CN114477185A - beta-SiC with lamellar structure and preparation method thereof - Google Patents
beta-SiC with lamellar structure and preparation method thereof Download PDFInfo
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Abstract
The method takes graphene as a carbon source, and the graphene and silicon powder are combusted and synthesized in a nitrogen atmosphere by igniting a chemical furnace to prepare the beta-SiC, the beta-SiC has a regular sheet layered structure, does not contain free silicon, and has high phase purity; beta-SiC nanowhiskers are present at the edges of the lamellar structure, which internally comprises mutually staggered, fine and short SiC nanowhiskers, and mutually connected SiC nanoparticles. The heat conductivity of the material and the toughness of the ceramic material are greatly improved, and the material can be applied to occasions with high thermal performance requirements such as electronic device packaging substrates and heat exchangers; and the preparation process is simple, the cost is low, the reaction time is short, and the method is favorable for industrial production.
Description
Technical Field
The invention relates to the field of silicon carbide ceramic materials, in particular to beta-SiC powder with a lamellar structure and a preparation method thereof.
Background
The silicon carbide ceramic has the characteristics of high hardness, high temperature resistance, oxidation resistance, good chemical stability and good thermal shock resistance, can be widely applied to the fields of machinery, aviation, chemical industry, metallurgy and the like, and is particularly suitable for the field with higher thermal performance requirement. Typical current methods for preparing beta-SiC include the following:
(1) as mentioned in CN107602131A, the reactive sintering method adopts silicon carbide coarse powder i, silicon carbide fine powder ii, graphene nanosheets, wood carbon black, silicon powder, a dispersing agent, and a binder, and prepares β -SiC by reactive sintering, wherein the graphene nanosheets provide a carbon source for the silicon carbon reaction, and the silicon carbide generated after the reaction with silicon has a typical layered structure, which can improve the mechanical properties of β -SiC. As mentioned in CN104926313A, dense silicon carbide can be prepared by mixing, molding, and reacting and sintering at high temperature using silicon carbide, graphene, carbon powder, surfactant, dispersant, etc. However, the reaction sintering method has complex raw materials, high energy consumption, long time, easy free silicon content and high industrial cost.
(2) The microwave reaction method, mentioned in Zhaohao in "preparation of silicon carbide by microwave and its electromagnetic shielding", adopts microwave reaction method, and makes different carbon sources react with silicon powder and silicon oxide powder to prepare beta-SiC product. Most of the nano wires, nano rods and micro-nano crystal grains are prepared by taking artificial graphite powder as a carbon source, and the content of the nano wires is low; mostly, the flaky graphite is used as a carbon source to prepare curled nanowires and nanorods; most of the graphene nanoplatelets are micro-nano crystal grains prepared by using the graphene nanoplatelets as a carbon source. Although pure phase beta-SiC can be generated, a graphene-like lamellar structure cannot be obtained, and thus mechanical properties are limited.
Disclosure of Invention
In order to overcome the defects, the invention provides a method for preparing beta-SiC powder with a lamellar structure by a high-temperature combustion synthesis method, which has the advantages of energy conservation, high efficiency and low cost, and the powder has controllable morphology and is beneficial to improving the mechanical property.
The technical scheme is as follows:
the beta-SiC ceramic material with the lamellar structure is characterized in that the lamellar structure is a lamellar structure with a completely open surface, the diameter of the lamellar layer is 4-30 mu m, and the thickness of the lamellar layer is 200-500 nm; the beta-SiC nanowhiskers exist at the edges of the lamellar structure, and the length-diameter ratio of the beta-SiC nanowhiskers is 10-30; the interior of the lamellar structure comprises mutually staggered, fine and short SiC nanowhiskers and mutually connected SiC nanoparticles.
