CN110683837A - Heat-conducting low-temperature co-fired ceramic material and preparation method thereof - Google Patents
Heat-conducting low-temperature co-fired ceramic material and preparation method thereof Download PDFInfo
- Publication number
- CN110683837A CN110683837A CN201911138228.6A CN201911138228A CN110683837A CN 110683837 A CN110683837 A CN 110683837A CN 201911138228 A CN201911138228 A CN 201911138228A CN 110683837 A CN110683837 A CN 110683837A
- Authority
- CN
- China
- Prior art keywords
- temperature
- powder
- heat
- based glass
- ceramic material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/36—Glass starting materials for making ceramics, e.g. silica glass
- C04B2235/365—Borosilicate glass
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6025—Tape casting, e.g. with a doctor blade
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a heat-conducting low-temperature co-fired ceramic material and a preparation method thereof. The material comprises the following components in percentage by weight: 100 parts of Bi-based glass, 80-150 parts of alumina ceramic powder and less than or equal to 3 parts of carbide, wherein the grain diameter of the alumina ceramic powder is 1-2 mu m; the method comprises the steps of mixing bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide, melting, quenching by water cooling, ball-milling the obtained Bi-based glass slag into powder, mixing with aluminum oxide ceramic powder, ball-milling the obtained mixed powder with a solvent, a dispersing agent, a binder, a plasticizer and a homogenizing agent in sequence, tape-casting the obtained stable and uniform slurry on a mold, drying, sequentially placing the obtained green ceramic chip at the temperature of 300-plus-one-material 600 ℃ for removing organic additives, and sintering and molding at the temperature of 800-plus-one-material 950 ℃ to obtain the target product. The heat-conducting property of the material is obviously improved, the dielectric property is obviously improved, and the material is very easy to be widely applied to the field of electronic packaging in a commercial mode.
Description
Technical Field
The invention relates to a ceramic material and a preparation method thereof, in particular to a heat-conducting low temperature co-fired ceramic (LTCC) material and a preparation method thereof.
Background
With the rapid development of the information-oriented industry, people have increasingly high requirements on miniaturization, integration and portability of electronic products. In order to modularize and highly integrate electronic components and circuits, it is necessary to further improve the packaging density of the circuits and the stability of the system. Low temperature co-fired ceramic is a technology for printing interconnecting conductors, components and circuits on unsintered cast ceramic material, pressing them together in a stack, and sintering into an integrated ceramic multilayer material, which provides a practical solution to achieve the above objectives. Recently, people have made continuous efforts to obtain low-temperature co-fired ceramic materials, such as a bismuth oxide-niobium oxide based LTCC substrate material and a preparation method thereof, disclosed in 2019, 8, 23 and 8 of chinese patent application CN 110156455 a. The LTCC substrate material mentioned in this patent application consists of Bi2O3-Nb2O5Ceramic powder, ZnO-B2O3-SiO2Microcrystalline glass and CuO-V2O5A sintering aid; the preparation method comprises the steps of respectively preparing raw materials of ceramic powder, microcrystalline glass and sintering aid, ball milling, screening, drying, crushing uniformly, calcining or smeltingGrinding the mixture and the crushed balls into powder, mixing the powder in proportion, and carrying out tape casting, laminated hot pressing and sintering treatment to obtain the product. Although the product reduces the sintering temperature of a green body and shortens the sintering time, the product has defects with the preparation method, firstly, the product has poor thermal conductivity, the application range is limited, and particularly, the product is used for circuit packaging with higher power; secondly, the preparation process is not only too complicated, but also does not allow to obtain products with high thermal conductivity.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a heat-conducting low-temperature co-fired ceramic material with higher heat-conducting property.
The invention also provides a preparation method of the heat-conducting low-temperature co-fired ceramic material.
In order to solve the technical problem of the invention, the adopted technical scheme is that the heat-conducting low-temperature co-fired ceramic material comprises the following components in percentage by weight:
100 parts by weight of a Bi-based glass,
alumina (Al)2O3) 80-150 parts by weight of ceramic powder,
carbide is less than or equal to 3 weight portions;
wherein the grain diameter of the alumina ceramic powder is 1-2 μm.
