CN110963800A - Aluminum nitride ceramic substrate and preparation method thereof - Google Patents
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Abstract
The invention relates to an aluminum nitride ceramic substrate and a preparation method thereof. The preparation method of the aluminum nitride ceramic substrate comprises the following steps: (1) uniformly mixing kaolin and dolomite, and calcining in an air atmosphere to obtain mixed powder A; (2) uniformly mixing aluminum nitride powder, fluorite and cerium oxide powder with the mixed powder A obtained in the step (1) to obtain mixed powder B, and carrying out ball milling; (3) uniformly mixing ferric nitrate powder, ammonium chloride powder and the mixed powder B after ball milling to obtain mixed powder C; (4) uniformly mixing polyvinyl alcohol with the mixed powder C to obtain mixed powder D; (5) and (4) pressing and forming the mixed powder D obtained in the step (4), and then sintering in vacuum to obtain the aluminum nitride ceramic substrate. The method has the advantages of wide raw material sources and simple and controllable process, and the obtained aluminum nitride ceramic substrate has the excellent performances of high density, high thermal conductivity, high insulativity, low dielectric constant, no toxicity, good processability, high temperature corrosion resistance and the like.
Description
Technical Field
The invention relates to a ceramic substrate and a preparation method thereof, in particular to an aluminum nitride ceramic substrate and a preparation method thereof.
Background
The information technology taking the semiconductor technology as the core technology brings great changes to the daily life of human beings, and the development of the 5G communication technology brings higher requirements on electronic component packaging materials and technologies.
The aluminum nitride ceramic substrate is the most ideal high-thermal-conductivity ceramic substrate in the field of 5G communication due to high thermal conductivity, no toxicity, excellent insulating property, wide raw material sources, good manufacturability and high-temperature corrosion resistance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the aluminum nitride ceramic substrate with the advantages of high density, high thermal conductivity, high insulativity, high-temperature corrosion resistance, no toxicity, excellent processability and the like and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for preparing an aluminum nitride ceramic substrate, comprising the steps of:
(1) uniformly mixing kaolin and dolomite, and calcining in an air atmosphere to obtain mixed powder A;
(2) uniformly mixing aluminum nitride powder, fluorite and cerium oxide powder with the mixed powder A obtained in the step (1) to obtain mixed powder B, and carrying out ball milling;
(3) uniformly mixing ferric nitrate powder, ammonium chloride powder and the mixed powder B after ball milling to obtain mixed powder C;
(4) uniformly mixing polyvinyl alcohol with the mixed powder C to obtain mixed powder D;
(5) and (4) pressing and forming the mixed powder D obtained in the step (4), and then sintering in vacuum to obtain the aluminum nitride ceramic substrate.
The invention starts from the requirements of the current 5G communication development and the large-scale integrated circuit development on the ceramic substrate with high thermal conductivity, high insulation, low dielectric constant and corrosion resistance, and prepares the aluminum nitride ceramic substrate with high density, high thermal conductivity, high insulation, high temperature corrosion resistance, no toxicity and excellent processing performance by selecting aluminum nitride powder, adding proper cosolvent and selecting a static pressure sintering combined method, thereby meeting the industrial requirements of 5G communication, large-scale integrated circuits and the like.
The preparation method has the advantages of wide raw material source, non-toxic raw materials and stable performance.
In a preferred embodiment of the method for producing an aluminum nitride ceramic substrate according to the present invention, the method for producing an aluminum nitride ceramic substrate comprises the following production raw materials in parts by weight: 8-12 parts of kaolin, 2-4 parts of dolomite, 78-82 parts of aluminum nitride powder, 0.5-1 part of fluorite, 0.5-1 part of cerium oxide powder, 0.8-1.2 parts of ferric nitrate powder, 0.8-1.2 parts of ammonium chloride powder and 4-6 parts of polyvinyl alcohol.
