CN115677353A - Aluminum nitride-based conductive ceramic and preparation method thereof - Google Patents
Aluminum nitride-based conductive ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aluminum nitride-based conductive ceramic and a preparation method thereof. Mixing aluminum nitride powder, metal powder, sintering aid powder, an organic solvent, a binder and a dispersant by a ball mill to obtain mixed slurry; carrying out vacuum defoaming treatment and molding on the mixed slurry to obtain a first biscuit; placing the first biscuit in a glue discharging furnace for glue discharging treatment to obtain a ceramic biscuit; placing the ceramic biscuit subjected to binder removal in a high-temperature furnace, and firing at high temperature in a nitrogen atmosphere to obtain a co-crystallized aluminum nitride-based conductive ceramic material; crushing and molding the co-crystallized aluminum nitride-based conductive ceramic material to obtain a second blank; and placing the second blank in a hot-pressing vibration sintering furnace for hot-pressing sintering to obtain the compact eutectic aluminum nitride-based conductive ceramic material. The invention effectively inhibits the growth of the aluminum nitride crystal grains and the metal crystals, and enables the aluminum nitride crystal grains and the metal crystals to be mutually infiltrated and diffused effectively, so that the sintered ceramic has uniform heat conduction.
Description
The technical field is as follows:
the invention belongs to the technical field of aluminum nitride-based ceramics, and particularly relates to an aluminum nitride-based conductive ceramic and a preparation method thereof.
Background art:
aluminum Nitride Ceramic (Aluminum Nitride Ceramic) is a novel Ceramic material with excellent comprehensive performance, is an ideal material for manufacturing a new generation of semiconductor and packaging electronic devices, has excellent performance, high thermal conductivity (theoretical thermal conductivity of 320W/m.k), high electrical insulation, low dielectric constant and loss, no toxicity and thermal expansion coefficient matched with silicon, and is widely applied to the fields of semiconductor manufacturing, electronic information, power electronics and the like.
The resistivity of aluminum nitride ceramics is generally greater than 10 14 Omega cm, the resistance value of the aluminum nitride ceramic is changed by doping different metal materials in the aluminum nitride powder during preparation, different effects can be generated for different formulas, and the aluminum nitride ceramic has good electrostatic adsorption function by changing the resistivity of the aluminum nitride ceramic; the aluminum nitride ceramic is changed into a conductive ceramic by changing the resistivity of the aluminum nitride ceramic. The application field of the aluminum nitride ceramic is expanded, and the aluminum nitride ceramic is widely applied to dielectric layers on J-R electrostatic chucks in the semiconductor field, key heating elements in industrial production of ceramic heating plates in semiconductor manufacturing and the like.
In the existing preparation process of the aluminum nitride-based conductive ceramic, in the sintering process, because the migration of a crystal boundary cannot be inhibited, the growth speed of aluminum nitride crystal grains and metal crystal grains is too high, and the aluminum nitride crystal grains and the metal crystal grains cannot be effectively infiltrated and diffused, so that the aluminum nitride-based conductive ceramic obtained by sintering has the advantages of uneven heat conduction, easy cracking, short service life and large electrical loss between metal and ceramic materials.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
The invention content is as follows:
the invention aims to provide an aluminum nitride-based conductive ceramic and a preparation method thereof, so as to overcome the technical problems that the sintered aluminum nitride-based conductive ceramic has uneven heat conduction and large electrical loss between metal and ceramic materials due to the fact that aluminum nitride grains and metal grains in the prior art grow at an excessively high speed in the sintering process and cannot be fully infiltrated and diffused mutually.
In order to realize the purpose, the invention provides a preparation method of aluminum nitride-based conductive ceramic, which comprises the following steps:
s01: mixing aluminum nitride powder, metal powder, sintering aid powder, an organic solvent, a binder and a dispersant by a ball mill to obtain mixed slurry;
s02: carrying out vacuum defoaming treatment on the mixed slurry to obtain a mixture;
s03: processing the mixture through a forming process to obtain a first biscuit;
s04: placing the first biscuit in a glue discharging furnace for glue discharging treatment to discharge organic matters in the first biscuit, thereby obtaining a ceramic biscuit without residual carbon;
s05: placing the ceramic biscuit subjected to binder removal in a high-temperature furnace, and firing at high temperature in a nitrogen atmosphere to obtain a co-crystallized aluminum nitride-based conductive ceramic material;
s06: crushing the co-crystallized aluminum nitride-based conductive ceramic material to obtain ceramic powder;
s07: processing the ceramic powder through a forming process to obtain a second biscuit;
s08: and placing the second blank in a hot-pressing vibration sintering furnace for hot-pressing vibration sintering to obtain the compact eutectic aluminum nitride-based conductive ceramic material.
