CN114195487B - Ceramic slurry, ceramic membrane tape, and preparation method and application thereof - Google Patents
Ceramic slurry, ceramic membrane tape, and preparation method and application thereof Download PDFInfo
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention discloses ceramic slurry, a ceramic membrane belt, a preparation method and application thereof. And carrying out tape casting on the ceramic slurry to obtain the ceramic membrane tape. According to the invention, the fluorinated acrylic resin and the polyether modified polysiloxane are combined for the first time and are used in the tape casting process, the advantages of the fluorinated acrylic resin and the polyether modified polysiloxane are integrated, the performance of the film belt is synergistically improved, the preparation of the high-thickness alumina film belt by the tape casting method is realized, and the problems of uneven density, poor flatness, low tensile strength and the like of the high-thickness ceramic film belt are solved. In addition, the casting technology is used for replacing the traditional dry pressing technology, so that the production efficiency is improved, and the production cost is reduced.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to ceramic slurry, a ceramic membrane strip, and a preparation method and application thereof.
Background
The high-thickness 99 alumina ceramic substrate has the advantages of excellent insulativity, high thermal conductivity, high-frequency dielectric property and the like, and is widely applied to thick-film integrated circuits, hybrid integrated circuits and various electronic components. The existing production process of 99 alumina green film belt with high thickness (more than 1.5 mm) is mainly dry pressing forming. However, dry compression molding also has certain limitations: 1) The density in the green body is different, the green sheet is easy to break during sintering, the shrinkage degree is different, the flatness of the surface of the green sheet is poor, secondary grinding and polishing are needed, the cost is high, and the production time is wasted; 2) The method is difficult to process thinner powder (less than 0.2 mm), and is easy to cause arch bridge effect, so that the powder cannot uniformly fill a die cavity, and the phenomenon of elastic after-effect is easy to occur, so that the slab cracks; 3) The production efficiency is low, and the large-scale production cost is high. In view of the above disadvantages, there is a need for a more suitable forming method to produce high thickness green alumina film tapes instead of dry press forming.
The tape casting process has the advantages of simple required equipment, high production efficiency, continuous operation and high degree of automation, and is often used for replacing a dry pressing process to prepare a ceramic substrate in production. However, casting is often used to produce ultra-thin film tapes, and once the thickness of the film tape is greatly increased, the uniformity and flatness of the film tape obtained by casting cannot be ensured, and it is difficult to produce an acceptable high-thickness alumina film tape. At present, the problems of uneven density, poor flatness, low tensile strength and the like commonly exist in high-thickness aluminum oxide film belts in the market.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides the ceramic slurry, and the ceramic slurry can be subjected to tape casting to prepare the high-thickness film belt with uniform density, flatness and high tensile strength.
Meanwhile, the invention also provides a preparation method and application of the ceramic slurry.
Specifically, the invention adopts the following technical scheme:
the first aspect of the invention provides a ceramic slurry, wherein the preparation raw materials of the ceramic slurry comprise ceramic powder and a mixed leveling agent, and the mixed leveling agent comprises fluorinated acrylic resin and polyether modified polysiloxane.
The ceramic slurry according to the first aspect of the present invention has at least the following advantageous effects:
when the ceramic slurry is applied to tape casting, as the polyether modified polysiloxane in the mixed leveling agent contains oleophobic siloxane chains, the polyether modified polysiloxane is more prone to escaping from the bulk phase of the ceramic slurry to a gas-liquid interface; in order to prevent the formation of a dense molecular layer on the surface of the slurry in the initial casting stage and to reduce the fluidity of the slurry, a fluorinated acrylic resin is added in order to disturb the dense silicone molecular layer and promote the fluidity of the slurry, and in order to fill the voids of the powder particles to form a three-dimensional network structure and to provide a certain strength to the film tape. Therefore, the ceramic slurry can be subjected to tape casting to prepare a high-thickness film belt with uniform density, flatness and high tensile strength by adding the mixed leveling agent consisting of the fluorinated acrylic resin and the polyether modified polysiloxane into the ceramic slurry.