In a preferred embodiment of the method for producing an aluminum nitride ceramic substrate according to the present invention, the method for producing an aluminum nitride ceramic substrate comprises the following production raw materials in parts by weight: 10 parts of kaolin, 2 parts of dolomite, 80 parts of aluminum nitride powder, 0.5 part of fluorite, 0.5 part of cerium oxide powder, 1 part of ferric nitrate powder, 1 part of ammonium chloride powder and 5 parts of polyvinyl alcohol.
As a preferred embodiment of the method for producing an aluminum nitride ceramic substrate according to the present invention, in the step (1), the conditions for calcination in an air atmosphere are: raising the temperature from room temperature to 850-950 ℃ in air atmosphere, wherein the temperature raising rate is 8-12 ℃/min, keeping the temperature for 40-80min, raising the temperature to 1000-1200 ℃ at the temperature raising rate of 4-6 ℃/min, and keeping the temperature for 140 min.
As a preferred embodiment of the method for producing an aluminum nitride ceramic substrate according to the present invention, in the step (1), the conditions for calcination in an air atmosphere are: heating from room temperature to 900 ℃ in air atmosphere at a heating rate of 10 ℃/min, keeping the temperature for 60min, heating to 1100 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 120 min.
As a preferred embodiment of the method for preparing the aluminum nitride ceramic substrate according to the present invention, in the step (2), a planetary ball mill is used for ball milling.
In a preferred embodiment of the method for producing an aluminum nitride ceramic substrate according to the present invention, in the step (5), the pressure for press molding is 100MPa and the time is 2 min.
As a preferred embodiment of the method for producing an aluminum nitride ceramic substrate according to the present invention, in the step (5), the conditions for sintering in vacuum are as follows: in vacuum, the temperature is raised to 650 ℃ at the temperature raising rate of 4-6 ℃/min, the temperature is maintained for 50-70min, then the temperature is raised to 1700 ℃ at the temperature raising rate of 8-12 ℃/min, and the temperature is maintained for 260 min.
As a preferred embodiment of the method for producing an aluminum nitride ceramic substrate according to the present invention, in the step (5), the conditions for sintering in vacuum are as follows: in vacuum, heating to 600 deg.C at a rate of 5 deg.C/min, maintaining for 60min, heating to 1600 deg.C at a rate of 10 deg.C/min, and maintaining for 240 min.
In addition, the invention also provides the aluminum nitride ceramic substrate prepared by the method. The aluminum nitride ceramic substrate has the advantages of high density, high thermal conductivity, high insulativity, high temperature corrosion resistance, no toxicity, excellent processability and the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation raw materials are wide in source, and the preparation process is simple and controllable;
(2) the aluminum nitride ceramic substrate prepared by the invention has the excellent performances of high density, high thermal conductivity, high insulativity, low dielectric constant, no toxicity, good processability, high temperature corrosion resistance and the like.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
In an embodiment of the aluminum nitride ceramic substrate and the method for preparing the same of the present invention, the method for preparing the aluminum nitride ceramic substrate includes:
(1) uniformly mixing 10 parts of kaolin and 2 parts of dolomite, pouring the mixture into a corundum crucible, then placing the crucible into a muffle furnace, heating the crucible to 900 ℃ from room temperature in air atmosphere, wherein the heating rate is 10 ℃/min, keeping the temperature for 60min, heating the crucible to 1100 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 120min, and then cooling the crucible along with the furnace to obtain mixed powder A;
(2) weighing 80 parts of aluminum nitride powder, 0.5 part of fluorite and 0.5 part of cerium oxide powder, pouring into the mixed powder A, uniformly mixing to obtain mixed powder B, placing the mixed powder B into a corundum cylinder body of a ball mill, ball-milling for 60min by using a planetary ball mill, weighing 1 part of ferric nitrate powder, pouring 1 part of ammonium chloride powder into the powder, and uniformly stirring by using a glass rod to obtain mixed powder C;
(3) weighing 5 parts of polyvinyl alcohol, pouring the mixed powder C and uniformly mixing to obtain powder D;
(4) placing the mixed powder D in a dry pressing grinding tool, and performing unidirectional pressure forming, keeping the pressure at 100MPa, and keeping the pressure for 2min to obtain a forming block;
(5) placing the molding block in a vacuum sintering furnace, heating to 600 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 60min, heating to 1600 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 240min, then turning off a power supply, keeping the vacuum condition for annealing treatment, and obtaining the high-performance aluminum nitride ceramic substrate after reaching the room temperature;
(6) and (4) after the vacuum furnace is cooled to room temperature, taking out the aluminum nitride ceramic substrate, and packaging according to requirements.