As a further improvement of the heat-conducting low-temperature co-fired ceramic material:
preferably, the Bi-based glass is made of bismuth trioxide (Bi)2O3) Boron oxide (B)2O3) Silicon oxide (SiO)2) Zinc oxide (ZnO) and aluminum oxide (Al)2O3) In a molar ratio of 1: 0.1-1: 0.05-0.2: 0.5-1: 0-0.2.
In order to solve another technical problem of the present invention, another technical solution is that the preparation method of the heat-conducting low-temperature co-fired ceramic material comprises a tape casting method, and particularly comprises the following steps:
step 1, firstly, according to the molar ratio of bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide of 1: 0.1-1: 0.05-0.2: 0.5-1: 0-0.2, mixing the five materials to obtain a mixture, melting the mixture at 900-1200 ℃, and performing water-cooling quenching to obtain Bi-based glass slag;
step 2, ball-milling the Bi-based glass slag into Bi-based glass powder with the particle size of less than or equal to 400nm, and mixing the Bi-based glass powder with alumina ceramic powder to obtain mixed powder;
step 3, firstly, according to the weight ratio of the Bi-based glass powder, the solvent and the dispersant in the mixed powder of 1: 0.1-2: 0.01-0.1, performing ball milling on the mixed powder, the solvent and the dispersant for 2-12 hours to obtain uniformly dispersed slurry, and then mixing the Bi-based glass powder, the binder, the plasticizer and the homogenizing agent in the uniformly dispersed slurry according to the weight ratio of 1: 0.05-0.1: 0.1-0.2: 0.005-0.05, and performing ball milling on the uniformly dispersed slurry, the binder, the plasticizer and the homogenizing agent for 2-12h to obtain stable and uniform slurry;
and 4, casting and molding the stable and uniform slurry on a mold, drying to obtain a raw ceramic chip, and sequentially placing the raw ceramic chip at the temperature of 300 ℃ and 600 ℃ for 1.5-2.5h to remove organic additives and at the temperature of 800 ℃ and 950 ℃ for 1.5-2.5h to sinter and mold to obtain the heat-conducting low-temperature co-fired ceramic material.
The preparation method of the low-temperature co-fired ceramic material with heat conduction is further improved as follows:
preferably, the solvent is ethanol, or xylene.
Preferably, the dispersant is castor oil, or fish oil, or a phosphate ester, or tributyl phosphate, or triethanolamine.
Preferably, the binder is polyvinyl alcohol, or polyvinyl butyral, or polyvinyl chloride, or polyvinylpyrrolidone, or polymethylmethacrylate.
Preferably, the plasticizer is one or two mixture of butyl benzyl phthalate, dibutyl phthalate, dimethyl phthalate, dioctyl phthalate and polyethylene glycol.
Preferably, the leveling agent is cyclohexanone, or cyclohexane.
Preferably, the mold is a polyimide flat sheet mold.
Preferably, the drying is air drying at room temperature.
Compared with the prior art, the beneficial effects are that:
firstly, the cross section of the prepared target product is respectively characterized by using a scanning electron microscope and an attached energy spectrum tester, and the result shows that the cross section of the target product is that alumina ceramic powder with the grain diameter of 1-2 mu m is uniformly dispersed in Bi-based glass, and the alumina ceramic powder is tightly combined with the Bi-based glass without gaps; the trace carbide contained in the material is the residue of organic additives, namely solvent, dispersant, binder, plasticizer and leveling agent after sintering. The target product mainly composed of the alumina ceramic powder and the Bi-based glass not only has low dielectric constant, low loss, high thermal conductivity and low cost due to the alumina ceramic, but also has the grain diameter of 1-2 mu m, and due to the selection of the Bi-based glass for reducing sintering temperature and improving the density of a sintered sheet, and the grain diameter of the Bi-based glass powder is preferably less than or equal to 400nm, and the Bi-based glass powder with large specific surface area and high surface activation energy is easy to melt and wet the alumina ceramic powder due to the optimized combination of the components and the contents between the Bi-based glass and the alumina ceramic powder, thereby laying a good foundation for the change of the heat conduction performance and the dielectric performance of the target product.
