CN103232042B - Metastable amorphous silicon monoxide nanowire and preparation method thereof - Google Patents
Metastable amorphous silicon monoxide nanowire and preparation method thereof Download PDFInfo
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- CN103232042B CN103232042B CN201310160668.8A CN201310160668A CN103232042B CN 103232042 B CN103232042 B CN 103232042B CN 201310160668 A CN201310160668 A CN 201310160668A CN 103232042 B CN103232042 B CN 103232042B
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Abstract
The invention belongs to the technical field of silicon oxide and compounds thereof, and relates to a metastable amorphous silicon monoxide (SiO) nanowire and a preparation method thereof. The preparation method comprises the following steps: 1, placing a silicon carbide block material into high-temperature pipe furnace equipment, electrifying to perform heating operation, heating the silicon carbide to 1200-1600 DEG C under the condition that air is introduced, and keeping the temperature for 30-200 minutes; 2, introducing argon gas, discharging the air in the high-temperature pipe furnace, and simultaneously placing silicon powder on the heated silicon carbide material in the argon gas atmosphere, wherein the silicon powder contains iron powder having a mass ratio of 1/10000-1/1000; and 3, electrifying the high-temperature pipe furnace equipment again to perform heating operation, wherein the heating temperature is 1200-1600 DEG C, and the temperature keeping time is 30-300 minutes. The metastable amorphous silicon monoxide nanowire prepared by the method is regular in morphology, uniform in size and high in purity, and is in an amorphous state; the atomic ratio of the silicon element to the oxygen element is 1:1; and the diameter is 30-40 nanometers, and the length is 20-40 micrometers.
Description
Technical field
The invention belongs to silicon oxide and compound technical thereof, relate to a kind of metastable state amorphous silicon monoxide (SiO) nano wire and preparation method thereof.
Background technology
Nano material, as nano wire, nanotube, nanometer rod and nano flower etc. have caused the extensive concern of material supply section scholar.They have important application in a lot of fields, as sensor, light and electroluminescence device, energy transformation and storing device, intelligent exchange and self-cleaning material etc.Silicon monoxide itself has the optics of unique structural performance and excellence, catalysis and chemical property etc.; make it there is application prospect widely in fields such as catalysis, sensing, opticglass, opticinstrument protective membrane, lithium ion battery, semi-conductors, and synthesize the study hotspot that silicon monoxide nano material becomes Material Field.
At present, industrial production silicon monoxide at high temperature with after elemental silicon effect can cool rapidly and obtains by silicon-dioxide.By SiO
2content is SiO 2 powder and the mixing of coal-tar pitch powder of 99.5%, C/SiO
2mixing mol ratio is 2.0, and mixture is through heating under reduced pressure process, and its temperature is 1600 DEG C, and pressure is 1.013kPa, generates SiO steam, pass into argon gas through reduction reaction, SiO devaporation is carried, makes the silicon monoxide powder of less than 0.1 μm.Or pass through SiO
2with the common heat of Si or by H
2, CO reduction can obtain SiO gaseous molecular.The method that SiO molecule can be lowered the temperature by liquid helium is captured in the lattice of Ar crystal.The nanometer powder of what but these methods generally obtained is all SiO.
And adopting these methods such as solid sintering technology, atom deposition method, the nano wire of acquisition is all its composition of non-stoichiometric is SiO
x(1<x<2), and the SiO nano wire of stoichiometric ratio does not obtain, and meanwhile, generates Si and SiO because SiO is easy to that disproportionation occurs
2deng by product, arrive the material that purity is higher scarcely ever, thus the extreme influence chemical purity of SiO, thus limit the application of this material.
Summary of the invention
For the problems referred to above, the invention provides a kind of metastable state amorphous silicon monoxide (SiO) nano wire and preparation method thereof, preparation method of the present invention is simple, prepared metastable state amorphous silicon monoxide (SiO) nano wire specific surface area is large, pattern is regular, size uniformity, and purity is high.
