CN112209722A - Silicon nitride composite material, preparation method thereof and heating element - Google Patents
Silicon nitride composite material, preparation method thereof and heating element Download PDFInfo
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Abstract
The invention relates to a silicon nitride composite material, a preparation method thereof and a heating body, wherein the silicon nitride composite material comprises 80-93 parts of silicon nitride powder, 5-15 parts of sintering aid, 1-5 parts of reinforcing agent and 1-5 parts of binder by mass; the reinforcing agent is selected from at least one of nitride whiskers with the length-diameter ratio of 1 (20-30) and carbide whiskers with the length-diameter ratio of 1 (20-30). By adopting specific components and proportions, the bending strength of the material can be enhanced and the thermal conductivity of the silicon nitride ceramic material can be improved through the combined action of the sintering aid, the binder and the nitride crystal whisker and/or the carbide crystal whisker with specific length-diameter ratio on the silicon nitride powder. When the silicon nitride composite material is applied to the heating field, the electric energy conversion efficiency of a heating body can be improved by 1-3 times, the service life of a device is further prolonged, and the purposes of energy conservation and consumption reduction are achieved.
Description
Technical Field
The invention relates to the technical field of silicon nitride material preparation, in particular to a silicon nitride composite material, a preparation method thereof and a heating body.
Background
The heating element is an important medium for converting electric energy into heat energy, and generally comprises a base body and a heating film loaded on the surface of the base body. Under the condition of electrifying, the heating film on the heating body converts electric energy into heat energy, and then the base body transfers the heat energy to objects needing to be heated, such as solvent, oil and the like. Most of the current heating markets adopt a quartz tube as a substrate of a tin dioxide heating film, but the quartz glass tube has low strength, bending strength of only 80 MPa and low thermal conductivity, the thermal conductivity of the quartz glass tube is less than 2W/m.k, and when the quartz glass tube is used as the substrate of a heating body, the power consumption of the heating body is high, so that the service life of the heating body is shortened, and the development of high-power heating products is greatly limited.
Silicon nitride (Si)3N4) The ceramic material has excellent comprehensive performance, the theoretical thermal conductivity of the single crystal silicon nitride is high, and the prepared ceramic material has excellent thermal radiation performance and heat cycle resistance. However, the silicon nitride ceramic material prepared by the traditional preparation method has low thermal conductivity and bending strength, and the existing silicon nitride ceramic material cannot be applied to the heating field with high requirements on thermal conductivity and mechanical impact.
Therefore, there is a need to develop a silicon nitride material with high bending strength and high thermal conductivity.
Disclosure of Invention
Based on the above, the invention provides the silicon nitride composite material with high bending strength and high heat conductivity, the preparation method thereof and the heating body.
The technical scheme of the invention is as follows.
The invention provides a silicon nitride composite material, which comprises 80-93 parts of silicon nitride powder, 5-15 parts of sintering aid, 1-5 parts of reinforcing agent and 1-5 parts of binder according to parts by mass;
the reinforcing agent is selected from at least one of nitride whiskers with the length-diameter ratio of 1 (20-30) and carbide whiskers with the length-diameter ratio of 1 (20-30).
In some of these embodiments, the sintering aid is selected from at least one of rare earth metal oxides, rare earth metal fluorides, and alkaline earth metal oxides.
In some of these embodiments, the sintering aid is selected from at least one of yttria, europia, ceria, neodymium fluoride, gadolinium fluoride, lanthanum fluoride, and magnesia;
the nitride whisker is a silicon nitride whisker, and/or the carbide whisker is a silicon carbide whisker.
The invention also provides a preparation method of the silicon nitride composite material, which comprises the following steps:
providing the following raw materials: 80-93 parts of silicon nitride powder, 5-15 parts of sintering aid, 1-5 parts of reinforcing agent and 1-5 parts of binder; the reinforcing agent is selected from at least one of nitride whiskers with the length-diameter ratio of 1 (20-30) and carbide whiskers with the length-diameter ratio of 1 (20-30);
mixing the raw materials in a solvent for pulping, then carrying out spray drying and granulation to obtain granulation powder;
preparing the granulated powder into a green body;
and sintering and molding the green body to obtain the silicon nitride composite material.
