CN107602154B - Bead string-shaped SiC/SiO2Heterostructure and method of synthesis - Google Patents
Bead string-shaped SiC/SiO2Heterostructure and method of synthesis Download PDFInfo
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- CN107602154B CN107602154B CN201710671398.5A CN201710671398A CN107602154B CN 107602154 B CN107602154 B CN 107602154B CN 201710671398 A CN201710671398 A CN 201710671398A CN 107602154 B CN107602154 B CN 107602154B
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Abstract
The invention discloses a bead string SiC/SiO2A heterostructure and a method of synthesizing the same. The invention relates to a bead-string SiC/SiO2The heterostructure consists of a SiC nanowire inner core and SiO wrapped on the SiC nanowire inner core2A coating layer, and arranged and distributed with SiO2SiO with coaxial coating layer and SiC nanowire inner core2And (4) ball composition. The synthesis method of the invention obtains SiC-Si ceramic composite powder by ball milling and sintering, and then obtains the bead-string SiC/SiO ceramic composite powder by further sintering and in-situ synthesis on the surface of the SiC-Si ceramic composite powder2A heterostructure. The synthesis method has simple and stable process, low cost and high efficiency, can realize large-scale industrial production, and can carry out bead string-shaped SiC/SiO by adjusting the preparation process2The morphology and size of the heterostructure is controlled.
Description
Technical Field
The invention relates to SiC/SiO2The technical field of heterostructure preparation, in particular to bead-string SiC/SiO2A heterostructure and a method of synthesizing the same.
Background
SiC/SiO2The heterostructure is a micro-nano material widely researched by people, and has excellent physical and chemical properties, such as high mechanical strength, good heat conduction performance, good thermal stability, wide band gap and the like. The method has wide application in the aspects of advanced nano composite materials, high-temperature electronic devices, microelectronic and optoelectronic devices, field emission displays, sensors and the like.
At present, SiC/SiO2The preparation method of the heterostructure mainly comprises a microwave method, a template method, a carbothermic method, a chemical vapor deposition method and the like. The literature "Wei J, Li K, Chen J, et al Synthesis and Growth mechanism of SiC/SiO2Nanochains Heterostructure by Catalyst-Free Chemical VaporDeposition[J]A chemical vapor deposition process for preparing SiC/SiO by chemical vapor deposition is reported in the Journal of the American Ceramic Society, 2013, 96(2):627-6332Nanochain heterojunctionA method of forming. The specific process comprises the following steps: adopts high-purity Si powder and SiO2The powder is taken as a raw material, ball milling and mixing are carried out according to the molar ratio of 1:1.3 to obtain mixed powder, the mixed powder is filled into a ceramic boat and covered by a porous graphite sheet; further use of WO3The powder and the C powder are fully mixed according to the molar ratio of 1:5, and are put into a ceramic boat and are put into a quartz tube furnace together. Then, under the condition that the argon flow is 25 sccm, the quartz tube is gradually heated to 1280 ℃, kept for 70 min and then slowly cooled to the room temperature. A small amount of SiC/SiO in a nano chain shape is obtained on the porous graphite sheet2The heterostructure deposits the product.
However, the above method has the following disadvantages: the preparation process is complex, the control precision is high (such as gas flow, positions of two precursors in a tube furnace and the like), and the process is unstable; the tungsten oxide raw material adopted by the precursor is expensive, and the preparation cost is high; synthetic SiC/SiO2The yield of the nano-chain heterostructure is low, only deposition by-products are generated, and the controllability of the shape and the size of the nano-chain heterostructure cannot be realized.
Disclosure of Invention
The invention aims to provide a bead-string SiC/SiO for overcoming the defects of the prior art2A heterostructure. The bead-string-shaped SiC/SiO2The heterostructure consists of a SiC nanowire inner core and SiO wrapped on the SiC nanowire inner core2A coating layer, and arranged and distributed with SiO2SiO with coaxial coating layer and SiC nanowire inner core2And (4) ball composition.