Preferably, the aspect ratio of the SiC nanowhiskers inside the lamellar structure is 5 to 12;
preferably, the size of SiC nano particles in the lamellar structure is 100-300 nm;
the invention also provides a preparation method of the beta-SiC ceramic material with the lamellar structure, which is characterized in that graphene is used as a carbon source, silicon powder is used as a silicon source, the silicon powder and the graphene are uniformly mixed, the mixture is dried and sieved, carbon-silicon mixed powder is filled into a reaction boat, thermite is used as a chemical furnace around the carbon-silicon mixed powder and is placed in a combustion synthesis reaction kettle, 1-3MPa nitrogen is introduced, and the carbon-silicon mixed powder is subjected to combustion synthesis reaction by igniting the chemical furnace to prepare the beta-SiC powder with the lamellar structure.
Preferably, the chemical furnace adopts Ti and C mixed powder and Al and Fe2O3The mixed powder is used as thermite, and a tungsten wire coil is arranged at one end of the powder.
The ignition chemical furnace is ignited by introducing alternating current into a tungsten wire coil.
Preferably, the Ti and C mixed powder accounts for 60-90% of the weight of the carbon-silicon mixed powder; the Al and Fe2O3The weight of the mixed powder is 10-40% of the weight of the carbon-silicon mixed powder.
Preferably, the molar ratio of the silicon source to the carbon source is 1:1-1: 1.2;
preferably, the silicon powder and the graphene are mixed by a wet method, and the weight of the silicon powder mixed with carbon and silicon is 1:1, stirring and wet mixing, continuously performing ultrasonic treatment in an ultrasonic instrument for 3 hours, and adding ethanol every 45min, wherein the adding amount of the ethanol for each time is 25 percent of the weight of the carbon-silicon mixed powder.
Preferably, the drying and sieving are carried out by putting the wet mixed powder into a drying oven at 80 ℃ for drying, and grinding the dried mixed powder through a 45-60-mesh sieve.
According to the invention, a chemical furnace is matched with a combustion synthesis method, the prepared beta-SiC can effectively retain a lamellar structure of graphene, the reaction principle is shown in fig. 1, the graphene has a completely open surface and a hexagonal network lattice structure with higher crystallinity, and the edge of the lamellar layer has active C atoms with relatively higher chemical activity due to a suspended C bond (as shown in fig. 1(a)), and meanwhile, in the preparation process of a product, the network lattice of the graphene can generate more defect sites, surface steps and locally broken C-C bonds under the high-temperature environment of ultrasonic mixing treatment and combustion synthesis, so that local active C atoms are also arranged in the lamellar layer of the graphene (as shown in fig. 1 (a)). In the reaction process, when the gas-phase silicon source (Si, SiO) diffuses to the surface of the graphene and reacts with the active C atoms in the graphene to form SiC crystal nuclei (as shown in fig. 1(b)), since the graphene has a lattice structure with high crystallinity and requires large energy for reaction, the SiC crystal nuclei grow in a one-dimensional direction according to a VS mechanism to form SiC nanowhiskers as the gas-phase silicon source is continuously deposited, and the SiC nanowhiskers are intertwined with each other to maintain a micron-scale lamellar structure (as shown in fig. 1(C)) within the limitation of a graphene lamellar carbon source. Because the activity of the C atoms at the edge of the graphene sheet layer is higher than the chemical activity of the C atoms in the surface of the sheet layer, SiC whiskers are formed at the edge firstly, the aspect ratio of the SiC whiskers at the edge is generally larger than that of the SiC whiskers in the sheet layer, and the formed SiC whiskers are somewhat very short due to the limitation of the activity of the C atoms in the sheet layer and can be directly regarded as SiC particles. Generally, the length of the SiC whisker and the thickness of the lamellar structure formed by the intertwining of the whisker are related to the activity of the fumed silicon source and the graphene, and the two are related to the reaction temperature and the reaction pressure, so that the reaction temperature and the reaction pressure during the combustion synthesis process determine the length of the SiC whisker and the thickness of the lamellar structure formed to some extent.