Preferably, in the technical scheme, 20-70 wt% of aluminum nitride powder, 1-5 wt% of metal powder, 0.2-0.7 wt% of sintering aid powder, 18-64 wt% of organic solvent, 6-32 wt% of binder and 0.15-1.6 wt% of dispersant are mixed by a ball mill to obtain mixed slurry.
Preferably, in the technical scheme, the aluminum nitride powder is carbon reduction method powder or powder generated by a direct nitridation method; the metal powder is Ti, mo, ta, W, taC, tiO 2 And TiN or a mixture of any one or more of TiN mixed in any ratio; the combustion improver is Y 2 O 3 、Al 2 O 3 、CaO、Li 2 O、YF 3 And CaF 2 Any one or a mixture of any several of them in any proportion.
Preferably, in the technical scheme, the organic solvent is butanone and/or absolute ethyl alcohol, the binder is polyvinyl butyral (PVB), and the dispersant is any one or a mixture of any several of fish oil, castor oil or triolein (GTO) in any proportion.
Preferably, in the technical scheme, the mixing time of the ball mill in the step S01 is 10-30h.
Preferably, in the technical scheme, after the mixed slurry is subjected to vacuum defoaming treatment in step S02, the mixture is subjected to granulation treatment to obtain granulated powder with the particle size of 30-80 μm.
Preferably, in the technical scheme, the granulation treatment is prepared by drying at the temperature of less than or equal to 150 ℃ or by a spray drying granulation tower.
Preferably, in the technical scheme, the forming process in the step S03 is dry pressing, a dry pressing grinding tool is designed according to the effective size of the vacuum graphite sintering furnace or the vacuum metal sintering furnace, and the prepared aluminum nitride granulation powder mixture is prepared into a biscuit with a corresponding shape and size through a dry press or a pressure forming machine.
Preferably, in the technical scheme, the product biscuit is placed in a glue discharging furnace in the step S04, and glue discharging treatment is carried out in a nitrogen atmosphere at the temperature of less than or equal to 800 ℃.
Preferably, in the technical scheme, in the step S05, sintering is carried out in a vacuum graphite sintering furnace or a metal vacuum sintering furnace under the atmosphere of argon with the vacuum degree of 10 Pa; the heating rate is 2 ℃/min when sintering is started, the temperature is kept for 120min after the temperature reaches 600 ℃, the temperature is continuously raised to 1100 ℃ at the heating rate of 1.5 ℃/min, and the temperature is kept for 30min; heating to 1450 ℃ at the heating rate of 1 ℃/min, preserving heat for 150min, cooling to 900 ℃ after heat preservation, cooling to 900 ℃ at the cooling rate of 5 ℃/min, and naturally cooling the material to room temperature along with the furnace after cooling to 900 ℃ to obtain the eutectic aluminum nitride-based conductive ceramic material.
Preferably, in the technical scheme, in the step S06, the ceramic powder with the average grain diameter of 30-90um is obtained through crushing by a roller crusher and a jaw crusher.
Preferably, in the technical scheme, the dry pressing blank is prepared by performing secondary dry pressing on a dry pressing grinding tool designed according to the final product graph in the step S07.
Preferably, in the technical scheme, the hot-pressing vibration sintering in the step S08 is performed in a nitrogen atmosphere, the vibration sintering temperature point is set to 1300 ℃, and the steps are as follows:
a) When the temperature in the furnace is less than 1300 ℃, uniformly boosting the pressure in the furnace to 30MPa, wherein the temperature rising rate in the furnace is 12 ℃/min, the boosting time and the temperature rising time are synchronous, and sintering is carried out on the second biscuit in the environment;
b) When the temperature in the furnace is =1300 ℃, starting to apply oscillation pressure of 25-35MPa on the basis of 30MPa pressure, wherein the oscillation frequency is 1Hz, and keeping the temperature for 30min;
c) Then under the same oscillation pressure, continuously heating to the target temperature at the heating rate of 3-5 ℃/min, keeping the temperature for 60-600min after the target temperature is reached, wherein the target temperature is less than or equal to 1860 ℃;
d) Unloading the oscillation pressure, keeping the constant pressure at 30MPa, cooling at the cooling rate of 5 ℃/min, unloading the constant pressure when the temperature in the furnace is cooled to 1400 ℃, cooling the material to room temperature along with the furnace, and taking out the material to obtain the compact eutectic aluminum nitride-based conductive ceramic material.
