CN115594510A - Silicon nitride heat-conducting substrate and preparation method thereof - Google Patents

Silicon nitride heat-conducting substrate and preparation method thereof Download PDF

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CN115594510A
CN115594510A CN202211451729.1A CN202211451729A CN115594510A CN 115594510 A CN115594510 A CN 115594510A CN 202211451729 A CN202211451729 A CN 202211451729A CN 115594510 A CN115594510 A CN 115594510A
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silicon nitride
heat
conducting substrate
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叶超超
赵紫娟
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Weifang University
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Abstract

The invention discloses a silicon nitride heat-conducting substrate and a preparation method thereof, relates to the technical field of semiconductor devices, aims to solve the problem of high heat-conducting property of the silicon nitride heat-conducting substrate, and realizes high strength and high heat-conducting property of silicon nitride through new raw materials and a new preparation method. The method comprises the following specific steps: mixing silicon magnesium nitride, yttrium hydride, beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to a target ratio, taking absolute ethyl alcohol as a medium, completing ball milling and mixing, drying and granulating, and preparing the silicon nitride heat-conducting substrate by two modes of tape casting air pressure and hot-pressing sintering. The silicon nitride heat-conducting substrate has the heat-conducting property of more than or equal to 80W (m.K) ‑1 Bending strength ofThe preparation method is 850MPa, has simple process, is suitable for preparation and product production of Guan Danhua silicon materials such as high-thermal conductivity silicon nitride, high-density silicon nitride, high-hardness silicon nitride and the like, and can be used for preparing electric automobile Inverters (IGBTs) and electronic packaging devices.

Description

Silicon nitride heat-conducting substrate and preparation method thereof
Technical Field
The invention relates to the technical field of semiconductor devices, in particular to a silicon nitride heat-conducting substrate and a preparation method thereof.
Background
With the rapid development of science and technology, electronic power equipment is moving towards high voltage, large current, large power and small bodyThe product is developed. However, the problem of heat dissipation of the substrate material has been a technical bottleneck that restricts the upgrade of the power equipment. Currently, aluminum nitride (AlN) has excellent thermal conductivity (200W. (m. K)) -1 ) They have already been put into practical use as substrate materials for electronic devices. However, alN has generally low mechanical properties and is easily hydrolyzed, which results in a short fatigue life of the substrate and high device cost and damage rate. Therefore, it is a major research direction to find a material with good thermal conductivity and excellent mechanical properties. Currently, silicon nitride (Si) 3 N 4 ) Is a novel high heat-conducting ceramic material which is concerned at home and abroad. From Si 3 N 4 Characterisation of the structure itself, single crystal beta-Si 3 N 4 Has good heat-conducting property under the condition of room temperature, and the theoretical thermal conductivity is as high as 200 to 450W (m.K) -1 (ii) a With Si 3 N 4 Has the characteristics of high strength, high toughness, low dielectric loss, low thermal expansion coefficient and the like. These excellent properties make Si 3 N 4 The ceramic has wide application prospect in the fields of heat conducting substrates of electric automobile Inverters (IGBT), electronic packaging devices (as shown in figure 1) and the like.
However, polycrystalline beta-Si 3 N 4 The thermal conductivity of (b) is much lower than the theoretical thermal conductivity, and the main reasons are two reasons: (1) In beta-Si 3 N 4 In the crystal grains, heat is transferred mainly by phonon vibration (lattice vibration), si 3 N 4 The oxygen impurity in the crystal boundary phase and crystal lattice in the ceramic can aggravate phonon scattering and reduce thermal conductivity (the thermal conductivity of the crystal boundary phase is very low, about 5W · (m.K)) -1 ）；（2）β-Si 3 N 4 Crystal rimcClose packed in the axial direction to result in beta-Si 3 N 4 Anisotropy of thermal conductivity of crystal: (aAndcthe theoretical thermal conductivity in the axial direction is 170W (m.K) -1 And 450W (m. K) -1 ). Therefore, how to reduce the oxygen impurity content in the grain boundary phase and the crystal lattice and control the orientation arrangement of the crystal grains to realize the improvement of the thermal conductivity becomes the key of the development and the application of the ceramic material in the direction of the heat conducting substrate.