Secondly, the prepared target product is tested for multiple times and multiple batches by using a thermal conductivity meter, and the result shows that the thermal conductivity coefficient is as high as 5W/m.K.
Thirdly, the preparation method is simple, scientific and efficient. Not only the target product with higher heat-conducting property, namely the heat-conducting low-temperature co-fired ceramic material is prepared; besides the obtained intermediate product, namely the green ceramic chip, has stronger bending property and tensile property, the heat conduction and dielectric property of the target product, namely the baked ceramic chip, are obviously improved; the method has the characteristics of simple and easy process, low cost and suitability for industrial mass production; thereby leading the target product to be easy to be widely applied to the electronic packaging field in a commercial way.
Drawings
FIG. 1 is one of the results of characterization of a cross section of an objective product obtained by the preparation method using a Scanning Electron Microscope (SEM). The SEM image shows the state of dispersion of the alumina ceramic powder in the high-density Bi-based glass matrix, and the bonding state between the two.
FIG. 2 is one of the results of characterization of a cross section of the objective product obtained using a scanning electron microscope and an energy spectrum (EDS) tester attached thereto. FIG. 2 is an SEM image of the target product shown in the drawing "a" and a drawing "b" which is a cross-sectional elemental content chart of the target product shown in the drawing "a".
Detailed Description
Preferred embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
First commercially available or manufactured on its own:
bismuth trioxide;
boron oxide;
silicon oxide;
zinc oxide;
alumina;
alumina ceramic powder with the grain diameter of 1-2 mu m;
ethanol and xylene as solvents;
castor oil, fish oil, phosphate, tributyl phosphate and triethanolamine as dispersants;
polyvinyl alcohol, polyvinyl butyral, polyvinyl chloride, polyvinyl pyrrolidone, and polymethyl methacrylate as a binder;
butyl benzyl phthalate, dibutyl phthalate, dimethyl phthalate, dioctyl phthalate and polyethylene glycol as plasticizers;
cyclohexanone and cyclohexane as leveling agents;
and (3) a polyimide.
Then:
example 1
Step 1, firstly, according to the molar ratio of bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide of 1: 0.1: 0.2: 0.5: 0.2, mixing the five to obtain a mixture. And then melting the mixture at 900 ℃, and then quenching by water cooling to obtain the Bi-based glass slag.
And step 2, ball-milling the Bi-based glass slag into Bi-based glass powder with the particle size of 360 nm. Then, the powder was mixed with alumina ceramic powder having a particle size of 2 μm to obtain a mixed powder.
Step 3, firstly, according to the weight ratio of the Bi-based glass powder, the solvent and the dispersant in the mixed powder of 1: 0.1: the mixed powder, the solvent and the dispersant are ball-milled for 2 hours according to the proportion of 0.1; wherein the solvent is ethanol, and the dispersant is castor oil, so as to obtain uniformly dispersed slurry. And then uniformly dispersing the Bi-based glass powder, the binder, the plasticizer and the homogenizing agent in the slurry according to the weight ratio of 1: 0.05: 0.2: 0.005, carrying out ball milling on the uniformly dispersed slurry, the binder, the plasticizer and the homogenizing agent for 2 hours; wherein, the adhesive is polyvinyl alcohol, the plasticizer is butyl benzyl phthalate, and the leveling agent is cyclohexanone, so as to obtain stable and uniform slurry.
And 4, casting the stable and uniform slurry on a polyimide flat plate die, and airing at room temperature to obtain the green ceramic chip. And then sequentially placing the green ceramic chip at 300 ℃ for 2.5h to remove organic additives and at 800 ℃ for 2.5h to sinter and form to prepare the heat-conducting low-temperature co-fired ceramic material similar to that shown in figure 1 and b in figure 2.