In some embodiments of the present invention, the mass ratio of the fluorinated acrylic resin to the polyether-modified polysiloxane is 1.5 to 7:1.
the addition of the fluorinated acrylic resin can disturb the polyether modified polysiloxane to form a dense organic silicon molecular layer and endow a film belt formed by casting with certain strength. But the proportion of fluorinated acrylic resin cannot be infinitely high:
1. when the leveling agent is completely made of fluorinated acrylic resin, (1) fluorinated acrylate continuously volatilizes in a large amount and cannot fill particle gaps, so that the problems of uneven particle accumulation and uneven film belt density are caused; (2) the fluorinated acrylate continuously volatilizes in a large amount, and the formation of B' nard vortex cannot be avoided, so that the surface of the membrane strip is uneven.
2. When the fluorinated acrylic resin: the mass ratio of the polyether modified polysiloxane is less than 1.5:1, the following adverse phenomena occur: (1) in the early stage of drying, the fluorinated acrylic resin is too little, the flowability is insufficient, the density is uneven, and the flatness is poor; (2) the polyether modified polysiloxane monomolecular layer is too thick, the volatilization of a solvent is influenced, longer drying time is needed, and the production efficiency is reduced.
3. Fluorinated acrylic resin: the mass ratio of the polyether modified polysiloxane is 1.5-7: when the thickness of the film belt is within the range of 1, the proportion of the fluorinated acrylic resin and the polyether modified polysiloxane is properly distributed, proportion unbalance does not occur in the early stage and the later stage of casting, and the prepared film belt has uniform density distribution, good flatness and higher strength.
4. Fluorinated acrylic resin: the mass ratio of the polyether modified polysiloxane is more than 7:1, (1) the polyether modified polysiloxane is too little, the surface of the slurry is difficult to cover in the later stage of casting, and a large amount of acrylic ester in the slurry volatilizes, so that the buffer effect cannot be brought, the particle stacking density is uneven, and the problem of uneven film belt density is caused; (2) the polyether modified polysiloxane cannot form a dense monomolecular layer on the surface of the slurry, so that the defects of vortex generation, corrugation on the surface of a substrate and the like are difficult to prevent.
5. When the polyether modified polysiloxane is completely used, (1) the polyether modified polysiloxane can greatly reduce the surface tension, and the fluidity of the slurry cannot be met; (2) the organic silicon monolayer is too thick, which affects the volatilization of the solvent.
Therefore, the mass ratio of the fluorinated acrylic resin to the polyether-modified polysiloxane is preferably 1.5 to 7:1.
in some embodiments of the present invention, the mass ratio of the fluorinated acrylic resin to the polyether-modified polysiloxane is 2 to 5:1.
in some embodiments of the present invention, the ceramic powder is 45 to 50wt% in the ceramic slurry.
In some embodiments of the present invention, the mixed leveling agent is present in the ceramic slurry in an amount of 5 to 10wt%. The leveling agent content is too low to achieve the leveling effect, and the blank sheet smoothness cannot be guaranteed; the content of the flatting agent is too high, the formed surface molecular film is too thick, the volatilization efficiency of the solvent is reduced, and the drying time is prolonged.
In some embodiments of the present invention, the raw materials for preparing the ceramic slurry further include a sintering aid, a dispersant, a plasticizer, and a solvent. Wherein, the sintering aid can reduce the temperature required by sintering; the dispersing agent inhibits the agglomeration of powder particles; the plasticizer can enhance the flexibility of the film strip; the solvent can disperse the ceramic powder and dissolve various auxiliaries, so that the slurry can reach proper viscosity.
In some embodiments of the present invention, the sintering aid is present in the ceramic slurry in an amount of 0.1 to 0.5wt%.
In some embodiments of the present invention, the dispersant is present in the ceramic slurry in an amount of 0.5 to 1wt%.
In some embodiments of the present invention, the plasticizer is present in the ceramic slurry in an amount of 3 to 5wt%.
In some embodiments of the present invention, the solvent is present in the ceramic slurry in an amount of 40 to 45wt%.
In some embodiments of the present invention, the ceramic powder comprises at least one of alumina powder, titania powder, and beryllia powder, and preferably comprises alumina powder.
In some embodiments of the invention, the ceramic powder has a purity of not less than 99%.
In some embodiments of the present invention, the ceramic powder has a particle size of 3 to 4 μm.
In some embodiments of the invention, the sintering aid comprises at least one of silica, magnesia, calcia.
In some embodiments of the invention, the dispersant comprises at least one of oleic acid, polyisobutylene, polyethylene glycol, polyvinylbutyral.
In some embodiments of the invention, the plasticizer comprises at least one of dibutyl phthalate, dioctyl phthalate, polyethylene.