In summary, si 3 N 4 Ceramics as a substrate material encounters a bottleneck in increasing thermal conductivity. The concrete points are as follows: (1) Due to alpha-Si 3 N 4 Excess SiO on the surface of the powder 2 The layer participates in the liquid phase sintering process, introduces excessive amorphous phase and lattice oxygen defects, thereby limiting Si 3 N 4 Ceramic heat conductivity; (2) Si 3 N 4 After sintering of the ceramic, because of beta-Si 3 N 4 The random arrangement of the crystal grains weakens the preferred orientation of the heat conduction performance and reduces the heat conductivity.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a silicon nitride heat conductive substrate and a method for preparing the same, which can reduce α -Si 3 N 4 Surface SiO 2 Layer, reducing oxygen impurity content in grain boundary phase and crystal lattice, and realizing beta-Si 3 N 4 Grain oriented growth and breakthrough of Si 3 N 4 The ceramic has more excellent performance due to technical bottleneck in the aspect of thermal conductivity, and can be used for electric automobile Inverters (IGBT) and electronic packaging devices.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of a silicon nitride heat-conducting substrate, which comprises the following steps:
mixing silicon magnesium nitride, yttrium hydride, beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Mixing the powder according to a ratio, performing ball milling, taking absolute ethyl alcohol as a ball milling medium, and performing the steps of granulation, tape casting, binder removal, sintering and post-treatment to obtain a silicon nitride heat-conducting substrate;
or silicon-magnesium nitride, yttrium hydride, beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Mixing the powder according to a ratio, carrying out ball milling, taking absolute ethyl alcohol as a ball milling medium, and carrying out granulation, hot-pressing sintering molding, sintering and post-treatment to obtain the silicon nitride heat-conducting substrate.
Further, the silicon magnesium nitride (MgSiN) 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The mass ratio of the powder is 2-6:4-8:10:80。
further, when tape casting is adopted, granulation is carried out by adopting a spray granulation mode, the granulated powder is put into slurry containing a forming binder, and the slurry is stirred, uniformly mixed and subjected to tape casting.
Furthermore, the forming binder is polyvinyl formal and polyvinyl acetal Ding Quanzhi, and the addition amount of the forming binder is 8% of the total weight of the material.
Further, when hot-pressing sintering molding is adopted, granulation is carried out by adopting a mechanical vibration or manual sieving granulation mode, and the granulated powder is placed in a hot-pressing die for hot-pressing molding.
Further, the glue discharging is vacuum glue discharging, protective atmosphere introducing or air furnace glue discharging. According to different molding modes and different binders, different glue discharging processes are selected, and vacuum glue discharging treatment, protective atmosphere glue discharging treatment or air furnace glue discharging treatment can be adopted. For example, polypropylene alcohol formal and polyvinyl butyral are selected as the binder, and need to be treated by a vacuum atmosphere furnace; the glue removing process is well known to those skilled in the art and will not be described herein.
Further, the sintering temperature is 1650-2000 ℃, and the air pressure sintering is preferred.
Further, the post-treatment is to perform mechanical processing according to different requirements of the silicon nitride heat-conducting substrate on the external dimensions. Preferably, after sintering, the silicon nitride ceramic block is cut into ceramic substrate pieces of 50-138 x 50-190 x 0.2-0.6 mm along a direction parallel to the hot pressing direction using diamond wires.
Further, the machining includes mechanical grinding, mechanical polishing, or vibratory polishing.
The silicon nitride heat-conducting substrate prepared by the preparation method comprises magnesium silicon nitride (MgSiN) 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 And (3) powder.
The silicon nitride heat-conducting substrate has the heat-conducting property of more than or equal to 80W (m.K) -1 The bending strength reaches 850MPa, and the process is simple,is suitable for preparation and product production of Guan Danhua silicon materials such as high-thermal-conductivity silicon nitride, high-density silicon nitride and high-hardness silicon nitride.
In order to realize the preparation and research of Guan Danhua silicon materials such as high-thermal-conductivity silicon nitride and high-density silicon nitride, a low-melting-point glass phase is formed by adding a non-oxide serving as a sintering aid to promote dissolution and diffusion, and finally the purpose of material densification is achieved. Firstly, in order to avoid the material performance degradation caused by the heat transfer inhibition due to the high oxygen content, the problem of sintering aid deoxidation must be solved, and the cost problem must be considered. Second, si 3 N 4 After sintering of the ceramic, because of beta-Si 3 N 4 The random arrangement of the crystal grains weakens the preferred orientation of the heat conduction performance and reduces the heat conductivity. This requires solving for beta-Si 3 N 4 The crystal grains are orderly arranged. The invention adopts new raw materials and a preparation method, and comprises the following steps: silicon magnesium nitride (MgSiN) is prepared by a new formula 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder is prepared according to the following proportion of 80 to 80 of 2-6:4-8 by mass ratio, so that the addition of the oxygen-free sintering aid is realized; secondly, the method comprises the following steps: cutting silicon nitride ceramic in the direction parallel to the hot pressing direction to realize beta-Si 3 N 4 The crystal grains are orderly arranged, and the heat conduction performance is improved.
The invention discloses the following technical effects:
(1) The invention utilizes magnesium silicon nitride (MgSiN) 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder is used as a brand new raw material, solves the problem of low heat conductivity caused by the oxygen content in the silicon nitride sintering aid, and adopts magnesium silicon nitride (MgSiN) 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Mixing the powder according to a target mass ratio, adding absolute ethyl alcohol, and combining subsequent mixing and granulating processes to obtain silicon nitride raw material powder; so that the ceramic substrate powder has obvious cost advantage and also has the advantage of low oxygen content.
(2) The invention adopts the technical proposal thatCutting the silicon nitride ceramics in the hot pressing direction to realize beta-Si 3 N 4 The crystal grains are orderly arranged, and the heat conduction performance, the toughness and the strength are high.
(3) The silicon nitride heat-conducting substrate for the electric automobile Inverter (IGBT) and the electronic packaging device has the advantages that the ceramic substrate is excellent in fatigue performance, excellent in abrasion resistance, long in service life and high in substrate use stability due to the adoption of the Mg system sintering aid.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the embodiments will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of a silicon nitride heat-conducting substrate in a new energy electric vehicle inverter;
FIG. 2 is a simulation of the microscopic grains of the thermocompression bonded silicon nitride thermal conductive substrate prepared in example 2;
FIG. 3 is a microstructure diagram of a hot-pressed sintered silicon nitride heat-conducting substrate prepared in example 2;
fig. 4 is a microstructure view of the cast air pressure sintered silicon nitride heat conducting substrate prepared in example 3.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated value or intervening value in a stated range, and any other stated or intervening value in a stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The embodiment of the invention provides a preparation method of a silicon nitride heat-conducting substrate, which comprises the following steps:
mixing silicon magnesium nitride, yttrium hydride, beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Mixing the powder according to a ratio, performing ball milling, taking absolute ethyl alcohol as a ball milling medium, and performing the steps of granulation, tape casting, binder removal, sintering and post-treatment to obtain a silicon nitride heat-conducting substrate;
or silicon-magnesium nitride, yttrium hydride, beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Mixing the powder according to a ratio, carrying out ball milling, taking absolute ethyl alcohol as a ball milling medium, and carrying out granulation, hot-pressing sintering molding, sintering and post-treatment to obtain the silicon nitride heat-conducting substrate.
In an embodiment of the present invention, magnesium silicon nitride (MgSiN) 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder mass ratio is 2-6:4-8.
In the embodiment of the invention, when the tape casting is adopted, the granulation is carried out by adopting a spray granulation mode, the granulated powder is put into slurry containing the forming binder, and the slurry is stirred, uniformly mixed and subjected to tape casting. The specific operation mode of spray granulation is the conventional operation means in the field, and is not the focus of the present invention, and is not described herein again.
In the embodiment of the invention, when the hot-pressing sintering molding is adopted, granulation is carried out by adopting a mechanical vibration or manual sieving granulation mode, and the granulated powder is placed in a hot-pressing die for hot-pressing molding. The specific operation modes of granulating by mechanical vibration or manual sieving are conventional operation means in the field, and are not the key points of the present invention, and are not described herein again.
In the embodiment of the invention, the rubber discharge is vacuum rubber discharge treatment, rubber discharge treatment by introducing protective atmosphere or rubber discharge treatment by an air furnace. According to different molding modes and different binders, different glue discharging processes are selected, and can be vacuum glue discharging treatment, glue discharging treatment by introducing protective atmosphere or air furnace glue discharging treatment, and the glue discharging processes are well known by persons skilled in the art and are not described herein. When the molding mode is hot press molding, no binder is needed; when the forming mode is tape casting, the binding agents are polypropylene alcohol formal and polyvinyl butyral, the vacuum furnace is adopted for glue discharging, and the adding amount of the binding agents is 8% of the total weight of the materials. The hot-pressing sintering molding and the tape casting molding method are conventional means in the field, are not the key point of the invention, and are not described again.
In the embodiment of the present invention, the sintering temperature is 1650-2000 ℃, and the gas pressure sintering is preferred.
Further, the post-treatment is to perform mechanical processing according to different requirements of the silicon nitride heat-conducting substrate on the external dimensions. Preferably, after sintering, the silicon nitride ceramic block is cut into ceramic substrate pieces of 50-138 x 50-190 x 0.2-0.6 mm along a direction parallel to the hot pressing direction using diamond wires.
Further, the machining includes mechanical grinding, mechanical polishing, or vibratory polishing.
The embodiment of the invention provides a silicon nitride heat-conducting substrate prepared by the preparation method, and the raw material of the silicon nitride heat-conducting substrate comprises magnesium silicon nitride (MgSiN) 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 And (3) powder.
The silicon nitride heat-conducting substrate has the heat-conducting property of more than or equal to 80W (m.K) -1 The bending strength reaches 850MPa, the process is simple, and the method is suitable for preparing Guan Danhua silicon materials such as high-thermal conductivity silicon nitride, high-density silicon nitride, high-hardness silicon nitride and the like and producing products.
The silicon nitride heat-conducting substrate is used for an electric automobile Inverter (IGBT) and an electronic packaging device.
In order to realize the preparation and research of Guan Danhua silicon materials such as high-thermal-conductivity silicon nitride and high-density silicon nitride, a low-melting-point glass phase is formed by adding a non-oxide serving as a sintering aid to promote dissolution and diffusion, and finally the purpose of material densification is achieved. Firstly, in order to avoid the material performance degradation caused by the heat transfer inhibition due to the high oxygen content, the problem of sintering aid deoxidation must be solved, and the cost problem must be considered. Second, si 3 N 4 After sintering of the ceramic, because of beta-Si 3 N 4 The random arrangement of the crystal grains weakens the preferred orientation of the heat conduction performance and reduces the heat conductivity. This requires solving for beta-Si 3 N 4 The crystal grains are orderly arranged. The invention adopts new raw materials and a preparation method, and comprises the following steps: silicon magnesium nitride (MgSiN) is prepared by a new formula 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder is prepared according to the following weight ratio of 1-30; secondly, the method comprises the following steps: cutting silicon nitride ceramics in a direction parallel to the hot pressing direction to realize beta-Si 3 N 4 The crystal grains are orderly arranged, and the heat conduction performance is improved.
Magnesium silicon nitride, yttrium hydride, beta-Si in examples and comparative examples of the present invention 3 N 4 Seed crystal and alpha-Si 3 N 4 Powder purchasingFrom Jiangsu Dongpu Fine ceramics, inc.
Example 1
A method for preparing a silicon nitride heat-conducting substrate for an electric automobile Inverter (IGBT) and an electronic packaging device by adopting hot-pressing sintering comprises the following steps:
silicon magnesium nitride (MgSiN) 2 ) Yttrium Hydride (YH) 2 ）、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to a mass ratio of 4; and then, moving the blank into a hot-pressing sintering furnace, carrying out heat preservation sintering at 1930 ℃ for 3h, carrying out diamond cutting processing on the hot-pressing sintered silicon nitride ceramic after sintering is finished, and cutting the silicon nitride ceramic block into a silicon nitride heat-conducting substrate (hot-pressing sintered silicon nitride ceramic heat-conducting substrate) with 138 × 190 × 0.32 mm by adopting a diamond line along a direction parallel to the hot-pressing direction.
The hot-pressed sintered silicon nitride ceramic heat-conducting substrate prepared in the embodiment has the following properties: thermal conductivity of 83W (m.K) -1 The bulk density is 3.24 g/cm 3 Flexural strength of 880 MPa and fracture toughness of 6.8 MPa 1/2 The Vickers hardness was 16.1 GPa.
Example 2
A method for preparing a silicon nitride heat-conducting substrate for an electric automobile Inverter (IGBT) and an electronic packaging device by adopting hot-pressing sintering comprises the following steps:
per MgSiN 2 、YH 2 And alpha-Si 3 N 4 Adding the powder into a ball milling tank according to a mass ratio of 4; performing gel removal sintering for 24 hours at 500 ℃ in a vacuum gel removal furnace; and then, moving the blank into a hot-pressing sintering furnace, carrying out heat preservation sintering at 1930 ℃ for 3h, carrying out diamond cutting processing on the hot-pressing sintered silicon nitride ceramic after sintering is finished, and cutting the silicon nitride ceramic block into 138 × 190 × 0.32 mm by adopting a diamond wire along a direction parallel to a hot-pressing direction to prepare the hot-pressing sintered silicon nitride ceramic heat-conducting substrate.
This example preparationThe simulation diagram of the microscopic crystal grains of the hot-pressing sintering silicon nitride ceramic heat-conducting substrate is shown in figure 2, and the microstructure diagram is shown in figure 3. The hot-pressed sintered silicon nitride ceramic heat-conducting substrate prepared by the embodiment has the following properties: thermal conductivity of 79W (m.K) -1 The bulk density is 3.25 g/cm 3 Flexural strength of 850MPa and fracture toughness of 7.1 MPa 1/2 The Vickers hardness was 15.6 GPa.
Example 3
Preparation of inverter (for electric automobile) by adopting tape casting air pressure sintering IGBT) and a method for manufacturing a silicon nitride heat-conducting substrate of an electronic packaging device:
per MgSiN 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to a mass ratio of 4; removing glue and sintering for 24 hours at 500 ℃ in a vacuum glue removing furnace; and putting the granulated powder into slurry of a forming binder, and stirring and uniformly mixing, wherein the forming binder is polypropylene alcohol formal and polyvinyl alcohol Ding Quanzhi (the mass ratio of the two is 1:1), and the addition amount of the forming binder is 8% of the total weight of the material. And after tape casting, drying the green body. Sintering by adopting air pressure, setting the highest sintering temperature at 1780 ℃, and preserving heat for 3 hours. After the sintering is finished, the sintering process is carried out, and (3) processing the silicon nitride ceramic by a grinding machine to prepare the casting air pressure sintered silicon nitride ceramic heat-conducting substrate.
The microstructure of the cast gas pressure sintered silicon nitride ceramic heat conducting substrate prepared in this example is shown in fig. 4. The performance of the tape casting air pressure sintering silicon nitride ceramic heat conducting substrate prepared by the embodiment is as follows: thermal conductivity of 75W (m.K) -1 The bulk density is 3.20 g/cm 3 The breaking strength is 720MPa, and the fracture toughness is 6.3 MPa 1/2 The Vickers hardness was 15.1 GPa.
Example 4
A method for preparing a silicon nitride heat-conducting substrate for an electric automobile Inverter (IGBT) and an electronic packaging device by adopting hot-pressing sintering comprises the following steps:
per MgSiN 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to the mass ratio of 3; and then, moving the blank into a hot-pressing sintering furnace, carrying out heat preservation sintering at 1930 ℃ for 3h, carrying out diamond cutting processing on the hot-pressing sintered silicon nitride ceramic after sintering is finished, and cutting the silicon nitride ceramic block into 138 × 190 × 0.32 mm silicon nitride heat-conducting substrates (hot-pressing sintered silicon nitride ceramic heat-conducting substrates) by adopting diamond wires along the direction parallel to the hot-pressing direction.
The hot-pressed sintered silicon nitride ceramic heat-conducting substrate prepared by the embodiment has the following properties: thermal conductivity of 72W (m.K) -1 The bulk density is 3.22 g/cm 3 The breaking strength is 852 MPa, and the fracture toughness is 6.5 MPa 1/2 The Vickers hardness was 15.8 GPa.
Example 5
A method for preparing a silicon nitride heat-conducting substrate for an electric automobile Inverter (IGBT) and an electronic packaging device by adopting hot-pressing sintering comprises the following steps:
per MgSiN 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to the mass ratio of 2; and then, moving the blank into a hot-pressing sintering furnace, carrying out heat preservation sintering at 1930 ℃ for 3h, carrying out diamond cutting processing on the hot-pressing sintered silicon nitride ceramic after sintering is finished, and cutting the silicon nitride ceramic block into 138 × 190 × 0.32 mm silicon nitride heat-conducting substrates (hot-pressing sintered silicon nitride ceramic heat-conducting substrates) by adopting diamond wires along the direction parallel to the hot-pressing direction.
The hot-pressed sintered silicon nitride ceramic heat-conducting substrate prepared by the embodiment has the following properties: thermal conductivity of 67W (m. K) -1 The bulk density is 3.20 g/cm 3 Flexural strength of 827 MPa and fracture toughness of 6.3 MPa 1/2 The Vickers hardness was 15.4 GPa.
Example 6
A method for preparing a silicon nitride heat-conducting substrate for an electric automobile Inverter (IGBT) and an electronic packaging device by adopting hot-pressing sintering comprises the following steps:
as MgSiN 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to a mass ratio of 6; and then, moving the blank into a hot-pressing sintering furnace, carrying out heat preservation sintering at 1930 ℃ for 3h, carrying out diamond cutting processing on the hot-pressing sintered silicon nitride ceramic after sintering is finished, and cutting the silicon nitride ceramic block into 138 × 190 × 0.32 mm silicon nitride heat-conducting substrates (hot-pressing sintered silicon nitride ceramic heat-conducting substrates) by adopting diamond wires along the direction parallel to the hot-pressing direction.
The hot-pressed sintered silicon nitride ceramic heat-conducting substrate prepared by the embodiment has the following properties: thermal conductivity of 70W (m.K) -1 The bulk density is 3.24 g/cm 3 Flexural strength of 861 MPa and fracture toughness of 7.0 MPa 1/2 The Vickers hardness was 15.8 GPa.
Example 7
A method for preparing a silicon nitride heat-conducting substrate for an electric automobile Inverter (IGBT) and an electronic packaging device by adopting tape casting air pressure sintering comprises the following steps:
as MgSiN 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to the mass ratio of 3; removing glue and sintering for 24 hours at 500 ℃ in a vacuum glue removing furnace; and putting the granulated powder into the slurry of a forming binder, and stirring and uniformly mixing, wherein the mass ratio of the polyvinyl formal to the polyvinyl acetal Ding Quanzhi (the mass ratio of the polyvinyl formal to the polyvinyl acetal is 1:1), and the addition amount of the polyvinyl formal to the polyvinyl acetal is 8% of the total weight of the material. And after tape casting, drying the green body. And (3) adopting air pressure sintering, setting the highest sintering temperature at 1780 ℃, and keeping the sintering time at 3h. And after sintering, processing the silicon nitride ceramic by using a grinding machine to prepare the casting air pressure sintering silicon nitride ceramic heat-conducting substrate.
The properties of the tape casting air pressure sintering silicon nitride ceramic heat conducting substrate prepared by the embodiment are as follows: thermal conductivityIs 70W (m.K) -1 The bulk density is 3.19 g/cm 3 Breaking strength of 695 MPa, fracture toughness of 5.9 MPa 1/2 The Vickers hardness was 15.1 GPa.
Example 8
A method for preparing a silicon nitride heat-conducting substrate for an electric automobile Inverter (IGBT) and an electronic packaging device by adopting hot-pressing sintering comprises the following steps:
per MgSiN 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Adding the powder into a ball milling tank according to a mass ratio of 4; and then, moving the blank into a hot-pressing sintering furnace, carrying out heat preservation sintering at 1930 ℃ for 3h, carrying out diamond cutting processing on the hot-pressing sintered silicon nitride ceramic after sintering is finished, and cutting the silicon nitride ceramic block into 138 × 190 × 0.32 mm silicon nitride heat-conducting substrates (hot-pressing sintered silicon nitride ceramic heat-conducting substrates) by adopting diamond wires along the direction perpendicular to the hot-pressing direction.