Example 2
Step 1, firstly, according to the molar ratio of bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide of 1: 0.3: 0.16: 0.63: 0.15 to obtain a mixture. And melting the mixture at 975 ℃, and then carrying out water-cooling quenching to obtain the Bi-based glass slag.
And step 2, firstly, ball-milling the Bi-based glass slag into Bi-based glass powder with the particle size of 370 nm. Then, the powder was mixed with alumina ceramic powder having a particle size of 1.8 μm to obtain a mixed powder.
Step 3, firstly, according to the weight ratio of the Bi-based glass powder, the solvent and the dispersant in the mixed powder of 1: 0.5: the mixed powder, the solvent and the dispersant are ball-milled for 4.5 hours according to the proportion of 0.078; wherein the solvent is ethanol, and the dispersant is castor oil, so as to obtain uniformly dispersed slurry. And then uniformly dispersing the Bi-based glass powder, the binder, the plasticizer and the homogenizing agent in the slurry according to the weight ratio of 1: 0.063: 0.18: the slurry, the binder, the plasticizer and the homogenizing agent which are uniformly dispersed are ball-milled for 4.5 hours together according to the proportion of 0.016; wherein, the adhesive is polyvinyl alcohol, the plasticizer is butyl benzyl phthalate, and the leveling agent is cyclohexanone, so as to obtain stable and uniform slurry.
And 4, casting the stable and uniform slurry on a polyimide flat plate die, and airing at room temperature to obtain the green ceramic chip. And then sequentially placing the green ceramic chip at 375 ℃ for 2.3h to remove organic additives and at 838 ℃ for 2.3h to sinter and form to obtain the heat-conducting low-temperature co-fired ceramic material similar to that shown in figure 1 and b in figure 2.
Example 3
Step 1, firstly, according to the molar ratio of bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide of 1: 0.6: 0.13: 0.75: 0.1, mixing the five to obtain a mixture. And then the mixture is melted at 1050 ℃ and then water-cooled and quenched to obtain the Bi-based glass slag.
And step 2, ball-milling the Bi-based glass slag into Bi-based glass powder with the particle size of 380 nm. Then, the powder was mixed with alumina ceramic powder having a particle size of 1.5 μm to obtain a mixed powder.
Step 3, firstly, according to the weight ratio of the Bi-based glass powder, the solvent and the dispersant in the mixed powder of 1: 1.05: 0.055, carrying out ball milling on the mixed powder, the solvent and the dispersing agent for 7 hours; wherein the solvent is ethanol, and the dispersant is castor oil, so as to obtain uniformly dispersed slurry. And then uniformly dispersing the Bi-based glass powder, the binder, the plasticizer and the homogenizing agent in the slurry according to the weight ratio of 1: 0.075: 0.15: 0.028, carrying out ball milling on the uniformly dispersed slurry, the binder, the plasticizer and the homogenizing agent for 7 hours; wherein, the adhesive is polyvinyl alcohol, the plasticizer is butyl benzyl phthalate, and the leveling agent is cyclohexanone, so as to obtain stable and uniform slurry.
And 4, casting the stable and uniform slurry on a polyimide flat plate die, and airing at room temperature to obtain the green ceramic chip. And sequentially placing the green ceramic chip at 450 ℃ for 2h to remove the organic additives and at 875 ℃ for 2h to sinter and form to obtain the heat-conducting low-temperature co-fired ceramic material shown in figure 1 and b in figure 2.
Example 4
Step 1, firstly, according to the molar ratio of bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide of 1: 0.8: 0.09: 0.88: 0.05, and mixing the five to obtain a mixture. And then the mixture is melted at 1125 ℃, and then water-cooled and quenched to obtain the Bi-based glass slag.
And 2, firstly, ball-milling the Bi-based glass slag into Bi-based glass powder with the particle size of 390 nm. Then, the powder was mixed with alumina ceramic powder having a particle size of 1.3 μm to obtain a mixed powder.