Preferably, in the technical scheme, the pressure of nitrogen in the furnace is maintained at 20KPa.
An aluminum nitride-based conductive ceramic material is prepared by the preparation method.
Compared with the prior art, the technical scheme of the application can effectively inhibit the growth of aluminum nitride grains and metal crystals by applying the oscillating pressure in the sintering process, and controls the grain sizes of the aluminum nitride grains and the metal crystals in a narrow size interval. The oscillation pressure strengthens the phenomena of plastic deformation, grain boundary slippage and the like of different material grains at high temperature, and inhibits the grain boundary migration, thereby inhibiting the over-rapid growth of the aluminum nitride-based conductive ceramic grains, and effectively infiltrating and diffusing the aluminum nitride grains and the metal crystals to obtain the compact eutectic aluminum nitride-based conductive ceramic material, and the invention has the following beneficial effects:
1. the invention provides an aluminum nitride-based conductive ceramic material, which forms a eutectic structure through high-temperature sintering, and is subjected to thermal shock sintering after secondary crushing, so that the defects and shortcomings of the traditional metal heating resistor are overcome and eliminated.
2. The invention provides different formulas of an aluminum nitride-based conductive ceramic material, and materials with different resistivities are prepared.
Description of the drawings:
FIG. 1 is a process flow diagram of a method for preparing an aluminum nitride-based conductive ceramic according to the present invention.
Fig. 2 is a metallographic structure diagram of the aluminum nitride-based conductive ceramic according to embodiment 1 of the present invention.
Fig. 3 is a metallographic structure diagram of the aluminum nitride-based conductive ceramic according to embodiment 2 of the present invention.
The specific implementation mode is as follows:
the following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Example 1
A preparation method of aluminum nitride-based conductive ceramic comprises the following steps:
s01: 50 percent of aluminum nitride powder (D50 =1.5 um) and 0.7 percent of Al 2 O 3 Ball milling the powder, 5% of TiN powder, 35% of butanone and absolute ethyl alcohol, 9% of polyvinyl butyral and 0.3% of fish oil for 5-20 hours by using a ball mill to obtain mixed slurry;
s02: carrying out vacuum defoaming treatment on the mixed slurry to obtain a mixture, and carrying out spray granulation (the average particle size is 30-80 um) on the mixture to prepare aluminum nitride mixture granulated powder;
s03: preparing the mixture of the granulation powder of the aluminum nitride-based conductive ceramic material into a biscuit with the thickness of 150x150x8mm by adopting a dry pressing grinding tool with the thickness of 150x150mm and a dry pressing machine or a pressure forming machine, wherein the pressure is 15Mpa/cm 2 ；
S04: placing the biscuit in a glue discharging furnace, and performing glue discharging treatment in a nitrogen atmosphere at the temperature of 800 ℃ to discharge organic matters in the first biscuit, thereby obtaining a ceramic biscuit without residual carbon;
s05: sintering in a vacuum graphite sintering furnace or a metal vacuum sintering furnace under the atmosphere of argon with the vacuum degree of 10 Pa; the heating rate is 2 ℃/min when sintering is started, the temperature is kept for 120min after the temperature reaches 600 ℃, the temperature is continuously raised to 1100 ℃ at the heating rate of 1.5 ℃/min, and the temperature is kept for 30min; heating to 1450 ℃ at a heating rate of 1 ℃/min, preserving heat for 150min, cooling to 900 ℃ after heat preservation, cooling to 900 ℃ at a cooling rate of 5 ℃/min, and naturally cooling the material to room temperature along with the furnace to obtain the eutectic aluminum nitride-based conductive ceramic material;
s06: crushing the co-crystallized aluminum nitride-based conductive ceramic material by a roller crusher and a jaw crusher to obtain ceramic powder with the average grain diameter of 60 mu m;
s07: preparing the ceramic powder into a biscuit of 150x150x8mm by a dry press or a pressure forming machine, wherein the pressure is 15Mpa/cm 2 Obtaining a second biscuit;
s08: placing the second element blank in a hot-pressing oscillation sintering furnace, carrying out hot-pressing oscillation sintering in a nitrogen atmosphere, setting an oscillation sintering temperature point to be 1300 ℃, uniformly boosting the pressure in the furnace to 30MPa when the temperature in the furnace is less than 1300 ℃, wherein the temperature rise rate in the furnace is 12 ℃/min, the boosting time is synchronous with the temperature rise time, and sintering the second element blank in the environment; when the temperature in the furnace is =1300 ℃, applying oscillation pressure of 35MPa on the basis of the pressure of 30MPa, wherein the oscillation frequency is 1Hz, and keeping the temperature for 30min; then under the same oscillation pressure, continuously heating to 1860 ℃ at the heating rate of 5 ℃/min, and preserving heat for 500min after reaching 1860 ℃; unloading the oscillation pressure, keeping the constant pressure at 30MPa, cooling at the cooling rate of 5 ℃/min, unloading the constant pressure when the temperature in the furnace is cooled to 1400 ℃, cooling the material to the room temperature along with the furnace, and taking out the material to obtain the compact eutectic aluminum nitride-based conductive ceramic material.
