CN107602154A - A kind of string-of-pearls-like SiC/SiO2Heterojunction structure and its synthetic method - Google Patents
A kind of string-of-pearls-like SiC/SiO2Heterojunction structure and its synthetic method Download PDFInfo
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Abstract
The invention discloses a kind of string-of-pearls-like SiC/SiO2Heterojunction structure and its synthetic method.String-of-pearls-like SiC/SiO of the present invention2Heterojunction structure is by including SiC nanowire inner core, the SiO being wrapped on SiC nanowire inner core2Clad, and arranged distribution and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball forms.Synthetic method of the present invention obtains SiC Si ceramic composite powders, then by further sintering, synthesizes to obtain the string-of-pearls-like SiC/SiO in SiC Si ceramic composite powder surface in situ by ball milling, sintering2Heterojunction structure.Simply, stably, cost is low for the synthetic method craft of the present invention, efficiently, large-scale industrial production can be achieved, and can be by adjusting preparation technology to string-of-pearls-like SiC/SiO2The pattern and size of heterojunction structure are controlled.
Description
Technical field
The present invention relates to SiC/SiO2A kind of heterojunction structure preparing technical field, and in particular to string-of-pearls-like SiC/SiO2It is heterogeneous
Structure and its synthetic method.
Background technology
SiC/SiO2Heterojunction structure is the widely studied a kind of micro Nano material of people, has excellent physical chemistry
Can, such as mechanical strength is high, heat-conductive characteristic is good, heat endurance is good, band gap is wide.In advanced nano composite material, high-temperature electronic
Device, microelectronics and opto-electronic device, FED and sensor etc. have a wide range of applications.
At present, SiC/SiO2The preparation method of heterojunction structure mainly includes microwave method, template, carbothermic method, chemistry
Vapour deposition process etc..Document " Wei J, Li K, Chen J, et al. Synthesis and Growth Mechanism
of SiC/SiO2 Nanochains Heterostructure by Catalyst-Free Chemical Vapor
Deposition[J]. Journal of the American Ceramic Society, 2013, 96(2):627-633”
In report and a kind of prepare SiC/SiO using chemical vapor deposition2The method of nano chain heterojunction structure.Concrete technology is：Using
High-purity Si powder and SiO2Powder is raw material, according to mol ratio 1:1.3 ball milling mixings obtain mixed powder, and the mixed powder is loaded and made pottery
In porcelain boat, and covered with porous stone ink sheet；WO is used again3Powder and C powder are according to mol ratio 1:5 are sufficiently mixed, and are fitted into ceramic boat,
It is placed in together in quartz tube furnace.Then under conditions of argon flow amount is 25 sccm, it is gradually heated up quartz ampoule to 1280 DEG C simultaneously
It is slowly cooled to room temperature after being incubated 70 min.A small amount of SiC/SiO in nanometer chain has been obtained on porous stone ink sheet2Hetero-junctions
Structure sedimentation products.
But the above method has the following disadvantages：Preparation process is complicated, requires that control precision is high（Such as gas flow, two
Kind presoma location etc. in tube furnace）, technique it is unstable；The tungsten oxide expensive raw material price that presoma uses, system
Standby cost is high；The SiC/SiO of synthesis2Nano chain heterojunction structure low yield, only deposition by-products, and its pattern can not be realized
With the controllability of size.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of string-of-pearls-like SiC/SiO2Heterojunction structure.
String-of-pearls-like SiC/SiO2Heterojunction structure is by including SiC nanowire inner core, the SiO being wrapped on SiC nanowire inner core2Clad,
And arranged distribution and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball forms.
The present invention also aims to provide a kind of described string-of-pearls-like SiC/SiO2The synthetic method of heterojunction structure.The party
Method obtains SiC-Si ceramic composite powders by ball milling, sintering, then by further sintering, in SiC-Si composite ceramic powder body surfaces
Face fabricated in situ obtains the string-of-pearls-like SiC/SiO2Heterojunction structure.The synthetic method craft is simple, inexpensive, efficient, prepares
Obtain substantial amounts of string-of-pearls-like SiC/SiO2Heterojunction structure, and can be by adjusting preparation technology to string-of-pearls-like SiC/SiO2Hetero-junctions
The pattern and size of structure are controlled.
The purpose of the present invention is achieved through the following technical solutions.