Step 3, firstly, according to the weight ratio of the Bi-based glass powder, the solvent and the dispersant in the mixed powder of 1: 1.45: the mixed powder, the solvent and the dispersant are ball-milled for 9.5 hours according to the proportion of 0.033; wherein the solvent is ethanol, and the dispersant is castor oil, so as to obtain uniformly dispersed slurry. And then uniformly dispersing the Bi-based glass powder, the binder, the plasticizer and the homogenizing agent in the slurry according to the weight ratio of 1: 0.088: 0.13: 0.039, carrying out ball milling on the uniformly dispersed slurry, the binder, the plasticizer and the homogenizing agent for 9.5 hours; wherein, the adhesive is polyvinyl alcohol, the plasticizer is butyl benzyl phthalate, and the leveling agent is cyclohexanone, so as to obtain stable and uniform slurry.
And 4, casting the stable and uniform slurry on a polyimide flat plate die, and airing at room temperature to obtain the green ceramic chip. And then sequentially placing the green ceramic chip at 525 ℃ for 1.8h to remove organic additives and at 913 ℃ for 1.8h to sinter and form, thus obtaining the heat-conducting low-temperature co-fired ceramic material similar to that shown in figure 1 and the b-diagram in figure 2.
Example 5
Step 1, firstly, according to the molar ratio of bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide of 1: 1: 0.05: 1: 0 to obtain a mixture. And then melting the mixture at 1200 ℃, and then quenching by water cooling to obtain the Bi-based glass slag.
And step 2, ball-milling the Bi-based glass slag into Bi-based glass powder with the particle size of 400 nm. And then mixing the powder with alumina ceramic powder with the particle size of 1 mu m to obtain mixed powder.
Step 3, firstly, according to the weight ratio of the Bi-based glass powder, the solvent and the dispersant in the mixed powder of 1: 2: the mixed powder, the solvent and the dispersant are ball-milled for 12 hours according to the proportion of 0.01; wherein the solvent is ethanol, and the dispersant is castor oil, so as to obtain uniformly dispersed slurry. And then uniformly dispersing the Bi-based glass powder, the binder, the plasticizer and the homogenizing agent in the slurry according to the weight ratio of 1: 0.1: 0.1: 0.05, carrying out ball milling on the uniformly dispersed slurry, the binder, the plasticizer and the homogenizing agent for 12 hours; wherein, the adhesive is polyvinyl alcohol, the plasticizer is butyl benzyl phthalate, and the leveling agent is cyclohexanone, so as to obtain stable and uniform slurry.
And 4, casting the stable and uniform slurry on a polyimide flat plate die, and airing at room temperature to obtain the green ceramic chip. And then sequentially placing the green ceramic chip at 600 ℃ for 1.5h to remove organic additives and at 950 ℃ for 1.5h to sinter and form to prepare the heat-conducting low-temperature co-fired ceramic material similar to that shown in figure 1 and the b-diagram in figure 2.
Ethanol or xylene as a solvent, castor oil or fish oil or phosphate or tributyl phosphate or triethanolamine as a dispersing agent, polyvinyl alcohol or polyvinyl butyral or polyvinyl chloride or polyvinyl pyrrolidone or polymethyl methacrylate as a binder, one or a mixture of two of butyl benzyl phthalate, dibutyl phthalate, dimethyl phthalate, dioctyl phthalate and polyethylene glycol as a plasticizer, and cyclohexanone or cyclohexane as a homogenizing agent are respectively selected, and the above examples 1 to 5 are repeated to prepare the heat-conducting low-temperature co-fired ceramic material shown in or similar to the graph in FIG. 1 and the graph b in FIG. 2.
It will be apparent to those skilled in the art that various modifications and variations can be made in the thermally conductive low temperature co-fired ceramic material and the method of making the same of the present invention without departing from the spirit or scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (10)
1. A heat-conducting low-temperature co-fired ceramic material comprises the following components in percentage by weight:
100 parts by weight of a Bi-based glass,
80-150 parts by weight of alumina ceramic powder,
carbide is less than or equal to 3 weight portions;
wherein the grain diameter of the alumina ceramic powder is 1-2 μm.