Because the synthesis experiment is completed under the conditions of a thermite chemical furnace and nitrogen atmosphere, when the nitrogen pressure is taken as a variable, the gas-phase silicon source is reduced along with the increase of the nitrogen pressure (1-3 MPa), so that the length of the formed whisker is shortened, and correspondingly, the thickness of a lamella is reduced to a certain extent; the thermite consists of Ti, C, Al and Fe2O3Composition, in which Ti reacts mildly with C and releases heat highly, Al and Fe2O3The reaction has intense and less exothermic heat, when the ratio of Ti to C is high, the temperature of the chemical furnace is slowly raised but can reach high temperature, the heat preservation time is long, when Al and Fe are in high2O3When the proportion is high, the temperature of the chemical furnace is quickly raised but the reaching temperature is low, and the heat preservation time is short. Therefore, the SiC crystal whiskers obtained by using a chemical furnace with higher proportion of Ti and C are longer, and correspondingly, the thickness of a sheet layer is larger.
Meanwhile, because Si/C is a weak exothermic reaction system, the adiabatic temperature is only 1600-1700K, the SiC is difficult to synthesize by combustion in a mode of directly igniting elements, and because the reactant consumption is less, the combustion synthesis needs to be carried out by means of Si nitridation under nitrogen and chemical furnace coupling heat release auxiliary Si/C system, so that the addition of SiC diluent is not needed.
The invention has the following beneficial effects:
1. the beta-SiC prepared by the combustion synthesis method has a regular sheet layered structure, does not contain free silicon, has high phase purity, greatly improves the thermal conductivity of the material and the toughness of the ceramic material, and can be applied to occasions with high thermal performance requirements, such as electronic device packaging substrates, heat exchangers and the like; and the preparation process is simple, the cost is low, the reaction time is short, and the method is favorable for industrial production.
2. According to the invention, graphene is used as a carbon source, on one hand, the carbon source is provided, on the other hand, the graphene provides a template for forming the flaky beta-SiC, as cracks develop along a flaky structure when the ceramic is broken, more breaking energy needs to be consumed, the fracture toughness of the ceramic is not easily increased, and a large number of nano whiskers exist on the flaky edge, so that the effects of enhancing and toughening are also achieved.
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The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 is a schematic diagram of the formation of a SiC sheet structure;
FIG. 2 is an XRD pattern of beta-SiC having a lamellar structure;
fig. 3 SEM images of reactant graphene and β -SiC having a lamellar structure, (a) SEM image of carbon source graphene; (b) (C) SEM image of the synthesized product under the condition that the mixed powder of Ti and C accounts for 80 percent of thermite and the nitrogen pressure of 1 MPa; (d) SEM image of the synthesized product under the condition that the mixed powder of Ti and C accounts for 90 percent of thermite and the nitrogen pressure of 1 MPa; (e) SEM image of the synthesized product under the condition that the mixed powder of Ti and C accounts for 70 percent of thermite and the nitrogen pressure of 2 MPa; (f) SEM image of the synthesized product under the condition that the mixed powder of Ti and C accounts for 60 percent of thermite and the nitrogen pressure of 3 MPa.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the embodiments described are only some representative embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Example 1
Selecting 12g of graphene, selecting 28g of silicon powder, mixing the silicon powder and the graphene to obtain 40g of carbon-silicon mixed powder, adding absolute ethyl alcohol with the weight ratio of the absolute ethyl alcohol to the carbon-silicon mixed powder of 1:1, stirring and wet mixing, and continuously carrying out ultrasonic treatment in an ultrasonic instrument for 3 hours, wherein the ethyl alcohol is added every 45 minutes because the ethyl alcohol can volatilize in the ultrasonic treatment process, and the adding amount of the ethyl alcohol is 25 percent of the weight of the carbon-silicon mixed powder. And then putting the wet mixed powder subjected to ultrasonic treatment into a drying box at 80 ℃ for drying, and grinding the dried mixed powder and sieving the ground mixed powder with a 45-mesh sieve for later use. Filling the ground and sieved carbon-silicon mixed powder into a stainless steel reaction boat lined with a carbon felt, wherein the mixed powder of Ti and C in a molar ratio of 1:1 accounts for 80 percent, and Al and Fe in a molar ratio of 1:12O3The thermite which accounts for 20 percent of the weight of the mixed powder is placed around the Si and C mixed powder to be used as a chemical furnace, a tungsten wire coil for ignition is placed at one end of the powder, and then the powder and the tungsten wire coil are placed in a closed combustion synthesis reaction kettle together. After the reaction kettle is vacuumized, high-purity nitrogen is filled into the reaction kettle under the pressure of 1 MPa. Then alternating current is introduced into the tungsten wire coil, a chemical furnace is ignited, and then the combustion synthesis reaction of the Si and C mixed powder is initiated, so that the beta-SiC powder with the lamellar structure is obtained. XRD shows that the product is pure-phase beta-SiC powder and does not contain free silicon, and Sf is caused by stacking layers of silicon carbide; according to SEM representation, most products integrally maintain a lamellar structure with the size and the appearance similar to those of graphene in appearance, the average diameter is 15 microns, the average thickness is 400nm, but from the smaller dimension, SiC nano whiskers with larger length-diameter ratios at the edges of the lamellar structure are mutually wound, the length-diameter ratio is about 20, the inner part of the lamellar structure is composed of mutually staggered, fine and short SiC nano whiskers and mutually connected and agglomerated SiC nano particles, the average length-diameter ratio of the short whiskers is about 10, and the average diameter of the nano particles is 150 nm.