A kind of string-of-pearls-like SiC/SiO2The synthetic method of heterojunction structure, comprises the following steps：
（1）Si powder, SiC powder and C powder are placed in polytetrafluoroethylene (PTFE) ball grinder, ball milling obtains mixed powder；
（2）Obtained mixed powder is placed in graphite crucible, then graphite crucible is put into sintering furnace, high temperature is carried out after heating
Sintering, is cooled to room temperature, obtains SiC-Si ceramic composite powders；
（3）Obtained SiC-Si ceramic composite powders is evenly laid out in having the porcelain Noah's ark of graphite paper substrates, and use graphite paper
Alumina tube furnace center is placed in after covering, high temperature sintering is carried out after heating, is cooled to room temperature, in SiC-Si ceramic composite powders
Surface in situ synthesizes to obtain the string-of-pearls-like SiC/SiO2Heterojunction structure.
Further, step（1）In, the purity of the Si powder is 99.5%, granularity is 300 mesh.
Further, step（1）In, the purity of the SiC powder is 98.5%, granularity is 300 mesh.
Further, step（1）In, the purity of the C powder is 99%, and granularity is 320 mesh.
Further, step（1）In, by the percentage for the gross mass for accounting for Si powder, SiC powder and C powder, Si powder 70~85%,
SiC powder 5~15%, C powder 7~15%.
Further, step（1）In, the ball material mass ratio of the ball milling is 1 ~ 3：1.
Further, step（1）In, the time of the ball milling is 2 ~ 4h.
Further, step（2）In, the heating is from room temperature liter with 5~10 DEG C/min heating rate by sintering furnace
Temperature is to 2000 ~ 2200 DEG C.
Further, step（2）In, the high temperature sintering is 1 ~ 3h of insulation at a temperature of 2000 ~ 2200 DEG C.
Further, step（2）In, the process of the heating and high temperature sintering is carried out under an argon atmosphere.
Further, step（3）In, it is described heating be with 5~10 DEG C/min heating rate by alumina tube furnace from
Room temperature is to 1250 ~ 1350 DEG C.
Further, step（3）In, the high temperature sintering is 1.5 ~ 3h of insulation at a temperature of 1250 ~ 1350 DEG C.
Further, step（3）In, the process of the heating and high temperature sintering is in 96vol% argon gas and 4vol% oxygen
Mixed-gas atmosphere under carry out.
Further, step（3）In, the flow of the mixed gas of the 96vol% argon gas and 4vol% oxygen for 180 ~
240 sccm。
The string-of-pearls-like SiC/SiO synthesized by the synthetic method described in any of the above-described2Heterojunction structure, described string-of-pearls-like
SiC/SiO2Heterojunction structure is by including SiC nanowire inner core, the SiO being wrapped on SiC nanowire inner core2Clad, and arrangement
Be distributed and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball forms；
Described string-of-pearls-like SiC/SiO2In heterojunction structure, " line " of bead string is SiO2The SiC nanowire inner core of clad parcel,
" pearl " of bead string be and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball；SiO2The SiC nanometers of clad parcel
" line " that line inner core is formed is by the SiO of arranged distribution2" pearl " that ball is formed is together in series, and forms string-of-pearls-like SiC/SiO2Hetero-junctions
Structure.
Further, a diameter of 10 ~ 50 nm of the SiC nanowire inner core.
Further, the SiO2A diameter of 200 ~ 400 nm of clad.
Further, the SiO2A diameter of 500 ~ 1500 nm of ball.
Compared with prior art, the invention has the advantages that and beneficial effect：
（1）The SiC/SiO of the present invention2Heterojunction structure is string-of-pearls-like SiC/SiO2Heterojunction structure；
（2）Simply, stably, cost is low for the synthetic method craft of the present invention, efficiently, large-scale industrial production can be achieved, and
Can be by adjusting preparation technology to string-of-pearls-like SiC/SiO2The pattern and size of heterojunction structure are controlled.
Brief description of the drawings
Fig. 1 is the string-of-pearls-like SiC/SiO synthesized in embodiment 22The transmission electron microscope of heterojunction structure（TEM）Figure；
Fig. 2 is the string-of-pearls-like SiC/SiO synthesized in embodiment 32The ESEM of heterojunction structure（SEM）Figure.
Embodiment
To more fully understand the present invention, below in conjunction with specific embodiments and the drawings, the present invention is further illustrated, but
The invention is not restricted to this.