In some embodiments, the step of sintering and shaping the green body specifically includes the following steps:
heating the green body to 900-1000 ℃ under the action of protective gas atmosphere and introduced hydrogen, and sintering at 900-1000 ℃ for 1-2 h; the flow rate of the introduced hydrogen is 30L/min-100L/min;
after the sintering at 900-1000 ℃, protective gas is filled to replace hydrogen, the temperature is continuously raised to 1300-1380 ℃ under the protective gas atmosphere for sintering for 2-5 h, and then the temperature is raised to 1650-1850 ℃ for sintering for 2-5 h.
In some of the embodiments, the temperature control procedure in the step of sintering and shaping the green body in step S30 is as follows:
heating to 900-1000 ℃ at constant speed within 10-20 h;
raising the temperature from 900-1000 ℃ to 1300-1380 ℃ at a constant speed within 5-10 h;
the temperature is raised from 1300 ℃ to 1380 ℃ to 1650 ℃ to 1850 ℃ at a constant speed within 5h to 10 h.
The invention also provides any one of the silicon nitride composite materials or the silicon nitride composite material prepared by any one of the preparation methods.
Further, the present invention provides a heating element comprising any one of the above silicon nitride composite materials or a silicon nitride composite material produced by any one of the above production methods.
In some embodiments, the heating element includes a substrate and a heating film loaded on the surface of the substrate, and the substrate is made of any one of the silicon nitride composite materials or the silicon nitride composite material prepared by any one of the preparation methods.
The present invention provides a heat generating device including any of the above heat generating bodies.
Advantageous effects
In the silicon nitride composite material, the specific components and the proportion are adopted, and the combined action of the sintering aid, the binder and the nitride crystal whisker and/or the carbide crystal whisker with the specific length-diameter ratio in a specific mass ratio on the silicon nitride powder can enhance the bending strength of the material and improve the thermal conductivity of the silicon nitride ceramic material. When the preparation method is applied to the preparation of heat-conducting products, the heat conductivity of the heat-conducting products can be improved, so that the device power of the heat-conducting products is improved, and the service life of the heat-conducting products is prolonged.
The preparation method of the silicon nitride composite material comprises the steps of preparing a green body by adopting specific components and proportions in the silicon nitride composite material; and sintering and molding the green body to obtain the silicon nitride composite material with high bending strength and high thermal conductivity.
Further, in the preparation method of the silicon nitride composite material, in the step of sintering and molding the green body, in the process of heating to 900-1000 ℃, hydrogen is introduced at the flow rate of 30-100L/min, the hydrogen can effectively raise the temperature of the colloid generated by the green body, purify the green body, effectively remove oxygen element contained in the green body material, reduce oxygen content in the grain boundary of the green body, and further improve the thermal conductivity and strength of the material.
The invention further provides a heating element, which comprises any one of the silicon nitride composite materials or the silicon nitride composite material prepared by any one of the preparation methods, and compared with the existing quartz heating tube, the heating element has the advantages that the energy conversion efficiency is improved by 1-3 times, and the service life is prolonged.
Drawings
FIG. 1 is a flow chart illustrating the preparation of the silicon nitride composite material according to example 1.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
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. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a silicon nitride composite material, which comprises 80-93 parts of silicon nitride powder, 5-15 parts of sintering aid, 1-5 parts of reinforcing agent and 1-5 parts of binder according to parts by mass;
wherein the reinforcing agent is at least one of nitride whiskers with the length-diameter ratio of 1 (20-30) and carbide whiskers with the length-diameter ratio of 1 (20-30).
In the silicon nitride composite material, the specific components and the proportion are adopted, and the combined action of the sintering aid, the binder and the silicon nitride whisker with the specific length-diameter ratio on the silicon nitride powder can enhance the bending strength of the material and improve the thermal conductivity of the silicon nitride ceramic material. When the preparation method is applied to the preparation of heat-conducting products, the heat conductivity of the heat-conducting products can be improved, so that the device power of the heat-conducting products is improved, and the service life of the heat-conducting products is prolonged.
