CN103523785A - Preparation method of silicon and silicon doped nanosheet - Google Patents
Preparation method of silicon and silicon doped nanosheet Download PDFInfo
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- CN103523785A CN103523785A CN201310487829.4A CN201310487829A CN103523785A CN 103523785 A CN103523785 A CN 103523785A CN 201310487829 A CN201310487829 A CN 201310487829A CN 103523785 A CN103523785 A CN 103523785A
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Abstract
The invention discloses a preparation method of silicon and a silicon doped silicon doped nanosheet. The preparation method is characterized by comprising the steps of using bulk silicon or bulk silicon doped with elements as an anode and taking a tungsten rod or a molybdenum rod as a cathode, and regulating the distance between the two electrodes to be 10-30mm; vacuumizing a reaction chamber, and filling hydrogen and inert gas according to a certain proportion; connecting automatic control direct-current arc metal nano powder production equipment to a cooling water system, conducing power supply and arcing, and regulating current and the distance between the two electrodes to obtain stable arc; under a hydrogen plasma heat source, evaporating the anode to be in gaseous silicon atom state, thus forming an atom cluster and coagulating nano powder, wherein the atom cluster and the nano powder are deposited on the inner wall of the water-cooled reaction chamber or are delivered into a trapping chamber along a circulating airflow; after completely depositing the nano powder, carrying out passivation, then collecting the powder body, and implementing primary sieving, wherein the silicon nanosheet is 3-500nm in size and 1-5nm in thickness. According to the method, the process is simple, the cost is low, harmful substance does not exist, the yield is high, output is great, and industrial production can be realized.
Description
Technical field
The invention belongs to nano material preparing technical field, relate to the preparation method of a kind of silicon and dopen Nano sheet thereof.
Background technology
The material with two-dimensional nanostructure, has attracted increasing people's attention in recent years.Than zero dimension and monodimension nanometer material, two-dimensional nano material has more avtive spot, presents how effective surface, makes two-dimensional nano material show good application prospect in fields such as the energy, environment, microelectronics.
Geim and the Novosselov of 2004 Nian You Britain graceful Chester universities successfully prepare mono-layer graphite, i.e. Graphene.Graphene has many peculiar and excellent performances: as very high Young's modulus, thermal conductivity, carrier mobility and specific surface area etc.Also there is the phenomenons such as fractional quantum hall effect, quantum Hall ferromegnetism and exciton band gap.In fields such as energy storage, liquid crystal device, electron device, biomaterial, sensing material and support of the catalyst, show many premium propertiess.In worldwide, caused research boom, thus, two professors have obtained 2010 years Nobel Prizes in physics.Silicon and carbon belong to IV main group element together, there is similar structure and character, therefore, there is theoretical investigation prediction silicon to have (silene or silicon nanometer sheet) with individual layer or which floor silicon two-dirnentional structure form, and the physical and chemical performance with same excellence the same as Graphene.Silicon is a kind of modern industry semiconductor material of excellent performance, and reserves are abundant, the semiconductor material being most widely used at present, if can explore a kind of simple, controlled, mode is prepared silicon two-dirnentional structure material cheaply, will inevitably cause change of semiconductor industry.Scientific worker has made a large amount of theoretical investigationes and experimental exploring to monolayer silicon nanometer sheet, and expectation can search out the synthetic individual layer of a kind of effective approach or have the silicon two-dirnentional structure of several layers.
Silicon two-dirnentional structure mainly contains the silene of individual layer and the silicon nanometer sheet of multilayer, wherein the definition of silene (silicene) is first mentioned [K.Takeda and K.Shiraishi by Takeda and Shiraishi Theoretical Calculation in 1994 first, Phys.Rev.B50, 14916 (1994) .], and in 2007 by Guzman-Verri called after silicene[G.G.Guzma ' n-Verri and L.C.Lew Yan Voon, Phys.Rev.B76, 075131 (2007) .], Patrick Vogt in 2012 first experimentally high vacuum epitaxial deposition prepare the single layer structure [Phys.Rev.Lett. of silicon, 108, 155501 (2012)].At present, the method for preparing multilayer silicon nanometer sheet has graphene oxide masterplate method [Z.Y.Lu, J.X.Zhu, D.H.Sim, et al., Chem.Mater., 2011,23,5293], chemistry peels off silicide method [Michelle J.S.Spencer, Tetsuya Morishita, et al., Phys.Chem.Chem.Phys., 2011,13,15418 – 15422], chemical vapour deposition [U.Kim, I.Kim, Y.Park, et al., ACS Nano., 2011,5 (3), 2176] etc.But the preparation method of above-mentioned relevant silicon nanometer sheet, inevitably exists the problems such as complex process, product is impure, cost is expensive, the most fatal shortcoming is that output is extremely low, seriously limits the practical application of silicon nanometer sheet.The present invention adopts DC arc plasma evaporation technique (China Patent No.: 200410021190.1), take bulk silicon as raw material, prepare silicon nanometer sheet.This method has that the reaction times is short, technique is simple, purity is high, especially can accomplish scale production.Use solid block silicon, in reaction process, without other impurity introducings, realize the high purity of product and the controllability of particle characteristics.The silicon nanometer sheet powder body material that adopts the present invention to prepare can be applicable to lithium ion battery, solar cell, photodetection, photochemical catalysis contaminant degradation, photochemical catalysis CO
2reduction equal energy source environmental area.
