at 600rpm for 30min to obtain a mixed slurry. Performing magnetic separation treatment on the mixed slurry by using a magnetic separator to obtain ceramic slurry; and performing ball milling treatment on the ceramic slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 2.0mm at the rotating speed of 30rpm for 360 min.
Example 2
30Kg of recovered ceramic, 6Kg of ceramic powder, 0.05Kg of dispersant, 30Kg of toluene, 20Kg of absolute ethanol and 0.1Kg of defoamer were stirred at 300rpm for 30min, and then left to stand for 30min, and then stirred at 300rpm for 30min to obtain a mixed slurry. Performing magnetic separation treatment on the mixed slurry by using a magnetic separator to obtain ceramic slurry; and performing ball milling treatment on the ceramic slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 3.0mm at the rotating speed of 30rpm for 360 min.
Example 3
Stirring 45Kg of recovered ceramic, 8Kg of ceramic powder, 0.25Kg of dispersant, 45Kg of toluene, 30Kg of absolute ethanol and 0.15Kg of defoamer at the rotation speed of 1000rpm for 10min, standing for 30min, and stirring at the rotation speed of 1000rpm for 10min to obtain a mixed slurry. Performing magnetic separation treatment on the mixed slurry by using a magnetic separator to obtain ceramic slurry; and performing ball milling treatment on the ceramic slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 2.0mm at the rotating speed of 50rpm for 240 min.
Example 4
Stirring 40Kg of recovered ceramic, 2Kg of ceramic powder, 0.05Kg of dispersant, 75Kg of solvent and 0.06Kg of defoamer for 30min at the rotating speed of 800rpm, wherein the solvent comprises 23Kg of toluene, 20Kg of ethanol, 2Kg of butanone and 0.4Kg of isopropanol; and standing for 30min, and stirring at the rotating speed of 800rpm for 30min to obtain the mixed slurry. Performing magnetic separation treatment on the mixed slurry by using a magnetic separator to obtain ceramic slurry; and performing ball milling treatment on the ceramic slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 6.0mm at the rotation speed of 30rpm for 240 min.
Example 5
30Kg of recovered ceramic, 6Kg of ceramic powder, 0.05Kg of dispersant, 45Kg of toluene and 0.6Kg of defoamer were stirred at 600rpm for 30min, and then left to stand for 30min, and then stirred at 600rpm for 30min to obtain a mixed slurry. Performing magnetic separation treatment on the mixed slurry by using a magnetic separator to obtain ceramic slurry; and performing ball milling treatment on the ceramic slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 2.0mm at the rotating speed of 30rpm for 360 min.
Example 6
50Kg of recovered ceramics, 0.1Kg of dispersant, 31Kg of toluene, 15.5Kg of anhydrous ethanol and 0.6Kg of defoamer were stirred at 600rpm for 30min, and then left to stand for 30min, and then stirred at 600rpm for 30min to obtain a mixed slurry. Performing magnetic separation treatment on the mixed slurry by using a magnetic separator to obtain ceramic slurry; and performing ball milling treatment on the ceramic slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 2.0mm at the rotation speed of 30rpm for 240 min.
Example 7
44Kg of recovered ceramic, 4Kg of ceramic powder, 47Kg of toluene and 0.6Kg of antifoaming agent were stirred at 600rpm for 30min, and then left to stand for 30min, and then stirred at 600rpm for 30min to obtain a mixed slurry. Performing magnetic separation treatment on the mixed slurry by using a magnetic separator to obtain ceramic slurry; and performing ball milling treatment on the ceramic slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 2.0mm at the rotation speed of 30rpm for 300 min.
Example 8
Stirring 30Kg of recovered ceramic, 6Kg of ceramic powder, 0.05Kg of dispersant, 30Kg of toluene, 20Kg of absolute ethyl alcohol and 0.1Kg of defoamer at the rotating speed of 300rpm for 30min, standing for 30min, and stirring at the rotating speed of 300rpm for 30min to obtain mixed slurry; and performing ball milling treatment on the mixed slurry to obtain ceramic slurry, and performing ball milling treatment on zirconia balls with the diameter of 3.0mm at the rotating speed of 30rpm for 360 min.
The ceramic slurries obtained by the treatments of examples 1 to 8 and the film sheets prepared from the ceramic slurries of examples 1 to 8 were used to fabricate a capacitor of 0805F/104M500 specification, and the results are shown in Table 1.