Preferably, the raw materials of the silicon nitride composite material comprise, by mass, 88 parts of silicon nitride powder, 10 parts of sintering aid, 2 parts of reinforcing agent and 3 parts of binder.
In some of these embodiments, the sintering aid is selected from at least one of rare earth metal oxides, rare earth metal fluorides, and alkaline earth metal oxides.
Preferably, the sintering aid is selected from the group consisting of rare earth metal oxides, rare earth metal fluorides and mixtures of alkaline earth metal oxides.
The bending strength and the thermal conductivity of the material can be further enhanced by combining other mass binders with the three sintering aids and the synergistic effect of the nitride whiskers and/or carbide whiskers with a specific length-diameter ratio on the silicon nitride powder.
It is understood that the rare earth metals include the rare earth elements found so far, including 17 elements of scandium, yttrium, lanthanoid, etc. in IIIB group of the periodic Table of elements; the alkaline earth metal refers to IIA group elements in the periodic table of elements, including seven elements such as beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr), barium (Ba), radium (Ra), and star (ubn).
In some embodiments, the sintering aid is at least one selected from the group consisting of yttrium oxide, europium oxide, cerium oxide, neodymium fluoride, gadolinium fluoride, lanthanum fluoride, and magnesium oxide.
In some of the embodiments, the sintering aid is magnesium oxide, neodymium fluoride, and yttrium oxide.
The binder may be any binder commonly used in the art, including but not limited to acrylic, cellulose, polyvinyl alcohol, polyvinyl butyral, and the like.
In some of these embodiments, the binder is polyvinyl butyral.
In some of these embodiments, the nitride whiskers are selected from at least one of aluminum nitride whiskers and silicon nitride whiskers; the carbide whisker is selected from at least one of silicon carbide whisker and aluminum carbide whisker.
In some of these embodiments, the nitride whiskers are silicon nitride whiskers, and/or the carbide whiskers are silicon carbide whiskers.
An embodiment of the present invention provides a method for preparing a silicon nitride composite material, including the following steps S10 to S40. The specific preparation process is shown in figure 1.
Step S10, providing the following raw materials: 80-93 parts of silicon nitride powder, 5-15 parts of sintering aid, 1-5 parts of reinforcing agent and 1-5 parts of binder; the reinforcing agent is selected from at least one of nitride whiskers with the length-diameter ratio of 1 (20-30) and carbide whiskers with the length-diameter ratio of 1 (20-30).
And S20, mixing the raw materials obtained in the step S10 in a solvent for pulping, and then carrying out spray drying and granulation to obtain granulated powder.
In some of the embodiments, in step S20, the particle size D50 of the slurry is less than or equal to 1 μm, and further, the particle size D50 of the slurry is 0.1 μm to 1 μm.
In some of these embodiments, the viscosity of the slurry in step S20 is 20mPa S to 50mPa S.
It is understood that, in step S20, the amount of the solvent is determined according to the viscosity of the slurry. The solvent may be selected from water or organic solvents commonly used in the art, such as ethanol and the like.
In some of these embodiments, the solvent is water in step S20.
In some embodiments, in step S20, the ball milling time is 1h to 5 h.
In some embodiments, in step S20, the granulated powder has a particle size of 50-80 microns.
Step S30, the granulated powder obtained in step S20 is made into a green body.
In some embodiments, in step S30, the step of forming the granulated powder into a green body is slip casting, dry pressing or isostatic pressing. In a specific example, isostatic pressing is adopted, and the specific steps are as follows:
and placing the obtained granulation powder in a die sleeve, then placing the die sleeve in wet isostatic pressing, and forming under the static pressure of 100-120 MPa to obtain a tubular green body. In a specific example, a tubular green body was obtained with a wall thickness of 1.5mm, a length of 300mm and an outer diameter of 23 mm.
It will be appreciated that after the green body is formed, the green body may be subjected to the necessary green body finishing operations as may be required for particular changes.
