CN105439148A - Preparation method of silene - Google Patents
Preparation method of silene Download PDFInfo
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- CN105439148A CN105439148A CN201510793100.9A CN201510793100A CN105439148A CN 105439148 A CN105439148 A CN 105439148A CN 201510793100 A CN201510793100 A CN 201510793100A CN 105439148 A CN105439148 A CN 105439148A
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- silene
- sputtering
- preparation
- cluster
- negative ion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
The invention provides a method for preparing silene. The method specifically comprises: processing silicon blocks into a concave tapered silicon target; mounting the silicon target on a sputtering target of a cesium sputtering negative ion source; sputtering the silicon target by using cesium ions; leading out Si<2-> cluster negative ion beams generated by sputtering from extraction electrode extraction holes, wherein Si<2-> cluster negative ions are uniformly deposited on an Ag (111) substrate through scanning electric field after being accelerated by extraction electrode voltage; and putting a sample into a vacuum chamber, sputtering the surface of the sample by Ar<+> ions, and then carrying out annealing treatment on the sample in an ultrahigh vacuum to finish the preparation of silene. According to the preparation method provided by the invention, by using the advantages of low energy of a single atom of low-energy cluster negative ion beams, and an accurate and controllable dose, the silene can be prepared directly by virtue of a direct deposition method.
Description
Technical field
The present invention relates to a kind of crystalline material, be specially method prepared by silene.
Background technology
Silene is a kind of Siliciumatom is the two-dimension nano materials that planar honeycomb shape arranges, and has good two dimensional crystal structure and electrical properties.Compared with the Graphene of zero band gap, silene has certain energy gap, therefore has wide practical use at semi-conductor electronic device and field of optoelectronic devices.The method preparing silene at present has epitaxy and ion injection method.
(1) epitaxy.Prepare silene in the world first and namely use this method, be i.e. silicon source evaporation epitaxial growth method.The special stratiform structural requirement of silene uses the specialized substrates materials such as silver-colored monocrystalline.But, when the atom evaporated is at substrate Epitaxial growth silene, owing to being subject to stronger interfacial interaction, silene there will be reconstruct, atomic shell warpage degree changes, some atom can rise, and some atom can decline, and causes structure cell to become large, symmetry reduces, or form few layer (few-layer) structure, thus destroy the dirac-fermi characteristic energy of silene, affect the performance of silene film material.
(2) ion beam.Draw cluster ions bundle by ion source, be injected into substrate material surface layer, through suitable thermal treatment, guide atom to separate out and nucleating growth, form individual layer or few layer two-dimensional material.Because the minority such as carbon, silicon element can form larger cluster ions line, therefore, ion beam can be used for the preparation of Graphene and silene.
On the other hand, the cluster ions bundle that ion source is drawn can also slow down, and forming energy, at the ultra-low energy cluster ions bundle of below 10eV/atom, is deposited directly to substrate surface and forms two-dimensional material.
The feature of cluster ions bundle is energy, the deposit dose controllable precise of atom, and the cluster ions arriving at substrate surface has single size, quality and energy, therefore can obtain the ultra-thin two-dimension material that thickness, degree of crystallinity are controlled.
Summary of the invention
The object of the present invention is to provide a kind of method preparing silylene material, high-purity silicon target is sputtered with cesium ion, produce the cluster negative ion beam of silicon, by the ionogenic target sputtering current of optimizing regulation, ionic fluid extraction voltage, obtain the silicon clusters negative ion of larger line, through magnetic core logical circuit deflection (quality choice) and two-dimensional electrostatic scanning, be injected into monocrystalline Ag (111) substrate surface.Then anneal in ultrahigh vacuum(HHV), the Siliciumatom being infused in substrate surface layer is reconstructed at Ag substrate surface, forms silene.
The present invention in order to achieve the above object, devises a kind of device preparing silylene material, and it forms primarily of ion source, scanning device, deposition target chamber and vacuum system.Ion source, scanning device, deposition target chamber are connected successively, are among vacuum system.The silicon clusters ionic fluid that ion source produces, obtains negative ion beam scanning on substrate, forms the even silene film of thickness.Principle sketch is as Fig. 1.
In order to improve silicon clusters line, sputtering target adopts specific recessed conical design (cone angle 45-60 degree, is shown in Figure of description 3), increases line and focuses on double effects, and adopting high-purity silico briquette to be processed into target, export with the line realizing optimizing to reach.