The crystal grain size of the aluminum nitride-based conductive ceramic material is 1.3-3.5 mu m, and the product density is 5.57g/cm 3 。
Aluminum nitride and titanium nitride are respectively taken, conductive ceramics are prepared by a conventional process, and a four-part sample A, B, C, D of the conductive ceramics prepared by the process is subjected to resistivity test on a high-precision direct-current low-resistance tester.
TABLE 1
| Sample numbering | Resistivity Ω · cm (room temperature) |
| A | ≥10 14 |
| B | 22×10 -6 |
| C | 6×10 4 |
| D | 4.3 |
As can be seen from Table 1, the resistivity of the aluminum nitride-based conductive ceramic prepared by the process is 4.3 omega cm at room temperature, which is far smaller than that of the conductive ceramic prepared by the conventional process, and can meet the requirements of dielectric layers on J-R electrostatic chucks in the semiconductor field, key heating elements in the industrial production of ceramic heating plates in the semiconductor manufacturing and other fields.
Example 2
A preparation method of aluminum nitride-based conductive ceramic comprises the following steps:
s01: 60 percent of aluminum nitride powder and 0.5 percent of Al 2 O 3 Ball milling the powder, 2% of Ti powder, 2% of Mo powder, 1% of Ta powder, 24% of butanone and absolute ethyl alcohol, 10% of polyvinyl butyral and 0.5% of fish oil for 10-30 hours by a ball mill to obtain a mixed powderMixing the slurry;
s02: carrying out vacuum defoaming treatment on the mixed slurry to obtain a mixture, and carrying out spray granulation (the average particle size is 30-80 um) on the mixture to prepare aluminum nitride mixture granulated powder;
s03: preparing the mixture of the granulation powder of the aluminum nitride-based conductive ceramic material into a biscuit with the thickness of 150x150x8mm by a dry pressing machine or a pressure forming machine by adopting a dry pressing grinding tool with the thickness of 150x150mm, wherein the pressure is 20Mpa/cm 2 ；
S04: placing the biscuit in a glue discharging furnace, and performing glue discharging treatment in a nitrogen atmosphere at the temperature of 800 ℃ to discharge organic matters in the first biscuit, thereby obtaining a ceramic biscuit without residual carbon;
s05: sintering in a vacuum graphite sintering furnace or a metal vacuum sintering furnace under the atmosphere of argon with the vacuum degree of 10 Pa; the heating rate is 2 ℃/min when sintering is started, the temperature is kept for 120min after the temperature reaches 600 ℃, the temperature is continuously raised to 1100 ℃ at the heating rate of 1.5 ℃/min, and the temperature is kept for 30min; heating to 1450 ℃ at a heating rate of 1 ℃/min, preserving heat for 150min, cooling to 900 ℃ after heat preservation is finished, cooling to 900 ℃ at a cooling rate of 5 ℃/min, and naturally cooling the material to room temperature along with the furnace after the temperature is reduced to 900 ℃ to obtain the eutectic aluminum nitride-based conductive ceramic material;
s06: crushing the co-crystallized aluminum nitride-based conductive ceramic material by a roller crusher and a jaw crusher to obtain ceramic powder with the average grain diameter of 60 mu m;
s07: preparing the ceramic powder into a biscuit of 150x150x8mm by a dry press or a pressure forming machine, wherein the pressure is 20Mpa/cm 2 Obtaining a second biscuit;
s08: placing the second element blank in a hot-pressing oscillation sintering furnace, carrying out hot-pressing oscillation sintering in a nitrogen atmosphere, setting an oscillation sintering temperature point to be 1300 ℃, uniformly boosting the pressure in the furnace to 30MPa when the temperature in the furnace is less than 1300 ℃, wherein the temperature rise rate in the furnace is 12 ℃/min, the boosting time is synchronous with the temperature rise time, and sintering the second element blank in the environment; when the temperature in the furnace is =1300 ℃, applying oscillation pressure of 30MPa on the basis of the pressure of 30MPa, wherein the oscillation frequency is 1Hz, and keeping the temperature for 30min; then under the same oscillation pressure, continuously heating to 1800 ℃ at the heating rate of 4 ℃/min, and preserving heat for 400min after the temperature reaches 1800 ℃; unloading the oscillation pressure, keeping the constant pressure at 30MPa, cooling at the cooling rate of 5 ℃/min, unloading the constant pressure when the temperature in the furnace is cooled to 1400 ℃, cooling the material to room temperature along with the furnace, and taking out the material to obtain the compact eutectic aluminum nitride-based conductive ceramic material.