And S40, sintering and molding the green body obtained in the step S30 to obtain the silicon nitride composite material.
The preparation method of the silicon nitride composite material comprises the steps of preparing a green body by adopting specific components and proportions in the silicon nitride composite material; and sintering and molding the green body to obtain the silicon nitride composite material with high bending strength and high thermal conductivity.
In some embodiments, the step of sintering and shaping the green body obtained in step S30 in step S40 specifically includes the following steps:
heating the green body to 900-1000 ℃ under the action of protective gas atmosphere and introduced hydrogen, and sintering at 900-1000 ℃ for 1-2 h; the flow rate of the introduced hydrogen is 30L/min-100L/min;
after the sintering at 900-1000 ℃, protective gas is filled to replace hydrogen, the temperature is continuously raised to 1300-1380 ℃ under the protective gas atmosphere for sintering for 2-5 h, and then the temperature is raised to 1650-1850 ℃ for sintering for 2-5 h.
In the step of sintering and molding the green body, hydrogen is introduced in the process of raising the temperature to 900-1000 ℃, and the introduction of hydrogen is stopped after the temperature is raised to 900-1000 ℃.
In the step S40, in the process of heating to 900-1000 ℃, hydrogen is introduced at a flow rate of 30-100L/min, and the introduction of hydrogen can effectively heat the colloid generated by the green body and purify the green body, thereby effectively removing the oxygen element contained in the green body material, reducing the oxygen content in the grain boundary of the green body, and further improving the thermal conductivity and strength of the material.
In the step of sintering and shaping the green body in the step S40, the green body is placed in a vacuum environment before the step of heating the green body to 900 to 1000 ℃ under the action of a protective gas atmosphere and hydrogen gas.
In some embodiments, in the step of sintering and shaping the green body in step S40, after sintering at 900-1000 ℃ and maintaining the temperature, 1-10 Mpa of protective gas is introduced to replace hydrogen.
The protective gas used in step S40 includes an inert gas and nitrogen. In one particular example, the protective gas is nitrogen.
In some of the embodiments, the temperature control procedure in the step of sintering and shaping the green body in step S40 is as follows:
heating to 900-1000 ℃ at constant speed within 10-20 h;
raising the temperature from 900-1000 ℃ to 1300-1380 ℃ at a constant speed within 5-10 h;
the temperature is raised from 1300 ℃ to 1380 ℃ to 1650 ℃ to 1850 ℃ at a constant speed within 5h to 10 h.
In some embodiments, step S40 includes cutting and polishing the silicon nitride composite material after the green body sintering and forming step.
It is understood that the silicon nitride composite material may be cut and polished or not cut and polished according to the requirements of practical application.
Further, an embodiment of the present invention provides an application of any one of the above silicon nitride composite materials or the silicon nitride composite material prepared by any one of the above preparation methods in preparing a heat conductive product.
When the silicon nitride composite material is applied to preparing a heat-conducting product, the heat conductivity of the heat-conducting product can be improved, so that the device power of the heat-conducting product is improved, and the service life of the heat-conducting product is prolonged.
Such thermally conductive articles include, but are not limited to: heat conducting gasket, heat conducting ceramic, heating body in heater, heat conducting glass and heat conducting device in heating equipment.
Further, an embodiment of the present invention provides a heat-generating body including the silicon nitride composite material described above or the silicon nitride composite material produced by the above-described production method.
Compared with the existing quartz heating tube, the power-increasing conversion efficiency of the heating body is improved by 1-3 times, and the service life is prolonged.
In some embodiments, the heating element includes a substrate and a heating film loaded on the surface of the substrate, and the substrate is made of any one of the silicon nitride composite materials or the silicon nitride composite material prepared by any one of the preparation methods.
In a specific example, the heat generating film is a tin dioxide film. Further, an embodiment of the present invention also provides a heat-generating device including any of the heat-generating bodies described above.
The heating device includes, but is not limited to, a heating device, a water heater, a heating tile, a heating plate, an electric heating plate, and the like.
In some embodiments, the heat generating device includes a case and a heat generating medium, the heat generating medium being any of the heat generating bodies described above.