For achieving the above object, the invention provides following technical scheme:
A preparation method for metastable state amorphous silicon monoxide nano wire, wherein, comprises the following steps:
Step 1: the carbofrax material of block is put into high-temperature tubular furnace apparatus electrified regulation, is heated to 1200-1600 DEG C of scope, and is incubated 30-200 minute under the condition passing into air by silicon carbide;
Step 2: pass into argon gas, discharges the air in high temperature process furnances, meanwhile, under the atmosphere of argon gas, is positioned over by silica flour above heated carbofrax material, and containing mass ratio in wherein said silica flour is the iron powder of 1/10000 to 1/1000;
Step 3: by high-temperature tubular furnace apparatus again electrified regulation, Heating temperature is 1200-1600 DEG C, soaking time 30-300 minute.
In described step 1, the Heating temperature of carbofrax material is 1300 DEG C-1500 DEG C.
In described step 1, the Heating temperature of carbofrax material is 1200 DEG C, 1400 DEG C or 1600 DEG C.
In described step 3, Heating temperature is 1300 DEG C-1500 DEG C.
In described step 3, Heating temperature is 1200 DEG C, 1400 DEG C or 1600 DEG C.
In described step 2, in described silica flour, the mass ratio of iron powder is 1/1000,1/5000 or 1/10000.
In described step 1, described soaking time is 30 minutes, 60 minutes or 300 minutes.
In described step 3, described soaking time is 30 minutes, 60 minutes or 300 minutes.
Described silicon carbide and described silica flour mass ratio are greater than 10:1, are less than 1000:1.
The granularity of described silica flour is 1-10 micron, and purity is greater than 99%.
Adopt the silicon monoxide nano wire prepared by aforementioned preparation process, wherein, described silicon monoxide nano wire is non-crystalline state, and diameter is 30-40 nanometer, and length is 20-40 micron, and wherein the atomic ratio of silicon and oxygen element is 1:1.
Compared with prior art, beneficial effect of the present invention is:
1, the preparation method of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention is simple, and easy to operate, raw material is easy to get, and is easy to large-scale industrial production.
2, in preparation method of the present invention, participate in react reactant can have very wide concentration range, be easy to realize large-scale industrial production.
3, preparation method of the present invention does not use toxicant, environmentally safe.
4, in preparation method of the present invention, do not need to add tensio-active agent, catalyzer etc., product is easy to be separated, and impurity is little, easily obtains highly purified product.
5, metastable state amorphous silicon monoxide nano wire pattern rule of the present invention, size uniformity, purity is high and be non-crystalline state, the atomic ratio of silicon and oxygen element is 1:1, and its diameter is 30-40 nanometer, and length is 20-40 micron.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph (SEM) of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention, and its enlargement ratio is 5000 times;
Fig. 2 is the electron scanning micrograph (SEM) of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention, and its enlargement ratio is 10000 times;
Fig. 3 is the energy spectrum analysis curve of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention;
Fig. 4 is the X ray diffracting spectrum (XRD) of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention;
Fig. 5 is the FTIR spectrum (FTIR) of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention;
Fig. 6 is the Raman spectrum (Raman) of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention;
Fig. 7 is the photoluminescence spectrum (PL) of metastable state amorphous silicon monoxide (SiO) nano wire of the present invention.
Embodiment
Below, by reference to the accompanying drawings with embodiment, further to explaining the present invention in detail.
Adopt preparation method of the present invention to prepare metastable state amorphous silicon monoxide (SiO) nano wire, key step is as follows:
(1) carbofrax material of block is put into high-temperature tubular furnace apparatus, by high temperature process furnances electrified regulation, silicon carbide is heated to 1400 DEG C under the condition of air, be incubated 60 minutes;
(2) pass at argon gas, the air in tube furnace discharged, meanwhile, under the atmosphere of argon gas, by a certain amount of silica flour (containing mass ratio be ten thousand/ iron powder, wherein iron powder is catalyzer) be positioned over above heated carbofrax material;
(3) again by high-temperature tubular furnace apparatus electrified regulation, temperature is 1500 DEG C, soaking time 60 minutes, and the white product that will obtain after cooling is taken out, obtain white product and be metastable state amorphous silicon monoxide (SiO) nano wire.