The crystal grain size of the aluminum nitride-based conductive ceramic material is 1.1-4.5 mu m, and the product density is 5.21g/cm 3 . The electrical properties were measured, the resistance was 55.48 Ω and the resistivity was 8.3 Ω · cm.
Aluminum nitride, titanium, molybdenum and tantalum are respectively taken, conductive ceramics are prepared by a conventional process, seven samples A, B, C, D, E, F of the conductive ceramics prepared by the process are subjected to resistivity test on a high-precision direct-current low-resistance tester.
TABLE 2
| Sample numbering | Resistivity Ω cm (room temperature) |
| A | ≥10 14 |
| B | 4.2×10 -5 |
| C | 5.34×10 -6 |
| D | 1.31×10 -5 |
| E | 2.8×10 4 |
| F | 8.3 |
As can be seen from Table 2, the resistivity of the aluminum nitride-based conductive ceramic prepared by the process is 8.3 omega cm at room temperature, which is far smaller than that of the conductive ceramic prepared by the conventional process, and can meet the requirements of dielectric layers on J-R electrostatic chucks in the semiconductor field, key heating elements in the industrial production of ceramic heating plates in the semiconductor manufacturing and other fields.
The application of the oscillating pressure in the sintering process can effectively inhibit the growth of aluminum nitride grains and metal crystals and control the grain sizes of the aluminum nitride grains and the metal crystals within a narrow size interval. The main mechanism of grain growth at the later stage of sintering is grain boundary migration, the grain boundary migration mechanism needs to be inhibited to control the grain growth, the densification mechanisms such as grain boundary diffusion and lattice diffusion are enhanced, the vibration pressure enhances the phenomena of plastic deformation, grain boundary slippage and the like of grains of different materials at high temperature, and the grain boundary migration is inhibited, so that the excessive growth of the aluminum nitride-based conductive ceramic grains is inhibited, and the aluminum nitride grains and the metal crystals are effectively infiltrated and diffused.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (12)
1. A preparation method of aluminum nitride-based conductive ceramic comprises the following steps:
s01: 20 to 70 weight percent of aluminum nitride powder and 1 to 5 weight percent of goldMixing powder, 0.2-0.7 wt% of sintering aid powder, 18-64 wt% of organic solvent, 6-32 wt% of binder and 0.15-1.6 wt% of dispersant by a ball mill to obtain mixed slurry; the metal powder is Ti, mo, ta, W, taC, tiO 2 And TiN or a mixture of any one or more of TiN mixed in any ratio; the combustion improver is Y 2 O 3 、Al 2 O 3 、CaO、Li 2 O、YF 3 And CaF 2 Any one or a mixture of any several of the above in any proportion; the organic solvent is butanone and/or absolute ethyl alcohol, the adhesive is polyvinyl butyral (PVB), and the dispersant is any one or a mixture of any more of fish oil, castor oil or triolein (GTO) in any proportion;
s02: carrying out vacuum defoaming treatment on the mixed slurry to obtain a mixture;
s03: processing the mixture through a forming process to obtain a first biscuit;
s04: placing the first biscuit in a glue discharging furnace for glue discharging treatment to discharge organic matters in the first biscuit, thereby obtaining a ceramic biscuit without residual carbon;
s05: placing the ceramic biscuit subjected to binder removal in a high-temperature furnace, and firing at high temperature in a nitrogen atmosphere to obtain a co-crystallized aluminum nitride-based conductive ceramic material;
s06: crushing the co-crystallized aluminum nitride-based conductive ceramic material to obtain ceramic powder;
s07: processing the ceramic powder through a forming process to obtain a second biscuit;
s08: and placing the second blank in a hot-pressing vibration sintering furnace for hot-pressing sintering to obtain the compact eutectic aluminum nitride-based conductive ceramic material.
2. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: the aluminum nitride powder is carbon reduction powder or powder generated by direct nitridation.
3. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: the mixing time of the ball mill in the step S01 is 10-30h.
4. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: and step S02, after the mixed slurry is subjected to vacuum defoaming treatment, granulating the mixture to obtain granulated powder with the particle size of 30-80 microns.
5. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: the granulation treatment is prepared by drying at a temperature of less than or equal to 150 ℃ or by a spray drying granulation tower.
6. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: the forming process in the step S03 is dry pressing forming, a dry pressing grinding tool is designed according to the effective size of the vacuum graphite sintering furnace or the vacuum metal sintering furnace, and the prepared aluminum nitride granulation powder mixture is prepared into a biscuit with a corresponding shape and size through a dry press or a pressure forming machine.
7. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: and S04, placing the product biscuit in a glue discharging furnace, and performing glue discharging treatment in a nitrogen atmosphere at the temperature of less than or equal to 800 ℃.
8. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: sintering in a vacuum graphite sintering furnace or a metal vacuum sintering furnace under the atmosphere of argon with the vacuum degree of 10Pa in the step S05; the heating rate is 2 ℃/min when sintering is started, the temperature is kept for 120min when the temperature reaches 600 ℃, the temperature is continuously raised to 1100 ℃ at the heating rate of 1.5 ℃/min, and the temperature is kept for 30min; heating to 1450 ℃ at the heating rate of 1 ℃/min, preserving heat for 150min, cooling to 900 ℃ after heat preservation, cooling to 900 ℃ at the cooling rate of 5 ℃/min, and naturally cooling the material to room temperature along with the furnace after cooling to 900 ℃ to obtain the eutectic aluminum nitride-based conductive ceramic material.
9. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: and in the step S06, the ceramic powder with the average grain diameter of 30-90um is obtained by crushing through a roller crusher and a jaw crusher.
10. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: and in the step S07, performing secondary dry pressing forming on the dry pressing grinding tool designed according to the final product graph to prepare a dry pressing biscuit.
11. The method for producing an aluminum nitride-based conductive ceramic according to claim 1, characterized in that: step S08, carrying out hot-pressing vibration sintering in a nitrogen atmosphere, setting the vibration sintering temperature point to be 1300 ℃, and comprising the following steps:
a) When the temperature in the furnace is less than 1300 ℃, uniformly boosting the pressure in the furnace to 30MPa, wherein the temperature rising rate in the furnace is 12 ℃/min, the boosting time and the temperature rising time are synchronous, and sintering is carried out on the second biscuit in the environment;
b) When the temperature in the furnace is =1300 ℃, applying oscillation pressure of 25-35MPa on the basis of 30MPa pressure, wherein the oscillation frequency is 1Hz, and keeping the temperature for 30min;
c) Then under the same oscillation pressure, continuously heating to the target temperature at the heating rate of 3-5 ℃/min, keeping the temperature for 60-600min after the target temperature is reached, wherein the target temperature is less than or equal to 1860 ℃;
d) Unloading the oscillation pressure, keeping the constant pressure at 30MPa, cooling at the cooling rate of 5 ℃/min, unloading the constant pressure when the temperature in the furnace is cooled to 1400 ℃, cooling the material to the room temperature along with the furnace, and taking out the material to obtain the compact eutectic aluminum nitride-based conductive ceramic material.
12. An aluminum nitride-based conductive ceramic material, characterized in that: prepared by the preparation method of any one of claims 1 to 11.
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