2. The heat-conducting low-temperature co-fired ceramic material as claimed in claim 1, wherein the Bi-based glass is prepared from bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide in a molar ratio of 1: 0.1-1: 0.05-0.2: 0.5-1: 0-0.2.
3. A preparation method of the heat-conducting low-temperature co-fired ceramic material as claimed in claim 1, which comprises a tape casting method, and is characterized by comprising the following steps:
step 1, firstly, according to the molar ratio of bismuth trioxide, boron oxide, silicon oxide, zinc oxide and aluminum oxide of 1: 0.1-1: 0.05-0.2: 0.5-1: 0-0.2, mixing the five materials to obtain a mixture, melting the mixture at 900-1200 ℃, and performing water-cooling quenching to obtain Bi-based glass slag;
step 2, ball-milling the Bi-based glass slag into Bi-based glass powder with the particle size of less than or equal to 400nm, and mixing the Bi-based glass powder with alumina ceramic powder to obtain mixed powder;
step 3, firstly, according to the weight ratio of the Bi-based glass powder, the solvent and the dispersant in the mixed powder of 1: 0.1-2: 0.01-0.1, performing ball milling on the mixed powder, the solvent and the dispersant for 2-12 hours to obtain uniformly dispersed slurry, and then mixing the Bi-based glass powder, the binder, the plasticizer and the homogenizing agent in the uniformly dispersed slurry according to the weight ratio of 1: 0.05-0.1: 0.1-0.2: 0.005-0.05, and performing ball milling on the uniformly dispersed slurry, the binder, the plasticizer and the homogenizing agent for 2-12h to obtain stable and uniform slurry;
and 4, casting and molding the stable and uniform slurry on a mold, drying to obtain a raw ceramic chip, and sequentially placing the raw ceramic chip at the temperature of 300 ℃ and 600 ℃ for 1.5-2.5h to remove organic additives and at the temperature of 800 ℃ and 950 ℃ for 1.5-2.5h to sinter and mold to obtain the heat-conducting low-temperature co-fired ceramic material.
4. A method for preparing a heat-conducting low-temperature co-fired ceramic material according to claim 3, wherein the solvent is ethanol or xylene.
5. A method for preparing a heat-conducting low-temperature co-fired ceramic material as claimed in claim 3, wherein the dispersant is castor oil, or fish oil, or phosphate, or tributyl phosphate, or triethanolamine.
6. A method for preparing a heat-conducting low-temperature co-fired ceramic material as claimed in claim 3, wherein the binder is polyvinyl alcohol, polyvinyl butyral, polyvinyl chloride, polyvinyl pyrrolidone, or polymethyl methacrylate.
7. The method for preparing the heat-conducting low-temperature co-fired ceramic material according to claim 3, wherein the plasticizer is one or a mixture of two of butyl benzyl phthalate, dibutyl phthalate, dimethyl phthalate, dioctyl phthalate and polyethylene glycol.
8. A method for preparing a heat-conducting low-temperature co-fired ceramic material as claimed in claim 3, wherein the homogenizing agent is cyclohexanone or cyclohexane.