In some embodiments of the invention, the solvent comprises at least one of isopropanol, toluene, ethanol.
The second aspect of the present invention provides a method for preparing the ceramic slurry, comprising the steps of: mixing the preparation raw materials to obtain the ceramic slurry.
After the feedstock is to be prepared, a slurry may be formed by milling (preferably ball milling). The particle size of the ceramic slurry after grinding is 2.5-3 μm, and the viscosity is 1200-1500 cps (25 ℃).
In a third aspect of the present invention, there is provided a ceramic membrane tape, wherein the raw material for preparing the ceramic membrane tape comprises the above ceramic slurry.
In some embodiments of the invention, the ceramic membrane tape has a thickness > 1.5mm, preferably ≧ 1.8mm, more preferably 1.8-2.2 mm.
In some embodiments of the invention, the ceramic membrane strip has a thickness variation range of 0.05mm or less, more preferably 0.04mm or less, 0.03mm or less, or 0.02mm or less.
In some embodiments of the invention, the density of the ceramic film tape is > 1.6g/cm 3 Preferably > 1.8g/cm 3 More preferably 1.8 to 2.1g/cm 3 。
In some embodiments of the invention, the ceramic film strip has a density that fluctuates by less than or equal to 0.05mm, more preferably less than or equal to 0.04mm, less than or equal to 0.03mm, less than or equal to 0.02mm, or less than or equal to 0.01mm.
The fourth aspect of the present invention provides a method for producing the above ceramic membrane tape, comprising the steps of: and carrying out tape casting on the ceramic slurry, and forming to obtain the ceramic membrane band.
In some embodiments of the present invention, the method further comprises a step of filtering and defoaming the ceramic slurry before the casting.
In some embodiments of the invention, the forming further comprises a drying step. The drying comprises two stages of low-temperature drying and high-temperature drying. Wherein the low-temperature drying temperature is 60-90 ℃, and the time is 10-15 min, preferably 11-14 min; the high-temperature drying temperature is 110-140 ℃, and the time is 10-15 min, preferably 10-13 min.
The invention also provides application of the ceramic film strip in manufacturing electronic components. The electronic components may include integrated circuits and the like.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the mixed leveling agent consisting of the fluorinated acrylic resin and the polyether modified polysiloxane is added into the ceramic slurry, and the ceramic slurry can be applied to the preparation of the ceramic membrane band by tape casting. After the slurry flows through a scraper, the slurry enters a low-temperature drying area (60-90 ℃), and due to the fact that the hydrophilic groups of the fluorinated acrylic resin in the leveling agent enhance the wettability of the slurry, the fluidity of the slurry is enhanced, and the spreading and uniformity degree of the slurry is promoted. During casting, the slurry flows from a surface of low surface tension to a surface of high surface tension, and the rapid flow produces a rippled surface. The fluorinated acrylic resin can gather on the surface of the sizing agent to stabilize the liquid level, thereby avoiding the situation. In addition, a part of the fluorinated acrylic resin can be freely dispersed around the powder particles in a curled form to fill gaps among the particles, so that the buffer effect is achieved, excessive accumulation of the particles is avoided, and uneven density of a green body is prevented.
The slurry passes through a high-temperature drying area (110-140 ℃) in the later period of casting, most of the solvent is volatilized at the moment, the medium with lower density and lower viscosity is brought to the surface and forms a vortex, the vortex in the horizontal plane is called as a B' nard vortex, and the ceramic powder particles in the slurry are also brought to form an uneven surface. Meanwhile, the fluorinated acrylic resin has the characteristic of no temperature resistance, and a large amount of volatilization of the fluorinated acrylic resin can be caused by high temperature, so that the original function is lost. The leveling system has the advantages that after the fluorinated acrylic resin on the surface is volatilized, the polyether organic silicon can form a dense monomolecular layer on a gas-liquid interface to replace the fluorinated acrylic resin to stabilize the interface, the surface tension of the slurry is greatly reduced, and the formation of B' nard vortex is avoided; on the other hand, the fluorinated acrylic resin in the film is prevented from being excessively volatilized, and after the small molecular solvent is volatilized, the fluorinated acrylic resin is cured into a three-dimensional network structure, so that the ceramic particles are prevented from being settled, and a certain strength is given to the film.