Embodiment 1
String-of-pearls-like SiC/SiO2The synthesis of heterojunction structure, specifically comprises the following steps：
（1）70 g Si powder is weighed respectively（Purity is 99.5%, granularity is 300 mesh）, 15 g SiC powder（Purity is 98.5%, grain
Spend for 300 mesh）With 15 g C powder（Purity is 99%, granularity is 320 mesh）, it is placed in polytetrafluoroethylene (PTFE) ball grinder, ball milling（Ball material
Mass ratio is 1：1）4 h are mixed, obtain mixed powder；
（2）Obtained mixed powder is put into graphite crucible, then is put into together in pyroreaction sintering furnace, with 5 DEG C/min's
Programming rate rises to 2000 DEG C from room temperature, is incubated 3 h, is warming up to insulation whole process by Ar gas shieldeds, it is naturally cold to be then turned off power supply
But to room temperature, SiC-Si ceramic composite powders are obtained；
（3）Obtained SiC-Si ceramic composite powders is evenly laid out in having the porcelain Noah's ark of graphite paper substrates, and use graphite paper
Alumina tube furnace center is placed in after covering, in the 96vol% argon gas and the mixed gas of 4vol% oxygen that flow is 180 sccm
Under atmosphere, tube furnace is gradually heated up to 1250 DEG C with 5 DEG C/min speed, and is incubated 1.5 h, then naturally cools to room temperature,
Synthesize to obtain string-of-pearls-like SiC/SiO in SiC-Si ceramic composite powder surface in situ2Heterojunction structure.
To the string-of-pearls-like SiC/SiO of synthesis2Heterojunction structure carries out TEM and SEM and characterized, and TEM figures and SEM figures are respectively referring to figure
1 and Fig. 2, string-of-pearls-like SiC/SiO2Heterojunction structure is by including SiC nanowire inner core, the SiO being wrapped on SiC nanowire inner core2Bag
Coating, and arranged distribution and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball forms；And string-of-pearls-like SiC/
SiO2In heterojunction structure, " line " of bead string is SiO2The SiC nanowire inner core of clad parcel, " pearl " of bead string are and SiO2Bag
Coating and the concentric SiO of SiC nanowire inner core2Ball；SiO2" line " that the SiC nanowire inner core of clad parcel is formed will be arranged
The SiO of column distribution2" pearl " that ball is formed is together in series, and forms string-of-pearls-like SiC/SiO2Heterojunction structure.
Meanwhile string-of-pearls-like SiC/SiO2In heterojunction structure, a diameter of 10 ~ 25 nm, SiO of SiC nanowire inner core2Clad
A diameter of 200 ~ 250 nm, SiO2A diameter of 500 ~ 550 nm of ball.
Embodiment 2
（1）81 g Si powder is weighed respectively（Purity is 99.5%, granularity is 300 mesh）, 12 g SiC powder（Purity is 98.5%, grain
Spend for 300 mesh）With 7 g C powder（Purity is 99%, granularity is 320 mesh）, it is placed in polytetrafluoroethylene (PTFE) ball grinder, ball milling（Ball material
Mass ratio is 2：1）3 h are mixed, obtain mixed powder；
（2）Obtained mixed powder is put into graphite crucible, then is put into together in pyroreaction sintering furnace, with 7 DEG C/min's
Programming rate rises to 2100 DEG C from room temperature, is incubated 2 h, is warming up to insulation whole process by Ar gas shieldeds, it is naturally cold to be then turned off power supply
But to room temperature, SiC-Si ceramic composite powders are obtained；
（3）Obtained SiC-Si ceramic composite powders is evenly laid out in having the porcelain Noah's ark of graphite paper substrates, and use graphite paper
Alumina tube furnace center is placed in after covering, in the 96vol% argon gas and the mixed gas of 4vol% oxygen that flow is 220 sccm
Under atmosphere, tube furnace is gradually heated up to 1300 DEG C with 8 DEG C/min speed, and is incubated 2 h, then naturally cools to room temperature,
SiC-Si ceramic composite powder surface in situ synthesizes to obtain string-of-pearls-like SiC/SiO2Heterojunction structure.
To the string-of-pearls-like SiC/SiO of synthesis2Heterojunction structure carries out TEM and SEM and characterized, wherein, TEM figures as shown in figure 1,
SEM figures are referring to Fig. 2, string-of-pearls-like SiC/SiO2Heterojunction structure by including SiC nanowire inner core, be wrapped on SiC nanowire inner core
SiO2Clad, and arranged distribution and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball forms；And pearl
String-like SiC/SiO2In heterojunction structure, " line " of bead string is SiO2The SiC nanowire inner core of clad parcel, " pearl " of bead string are
With SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball；SiO2What the SiC nanowire inner core of clad parcel was formed
" line " is by the SiO of arranged distribution2" pearl " that ball is formed is together in series, and forms string-of-pearls-like SiC/SiO2Heterojunction structure.