Example 2
The experimental conditions as in example 1 were adopted, wherein 12g of graphene and 33.6g of silicon powder were selected, the silicon powder and the graphene were mixed to obtain 45.6g of carbon-silicon mixed powder, the thermite was Ti and C mixed powder accounting for 90%, and Al and Fe were adopted2O3The mixed powder accounts for 10 percent; and grinding the dried mixed powder and sieving the ground mixed powder with a 60-mesh sieve for later use. The other conditions were the same as in example 1. XRD shows that the product is pure phase beta-SiC powder and does not contain free silicon; the SiC nano-whisker with the long diameter larger than that of the edge of the lamellar structure is mutually wound, the length-diameter ratio is about 25, the SiC nano-whisker with the long diameter larger than that of the edge of the lamellar structure is formed by mutually staggered, fine and short SiC nano-whiskers and mutually connected and agglomerated SiC nano-particles, the length-diameter ratio of the short nano-whiskers is about 12 on average, and the average diameter of the nano-particles is 200 nm.
Example 3
The experimental conditions as in example 1 were adopted, wherein the thermite is 70% of Ti and C mixed powder, and Al and Fe2O3The mixed powder accounts for 30 percent; after the reaction kettle is vacuumized, high-purity nitrogen gas is filled into the reaction kettle for 2 MPa. The other conditions were the same as in example 1. XRD shows that the product is pure phase beta-SiC powder and does not contain free silicon; the SiC nano-whiskers with the average diameter of 20 microns and the average thickness of 200nm are mutually wound at the edge of the lamellar structure and have the length-diameter ratio of about 17, and the SiC nano-whiskers with the larger length-diameter ratio are arranged in the lamellar structure and consist of mutually staggered, fine and short SiC nano-whiskers and mutually connected and agglomerated SiC nano-particles, the length-diameter ratio of the short nano-whiskers is about 8 on average, and the average diameter of the nano-particles is 180 nm.
Example 4
The experimental conditions as in example 1 were adopted, wherein the thermite is 60% of Ti and C mixed powder, and Al and Fe2O3The mixed powder accounts for 40 percent; after the reaction kettle is vacuumized, high-purity nitrogen is filled into the reaction kettle under the pressure of 1 MPa. The other conditions were the same as in example 1. XRD shows that the product is pure phase beta-SiC powder and does not contain free silicon; characterized by SEM and had a lamellar structure with an average diameter of 30 μm and an average thickness of 200nm at the edges of the lamellar structureThe SiC nano whiskers with larger length-diameter ratio are mutually wound, the length-diameter ratio is about 15, and the interior of the lamellar structure is formed from mutually-staggered, fine and short SiC nano whiskers and mutually-connected and agglomerated SiC nano particles, the average length-diameter ratio of the short whiskers is about 7, and the average diameter of the nano particles is 280 nm.