The invention also aims to provide the bead-string-shaped SiC/SiO2A method for synthesizing a heterostructure. The method comprises the steps of obtaining SiC-Si ceramic composite powder through ball milling and sintering, and then obtaining the bead-string SiC/SiO through further sintering and in-situ synthesis on the surface of the SiC-Si ceramic composite powder2A heterostructure. The synthesis method has simple process, low cost and high efficiency, and a large amount of bead-string-shaped SiC/SiO can be prepared2Heterostructure, and can be prepared by adjusting preparation process to bead-string-shaped SiC/SiO2The morphology and size of the heterostructure is controlled.
The purpose of the invention is realized by the following technical scheme.
Bead string-shaped SiC/SiO2A method of synthesis of a heterostructure comprising the steps of:
(1) placing Si powder, SiC powder and C powder in a polytetrafluoroethylene ball milling tank, and carrying out ball milling to obtain mixed powder;
(2) placing the obtained mixed powder into a graphite crucible, then placing the graphite crucible into a sintering furnace, heating, sintering at high temperature, and cooling to room temperature to obtain SiC-Si ceramic composite powder;
(3) uniformly spreading the obtained SiC-Si ceramic composite powder in a ceramic square boat with a graphite paper substrate, covering the ceramic square boat with graphite paper, placing the ceramic square boat in the center of an alumina tube furnace, heating, sintering at high temperature, cooling to room temperature, and synthesizing in situ on the surface of the SiC-Si ceramic composite powder to obtain the bead-string SiC/SiO2A heterostructure.
Further, in the step (1), the purity of the Si powder is 99.5%, and the particle size is 300 mesh.
Further, in the step (1), the purity of the SiC powder is 98.5%, and the particle size is 300 meshes.
Further, in the step (1), the purity of the C powder is 99%, and the granularity is 320 meshes.
Further, in the step (1), the Si powder accounts for 70-85%, the SiC powder accounts for 5-15% and the C powder accounts for 7-15% of the total mass of the Si powder, the SiC powder and the C powder.
Further, in the step (1), the mass ratio of ball materials of the ball mill is 1-3: 1.
further, in the step (1), the ball milling time is 2-4 h.
Further, in the step (2), the temperature of the sintering furnace is raised from room temperature to 2000-2200 ℃ at a temperature raising rate of 5-10 ℃/min.
Further, in the step (2), the high-temperature sintering is carried out at the temperature of 2000-2200 ℃ for 1-3 h.
Further, in the step (2), the heating and high-temperature sintering processes are all performed under an argon atmosphere.
Further, in the step (3), the temperature of the tubular aluminum oxide furnace is raised from room temperature to 1250-1350 ℃ at a temperature raising rate of 5-10 ℃/min.
Further, in the step (3), the high-temperature sintering is carried out for 1.5-3 hours at the temperature of 1250-1350 ℃.
Further, in the step (3), the processes of heating and high-temperature sintering are all performed under a mixed gas atmosphere of 96vol% argon and 4vol% oxygen.
Further, in the step (3), the flow rate of the mixed gas of 96vol% argon and 4vol% oxygen is 180 to 240 sccm.
Bead-string-shaped SiC/SiO synthesized by any one of the synthesis methods2Heterostructure, said beaded SiC/SiO2The heterostructure consists of a SiC nanowire inner core and SiO wrapped on the SiC nanowire inner core2A coating layer, and arranged and distributed with SiO2SiO with coaxial coating layer and SiC nanowire inner core2Ball composition;
the bead string SiC/SiO2In the heterostructure, the "line" of the bead string is SiO2The coating layer wraps the SiC nanowire inner core, and the bead of the bead string is made of SiO2SiO with coaxial coating layer and SiC nanowire inner core2A ball; SiO 22The SiO of the coating layer wrapped SiC nanowire inner core is arranged and distributed2The 'beads' formed by the balls are connected in series to form bead-string-shaped SiC/SiO2A heterostructure.
Further, the diameter of the SiC nanowire inner core is 10-50 nm.
Further, the SiO2The diameter of the coating layer is 200-400 nm.
Further, the SiO2The diameter of the sphere is 500-1500 nm.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) SiC/SiO of the invention2The heterostructure is bead-string SiC/SiO2A heterostructure;
(2) the synthetic method of the invention has simple and stable process, low cost and high efficiency, can realize large-scale industrial production,moreover, the bead-string-shaped SiC/SiO can be prepared by adjusting the preparation process2The morphology and size of the heterostructure is controlled.