Example 2
In an embodiment of the aluminum nitride ceramic substrate and the method for preparing the same of the present invention, the method for preparing the aluminum nitride ceramic substrate includes:
(1) uniformly mixing 8 parts of kaolin and 4 parts of dolomite, pouring the mixture into a corundum crucible, then placing the crucible into a muffle furnace, heating the crucible to 850 ℃ from room temperature in air atmosphere, wherein the heating rate is 8 ℃/min, keeping the temperature for 80min, heating the crucible to 1000 ℃ at the heating rate of 4 ℃/min, keeping the temperature for 140min, and then cooling the crucible along with the furnace to obtain mixed powder A;
(2) weighing 78 parts of aluminum nitride powder, 1 part of fluorite and 1 part of cerium oxide powder, pouring into the mixed powder A, uniformly mixing to obtain mixed powder B, placing the mixed powder B into a corundum cylinder body of a ball mill, carrying out ball milling for 60min by using a planetary ball mill, weighing 0.8 part of ferric nitrate powder and 1.2 parts of ammonium chloride powder, pouring into the powder, and uniformly stirring by using a glass rod to obtain mixed powder C;
(3) weighing 6 parts of polyvinyl alcohol, pouring the mixed powder C and uniformly mixing to obtain powder D;
(4) placing the mixed powder D in a dry pressing grinding tool, and performing unidirectional pressure forming, keeping the pressure at 100MPa, and keeping the pressure for 2min to obtain a forming block;
(5) placing the molding block in a vacuum sintering furnace, heating to 550 ℃ at the heating rate of 4 ℃/min, keeping the temperature for 70min, heating to 1700 ℃ at the heating rate of 12 ℃/min, keeping the temperature for 220min, then turning off a power supply, keeping the vacuum condition for annealing treatment, and obtaining the high-performance aluminum nitride ceramic substrate after reaching the room temperature;
(6) and (4) after the vacuum furnace is cooled to room temperature, taking out the aluminum nitride ceramic substrate, and packaging according to requirements.
Example 3
In an embodiment of the aluminum nitride ceramic substrate and the method for preparing the same of the present invention, the method for preparing the aluminum nitride ceramic substrate includes:
(1) uniformly mixing 12 parts of kaolin and 3 parts of dolomite, pouring the mixture into a corundum crucible, then placing the crucible into a muffle furnace, heating the crucible to 950 ℃ from room temperature in air atmosphere at a heating rate of 12 ℃/min, preserving heat for 40min, heating the crucible to 1200 ℃ at a heating rate of 6 ℃/min, keeping the temperature for 100min, and then cooling the crucible along with the furnace to obtain mixed powder A;
(2) weighing 82 parts of aluminum nitride powder, 0.8 part of fluorite and 0.8 part of cerium oxide powder, pouring into the mixed powder A, uniformly mixing to obtain mixed powder B, placing the mixed powder B into a corundum cylinder body of a ball mill, ball-milling for 60min by using a planetary ball mill, weighing 1.2 parts of ferric nitrate powder and 0.8 part of ammonium chloride powder, pouring into the powder, and uniformly stirring by using a glass rod to obtain mixed powder C;
(3) weighing 4 parts of polyvinyl alcohol, pouring the mixed powder C and uniformly mixing to obtain powder D;
(4) placing the mixed powder D in a dry pressing grinding tool, and performing unidirectional pressure forming, keeping the pressure at 100MPa, and keeping the pressure for 2min to obtain a forming block;
(5) placing the molding block in a vacuum sintering furnace, heating to 650 ℃ at the heating rate of 6 ℃/min, keeping the temperature for 50min, heating to 1500 ℃ at the heating rate of 8 ℃/min, keeping the temperature for 260min, then turning off a power supply, keeping the vacuum condition for annealing treatment, and obtaining the high-performance aluminum nitride ceramic substrate after reaching the room temperature;
(6) and (4) after the vacuum furnace is cooled to room temperature, taking out the aluminum nitride ceramic substrate, and packaging according to requirements.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of an aluminum nitride ceramic substrate is characterized by comprising the following steps:
(1) uniformly mixing kaolin and dolomite, and calcining in an air atmosphere to obtain mixed powder A;
(2) uniformly mixing aluminum nitride powder, fluorite and cerium oxide powder with the mixed powder A obtained in the step (1) to obtain mixed powder B, and carrying out ball milling;
(3) uniformly mixing ferric nitrate powder, ammonium chloride powder and the mixed powder B after ball milling to obtain mixed powder C;
(4) uniformly mixing polyvinyl alcohol with the mixed powder C to obtain mixed powder D;
(5) and (4) pressing and forming the mixed powder D obtained in the step (4), and then sintering in vacuum to obtain the aluminum nitride ceramic substrate.