In the present embodiment, main generation is reacted as follows:
SiC+2O
2→SiO
2+CO
2
The metastable state amorphous silicon monoxide of this enforcement is tested as follows:
1. sem analysis
Fig. 1-2 is the electron scanning micrograph of the metastable state amorphous silicon monoxide nano wire of the present embodiment, and its enlargement ratio is respectively 5000 times and 10000 times.As can be seen from Fig. 1-2, gained nano material size uniformity, in wire, diameter is 30-40 nanometer, and length is 20-40 micron.
2. EDX analyzes
Fig. 3 is the energy spectrum analysis curve of the metastable state amorphous silicon monoxide nano wire of the present embodiment; Its test result is for shown in table 1.Adopt the composition of power spectrum EDX to material to detect, its Surface scan analytical results only finds Si and O two kinds of elements, and the atomic ratio of these two kinds of elements is 1:1, and the SiO nano wire for stoichiometric ratio of the material of preparation is described, is not SiO
2or SiO
xnano wire.
Table 1. power spectrum test result
| Element | Wt% | At% |
| OK | 37.19 | 50.97 |
| SiK | 62.81 | 49.03 |
| Matrix | Correction | ZAF |
3. XRD analysis
Fig. 4 is the X ray diffracting spectrum of metastable state amorphous silicon monoxide (SiO) nano wire of the present embodiment.As can be seen from Figure 4, there is obvious " steamed bun peak " in the diffraction peak of the nano material of preparation, illustrate that the nano material prepared is amorphous material, with document Enhanced cycleperformance of SiO-C composite anode for lithium-ion batteries, in Journal ofPower Sources 170 (2007) 456 – 459, the diffraction peak of the SiO powdered material of report is consistent, illustrates that the nano wire of synthesis is amorphous silicon monoxide (SiO).XRD detected result is that 1:1 is consistent with the atomic ratio of EDX analytical results Si and O above, and this just illustrates that the material of preparation is amorphous silicon monoxide (SiO) nano wire.
4. FTIR analyzes
Fig. 5: the FTIR collection of illustrative plates of high-purity amorphous silicon monoxide (SiO) nano wire
Fig. 5 is the FTIR spectrum of metastable state amorphous silicon monoxide (SiO) nano wire of the present embodiment, and as can be seen from Figure 5, the FTIR spectrogram of SiO nano wire has two absorption peaks in 800 and 1066nm place.And amorphous silica lateral optical phonon (TO) stretching vibration peak of FTIR spectrogram between 400 ~ 2000nm of typical amorphous silica: the peak at 482nm place is the rocking vibration absorption peak of Si-O-Si, the peak at 806nm place is the stretching vibration absorption peak of O-Si-O, and 1095nm place is the asymmetric stretching vibration absorption peak of Si-O; Stronger peak appears at 1095nm place, illustrates that the randomness of amorphous oxide silicon nanowires is strong.But the examination of infrared spectrum analysis of the SiO nano wire of the present embodiment, not typical amorphous silica FTIR spectrogram in peak corresponding, that is the SiO nano wire of the present embodiment is different from traditional nanometer silica line.
5. Raman analyzes
Fig. 6 is the Raman spectrum of metastable state amorphous silicon monoxide (SiO) nano wire of the present embodiment.As can be seen from Figure 6, the Raman spectrogram of SiO nano wire has two peaks in 321 and 378nm place.And the Raman spectrogram of typical amorphous silica is at 502nm.But the Raman spectrum test of the SiO nano wire of the present embodiment is analyzed, not typical amorphous silica Raman spectrogram in peak corresponding, that is the SiO nano wire of the present embodiment is different from traditional nanometer silica line.