Drawings
FIG. 1 shows a beaded SiC/SiO solid phase catalyst synthesized in example 22Transmission Electron Microscopy (TEM) images of the heterostructure;
FIG. 2 shows a beaded SiC/SiO solid phase catalyst synthesized in example 32Scanning Electron Microscope (SEM) images of the heterostructure.
Detailed Description
For a better understanding of the invention, the invention will be further described with reference to specific embodiments and the accompanying drawings, to which, however, the invention is not restricted.
Example 1
Bead string SiC/SiO2The synthesis of the heterostructure specifically comprises the following steps:
(1) respectively weighing 70 g of Si powder (with the purity of 99.5 percent and the granularity of 300 meshes), 15 g of SiC powder (with the purity of 98.5 percent and the granularity of 300 meshes) and 15 g of C powder (with the purity of 99 percent and the granularity of 320 meshes), placing the powders into a polytetrafluoroethylene ball milling tank, and ball milling (ball-material mass ratio of 1: 1) for mixing for 4 hours to obtain mixed powder;
(2) putting the obtained mixed powder into a graphite crucible, putting the graphite crucible and the graphite crucible into a high-temperature reaction sintering furnace together, heating the mixed powder from room temperature to 2000 ℃ at a heating rate of 5 ℃/min, preserving heat for 3 hours, heating the mixed powder until the whole heat preservation process is protected by Ar gas, and then closing a power supply to naturally cool the mixed powder to the room temperature to obtain SiC-Si ceramic composite powder;
(3) evenly spreading the obtained SiC-Si ceramic composite powder in a ceramic square boat with a graphite paper substrate, covering the ceramic square boat with graphite paper, placing the ceramic square boat in the center of an alumina tube furnace, gradually heating the tube furnace to 1250 ℃ at the speed of 5 ℃/min under the atmosphere of mixed gas of 96vol% argon and 4vol% oxygen with the flow of 180 sccm, preserving the heat for 1.5 h, naturally cooling to room temperature, and carrying out in-situ synthesis on the surface of the SiC-Si ceramic composite powder to obtain the SiC/SiO in the shape of beads2A heterostructure.
For synthetic bead-string SiC/SiO2TEM and SEM characterization of the heterostructure, TEM and SEM images see FIGS. 1 and 2, respectively, bead clustersSiC/SiO solid2The heterostructure consists of a SiC nanowire inner core and SiO wrapped on the SiC nanowire inner core2A coating layer, and arranged and distributed with SiO2SiO with coaxial coating layer and SiC nanowire inner core2Ball composition; and the bead-string-shaped SiC/SiO2In the heterostructure, the "line" of the bead string is SiO2The coating layer wraps the SiC nanowire inner core, and the bead of the bead string is made of SiO2SiO with coaxial coating layer and SiC nanowire inner core2A ball; SiO 22The SiO of the coating layer wrapped SiC nanowire inner core is arranged and distributed2The 'beads' formed by the balls are connected in series to form bead-string-shaped SiC/SiO2A heterostructure.
Meanwhile, the bead-string-shaped SiC/SiO2In the heterostructure, the diameter of the SiC nanowire inner core is 10-25 nm, and SiO is2The diameter of the coating layer is 200-250 nm, SiO2The diameter of the sphere is 500-550 nm.
Example 2
(1) Respectively weighing 81 g of Si powder (with the purity of 99.5 percent and the granularity of 300 meshes), 12 g of SiC powder (with the purity of 98.5 percent and the granularity of 300 meshes) and 7 g of C powder (with the purity of 99 percent and the granularity of 320 meshes), placing the powders in a polytetrafluoroethylene ball milling tank, and mixing the powders for 3 hours to obtain mixed powder material, wherein the ball-material mass ratio is 2: 1;
(2) putting the obtained mixed powder into a graphite crucible, putting the graphite crucible and the graphite crucible into a high-temperature reaction sintering furnace together, heating the mixed powder from room temperature to 2100 ℃ at a heating rate of 7 ℃/min, preserving the heat for 2 hours, heating the mixed powder until the whole heat preservation process is protected by Ar gas, and then closing a power supply to naturally cool the mixed powder to the room temperature to obtain SiC-Si ceramic composite powder;
(3) evenly spreading the obtained SiC-Si ceramic composite powder in a ceramic square boat with a graphite paper substrate, covering the ceramic square boat with graphite paper, placing the ceramic square boat in the center of an alumina tube furnace, gradually heating the tube furnace to 1300 ℃ at the speed of 8 ℃/min under the atmosphere of mixed gas of 96vol% argon and 4vol% oxygen with the flow of 220 sccm, preserving the temperature for 2 h, naturally cooling to room temperature, and carrying out in-situ synthesis on the surface of the SiC-Si ceramic composite powder to obtain the bead-string SiC/SiO2A heterostructure.