For example, the warmer comprises a shell and a heating medium, wherein the heating medium is any one of the heating bodies, and the heating body can be in a plate shape, a tubular shape or other shapes according to actual requirements.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The silicon nitride composite material and the method for producing the same and the use thereof according to the present invention are exemplified herein, but the present invention is not limited to the following examples.
Example 1
1) Providing the following components: 85 parts of silicon nitride powder, 2 parts of magnesium oxide, 5 parts of neodymium fluoride, 3 parts of yttrium oxide, 5 parts of a binder and 3 parts of silicon nitride whiskers, wherein the length-diameter ratio of the silicon nitride whiskers is 1: 30.
2) Putting the components in the step 1) into a ball mill, adding a certain amount of deionized water, and carrying out ball milling for 2 hours to obtain slurry, wherein the viscosity of the slurry is 25mpa · s, and the particle size D50 of the slurry is measured by sampling and is 0.9 μm; then the material is taken out and dried in a spray drying granulation tower with the outlet temperature of 105 ℃ to obtain the granulation powder.
3) And (3) filling the powder obtained in the step 2) into a rubber die sleeve, and placing the rubber die sleeve into wet isostatic pressing to form under the pressure of 120MPa to obtain a tubular green body. The tubular green body had a wall thickness of 1.5mm, a length of 300mm and an outer diameter of 23 mm.
4) Putting the tubular green body obtained in the step 3) into a sintering furnace, closing the furnace, vacuumizing, filling nitrogen until the vacuum surface shows that the vacuum surface shows 20pa, starting heating, uniformly heating from room temperature to 1000 ℃ within 15 hours, then carrying out heat preservation sintering for 1 hour, and introducing hydrogen at the flow rate of 50L/min in the heating process; when the temperature is raised to 1000 ℃, the hydrogen is replaced, and then high-purity nitrogen of 2Mpa is filled; uniformly heating from 1000 ℃ to 1300 ℃ within 6 hours, and sintering at 1300 ℃ for 2 hours; then uniformly heating from 1300 ℃ to 1750 ℃ within 8 hours, and sintering for two hours under the condition of heat preservation; finally, slowly cooling from 1750 ℃ to 1000 ℃ in 4 hours, and then cooling along with the furnace to obtain the tubular silicon nitride composite material.
5) Cutting the tubular silicon nitride composite material obtained in the step 4) in length, and polishing and grinding the surface of the tubular silicon nitride composite material to obtain the tubular silicon nitride composite material. And covering a layer of tin dioxide heating film on the surface of the tubular silicon nitride composite material substrate to obtain the heating tube.
Example 2
1) Providing the following components: 80 parts of silicon nitride powder, 3 parts of magnesium oxide, 5 parts of neodymium fluoride, 5 parts of yttrium oxide, 5 parts of a binder and 5 parts of silicon nitride whiskers, wherein the length-diameter ratio of the silicon nitride whiskers is 1: 30.
2) Same as example 1, step 2).
3) Same as example 1, step 3).
4) Putting the tubular green body obtained in the step 3) into a sintering furnace, closing the furnace, vacuumizing, filling nitrogen until the vacuum table shows 20pa, starting heating, uniformly heating from room temperature to 1000 ℃ within 15 hours, then carrying out heat preservation sintering for 1 hour, and introducing hydrogen at the flow rate of 30L/min in the heating process; when the temperature is raised to 1000 ℃, the hydrogen is replaced, and then high-purity nitrogen of 2Mpa is filled; raising the temperature from 1000 ℃ to 1380 ℃ at a constant speed within 6 hours, and sintering at 1300 ℃ for 2 hours; then uniformly heating from 1380 ℃ to 1850 ℃ in 8 hours, and sintering for two hours in a heat preservation way; finally, slowly reducing the temperature from 1850 ℃ to 1000 ℃ in 4 hours, and then reducing the temperature along with the furnace to obtain the tubular silicon nitride composite material. 5) Same as example 1, step 5).