Meanwhile string-of-pearls-like SiC/SiO2In heterojunction structure, a diameter of 25 ~ 35 nm, SiO of SiC nanowire inner core2Clad
A diameter of 250 ~ 280 nm, SiO2A diameter of 550 ~ 700 nm of ball.
Compared to string-of-pearls-like SiC/SiO in embodiment 12The size of heterojunction structure, corresponding raw material composition and SiC-Si potteries
The temperature that porcelain composite granule sinters in tube furnace can be seen that embodiment 2 by improving the content of Si powder and in tube furnace
Sintering temperature so that SiC nanowire inner core, SiO2Clad and SiO2The size of ball increased.
Embodiment 3
（1）85 g Si powder is weighed respectively（Purity is 99.5%, granularity is 300 mesh）, 5 g SiC powder（Purity is 98.5%, grain
Spend for 300 mesh）With 10 g C powder（Purity is 99%, granularity is 320 mesh）, it is placed in polytetrafluoroethylene (PTFE) ball grinder, ball milling（Ball material
Mass ratio is 3：1）2 h are mixed, obtain mixed powder；
（2）Obtained mixed powder is put into graphite crucible, then is put into together in pyroreaction sintering furnace, with 10 DEG C/min's
Programming rate rises to 2200 DEG C from room temperature, is incubated 1 h, is warming up to insulation whole process by Ar gas shieldeds, it is naturally cold to be then turned off power supply
But to room temperature, SiC-Si ceramic composite powders are obtained；
（3）Obtained SiC-Si ceramic composite powders is evenly laid out in having the porcelain Noah's ark of graphite paper substrates, and use graphite paper
Alumina tube furnace center is placed in after covering, in the 96vol% argon gas and the mixed gas of 4vol% oxygen that flow is 240 sccm
Under atmosphere, tube furnace is gradually heated up to 1350 DEG C with 10 DEG C/min speed, and is incubated 3 h, then naturally cools to room temperature,
SiC-Si ceramic composite powder surface in situ synthesizes to obtain string-of-pearls-like SiC/SiO2Heterojunction structure.
To the string-of-pearls-like SiC/SiO of synthesis2Heterojunction structure carries out TEM and SEM and characterized, wherein, TEM figures are referring to Fig. 1, SEM
Figure is as shown in Fig. 2 string-of-pearls-like SiC/SiO2Heterojunction structure by including SiC nanowire inner core, be wrapped on SiC nanowire inner core
SiO2Clad, and arranged distribution and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball forms；And bead string
Shape SiC/SiO2In heterojunction structure, " line " of bead string is SiO2The SiC nanowire inner core of clad parcel, " pearl " of bead string be with
SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball；SiO2What the SiC nanowire inner core of clad parcel was formed
" line " is by the SiO of arranged distribution2" pearl " that ball is formed is together in series, and forms string-of-pearls-like SiC/SiO2Heterojunction structure.
Meanwhile string-of-pearls-like SiC/SiO2In heterojunction structure, a diameter of 35 ~ 50 nm, SiO of SiC nanowire inner core2Clad
A diameter of 280 ~ 400 nm, SiO2A diameter of 700 ~ 1500 nm of ball.
Compared to string-of-pearls-like SiC/SiO in Examples 1 and 22Size, raw material composition and the SiC-Si ceramics of heterojunction structure
The temperature that composite granule sinters in tube furnace can be seen that embodiment 3 by further improving the content of Si powder and in tubular type
Sintering temperature in stove so that SiC nanowire inner core, SiO2Clad and SiO2The size of ball further increases.
Claims (10)
- A kind of 1. string-of-pearls-like SiC/SiO2The synthetic method of heterojunction structure, it is characterised in that comprise the following steps：（1）Si powder, SiC powder and C powder are placed in polytetrafluoroethylene (PTFE) ball grinder, ball milling obtains mixed powder；（2）Obtained mixed powder is placed in graphite crucible, then graphite crucible is put into sintering furnace, high temperature is carried out after heating Sintering, is cooled to room temperature, obtains SiC-Si ceramic composite powders；（3）Obtained SiC-Si ceramic composite powders is evenly laid out in having the porcelain Noah's ark of graphite paper substrates, and use graphite paper Alumina tube furnace center is placed in after covering, high temperature sintering is carried out after heating, is cooled to room temperature, in SiC-Si ceramic composite powders Surface in situ synthesizes to obtain the string-of-pearls-like SiC/SiO2Heterojunction structure.