For synthetic beadsString-shaped SiC/SiO2The heterostructure is subjected to TEM and SEM characterization, wherein a TEM image is shown in FIG. 1, an SEM image is shown in FIG. 2, and the SiC/SiO in bead strings2The heterostructure consists of a SiC nanowire inner core and SiO wrapped on the SiC nanowire inner core2A coating layer, and arranged and distributed with SiO2SiO with coaxial coating layer and SiC nanowire inner core2Ball composition; and the bead-string-shaped SiC/SiO2In the heterostructure, the "line" of the bead string is SiO2The coating layer wraps the SiC nanowire inner core, and the bead of the bead string is made of SiO2SiO with coaxial coating layer and SiC nanowire inner core2A ball; SiO 22The SiO of the coating layer wrapped SiC nanowire inner core is arranged and distributed2The 'beads' formed by the balls are connected in series to form bead-string-shaped SiC/SiO2A heterostructure.
Meanwhile, the bead-string-shaped SiC/SiO2In the heterostructure, the diameter of the SiC nanowire inner core is 25-35 nm, and SiO is2The diameter of the coating layer is 250-280 nm and SiO2The diameter of the sphere is 550-700 nm.
Compared with the bead-string SiC/SiO in example 12The size of the heterostructure, the corresponding raw material composition and the sintering temperature of the SiC-Si ceramic composite powder in the tube furnace can be seen, and example 2 enables the SiC nanowire core, SiO, by increasing the Si powder content and the sintering temperature in the tube furnace2Coating layer and SiO2The size of the ball increases.
Example 3
(1) Respectively weighing 85 g of Si powder (with the purity of 99.5 percent and the granularity of 300 meshes), 5 g of SiC powder (with the purity of 98.5 percent and the granularity of 300 meshes) and 10 g of C powder (with the purity of 99 percent and the granularity of 320 meshes), placing the powders in a polytetrafluoroethylene ball milling tank, and ball milling (ball material mass ratio of 3: 1) for mixing for 2 hours to obtain mixed powder;
(2) putting the obtained mixed powder into a graphite crucible, putting the graphite crucible and the graphite crucible into a high-temperature reaction sintering furnace together, heating the mixed powder from room temperature to 2200 ℃ at the heating rate of 10 ℃/min, preserving the heat for 1 h, heating the mixed powder until the whole heat preservation process is protected by Ar gas, and then closing a power supply to naturally cool the mixed powder to the room temperature to obtain SiC-Si ceramic composite powder;
(3) evenly spreading the obtained SiC-Si ceramic composite powder in a ceramic square boat with a graphite paper substrate, covering the ceramic square boat with graphite paper, placing the ceramic square boat in the center of an alumina tube furnace, gradually heating the tube furnace to 1350 ℃ at the speed of 10 ℃/min under the atmosphere of mixed gas of 96vol% argon and 4vol% oxygen with the flow of 240 sccm, preserving the heat for 3 hours, naturally cooling to room temperature, and carrying out in-situ synthesis on the surface of the SiC-Si ceramic composite powder to obtain the bead-string SiC/SiO2A heterostructure.
For synthetic bead-string SiC/SiO2Performing TEM and SEM characterization on the heterostructure, wherein a TEM image is shown in figure 1, an SEM image is shown in figure 2, and the heterostructure is in a bead string shape like SiC/SiO2The heterostructure consists of a SiC nanowire inner core and SiO wrapped on the SiC nanowire inner core2A coating layer, and arranged and distributed with SiO2SiO with coaxial coating layer and SiC nanowire inner core2Ball composition; and the bead-string-shaped SiC/SiO2In the heterostructure, the "line" of the bead string is SiO2The coating layer wraps the SiC nanowire inner core, and the bead of the bead string is made of SiO2SiO with coaxial coating layer and SiC nanowire inner core2A ball; SiO 22The SiO of the coating layer wrapped SiC nanowire inner core is arranged and distributed2The 'beads' formed by the balls are connected in series to form bead-string-shaped SiC/SiO2A heterostructure.