9. The method of claim 3, wherein the mold is a polyimide flat film.
10. A method of preparing a thermally conductive low temperature co-fired ceramic material as claimed in claim 3, wherein the drying is air drying at room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911138228.6A CN110683837A (en) | 2019-11-20 | 2019-11-20 | Heat-conducting low-temperature co-fired ceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911138228.6A CN110683837A (en) | 2019-11-20 | 2019-11-20 | Heat-conducting low-temperature co-fired ceramic material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110683837A true CN110683837A (en) | 2020-01-14 |
Family
ID=69117035
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911138228.6A Pending CN110683837A (en) | 2019-11-20 | 2019-11-20 | Heat-conducting low-temperature co-fired ceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110683837A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143166A (en) * | 2020-09-11 | 2020-12-29 | 北京理工大学 | Ceramic-reinforced boron phenolic resin-based composite material and preparation method thereof |
| CN113402283A (en) * | 2020-03-16 | 2021-09-17 | 中国科学院上海硅酸盐研究所 | Low-temperature co-fired ceramic substrate and preparation method thereof |
| CN114628058A (en) * | 2022-05-16 | 2022-06-14 | 西安宏星电子浆料科技股份有限公司 | Copper terminal electrode slurry for multilayer chip ceramic capacitor and preparation method thereof |
-
2019
- 2019-11-20 CN CN201911138228.6A patent/CN110683837A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| I.J.INDUJA: "LTCC tapes based on Al2O3–BBSZ glass with improved thermal conductivity", 《CERAMICS INTERNATIONAL》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113402283A (en) * | 2020-03-16 | 2021-09-17 | 中国科学院上海硅酸盐研究所 | Low-temperature co-fired ceramic substrate and preparation method thereof |
| CN112143166A (en) * | 2020-09-11 | 2020-12-29 | 北京理工大学 | Ceramic-reinforced boron phenolic resin-based composite material and preparation method thereof |
| CN114628058A (en) * | 2022-05-16 | 2022-06-14 | 西安宏星电子浆料科技股份有限公司 | Copper terminal electrode slurry for multilayer chip ceramic capacitor and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110683837A (en) | Heat-conducting low-temperature co-fired ceramic material and preparation method thereof | |
| CN101321415B (en) | Rare earth thick film circuit electrical heating element based on aluminum nitride minicrystal ceramic substrates and its preparation technique | |
| CN100503507C (en) | Low temperature sintered 99 aluminium oxide ceramic and its production method and use | |
| CN102030538B (en) | Production method of aluminum nitride ceramic and aluminum nitride ceramic prepared by same | |
| US5318743A (en) | Processes for producing a thermoelectric material and a thermoelectric element | |
| CN106631039A (en) | Preparation method of silicon nitride ceramic substrate | |
| CN101386539A (en) | Aluminium nitride ceramics material and preparation method thereof | |
| CN110357590A (en) | Devitrified glass and high-flexural strength low-temperature co-burning ceramic material and preparation method thereof | |
| CN110128115A (en) | A kind of method that flash burning prepares oxide eutectic ceramics | |
| CN105990511A (en) | Method of preparing homogeneous block thermoelectric material through one-step in situ reaction | |
| CN1937856A (en) | Rare earth basic-metal resistance size for metal base board based rare earth thick film circuit and its preparing process | |
| CN107396466A (en) | Electric slurry and preparation method thereof, thick film circuit chip thermal source and preparation method thereof | |
| CN111320469A (en) | Manufacturing method of NTC thermistor material | |
| CN105347781B (en) | A kind of ceramic material and preparation method thereof | |
| CN113161035A (en) | General silver paste for lead-free piezoelectric ceramic and preparation method thereof | |
| CN112225186A (en) | Preparation method of spherical boron nitride | |
| CN106906388B (en) | A kind of preparation method of silumin | |
| CN108658600B (en) | Cu2-xUltralow temperature sintering method of S thermoelectric material | |
| CN111018539A (en) | Low-temperature co-fired ceramic material of dual-phase ceramic filler and preparation method thereof | |
| CN104230344A (en) | Low-temperature sintering preparation method of AlN ceramic added with multi-element sintering aid | |
| CN103094694B (en) | A kind of Metamaterial dielectric substrate and processing method thereof | |
| CN106542828A (en) | A kind of aluminium nitride ceramics of low-temperature sintering high heat conductance and preparation method thereof | |
| CN106810078B (en) | A kind of devitrified glass series microwave dielectric material of sintered at ultra low temperature and preparation method thereof | |
| CN107263671B (en) | A kind of preparation method of the composite modified aluminium nitride chip of resistance to shrinkage type of twin crystal palpus | |
| CN113782250B (en) | High-thixotropy low-temperature co-fired ceramic inner electrode silver paste and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |