CN114477111B - Equiaxed beta-Si 3 N 4 Powder and preparation process thereof - Google Patents
Equiaxed beta-Si 3 N 4 Powder and preparation process thereof Download PDFInfo
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- CN114477111B CN114477111B CN202011168279.6A CN202011168279A CN114477111B CN 114477111 B CN114477111 B CN 114477111B CN 202011168279 A CN202011168279 A CN 202011168279A CN 114477111 B CN114477111 B CN 114477111B
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention adopts combustion synthesis method to prepare single-phase and high-purity equiaxed beta-Si 3 N 4 Powder body, silicon powder and diluent beta-Si 3 N 4 The grain diameter and the silicon powder content of the silicon powder are controlled by adding the additive CaO to obtain equiaxed beta-Si 3 N 4 The powder has an aspect ratio of 1-4, a length of 1-10 μm and a diameter of 1-3 μm, and no free Si. The method has the advantages of short reaction period, simple process, low cost, capability of meeting the requirement of industrial mass production, high quality and use as the heat conducting filler.
Description
Technical Field
The invention relates to a preparation process of silicon nitride ceramics, in particular to an equiaxed beta-Si 3 N 4 The preparation process of the powder.
Background
In recent years, electronic devices are continuously developed towards integration, miniaturization and high frequency, and the problem of heat dissipation of chips has become a bottleneck problem for further development of electronic devices. The improvement of the thermal conductivity of the thermal interface material is particularly important for improving the heat dissipation capacity of the whole chip, and the selection of the heat conducting filler with excellent performance is more important for obtaining the thermal interface material with high thermal conductivity. The silicon nitride material has the characteristics of high strength, high temperature resistance, oxidation resistance, corrosion resistance, strong chemical stability, large heat conduction coefficient and low thermal expansion coefficient, in particular to beta-Si 3 N 4 The intrinsic heat conductivity of the material can reach 320W/mK, and the material can be widely used as a heat conducting filler in electronic packaging materials. However, beta-Si 3 N 4 Is hexagonal, usually in the form of anisotropic rod-like crystals, and beta-Si with high aspect ratio 3 N 4 The wettability between the particles and the polymer is poor, and the interface thermal resistance is large, so that the thermal conductivity of the thermal interface material cannot meet the commercial requirement. The spherical particles have good fluidity in the matrix, and can effectively reduce interface thermal resistance while improving the filling quantity, so that the equiaxed beta-Si 3 N 4 The acquisition of the particles is critical to the synthesis of highly thermally conductive composites.
Currently equiaxed beta-Si 3 N 4 The preparation process of the powder comprises the following steps:
(1) By direct nitriding, e.g. as mentioned in CN110357050A in Si, beta-Si 3 N 4 、CaF 2 The powder is taken as raw material, evenly mixed by a mixer and then mixed in NH 3 Direct nitridation under atmosphere to equiaxed beta-Si 3 N 4 The powder, although the method is simple in operation and the reaction process is not complex, the reaction process is long in time and the CaF is practical 2 The additive is corrosive.
(2) Carbothermal reduction, e.g. Sun et al at university of Qinghai, siO 2 Carbon black and CaO are used as raw materials, and the raw materials are N 2 Synthesis of equiaxed beta-Si by carbothermal reduction in an atmosphere 3 N 4 Although the reaction raw materials are simple and easy to obtain, the method synthesizes equiaxed beta-Si 3 N 4 CO toxic gas is generated in the process of (2), and the method is harmful to the environment.
Disclosure of Invention
The invention aims to solve the technical problems and provide an equiaxed beta-Si 3 N 4 Powder and preparation process thereof, and preparation of high-purity, low-defect and completely nitrided beta-Si 3 N 4 The powder can be applied to the heat conduction filler of the packaging material.
The technical scheme provided by the invention is as follows:
equiaxed beta-Si 3 N 4 The powder is characterized in that the equiaxed beta-Si 3 N 4 The powder is prepared by a combustion synthesis method and comprises the following raw materials in parts by weight: 36-48.75wt% of silicon powder and diluent beta-Si 3 N 4 41.25-61.5wt% and additive CaO2.5-10 wt%, wherein Si: beta-Si 3 N 4 The ratio of silicon powder to silicon powder is 1:1-2:3, and the grain diameter of the silicon powder is 2-5 mu m; the equiaxed beta-Si 3 N 4 The aspect ratio of the powder is 1-4, the length is 1-10 mu m, the diameter is 1-3 mu m, and free Si is not generated.
Further, the content of the silicon powder is 36%,38%,39% and 45% of the total amount of the powder mixture required for synthesis.
Further, the method comprises the steps of,preferably diluent axis beta-Si 3 N 4 The morphology is bar-shaped crystal, and the length-diameter ratio is 4-5.
Further, the CaO addition amount of the additive is 5-10wt%.
Equiaxed beta-Si 3 N 4 The preparation process of the powder is characterized by comprising the following process steps:
(1) Mixing the raw materials: 36-48.75wt% of silicon powder, beta-Si 3N441.25-61.5% of diluent and 2.5-10% of additive CaO are adopted as raw materials, ethanol is adopted as grinding medium to ball mill the powder mixture for 1.5-5 hours, and the mixture is uniformly mixed;
(2) Drying and sieving: drying the mixture slurry for 20-48 hours, and sieving the powder mixture;
(3) And (3) combustion synthesis: filling the powder mixture into a porous graphite mold, placing the graphite mold into a combustion reaction kettle, and introducing nitrogen gas with the pressure of 2-5 MPa into the kettle; the powder mixture was ignited by a tungsten coil embedded in titanium powder at the top of the die with an ignition current of 10A and burned in an N2 atmosphere to form a pure phase, equiaxed beta-Si 3N4 powder.
Further, it is preferable that the powder mixture is sieved through a 200 mesh sieve.
Further, in the step (3), siO on the surfaces of CaO and silicon powder in the combustion synthesis 2 The amorphous layer is eutectic to form Ca-O-Si amorphous liquid phase layer.
beta-Si is well known 3 N 4 The generation mechanism of the powder is a dissolution and precipitation mechanism, and the content of high-temperature liquid phase Si in the reaction process is more or less than that of beta-Si 3 N 4 Is particularly important, and the presence of the liquid phase additive increases the combustion temperature and increases the content of liquid phase Si. The invention adds CaO into the system, the CaO can be combined with SiO on the surface of the silicon powder 2 Eutectic formation of the amorphous layer into a Ca-O-Si amorphous liquid phase layer, the presence of the liquid phase layer promoting beta-Si 3 N 4 Dissolving and separating out phases; and is rich in Ca x Si y O z beta-Si in the case of liquids 3 N 4 Then tends to grow along the lowest energy direction of the solid-liquid interface, thereby obtaining equiaxed columnar beta-Si 3 N 4 The die is shown in fig. 1.
Preparation of beta-Si by combustion synthesis 3 N 4 In the process, the reaction of nitrogen and silicon is an outside-in process, which firstly occurs on the surface of silicon powder, and for silicon powder with larger particle size (such as silicon powder with 5 mu m), the specific surface area is smaller, the energy is too low, the energy required by the complete nitridation of the silicon powder from outside to inside cannot be provided, the situation of incomplete nitridation of the silicon powder is easily caused, and the requirement of the current enterprises on the quality of silicon nitride is difficult to be met; the silicon powder (for example, 100 nm) with smaller particle size cannot be uniformly mixed in the mixing process, so that the particle size of the silicon powder is required to be strictly matched in the synthesis process; on the other hand, the content of the silicon powder has great influence on the complete nitridation of the silicon powder, and if the content of CaO is certain, the content of Si/beta-Si 3 N 4 The ratio of the silicon powder to the nitrogen is too large, namely the silicon powder is large in ratio, and free silicon is generated because the silicon powder cannot completely react with the nitrogen, so that the control of the silicon powder content is particularly important.
The invention adopts the combustion synthesis method to prepare single-phase and high-purity equiaxed beta-Si 3N4 powder, has short reaction period, simple process and low cost, and the prepared beta-Si 3N4 powder has no free silicon, has the length-diameter ratio of 1-4, the diameter of 1-3 mu m and the length of 1-10 mu m, can meet the requirement of industrial mass production, has high quality and can use the heat conducting filler.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 preparation of equiaxed beta-Si by combustion synthesis 3 N 4 A powder reaction schematic diagram.
FIG. 2 equiaxed beta-Si prepared by combustion synthesis 3 N 4 XRD pattern of powder.
FIG. 3 equiaxed beta-Si at 10% CaO addition in example 1 of the invention 3 N 4 Powder SEM morphology.
FIG. 4 shows equiaxed beta-Si at 5% CaO addition in example 4 of the invention 3 N 4 Powder SEM morphology.
FIG. 5. Beta. -Si in example 5 of the present invention without CaO addition 3 N 4 Powder SEM morphology.
Detailed Description
The invention will be further illustrated by the following examples. The technical scheme of the invention and the protection scope thereof include but are not limited to the following examples.
Example 1
54g of Si powder with the particle size of 2 mu m and 24.6 mu m beta-Si 3 N 4 81g of powder and 15g (with the ratio of 10%) of commercial CaO powder are taken as raw materials, wherein Si and beta-Si are taken as raw materials 3 N 4 The mass ratio of the powder is 2/3, and the total weight of the raw material powder is 150g; ball milling the powder mixture for 2 hours by using ethanol as a grinding medium, uniformly mixing, drying the slurry for 24 hours, and sieving the powder mixture by a 200-mesh sieve; filling the powder mixture into a porous graphite mold, and placing the graphite mold into a 20L combustion reaction kettle, wherein the kettle is filled with nitrogen under the pressure of 2MPa (the purity is 99.99 percent); the powder mixture was ignited by a tungsten coil embedded in the titanium powder at the top of the mold with an ignition current of 10A; after the reaction was completed, a sample was collected. The XRD pattern can find that the pure phase beta-Si is prepared 3 N 4 No diffraction peak of residual Si and CaO phases. The scanning electron microscope can find that the equiaxial columnar high-dispersion beta-Si can be obtained 3 N 4 Wherein the aspect ratio is on average 1.2, the length is about 1.2 μm and the diameter is 1 μm.
Example 2
67.5g of Si powder with the particle size of 2 mu m and 24.6 mu m of beta-Si 3 N 4 67.5g of powder and 15g (with the ratio of 10%) of commercial CaO powder are taken as raw materials, wherein Si and beta-Si are taken as raw materials 3 N 4 The mass ratio of the powder is 1/1, and the total weight of the raw material powder is 150g; ball milling the powder mixture for 2 hours by using ethanol as a grinding medium, uniformly mixing, drying the slurry for 24 hours, and sieving the powder mixture by a 200-mesh sieve; filling the powder mixture into a porous graphite mold, and placing the graphite mold into a 20L combustion reaction kettle, wherein the kettle is filled with nitrogen under the pressure of 2MPa (the purity is 99.99 percent); the powder mixture was ignited by a tungsten coil embedded in the titanium powder at the top of the mold with an ignition current of 10A; after the reaction was completed, a sample was collected. Detection of sample as single beta-Si by XRD powder diffractometer 3 N 4 And (3) phase (C). SEM morphology observation of equiaxed beta-Si 3 N 4 Averaging of the productsThe aspect ratio was 2.5, the length was about 2.5 μm, and the diameter was about 1. Mu.m.
Example 3
54g of Si powder with the particle size of 2 mu m and 24.6 mu m beta-Si 3 N 4 81g of powder and 15g (with the ratio of 10%) of commercial CaO powder are taken as raw materials, wherein Si and beta-Si are taken as raw materials 3 N 4 The mass ratio of the powder is 2/3, and the total weight of the raw material powder is 150g; ball milling the powder mixture for 2 hours by using ethanol as a grinding medium, uniformly mixing, drying the slurry for 24 hours, and sieving the powder mixture by a 200-mesh sieve; filling the powder mixture into a porous graphite mold, and placing the graphite mold into a 20L combustion reaction kettle, wherein the kettle is filled with nitrogen under the pressure of 5MPa (the purity is 99.99 percent); the powder mixture was ignited by a tungsten coil embedded in the titanium powder at the top of the mold with an ignition current of 10A; after the reaction was completed, a sample was collected. The XRD pattern can find that the pure phase beta-Si is prepared 3 N 4 Free silicon is not contained. The scanning electron microscope can find that the equiaxial columnar high-dispersion beta-Si can be obtained 3 N 4 Wherein the average aspect ratio is about 4, the length is about 10 μm, and the diameter is about 2.5 μm.
Example 4
57g of Si powder with the particle size of 5 mu m and 24.6 mu m of beta-Si 3 N 4 85.5g of powder as raw material and 7.5g (5% of commercial CaO powder) of Si and beta-Si 3 N 4 The mass ratio of the powder is 2/3, and the total weight of the raw material powder is 150g; ball milling the powder mixture for 2 hours by using ethanol as a grinding medium, uniformly mixing, drying the slurry for 24 hours, and sieving the powder mixture by a 200-mesh sieve; filling the powder mixture into a porous graphite mold, and placing the graphite mold into a 20L combustion reaction kettle, wherein the kettle is filled with nitrogen under the pressure of 2MPa (the purity is 99.99 percent); the powder mixture was ignited by a tungsten coil embedded in the titanium powder at the top of the mold with an ignition current of 10A; after the reaction was completed, a sample was collected. Detection of beta-Si only in sample by XRD powder diffractometer 3 N 4 The phase has no diffraction peak of residual Si and CaO phases. As can be seen from the SEM image, beta-Si 3 N 4 The average aspect ratio of the product was 2.5, the average length was about 5 μm and the average diameter was 2. Mu.m, wherein very small particles may be due to the sample preparation processSome of the structures may be destroyed, and the evaluation of the whole microstructure is not affected.
Example 5
58.5g of Si powder with the particle size of 2 mu m and 24.6 mu m of beta-Si 3 N 4 87.75g of powder as raw material and 3.75g (with the ratio of 2.5%) of commercial CaO powder, wherein Si and beta-Si 3 N 4 The mass ratio of the powder is 2/3, and the total weight of the raw material powder is 150g; ball milling the powder mixture for 2 hours by using ethanol as a grinding medium, uniformly mixing, drying the slurry for 24 hours, and sieving the powder mixture by a 200-mesh sieve; filling the powder mixture into a porous graphite mold, and placing the graphite mold into a 20L combustion reaction kettle, wherein the kettle is filled with nitrogen under the pressure of 5MPa (the purity is 99.99 percent); the powder mixture was ignited by a tungsten coil embedded in the titanium powder at the top of the mold with an ignition current of 10A; after the reaction was completed, a sample was collected. Detection of beta-Si only in sample by XRD powder diffractometer 3 N 4 The phase has no diffraction peak of residual Si and CaO phases. beta-Si 3 N 4 The average aspect ratio of the product was 1.5, the average length was about 1.5 μm and the average diameter was 12 μm.
Comparative example
60g of Si powder with the particle size of 2 mu m and 90g of beta-Si 3N4 powder with the particle size of 24.6 mu m are taken as raw materials, wherein the mass ratio of Si to beta-Si 3N4 is 2/3, and the total weight of the raw material powder is 150g; ball milling the powder mixture for 2 hours by using ethanol as a grinding medium, uniformly mixing, drying the slurry for 24 hours, and sieving the powder mixture by a 200-mesh sieve; filling the powder mixture into a porous graphite mold, and placing the graphite mold into a 20L combustion reaction kettle, wherein the kettle is filled with nitrogen under the pressure of 2MPa (the purity is 99.99 percent); the powder mixture was ignited by a tungsten coil embedded in the titanium powder at the top of the mold with an ignition current of 10A; after the reaction was completed, a sample was collected. The sample was examined by XRD powder diffractometer for a single beta-Si 3N4 phase. The beta-Si 3N4 product has different particle sizes, obvious coarse particles and fine particles, long particles and short particles, larger difference between the length-diameter ratios of different particles and obvious agglomeration phenomenon.
The above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (3)
1. Equiaxial beta-Si synthesized by combustion 3 N 4 The powder is characterized in that the equiaxed beta-Si 3 N 4 The powder is prepared by combustion synthesis method, si powder is used as raw material, beta-Si is used 3 N 4 As a diluent, caO is used as an additive, and the following ingredients are mixed according to the weight ratio: 36-48.75wt% of Si powder and a diluent beta-Si 3 N 4 41.25-61.5wt% and additive CaO2.5-10 wt%, wherein the grain size of the silicon powder is 2-5 mu m, and the diluent is beta-Si 3 N 4 The morphology is bar-shaped crystal, and the length-diameter ratio is 4-5; the equiaxed beta-Si 3 N 4 The change range of the length-diameter ratio of the powder is 1-4, the length is 1-10 mu m, the diameter is 1-3 mu m, and free Si is avoided.
2. The combustion synthesized equiaxed beta-Si according to claim 1 3 N 4 The powder is characterized in that the addition amount of the additive CaO is 5-10wt%.
3. The combustion synthesized equiaxed beta-Si according to claim 1 3 N 4 The powder is characterized in that SiO on the surfaces of CaO and Si powder in combustion synthesis 2 The amorphous layer is eutectic to form Ca-O-Si amorphous liquid phase layer.
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