6. PL analyzes
Fig. 7 is the photoluminescence spectrum of metastable state amorphous silicon monoxide (SiO) nano wire of the present embodiment.As can be seen from Figure 7, the PL spectrogram of SiO nano wire has two peaks in 421 and 520nm place.And the PL spectrogram of typical amorphous silica is at 700nm.But at present the PL spectrum test of the SiO nano wire of the present embodiment is analyzed, not typical amorphous silica PL spectrogram in peak corresponding, that is the SiO nano wire of the present embodiment is different from traditional nanometer silica line.
Can find from above-mentioned test result; adopt metastable state amorphous silicon monoxide (SiO) nano wire prepared by preparation method of the present invention; there are larger specific surface area, pattern rule, size more homogeneous; therefore; this metastable state amorphous silicon monoxide (SiO) nano wire is expected to there is potential using value in fields such as catalysis, sensing, opticglass, opticinstrument protective membrane, lithium ion battery, semi-conductors, has good application and industrialization prospect.
Claims (11)
1. the preparation method of a metastable state amorphous silicon monoxide nano wire, it is characterized in that: prepared silicon monoxide nano wire is non-crystalline state, diameter is 30-40 nanometer, and length is 20-40 micron, wherein the atomic ratio of silicon and oxygen element is 1:1, comprises the following steps:
Step 1: the carbofrax material of block is put into high-temperature tubular furnace apparatus electrified regulation, is heated to 1200-1600 DEG C of scope, and is incubated 30-200 minute under the condition passing into air by silicon carbide;
Step 2: pass into argon gas, discharges the air in high temperature process furnances, meanwhile, under the atmosphere of argon gas, is positioned over by silica flour above heated carbofrax material, and containing mass ratio in wherein said silica flour is the iron powder of 1/10000 to 1/1000;
Step 3: by high-temperature tubular furnace apparatus again electrified regulation, Heating temperature is 1200-1600 DEG C, soaking time 30-300 minute.
2. preparation method according to claim 1, is characterized in that: in described step 1, and the Heating temperature of carbofrax material is 1300 DEG C-1500 DEG C.
3. preparation method according to claim 1, is characterized in that: in described step 1, and the Heating temperature of carbofrax material is 1200 DEG C, 1400 DEG C or 1600 DEG C.
4. preparation method according to claim 1, is characterized in that: in described step 3, and Heating temperature is 1300 DEG C-1500 DEG C.
5. preparation method according to claim 1, is characterized in that: in described step 3, and Heating temperature is 1200 DEG C, 1400 DEG C or 1600 DEG C.
6. preparation method according to claim 1, is characterized in that: in described step 2, and in described silica flour, the mass ratio of iron powder is 1/1000,1/5000 or 1/10000.
7. preparation method according to claim 1, is characterized in that: in described step 1, and described soaking time is 30 minutes or 60 minutes.
8. preparation method according to claim 1, is characterized in that: in described step 3, and described soaking time is 30 minutes, 60 minutes or 300 minutes.
9. preparation method according to claim 1, is characterized in that: described silicon carbide and described silica flour mass ratio are greater than 10:1, are less than 1000:1.
10. preparation method according to claim 1, is characterized in that: the granularity of described silica flour is 1-10 micron, and purity is greater than 99%.
11. 1 kinds adopt the silicon monoxide nano wire prepared by preparation method according to claim 1, and it is characterized in that: described silicon monoxide nano wire is non-crystalline state, diameter is 30-40 nanometer, and length is 20-40 micron, and wherein the atomic ratio of silicon and oxygen element is 1:1.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740094A (en) * | 2005-06-23 | 2006-03-01 | 复旦大学 | Synthesis of nanometer single-crystal silica line |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740094A (en) * | 2005-06-23 | 2006-03-01 | 复旦大学 | Synthesis of nanometer single-crystal silica line |
Non-Patent Citations (2)
| Title |
|---|
| Synthesis and photoluminescence of aligned SiOx nanowire arrays;G.W. Meng;《Applied Physics A》;20031231;第76卷;第119-121页 * |
| 梁训裕等.碳化硅耐火材料.《碳化硅耐火材料》.1981, * |
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