In short, the invention starts from the later period before and after the casting and drying, combines the fluorinated acrylic resin and the polyether modified polysiloxane for the first time and uses the fluorinated acrylic resin and the polyether modified polysiloxane in the casting and forming process, integrates the advantages of the fluorinated acrylic resin and the polyether modified polysiloxane, creatively discovers and utilizes the protective effect of the polyether modified polysiloxane on the fluorinated acrylic resin in the casting process, and synergistically improves the performance of the film belt. In the early stage of drying, the fluidity and the stability of the slurry are improved through the wettability of the fluorinated acrylic resin, in the later stage of drying, the polyether modified polysiloxane in the flatting agent system makes up the defect that the fluorinated acrylic resin is not resistant to high temperature, a molecular layer is formed on the surface of the slurry, the volatilization amount of the fluorinated acrylic resin is obviously reduced, the fluorinated acrylic resin is solidified in the slurry, a three-dimensional network structure is formed, and certain strength is endowed to the membrane. The mixed leveling agent avoids the defect that the fluorinated acrylic resin is not resistant to temperature, realizes the preparation of the high-thickness alumina membrane band by a tape casting method, and solves the problems of uneven density, poor flatness, low tensile strength and the like of the high-thickness ceramic membrane band.
In addition, the casting technology is used for replacing the traditional dry pressing technology, so that the production efficiency is improved, and the production cost is reduced.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples. The starting materials used in the following examples, unless otherwise specified, are available from conventional commercial sources; the processes used, unless otherwise specified, are conventional in the art.
The raw material composition of the alumina slurry is shown in the following table 1.
TABLE 1 raw material composition of alumina slurry
In table 1, the sintering aid is silicon dioxide, the dispersant is oleic acid, the plasticizer is dibutyl phthalate, and the solvent is isopropanol.
Ceramic slurry was prepared and used to prepare alumina ceramic membrane tape as follows:
(1) Fully mixing 99 alumina powder, a mixed leveling agent, a sintering aid, a dispersing agent, a plasticizer and a solvent according to the proportion shown in the table 1, and performing ball milling to prepare ceramic slurry;
(2) Filtering the ceramic slurry obtained in the step (1), and then putting the ceramic slurry into a defoaming cylinder for defoaming;
(3) Casting the defoamed ceramic slurry in a casting machine to obtain a green body after molding;
(4) And (4) drying the green body obtained by casting in the step (3) by a drying oven (the drying procedure is 70 ℃/12min → 125 ℃/11 min), so as to obtain the high-thickness 99 alumina ceramic film belt.
The performance of the 99 alumina ceramic membrane tape was tested as follows, and the test results are shown in table 2.
(1) Green density:
(1) the film strips (100 mm. Times.100 mm) were cut at 3 random positions along each side in the casting direction, and the cut green film strips were directly weighed to obtain M.
(2) Putting the membrane belt into a liquid immersion groove, putting the liquid immersion groove into a vacuum device, vacuumizing for 10min at a vacuum degree of not less than 0.095MPa, then injecting distilled water in 3min until the membrane belt is immersed in the liquid level, continuing vacuumizing for 30min, then opening the vacuum device, taking out the liquid immersion groove, taking out the membrane belt, wiping off redundant liquid on the surface, and immediately weighing M1.
(3) The wire frame is hung at one end of a balance and is sunk in a container containing distilled water, then a sample saturated with the distilled water is placed in the wire frame and is not in contact with any part of the container, the liquid level is kept 60mm above the membrane strip, and M2 is weighed.
Calculating the formula: d = M/(M1-M2) × D
D: green density (g/cm) 3 )；
d: density of distilled water (g/cm) 3 )。
(2) Tensile strength:
(1) the measuring tool measures the length and width of the faying surface of the test sample.
(2) The test specimen is symmetrically clamped in upper and lower clamps of a universal tester, and the distance from the clamping position to the overlapping end is (50 +/-1) mm.
(3) The test instrument was started at a speed of within 5mm/min and loaded at a steady speed. The maximum load of the specimen to shear failure was recorded.
Calculating the formula: a = p/(b x d)
a is tensile strength (MPa);
p is the maximum load (N);
b is the specimen width (mm);
d is the specimen thickness (mm).
(3) Thickness of the film tape:
and measuring more than three points on each side of each coil of blank roll in the casting direction by using a spiral micrometer, and taking and recording the maximum value/the minimum value.
(4) Appearance:
and observing whether the film belt has the defects of fluctuation, grains, depression and the like by naked eyes.