The hot-pressed sintered silicon nitride ceramic heat-conducting substrate prepared by the embodiment has the following properties: thermal conductivity of 45W (m.K) -1 The bulk density is 3.24 g/cm 3 The breaking strength is 740 MPa, and the fracture toughness is 7.1 MPa 1/2 The Vickers hardness was 15.3 GPa.
Comparative example 1
The same as example 1, except that the silicon nitride heat-conducting substrate is made of MgSiN 2 And YH 2 And alpha-Si 3 N 4 Powder of not added with beta-Si 3 N 4 And (4) seed crystals.
The silicon nitride ceramic heat-conducting substrate prepared by the comparative example has the following properties: the thermal conductivity is 79W (m.K) -1 The bulk density is 3.24 g/cm 3 Flexural strength of 880 MPa and fracture toughness of 6.8 MPa 1/2 The Vickers hardness was 16.1 GPa. The reason for the lower thermal conductivity than in example 1 is β -Si 3 N 4 The seed crystal can improve the transmission channel of the lattice vibration.
Comparative example 2
The difference from example 1 is only that the preparation method of the silicon nitride heat-conducting substrate is a casting method.
The silicon nitride ceramic heat-conducting substrate prepared by the comparative example has the following properties: thermal conductivity of 75W (m.K) -1 The bulk density is 3.20 g/cm 3 The breaking strength is 720MPa, and the fracture toughness is 6.3 MPa 1/2 The Vickers hardness was 15.1 GPa. The reason why the thermal conductivity is lower than that of example 1 is that the density of the tape casting method is lower than that of the hot press sintering, resulting in lower thermal conductivity.
Comparative example 3
The difference from example 1 is only that MgSiN is used as a raw material for preparing a silicon nitride heat-conducting substrate 2 And YH 2 The mixture ratio is different, specifically, mgSiN is used as the material in example 1 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder mass ratio is 4 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 And (3) adding the powder into a ball milling tank according to the mass ratio of 3.
The silicon nitride ceramic heat-conducting substrate prepared by the comparative example has the following properties: thermal conductivity of 72W (m.K) -1 The bulk density is 3.22 g/cm 3 The breaking strength is 852 MPa, and the fracture toughness is 6.5 MPa 1/2 The Vickers hardness was 15.8 GPa. The reason why the thermal conductivity was lower than that of example 1 is magnesium silicon nitride (MgSiN) 2 ) And Yttrium Hydride (YH) 2 ) The proportion change causes the grain boundary phase proportion and the density change, and the thermal conductivity is lower.
Comparative example 4
The difference from example 1 is only that MgSiN is used as a raw material for preparing a silicon nitride heat-conducting substrate 2 And YH 2 The mixture ratio is different, specifically, the MgSiN is adopted according to example 1 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder mass ratio is 4 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 And (3) adding the powder into a ball milling tank according to the mass ratio of 2.
Nitridation prepared by this comparative exampleThe silicon ceramic heat-conducting substrate has the following properties: thermal conductivity of 67W (m.K) -1 The bulk density is 3.20 g/cm 3 Flexural strength of 827 MPa and fracture toughness of 6.3 MPa 1/2 The Vickers hardness was 15.4 GPa. The reason why the thermal conductivity was lower than that of example 1 is MgSiN 2 And YH 2 The proportion change causes the grain boundary phase proportion and the density change, and the thermal conductivity is lower.
Comparative example 5
The difference from example 1 is only that MgSiN is used as a raw material for preparing a silicon nitride heat-conducting substrate 2 And YH 2 In particular, example 1 according to MgSiN 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder mass ratio is 4 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 And (3) adding the powder into a ball milling tank according to the mass ratio of 6.
The silicon nitride ceramic heat conducting substrate prepared by the comparative example has the following properties: has thermal conductivity of 70W (m.K) -1 The bulk density is 3.24 g/cm 3 Flexural strength of 861 MPa and fracture toughness of 7.0 MPa 1/2 The Vickers hardness was 15.8 GPa. The reason why the thermal conductivity was lower than that of example 1 is MgSiN 2 And YH 2 The proportion change causes the grain boundary phase proportion and the density change, and the thermal conductivity is lower.