- A kind of 2. string-of-pearls-like SiC/SiO according to claim 12The synthetic method of heterojunction structure, it is characterised in that step （1）In, the purity of the Si powder is 99.5%, granularity is 300 mesh；The purity of the SiC powder is 98.5%, granularity is 300 mesh；Institute The purity for stating C powder is 99%, and granularity is 320 mesh.
- A kind of 3. string-of-pearls-like SiC/SiO according to claim 12The synthetic method of heterojunction structure, it is characterised in that step （1）In, by the percentage for the gross mass for accounting for Si powder, SiC powder and C powder, Si powder 70~85%, SiC powder 5~15%, C powder 7~15%.
- A kind of 4. string-of-pearls-like SiC/SiO according to claim 12The synthetic method of heterojunction structure, it is characterised in that step （1）In, the ball material mass ratio of the ball milling is 1 ~ 3：1；The time of the ball milling is 2 ~ 4h.
- A kind of 5. string-of-pearls-like SiC/SiO according to claim 12The synthetic method of heterojunction structure, it is characterised in that step （2）In, the heating is from room temperature to 2000 ~ 2200 DEG C with 5~10 DEG C/min heating rate by sintering furnace；The height Temperature sintering is 1 ~ 3h of insulation at a temperature of 2000 ~ 2200 DEG C.
- A kind of 6. string-of-pearls-like SiC/SiO according to claim 12The synthetic method of heterojunction structure, it is characterised in that step （2）In, the process of the heating and high temperature sintering is carried out under an argon atmosphere.
- A kind of 7. string-of-pearls-like SiC/SiO according to claim 12The synthetic method of heterojunction structure, it is characterised in that step （3）In, the heating is from room temperature to 1250 ~ 1350 DEG C with 5~10 DEG C/min heating rate by alumina tube furnace； The high temperature sintering is 1.5 ~ 3h of insulation at a temperature of 1250 ~ 1350 DEG C.
- A kind of 8. string-of-pearls-like SiC/SiO according to claim 12The synthetic method of heterojunction structure, it is characterised in that step （3）In, the process of the heating and high temperature sintering is carried out under the mixed-gas atmosphere of 96vol% argon gas and 4vol% oxygen； The flow of the mixed gas of the 96vol% argon gas and 4vol% oxygen is 180 ~ 240 sccm.
- 9. the string-of-pearls-like SiC/SiO synthesized by the synthetic method described in any one of claim 1 ~ 82Heterojunction structure, its feature exist In described string-of-pearls-like SiC/SiO2Heterojunction structure is by including SiC nanowire inner core, the SiO being wrapped on SiC nanowire inner core2 Clad, and arranged distribution and SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball forms；Described bead string Shape SiC/SiO2In heterojunction structure, " line " of bead string is SiO2The SiC nanowire inner core of clad parcel, " pearl " of bead string be with SiO2Clad and the concentric SiO of SiC nanowire inner core2Ball.
- A kind of 10. string-of-pearls-like SiC/SiO according to claim 92Heterojunction structure, it is characterised in that the SiC nanowire A diameter of 10 ~ 50 nm of inner core；The SiO2A diameter of 200 ~ 400 nm of clad；The SiO2A diameter of the 500 of ball ~ 1500 nm。
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| CN112062573A (en) * | 2020-09-11 | 2020-12-11 | 郑州大学 | Sheet SiC-SiO2 composite material and preparation method thereof |
| CN115058885A (en) * | 2022-06-13 | 2022-09-16 | 西北工业大学 | Carbon fiber cloth surface oriented SiC nanowire array and preparation method thereof |
| CN115716759A (en) * | 2022-10-26 | 2023-02-28 | 南京工业大学 | Porous SiC nanowire film with high flexibility and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109437912A (en) * | 2018-12-05 | 2019-03-08 | 南昌航空大学 | A kind of preparation method of the silica in situ cladding silicon carbide nuclear-shell structured nano-composite material of morphology controllable |
| CN112062573A (en) * | 2020-09-11 | 2020-12-11 | 郑州大学 | Sheet SiC-SiO2 composite material and preparation method thereof |
| CN112062573B (en) * | 2020-09-11 | 2022-09-06 | 郑州大学 | Sheet SiC-SiO2 composite material and preparation method thereof |
| CN115058885A (en) * | 2022-06-13 | 2022-09-16 | 西北工业大学 | Carbon fiber cloth surface oriented SiC nanowire array and preparation method thereof |
| CN115058885B (en) * | 2022-06-13 | 2024-01-30 | 西北工业大学 | Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof |
| CN115716759A (en) * | 2022-10-26 | 2023-02-28 | 南京工业大学 | Porous SiC nanowire film with high flexibility and preparation method thereof |
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