Meanwhile, the bead-string-shaped SiC/SiO2In the heterostructure, the diameter of the SiC nanowire inner core is 35-50 nm, and SiO is2The diameter of the coating layer is 280-400 nm, and SiO is2The diameter of the ball is 700-1500 nm.
In comparison with the beaded SiC/SiO of examples 1 and 22The size of the heterostructure, the raw material composition and the sintering temperature of the SiC-Si ceramic composite powder in the tube furnace can be seen, and example 3 allows the SiC nanowire core, SiO, to be grown by further increasing the Si powder content and the sintering temperature in the tube furnace2Coating layer and SiO2The size of the ball is further increased.
Claims (5)
1. Bead string-shaped SiC/SiO2A method of synthesizing a heterostructure comprisingThe method comprises the following steps:
(1) putting Si powder, SiC powder and C powder into a polytetrafluoroethylene ball milling tank, and carrying out ball milling to obtain mixed powder, wherein the mixed powder comprises 70-85% of Si powder, 5-15% of SiC powder and 7-15% of C powder in percentage by mass of the total mass of the Si powder, the SiC powder and the C powder; the ball-milling ball material mass ratio is 1-3: 1; the ball milling time is 2-4 h;
(2) placing the obtained mixed powder into a graphite crucible, then placing the graphite crucible into a sintering furnace, heating, sintering at high temperature, and cooling to room temperature to obtain SiC-Si ceramic composite powder; the temperature rise is to raise the temperature of the sintering furnace from room temperature to 2000-2200 ℃ at a temperature rise rate of 5-10 ℃/min; the high-temperature sintering is carried out for 1-3 h at the temperature of 2000-2200 ℃;
(3) uniformly spreading the obtained SiC-Si ceramic composite powder in a ceramic square boat with a graphite paper substrate, covering the ceramic square boat with graphite paper, placing the ceramic square boat in the center of an alumina tube furnace, and heating the ceramic square boat at a temperature rising rate of 5-10 ℃/min to heat the alumina tube furnace from room temperature to 1250-1350 ℃; the high-temperature sintering is carried out for 1.5-3 h at 1250-1350 ℃; cooling to room temperature, and in-situ synthesizing on the surface of the SiC-Si ceramic composite powder to obtain the bead-string SiC/SiO2A heterostructure.
2. The beaded SiC/SiO of claim 12The synthesis method of the heterostructure is characterized in that in the step (1), the purity of the Si powder is 99.5%, and the granularity is 300 meshes; the purity of the SiC powder is 98.5%, and the granularity is 300 meshes; the purity of the C powder is 99%, and the granularity is 320 meshes.
3. The beaded SiC/SiO of claim 12The synthesis method of the heterostructure is characterized in that in the step (2), the heating and high-temperature sintering processes are all carried out in an argon atmosphere.
4. The beaded SiC/SiO of claim 12A method for synthesizing a heterostructure, wherein in the step (3), the temperature is raised and the temperature is raisedThe warm sintering process is carried out in the mixed gas atmosphere of 96vol% argon and 4vol% oxygen; the flow rate of the mixed gas of 96vol% argon and 4vol% oxygen is 180-240 sccm.
5. Bead-string-shaped SiC/SiO synthesized by the synthesis method according to any one of claims 1 to 42The heterostructure is characterized in that the bead-string SiC/SiO2The heterostructure consists of a SiC nanowire inner core and SiO wrapped on the SiC nanowire inner core2A coating layer, and arranged and distributed with SiO2SiO with coaxial coating layer and SiC nanowire inner core2Ball composition; the bead string SiC/SiO2In the heterostructure, the "line" of the bead string is SiO2The coating layer wraps the SiC nanowire inner core, and the bead of the bead string is made of SiO2SiO with coaxial coating layer and SiC nanowire inner core2A ball; the diameter of the SiC nanowire inner core is 10-50 nm; the SiO2The diameter of the coating layer is 200-400 nm; the SiO2The diameter of the sphere is 500-1500 nm.
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