China's granted patent: automatically control direct current arc metal nano powder production unit (ZL200410021190.1), its equipment consists of the powder generation chamber, powder granularity grading room, powder dust trapping chamber, powder handling chamber, pumped vacuum systems, gas recycle pump, hydraulic power actuating system, water-cooling system, the programming Control system that connect successively; Powder generates in chamber anode and negative electrode is installed, and is connected with programming Control system with external hydraulic transmission through powder generation locular wall; Powder granularity grading room is that double-walled water cooled housing and cooled with liquid nitrogen tank form; Hydraulic power actuating system is mobile by control cathode dimension and anode dimension moves hydraulic tank and transmission rod form.This equipment packs material into anode and becomes a part for anode, and with the gap of negative electrode formation 10-30mm, integral device vacuumizes, logical water coolant.Pass into after reactive gas and condensed gas, start starting the arc device and power supply, between yin, yang electrode, form electric arc, material start vaporizer also forms nano-powder.This equipment can be realized silicon nanometer sheet powder and produce in a large number.
Summary of the invention
The invention provides a kind of preparation method of silicon nanometer sheet, realize the preparation of mass-producing, highly purified silicon nanometer sheet powder, and the preparation of the controlled nano-powder material of phase composite, shape characteristic.
The present invention uses automatic control DC arc plasma equipment, using bulk silicon as raw material and as anode, and tungsten bar, as negative electrode, passes into the mixed gas of rare gas element and hydrogen, and evaporation raw material also obtains silicon nanometer sheet powder.Concrete steps are as follows:
(1) using buik silicon as anode, tungsten bar or molybdenum bar are negative electrode, regulate two interpole gaps at 10～30mm;
(2) reaction chamber is vacuumized, be filled with hydrogen and rare gas element.
(3) will automatically control direct current arc metal nano powder production unit and be connected with cooling water system, and switch on power and form stable electric arc;
(4) under hydrogen plasma Source, anode is evaporated to gas-phase silicon atomic state, forms elementide and is condensed on the reaction chamber wall that nano-powder is deposited on water-cooled, or being delivered in dust trapping chamber with circulating current.After nano-powder deposits completely, after passivation technology, collect powder, and tentatively sieve, obtain single-phase silicon nanometer sheet.
After the preliminary screening described in step (4), silicon nanometer sheet is of a size of 3-500nm at two-dimensional directional, individual layer silene thickness-5nm.
In step (2), described rare gas element is a kind of or its mixed gas in argon gas, helium, neon, and the air pressure of reaction chamber is 0.005MPa～0.09MPa, and described hydrogen is 1:1～9 with the air pressure of rare gas element ratio.
In step (1), described buik silicon is solid silicon or the silico briquette suppressed by silica flour, and the purity of its silicon is more than 97%.Other elements that can adulterate in buik silicon, its atomic mass concentration is no more than 3%.In buik silicon, can doped element be: alkali earth metal Be, Mg, Ca, Sr, Ba; Transition metal Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Re, Re, Ru, Os, Co, Rh, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd; Main Group Metal Elements Al, Ga, In, Tl, Ge, Sn, Pb, Sb, Bi; A kind of and several in thulium Sc, Y, Ce, Pr, Nb, Sm, Gd, Er, Tm, Yb, Lu.
The invention solves the difficult problem in the preparation of silicon two-dirnentional structure material.Silicon nanometer sheet, as a kind of two-dimensional nano material of novelty, can, for basic scientific research, also can be applicable to the fields such as the energy, environment.Preparation method of the present invention has that process is simple, solid feed is with low cost, do not produce objectionable impurities, and has that productive rate is high, turnout is large, can realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the images of transmissive electron microscope of the synthetic silicon nanometer sheet of embodiment 1.
Fig. 2 is the X-ray diffraction collection of illustrative plates of the synthetic silicon nanometer sheet of embodiment 1.