Example 3
1) Providing the following components: 94 parts of silicon nitride powder, 1 part of magnesium oxide, 3 parts of neodymium fluoride, 2 parts of yttrium oxide, 2 parts of a binder and 1 part of silicon nitride whisker, wherein the length-diameter ratio of the silicon nitride whisker is 1: 30.
2) Same as example 1, step 2).
3) Same as example 1, step 3).
4) Putting the tubular green body obtained in the step 3) into a sintering furnace, closing the furnace, vacuumizing, filling nitrogen until the vacuum table shows 20pa, starting heating, uniformly heating from room temperature to 1000 ℃ within 15 hours, then carrying out heat preservation sintering for 1 hour, and introducing hydrogen at the flow rate of 100L/min in the heating process; when the temperature is raised to 1000 ℃, the hydrogen is replaced, and then high-purity nitrogen of 2Mpa is filled; uniformly heating from 1000 ℃ to 1350 ℃ within 6 hours, and sintering at 1300 ℃ for 2 hours; then uniformly heating from 1350 ℃ to 1800 ℃ within 8 hours, and sintering for two hours in a heat preservation way; finally, slowly cooling from 1800 ℃ to 1000 ℃ in 4 hours, and then cooling along with the furnace to obtain the tubular silicon nitride composite material.
5) Same as example 1, step 5).
Example 4
1) Providing the following components: 88 parts of silicon nitride powder, 5 parts of magnesium oxide, 2 parts of neodymium fluoride, 3 parts of yttrium oxide, 3 parts of a binder and 2 parts of silicon nitride whiskers, wherein the length-diameter ratio of the silicon nitride whiskers is 1: 20.
The remaining steps and process conditions were the same as in example 1.
Example 5
1) Example 5 is essentially the same as example 1 except that step 1) in example 5 provides the following components: 90 parts of silicon nitride powder, 2 parts of magnesium oxide, 4 parts of neodymium fluoride, 1 part of yttrium oxide, 4 parts of a binder and 2 parts of silicon nitride whiskers, wherein the length-diameter ratio of the silicon nitride whiskers is 1: 30.
Example 6
1) Providing the following components: 85 parts of silicon nitride powder, 2 parts of magnesium oxide, 5 parts of neodymium fluoride, 3 parts of yttrium oxide, 5 parts of a binder and 3 parts of silicon carbide whiskers, wherein the length-diameter ratio of the silicon carbide whiskers is 1: 30.
The rest of the procedure was the same as in example 1.
Example 7
1) Example 7 is essentially the same as example 1 except that step 1) in example 7 provides the following components: 85 parts of silicon nitride powder, 5 parts of magnesium oxide, 5 parts of neodymium fluoride, 5 parts of a binder and 3 parts of silicon nitride whiskers, wherein the length-diameter ratio of the silicon nitride whiskers is 1: 30.
Comparative example 1
Comparative example 1 is essentially the same as example 1 except that step 1) of comparative example 1 provides the following components: 85 parts of silicon nitride powder, 2 parts of magnesium oxide, 5 parts of neodymium fluoride, 3 parts of yttrium oxide, 6 parts of a binder and 1 part of silicon nitride whisker, wherein the length-diameter ratio of the silicon nitride whisker is 1: 30.
The remaining steps and process conditions were the same as in example 1
Comparative example 2
Comparative example 1 is essentially the same as example 1 except that step 1) of comparative example 1 provides the following components: 85 parts of silicon nitride powder, 2 parts of magnesium oxide, 5 parts of neodymium fluoride, 3 parts of yttrium oxide, 5 parts of a binder and 3 parts of silicon nitride whiskers, wherein the length-diameter ratio of the silicon nitride whiskers is 1: 15.
The binders used in examples 1 to 7 and comparative examples 1 to 2 were all polyvinyl butyral, and the raw material compositions and the formulation ratios thereof in examples 1 to 7 and comparative examples 1 to 2 are shown in table 1.
TABLE 1
Example 8
1. The tubular silicon nitride composite materials prepared in the embodiments 1-7 and the comparative examples 1-2 are subjected to bending strength and thermal conductivity tests, and the bending strength test standard refers to GB/T23806-2009; the test of the thermal conductivity is referred to the GB/T22588-2008 standard.