TABLE 2.99 alumina ceramic Membrane strip Properties
It can be seen from comparing example 1 with comparative example 1 that the proportion of the fluorinated acrylate in the leveling agent is too small, so that the fluidity of the casting slurry is insufficient, and further the density of the film tape is not uniform, and because the proportion of the fluorinated acrylate is too small, the gaps between the particles are difficult to completely fill, a stable three-dimensional network structure cannot be formed after drying, and the tensile strength of the film tape is reduced.
As can be seen from the comparison between example 1 and comparative example 2, too little leveling agent can not cover the surface of the slurry, so that the fluidity of the slurry is too low, and the density of the film tape is uneven; and the content of the fluorinated acrylate in the slurry is too low due to too little leveling agent, so that the tensile strength of the membrane tape is reduced, and the content of the polyether modified polysiloxane in the slurry is too low, so that a dense molecular layer cannot be formed after casting to prevent the generation of eddy current, and the slurry has poor flatness and has ripples.
As can be seen from the comparison between example 7 and comparative example 3, the proportion of fluorinated acrylate is too large, the volatilization time required in the post-casting period is increased, the remained fluorinated acrylate is increased and is gathered on the surface of the slurry, the polyether modified polysiloxane is difficult to form a dense monomolecular layer, the problem of eddy current cannot be avoided, and the slurry has poor flatness, large thickness fluctuation and corrugation.
As can be seen from the comparison between example 7 and comparative example 4, the content of the leveling agent is too much, so that fluorinated acrylate and polyether modified polysiloxane are greatly gathered on the surface of the slurry, the normal volatilization of the solvent is prevented in the early stage of casting (low temperature region), the slurry with a large amount of solvent remained enters the later stage of casting (high temperature region), the solvent is violently volatilized, the defects of bubbles, ripples and the like are formed on the surface of the membrane strip, and the thickness and the strength of the membrane strip are influenced.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. Ceramic slurry, characterized in that: the preparation raw materials of the ceramic slurry comprise ceramic powder and a mixed leveling agent, wherein the mixed leveling agent comprises fluorinated acrylic resin and polyether modified polysiloxane;
the mass ratio of the fluorinated acrylic resin to the polyether modified polysiloxane is 1.5-7: 1; the proportion of the mixed leveling agent in the ceramic slurry is 5-10 wt%.
2. The ceramic slurry according to claim 1, wherein: the mass ratio of the fluorinated acrylic resin to the polyether modified polysiloxane is 2-5: 1.
3. the ceramic slurry according to claim 1, wherein: the ceramic powder accounts for 45-50 wt% of the ceramic slurry.
4. The ceramic slurry according to any one of claims 1 to 3, characterized in that: the ceramic powder comprises at least one of alumina powder, titanium dioxide powder and beryllium oxide powder.
5. The ceramic slurry according to claim 4, wherein: the ceramic powder comprises alumina powder.
6. A method for producing a ceramic slurry according to any one of claims 1 to 5, characterized in that: the method comprises the following steps: mixing the preparation raw materials to obtain the ceramic slurry.
7. Ceramic membrane area, its characterized in that: the raw material for producing the ceramic membrane tape comprises the ceramic slurry according to any one of claims 1 to 5.
8. A method of producing a ceramic membrane tape according to claim 7, characterized in that: the method comprises the following steps: casting the ceramic slurry according to any one of claims 1 to 5 to obtain a ceramic film tape after molding.
9. Use of the ceramic film tape according to claim 7 for the manufacture of electronic components.
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| CN109054556A (en) * | 2018-07-11 | 2018-12-21 | 合肥信亚达智能科技有限公司 | A kind of water nano compound heat-insulation coating and preparation method thereof |
| CN110204306B (en) * | 2019-04-08 | 2022-03-25 | 江西和美陶瓷有限公司 | Silk fine matt ceramic tile and preparation method thereof |
| CN111548101B (en) * | 2020-06-29 | 2022-05-13 | 广东平坦适环保材料有限公司 | Cement-based efficient permeable crystallization type waterproof material and preparation method thereof |
| CN112608154A (en) * | 2020-12-28 | 2021-04-06 | 合肥圣达电子科技实业有限公司 | Silicon nitride ceramic slurry and preparation method and application thereof |
| CN113024740A (en) * | 2021-03-10 | 2021-06-25 | 鸿鑫三维科技(东莞)有限公司 | 3D printing material and 3D printing method |
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