Comparative example 6
The same as example 1, except that the preparation method of the silicon nitride heat-conducting substrate is a casting method and MgSiN 2 And yttrium hydride YH 2 The mixture ratio is different, specifically, the sintering is completed by hot-pressing sintering in the embodiment 1, the powder is firstly granulated by spraying, and then the densification is completed by tape casting and air pressure sintering in the comparative example, the MgSiN is adopted as the material in the embodiment 1 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder mass ratio is 4 2 、YH 2 、β-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 And (2) adding the powder into a ball milling tank according to the mass ratio of 3.
The silicon nitride ceramic heat-conducting substrate prepared by the comparative example has the following properties: thermal conductivity of 75W (m.K) -1 The bulk density is 3.22 g/cm 3 Flexural strength of 750 MPa and fracture toughness of 6.3 MPa 1/2 The Vickers hardness was 15.1 GPa. The reason that the thermal conductivity is lower than that of the embodiment 1 is that the density of the tape casting method is lower than that of hot-pressing sintering, so that the thermal conductivity is lower; second, mgSiN 2 And YH 2 The proportion change causes the grain boundary phase proportion and the density change, which results in lower thermal conductivity.
Comparative example 7
The difference from example 1 is that in example 8, a silicon nitride ceramic block was cut in a direction perpendicular to the hot pressing direction.
The silicon nitride ceramic heat-conducting substrate prepared by the comparative example has the following properties: thermal conductivity of 45W (m.K) -1 The bulk density is 3.24 g/cm 3 The breaking strength is 740 MPa, and the fracture toughness is 7.1 MPa 1/2 The Vickers hardness was 15.3 GPa. The reason for the lower thermal conductivity than in example 1 is β -Si 3 N 4 The grains have anisotropy, resulting in a thermal conductivity parallel to the hot pressing direction that is significantly higher than the thermal conductivity perpendicular to the hot pressing direction.
The above-described embodiments are only intended to illustrate the preferred embodiments of the present invention, and not to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims (9)

1. A preparation method of a silicon nitride heat conduction substrate is characterized by comprising the following steps:
mixing silicon magnesium nitride, yttrium hydride, beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Mixing powder, ball-milling, taking absolute ethyl alcohol as a ball-milling medium, and performing the steps of granulation, tape casting, binder removal, sintering and post-treatment to obtain a silicon nitride heat-conducting substrate;
or silicon-magnesium nitride, yttrium hydride, beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 Mixing the powder according to a ratio, carrying out ball milling, taking absolute ethyl alcohol as a ball milling medium, and carrying out granulation, hot-pressing sintering molding, sintering and post-treatment to obtain the silicon nitride heat-conducting substrate.
2. The method according to claim 1, wherein the silicon-magnesium nitride, yttrium hydride, β -Si 3 N 4 Seed crystal and alpha-Si 3 N 4 The powder mass ratio is 2-6:4-8.
3. The preparation method according to claim 1, wherein when the tape casting is adopted, the granulation is carried out by spray granulation, the granulated powder is put into slurry containing the forming binder, and the slurry is stirred, mixed and cast.
4. The preparation method of claim 3, wherein the forming binder is polypropylene acetal and polyvinyl acetal Ding Quanzhi, and the addition amount is 8% of the total weight of the material.
5. The method according to claim 1, wherein when the hot-press sintering is adopted, the granulation is carried out by mechanical vibration or manual sieving granulation, and the granulated powder is placed in a hot-press mold and hot-press molded.
6. The preparation method according to claim 1, wherein the glue discharging is vacuum glue discharging, protective atmosphere introducing or air furnace glue discharging.
7. The method of claim 1, wherein the sintering temperature is 1650-2000 ℃.
8. The preparation method according to claim 1, wherein the post-treatment is machining according to different requirements of the silicon nitride heat-conducting substrate on the external dimensions.
9. NitrogenA silicon nitride heat-conducting substrate prepared by the method according to any one of claims 1 to 8, wherein the raw materials include magnesium silicon nitride, yttrium hydride, and beta-Si 3 N 4 Seed crystal and alpha-Si 3 N 4 And (3) powder.
CN202211451729.1A 2022-11-21 2022-11-21 Silicon nitride heat-conducting substrate and preparation method thereof Pending CN115594510A (en)

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