Fig. 3 is embodiment 2 gained silicon nanometer sheet Raman vibration collection of illustrative plates.
Fig. 4 is the cycle performance of lithium ion battery curve that embodiment 3 gained silicon nanometer sheet are made.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is further illustrated.
Embodiment 1:
Using high-purity silico briquette as anode, tungsten bar is negative electrode, adjusts two interpole gaps to 30mm.Reaction chamber is evacuated to approximately 10
-2pa, is filled with argon gas and hydrogen in the ratio of 2:1, reaches respectively 2 * 10
4pa and 1 * 10
4pa.Open cooling water system, switch on power and the starting the arc, adjusting electric current and two interpole gaps stabilising arc, evaporate block target, forms elementide and be gathered into nanometer sheet to be deposited in reaction chamber wall, through passivation technology, collects powder.
Embodiment 1 gained silicon nanometer sheet TEM image as shown in Figure 1, is shown as nano-sheet.
Embodiment 1 gained silicon nanometer sheet XRD figure spectrum as shown in Figure 2, is shown as single-phase silicon.
The thickness of embodiment 1 gained silicon nanometer sheet is about 1.5 nanometers.
Embodiment 2:
Using high-purity silico briquette as anode, tungsten bar is negative electrode, adjusts two interpole gaps to 30mm.Reaction chamber is evacuated to approximately 10
-2pa, is filled with helium and hydrogen in the ratio of 2:1, reaches respectively 2 * 10
4pa and 1 * 10
4pa.Open cooling water system, switch on power and the starting the arc, adjusting electric current and two interpole gaps stabilising arc, evaporate block target, forms elementide and be gathered into nanometer sheet to be deposited in reaction chamber wall, through passivation technology, collects powder.The silicon nanometer sheet preparing with respect to embodiment 1, in embodiment 2, the silicon nanometer sheet of preparation is more long and narrow, has banded pattern.
Embodiment 2 gained silicon nanometer sheet Raman collection of illustrative plates as shown in Figure 3, demonstrate the second order vibration performance peak of silicon two-dirnentional structure.
Embodiment 3:
By the silicon nanometer sheet of embodiment 1 preparation, conductive agent and Xylo-Mucine are more even than mixed grinding with the quality of 45:45:10, drip appropriate amount of deionized water, stir and obtain thick mud, are coated on the Copper Foil suppressing in advance 120 ℃ of dry 10h of vacuum.Then electrode slice is transferred to the glove box (Ar<0.1ppm, the O that are full of argon gas<sub TranNum="106">2</sub><0.1ppm) in, take lithium sheet as to electrode, electrolytic solution is 1M LiTFSI, and barrier film is Ceglard2400 microporous polypropylene membrane, is assembled into CR2025 type button half-cell.Adopt CHI660D-1 electrochemical workstation (Shanghai Chen Hua instrument company), carry out cyclic voltammetry, sweep velocity is 0.0001V/S, voltage range 0.01-2.5V.Employing Land CT2001A(Wuhan City Lan electricity Electronics Co., Ltd.) carry out cycle performance test, voltage range 0.01-1.2V.
The cycle performance of lithium ion battery curve that embodiment 3 gained silicon nanometer sheet are made as shown in Figure 4, stable cycle performance.
Embodiment 4:
Using high-purity silico briquette (99.999%) (containing 5 ‰ Fe, 2 ‰ Al, 0.2 ‰ Ti), respectively as anode, tungsten bar is negative electrode with doping silico briquette, adjust two interpole gaps to 30mm.Reaction chamber is evacuated to approximately 10
-2pa, is filled with argon gas and hydrogen in the ratio of 2:1, reaches respectively 2 * 10
4pa and 1 * 10
4pa.Open cooling water system, switch on power and the starting the arc, adjusting electric current and two interpole gaps stabilising arc, evaporate block target, forms elementide and be gathered into nanometer sheet to be deposited in reaction chamber wall, through passivation technology, collects respectively powder.
Photoelectric current test shows that the photoelectric current of silicon nanometer sheet prepared by HIGH-PURITY SILICON is about 1 μ A/cm
-2, the photoelectric current of doped silicon nanometer sheet prepared by the titanium doped silico briquette of iron aluminium is about 2 μ A/cm
-2, approximately improve 1 times.
Claims (10)
1. a preparation method for silicon and dopen Nano sheet thereof, uses the DC arc plasma equipment of automatically controlling, and its feature comprises the following steps,
(1) using buik silicon as anode, tungsten bar or molybdenum bar are negative electrode, regulate two interpole gaps at 10～30mm;
(2) reaction chamber is vacuumized, be filled with hydrogen and rare gas element.