2. The method for preparing an aluminum nitride ceramic substrate according to claim 1, wherein the method for preparing an aluminum nitride ceramic substrate comprises the following raw materials in parts by weight: 8-12 parts of kaolin, 2-4 parts of dolomite, 78-82 parts of aluminum nitride powder, 0.5-1 part of fluorite, 0.5-1 part of cerium oxide powder, 0.8-1.2 parts of ferric nitrate powder, 0.8-1.2 parts of ammonium chloride powder and 4-6 parts of polyvinyl alcohol.
3. The method for preparing an aluminum nitride ceramic substrate according to claim 2, wherein the method for preparing an aluminum nitride ceramic substrate comprises the following raw materials in parts by weight: 10 parts of kaolin, 2 parts of dolomite, 80 parts of aluminum nitride powder, 0.5 part of fluorite, 0.5 part of cerium oxide powder, 1 part of ferric nitrate powder, 1 part of ammonium chloride powder and 5 parts of polyvinyl alcohol.
4. The method for producing an aluminum nitride ceramic substrate according to claim 1, wherein in the step (1), the conditions for the calcination in the air atmosphere are: raising the temperature from room temperature to 850-950 ℃ in air atmosphere, wherein the temperature raising rate is 8-12 ℃/min, keeping the temperature for 40-80min, raising the temperature to 1000-1200 ℃ at the temperature raising rate of 4-6 ℃/min, and keeping the temperature for 140 min.
5. The method for producing an aluminum nitride ceramic substrate according to claim 4, wherein in the step (1), the conditions for the calcination in the air atmosphere are: heating from room temperature to 900 ℃ in air atmosphere at a heating rate of 10 ℃/min, keeping the temperature for 60min, heating to 1100 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 120 min.
6. The method of preparing an aluminum nitride ceramic substrate according to claim 1, wherein in the step (2), the ball milling is performed using a planetary ball mill.
7. The method of producing an aluminum nitride ceramic substrate according to claim 1, wherein the pressure for press molding in the step (5) is 100MPa for 2 min.
8. The method for preparing an aluminum nitride ceramic substrate according to claim 1, wherein in the step (5), the sintering conditions in vacuum are as follows: in vacuum, the temperature is raised to 650 ℃ at the temperature raising rate of 4-6 ℃/min, the temperature is maintained for 50-70min, then the temperature is raised to 1700 ℃ at the temperature raising rate of 8-12 ℃/min, and the temperature is maintained for 260 min.
9. The method for producing an aluminum nitride ceramic substrate according to claim 8, wherein in the step (5), the sintering conditions in vacuum are: in vacuum, heating to 600 deg.C at a rate of 5 deg.C/min, maintaining for 60min, heating to 1600 deg.C at a rate of 10 deg.C/min, and maintaining for 240 min.
10. An aluminium nitride ceramic substrate produced by the method of any one of claims 1 to 9.
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