2. The heating tubes prepared in the embodiments 1 to 7 and the comparative examples 1 to 2 are tested for electric energy conversion efficiency and service life, and the electric energy conversion efficiency test is in reference to the standard GB 4706.1-2005.
The results obtained are shown in table 2 below.
TABLE 2
As can be seen from the test data in Table 2, the tubular silicon nitride composite material prepared according to the technical scheme of the application has high bending strength which is larger than 650Mpa and high thermal conductivity which is larger than 60W/mk, and can obviously improve the heating efficiency of the heating tube, thereby improving the service life, saving energy and reducing consumption.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The silicon nitride composite material is characterized by comprising 80-93 parts by mass of silicon nitride powder, 5-15 parts by mass of sintering aid, 1-5 parts by mass of reinforcing agent and 1-5 parts by mass of binder;
the reinforcing agent is selected from at least one of nitride whiskers with the length-diameter ratio of 1 (20-30) and carbide whiskers with the length-diameter ratio of 1 (20-30).
2. The silicon nitride composite material of claim 1, wherein the sintering aid is selected from at least one of rare earth metal oxides, rare earth metal fluorides, and alkaline earth metal oxides.
3. The silicon nitride composite material according to claim 1, wherein the sintering aid is selected from at least one of yttrium oxide, europium oxide, cerium oxide, neodymium fluoride, gadolinium fluoride, lanthanum fluoride, and magnesium oxide;
the nitride whisker is a silicon nitride whisker, and/or the carbide whisker is a silicon carbide whisker.
4. A preparation method of a silicon nitride composite material is characterized by comprising the following steps:
providing the following raw materials: 80-93 parts of silicon nitride powder, 5-15 parts of sintering aid, 1-5 parts of reinforcing agent and 1-5 parts of binder; the reinforcing agent is selected from at least one of nitride whiskers with the length-diameter ratio of 1 (20-30) and carbide whiskers with the length-diameter ratio of 1 (20-30);
mixing the raw materials in a solvent for pulping, then carrying out spray drying and granulation to obtain granulation powder;
preparing the granulated powder into a green body;
and sintering and molding the green body to obtain the silicon nitride composite material.
5. The method according to claim 4, wherein the step of sintering and shaping the green body comprises the following steps:
heating the green body to 900-1000 ℃ under the action of protective gas atmosphere and introduced hydrogen, and sintering at 900-1000 ℃ for 1-2 h; the flow rate of the introduced hydrogen is 30L/min-100L/min;
after the sintering at 900-1000 ℃, protective gas is filled to replace hydrogen, the temperature is continuously raised to 1300-1380 ℃ under the protective gas atmosphere for sintering for 2-5 h, and then the temperature is raised to 1650-1850 ℃ for sintering for 2-5 h.
6. The method of claim 5, wherein the temperature control procedure in the step of sintering and shaping the green body is as follows:
heating to 900-1000 ℃ at constant speed within 10-20 h;
raising the temperature from 900-1000 ℃ to 1300-1380 ℃ at a constant speed within 5-10 h;
the temperature is raised from 1300 ℃ to 1380 ℃ to 1650 ℃ to 1850 ℃ at a constant speed within 5h to 10 h.
7. Use of the silicon nitride composite material according to any one of claims 1 to 3 or the silicon nitride composite material prepared by the preparation method according to any one of claims 3 to 6 in preparing a heat-conducting product.
8. A heat-generating body characterized in that the heat-generating body comprises the silicon nitride composite material as set forth in any one of claims 1 to 3 or the silicon nitride composite material produced by the production method as set forth in any one of claims 4 to 6.
9. The heat-generating body according to claim 8, characterized in that the heat-generating body comprises a base and a heat-generating film supported on the surface of the base, and the material of the base is the silicon nitride composite material according to any one of claims 1 to 3 or the silicon nitride composite material prepared by the preparation method according to any one of claims 4 to 6.
10. A heat-generating device characterized by comprising the heat-generating body as claimed in any one of claims 8 to 9.
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