Example 5
The experimental conditions as in example 1 were adopted, wherein the thermite is 60% of Ti and C mixed powder, and Al and Fe2O3The mixed powder accounts for 40 percent; after the reaction kettle is vacuumized, high-purity nitrogen is filled in the reaction kettle for 3 MPa. The other conditions were the same as in example 1. XRD shows that the product is pure phase beta-SiC powder and does not contain free silicon; the SiC nano-whisker with the long diameter larger than that of the edge of the lamellar structure is mutually wound, the length-diameter ratio is about 10, the SiC nano-whisker with the long diameter larger than that of the edge of the lamellar structure is formed by mutually staggered, fine and short SiC nano-whiskers and mutually connected and agglomerated SiC nano-particles, the length-diameter ratio of the short whiskers is about 5 on average, and the average diameter of the nano-particles is 300 nm.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present 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 solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The beta-SiC ceramic material with the lamellar structure is characterized in that the lamellar structure is a lamellar structure with a completely open surface, the diameter of the lamellar layer is 4-30 mu m, and the thickness of the lamellar layer is 200-500 nm; the beta-SiC nanowhiskers exist at the edges of the lamellar structure, and the length-diameter ratio of the beta-SiC nanowhiskers is 10-30; the interior of the lamellar structure comprises mutually staggered, fine and short SiC nanowhiskers and mutually connected SiC nanoparticles.
2. The beta-SiC ceramic material with a lamellar structure according to claim 1, characterized in that the SiC nanowhiskers inside the lamellar structure have an aspect ratio of 5 to 12.
3. The beta-SiC ceramic material having a lamellar structure according to claim 1, wherein the SiC nanoparticles inside the lamellar structure have a size of 100 to 300 nm.
4. The method for preparing beta-SiC ceramic material with lamellar structure according to claim 1, wherein graphene is used as carbon source, silicon powder is used as silicon source, the silicon powder and graphene are uniformly mixed, the mixture is dried and sieved, the carbon-silicon mixed powder is loaded into a reaction boat, the periphery of the carbon-silicon mixed powder is treated with thermite as chemical furnace and is placed in a combustion synthesis reaction kettle, 1-3MPa nitrogen is introduced, and the carbon-silicon mixed powder is subjected to combustion synthesis reaction by igniting the chemical furnace to prepare beta-SiC powder with lamellar structure.
5. The method for preparing beta-SiC ceramic material with lamellar structure according to claim 4, wherein said chemical furnace uses Ti, C mixed powder and Al, Fe2O3The mixed powder is used as thermite, and a tungsten wire coil is arranged at one end of the powder.
6. The preparation method of the beta-SiC ceramic material with the lamellar structure according to claim 5, wherein preferably, the Ti and C mixed powder accounts for 60-90% of the weight of the thermite powder; the Al and Fe2O3 mixed powder accounts for 10-40% of the weight of the thermite powder; more preferably, the molar ratio of Ti to C in the Ti/C mixed powder is 1:1, Al, Fe2O3Al and Fe in mixed powder2O3The molar ratio is 1:1.
7. the method for preparing a beta-SiC ceramic material having a lamellar structure according to claims 4 to 6, wherein said ignition chemical furnace is ignited by passing an alternating current through a coil of tungsten wire.
8. The method for preparing a beta-SiC ceramic material with a lamellar structure according to claim 4, wherein the molar ratio of the silicon source to the carbon source is 1:1-1: 1.2.
9. The preparation method of the beta-SiC ceramic material with the lamellar structure according to claim 4, wherein the silicon powder and the graphene are mixed by a wet method, and the weight of the silicon powder mixed with carbon and silicon is 1:1, stirring and wet mixing, continuously performing ultrasonic treatment in an ultrasonic instrument for 3 hours, and adding ethanol every 45min, wherein the adding amount of the ethanol for each time is 25 percent of the weight of the carbon-silicon mixed powder.
10. The method for preparing the beta-SiC ceramic material with the lamellar structure according to claim 9, wherein the drying and sieving are carried out by putting the wet mixed powder into a drying oven at 80 ℃ for drying, and grinding the dried mixed powder through a 45-60 mesh sieve.
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