(3) will automatically control direct current arc metal nano powder production unit and be connected with cooling water system, and switch on power and form stable electric arc;
(4) under hydrogen plasma Source, anode is evaporated to gas-phase silicon atomic state, forms elementide and is condensed on the reaction chamber wall that nano-powder is deposited on water-cooled, or being delivered in dust trapping chamber with circulating current; After nano-powder deposits completely, after passivation technology, collect powder, and tentatively sieve, obtain single-phase silicon nanometer sheet.
2. preparation method as claimed in claim 1, is characterized in that: after the preliminary screening described in step (4), silicon nanometer sheet is of a size of 3-500nm, thickness 1-5nm at two-dimensional directional.
3. preparation method as claimed in claim 1 or 2, is characterized in that, in step (1), described buik silicon is solid silicon or the silico briquette suppressed by silica flour, and the purity of its silicon is more than 97%.
4. preparation method as claimed in claim 3, is characterized in that, other elements that can adulterate in buik silicon, and doped element atomic mass concentration is no more than 3%; In buik silicon, can doped element be: alkali earth metal Be, Mg, Ca, Sr, Ba; Transition metal Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Re, Re, Ru, Os, Co, Rh, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd; Main Group Metal Elements Al, Ga, In, Tl, Ge, Sn, Pb, Sb, Bi; A kind of and several in thulium Sc, Y, Ce, Pr, Nb, Sm, Gd, Er, Tm, Yb, Lu.
5. the preparation method as described in claim 1,2,3 or 4, is characterized in that, in step (2), described rare gas element is a kind of or its mixed gas in argon gas, helium, neon.
6. the preparation method as described in claim 1,2,3 or 4, is characterized in that, the air pressure of reaction chamber is 0.005MPa～0.09MPa.
7. preparation method as claimed in claim 5, is characterized in that, the air pressure of reaction chamber is 0.005MPa～0.09MPa.
8. the preparation method as described in claim 1,2,3,4 or 7, is characterized in that, in step (2), described hydrogen is 1:1～9 with the air pressure of rare gas element ratio.
9. preparation method as claimed in claim 5, is characterized in that, in step (2), described hydrogen is 1:1～9 with the air pressure of rare gas element ratio.
10. preparation method as claimed in claim 6, is characterized in that, in step (2), described hydrogen is 1:1～9 with the air pressure of rare gas element ratio.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105399099A (en) * | 2015-11-17 | 2016-03-16 | 大连理工大学 | Preparation method of doped nano silicon material and application of doped nano silicon material in super photocapacitor field |
| CN108014783A (en) * | 2017-12-23 | 2018-05-11 | 马苗 | A kind of preparation method for colored dyes waste water composite nano materials of degrading |
| CN109225182A (en) * | 2018-09-04 | 2019-01-18 | 合肥工业大学 | A kind of ultra-thin silicon nanosheet photocatalyst and the preparation method and application thereof |
| CN109702344A (en) * | 2019-01-25 | 2019-05-03 | 大连理工大学 | Hot arc and laser composite heat power supply evaporate Multicarity nano powder preparing device |
| CN112496333A (en) * | 2020-11-26 | 2021-03-16 | 大连理工大学 | Preparation method and application of Si-Ti alloy nano powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399099A (en) * | 2015-11-17 | 2016-03-16 | 大连理工大学 | Preparation method of doped nano silicon material and application of doped nano silicon material in super photocapacitor field |
| CN108014783A (en) * | 2017-12-23 | 2018-05-11 | 马苗 | A kind of preparation method for colored dyes waste water composite nano materials of degrading |
| CN109225182A (en) * | 2018-09-04 | 2019-01-18 | 合肥工业大学 | A kind of ultra-thin silicon nanosheet photocatalyst and the preparation method and application thereof |
| CN109225182B (en) * | 2018-09-04 | 2021-07-23 | 合肥工业大学 | Ultrathin silicon nanosheet photocatalyst and preparation method and application thereof |
| CN109702344A (en) * | 2019-01-25 | 2019-05-03 | 大连理工大学 | Hot arc and laser composite heat power supply evaporate Multicarity nano powder preparing device |
| CN109702344B (en) * | 2019-01-25 | 2023-12-29 | 大连理工大学 | Thermal arc and laser composite heat source evaporation multi-cavity nano powder preparation device |
| CN112496333A (en) * | 2020-11-26 | 2021-03-16 | 大连理工大学 | Preparation method and application of Si-Ti alloy nano powder |
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Application publication date: 20140122 |