Wherein the viscosity of the slurry is obtained by adopting a Chuanyn viscosity cup test, the test temperature is 25 ℃, and the calculation formula is η - ηT+ (T-25)/4 wherein η is viscosity at 25 ℃ of ηTThe method comprises filling a Chuanyn cup with slurry, and calculating time from slurry flowing out to breakpoint by using stopwatch to be ηT；
The density of the slurry is obtained by testing a 100ml standard density cup, and the density rho of a formula is calculated to be m/V;
the density of the diaphragm is obtained by adopting a density board test, and rho is m/V;
the electric breakdown rate is tested by adopting an insulation resistance tester with the model number of NF2511A under the following test conditions: a 50V rated voltage test is used;
the compressive strength is obtained by testing an AC/DC dielectric analyzer with the model number of 1870, and the test conditions are as follows: the test was carried out using a voltage of 1500V, a current of 500uA, a boost time process of 1S.
TABLE 1
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 (9)
1. The preparation method of the ceramic slurry is characterized by comprising the following steps of:
according to the mass parts, 30-45 parts of recovered ceramics, 2-8 parts of ceramic powder, 0.05-0.25 part of dispersant, 45-80 parts of solvent and 0.03-0.15 part of defoamer are mixed to obtain mixed slurry, the mass ratio of the ceramic powder to the recovered ceramics is 1: 20-1: 5, and the solvent is at least one selected from toluene, xylene, butanone, methyl isobutyl ketone, ethanol, isopropanol, ethylene glycol, ethyl acetate and n-butanol; the recycled ceramic is unusable rim charge generated by cutting a membrane in the process of preparing the MLCC; the ceramic powder is at least one of barium titanate ceramic powder and aluminum oxide ceramic powder; and
and carrying out magnetic separation treatment on the mixed slurry to obtain the ceramic slurry.
2. The method of producing a ceramic slurry according to claim 1, wherein the reclaimed ceramic is a non-magnetic reclaimed ceramic, and the ceramic powder is a non-magnetic ceramic powder.
3. The method of producing a ceramic slurry according to claim 1, wherein the reclaimed ceramic is at least one of a barium titanate ceramic and an alumina ceramic.
4. The method for preparing ceramic slurry according to claim 1, wherein the solvent is selected from a mixed solution of toluene and ethanol, and the mass ratio of toluene to ethanol is 0.5: 1-2: 1.
5. The method for producing ceramic slurry according to claim 1, wherein the defoaming agent is at least one selected from the group consisting of a polyether-modified silicone oil defoaming agent, a mineral oil defoaming agent, a mixed silicone oil defoaming agent, a phenyl silicone oil defoaming agent, and a dimethyl silicone oil defoaming agent.
6. The method for preparing ceramic slurry according to claim 1, wherein the mixing process specifically comprises:
according to the mass parts, stirring 30 to 45 parts of recycled ceramics, 2 to 8 parts of ceramic powder, 0.05 to 0.25 part of dispersant, 45 to 80 parts of solvent and 0.03 to 0.15 part of defoamer at the rotating speed of 300 to 1000rpm for 10 to 60 min;
standing for 10-60 min; and
and then stirring at the rotating speed of 300-1000 rpm for 10-60 min.
7. The method for preparing ceramic slurry according to claim 1, further comprising, after the step of magnetically separating the mixed slurry to obtain ceramic slurry: and carrying out ball milling treatment on the ceramic slurry.
8. The method for preparing ceramic slurry according to claim 7, wherein the ceramic slurry is ball-milled using zirconia balls; the diameter of the zirconia ball is 2.0 mm-7.5 mm; the rotating speed of the ball milling treatment is 30-50 rpm.
9. A ceramic slurry, characterized in that the ceramic slurry is prepared by the method for preparing a ceramic slurry according to any one of claims 1 to 8.
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| CN104211377A (en) * | 2014-09-18 | 2014-12-17 | 福建省德化县南祥陶瓷有限公司 | Process for preparing ceramic craft by utilizing ceramic waste sludge |
| CN104591695A (en) * | 2015-02-03 | 2015-05-06 | 朱立民 | Manufacturing method of large-sized regenerated ceramic |
| CN106242513A (en) * | 2016-08-05 | 2016-12-21 | 卞广勇 | A kind of environment-friendly type building brick utilizing waste material to produce and production technology thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104211377A (en) * | 2014-09-18 | 2014-12-17 | 福建省德化县南祥陶瓷有限公司 | Process for preparing ceramic craft by utilizing ceramic waste sludge |
| CN104591695A (en) * | 2015-02-03 | 2015-05-06 | 朱立民 | Manufacturing method of large-sized regenerated ceramic |
| CN106242513A (en) * | 2016-08-05 | 2016-12-21 | 卞广勇 | A kind of environment-friendly type building brick utilizing waste material to produce and production technology thereof |
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