Ion source of the present invention is by caesium stove, ionization device, silicon target, a few part of extraction electrode is formed, ion source principle of work: the liquid metal caesium in caesium stove evaporates under heat effect, the surface of the concave type ionization device that the armouring tantalum wire that the caesium steam arrival big current produced heats is coiled into, the gas molecule of cold caesium runs into hot tantalum wire and ionizes, the cesium ion produced accelerates toward target motion under negative target voltage effect, Siliciumatom in target is spilt with the form of cluster negative ion, cluster negative ion accelerates toward extraction electrode motion under an extraction electrode negative voltage effect higher than target current potential, cluster negative ion draws [seeing Figure of description 2] by extraction electrode the most at last.
The present invention is using high-purity silicon target as sputtering target, and sputtering voltage Vsp is 5-6kV; The cluster negative ion beam of the silicon that sputtering produces is drawn by extraction electrode fairlead, probe voltage V
eXbe generally 10-20kV.The Si drawn
1-Si
7corresponding Cluster Beam as shown in Figure 4, V
eX=20.0kV.
Scanning device of the present invention adopts electrostatic scanning mode, and by 0-15kV continuously adjustable two-way choppy sea power drives, realize the Uniform Scanning of ionic fluid in XY direction, scanning device is arranged in the vacuum box between two 45 degree of magnet.
The preparation method of silene of the present invention, comprises the following steps:
(1) preparation of silicon target:
By purity be 99.9% silico briquette be processed into silicon target through workshop, the shape of silicon target is concave cone shape;
(2) silicon clusters ionic fluid is drawn:
Be arranged on sputtering target by above-mentioned silicon target, controlling the heating current 20-28A of tantalum wire, the sputtering voltage of sputtering silicon target is 5-6kV, and probe voltage is under the condition of 10-20kV, sputters silicon target with cesium ion, the Si that sputtering produces
2 -cluster negative ion beam is drawn by extraction electrode fairlead;
(3) cluster ion implantation:
By Si
2 -cluster negative ion beam is injected in monocrystalline Ag (111) substrate, forms silene;
(4) sputtering and anneal:
The sample injected is put to 2 × 10
-3-5 × 10
-3in vacuum chamber, with the Ar of 600eV
+ion pair surface sputters, to remove surface contaminant, then 8 × 10
-9-2 × 10
-8carry out anneal to sample under the ultrahigh vacuum(HHV) of Pa, annealing temperature is 400-500 DEG C, can complete the preparation of silene.
The angle of the bevel angle of the concave cone shape of described sputtering silicon target is 45-60
°, sputtering silicon target length is 15mm, and diameter is 7mm.
In step (2), the Si sputtered
2 -the energy of cluster negative ion beam is 5-20keV.Si
2 -cluster negative ion beam is Si
1-Si
7cluster Beam.
In step (3), the size of monocrystalline Ag (111) substrate is 5 × 5mm
2.
In step (3), Si
2 -cluster negative ion beam implantation dosage is 2 × 10
15atoms/cm
2.
In step (4), the vacuum tightness of sputtering is 4 × 10
-3; The vacuum tightness of annealing is 10
-8pa; Annealing temperature is 450 DEG C.
The invention has the beneficial effects as follows and provide a kind of method preparing silene, its advantage is; (1) number of the Siliciumatom injected can be read by line totalizing instrument, thus the silene thickness controllable precise of preparation; (2) can at room temperature deposit; (3) the good film of homogeneity can be prepared under scan action.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention schematic diagram.1. negative cluster beam, 2. scanning electric field, 3. specimen holder, 4. retarding field, 5. line totalizing instrument.
Fig. 2 is ionogenic structure iron of the present invention.6. caesium stoves, 7. ionization device, 8. refrigerant, 9. silicon target, 10. cathode insulation in figure.
The schematic shapes of the sputtering target of Fig. 3 designed by the present invention.
Fig. 4 is the Si that the sputtering of this device produces
1-Si
7corresponding Cluster Beam.
The XPS figure of the silicon fiml of Fig. 5 prepared by this device.Wherein (a) is that figure, (b) after 400 DEG C of sputterings are 450 DEG C of annealing figure, (c) is 500 DEG C of annealing figure.
The LEED figure of the silicon fiml of Fig. 6 prepared by this device.Wherein (a) is 400 DEG C of annealing figure, (b) be 450 DEG C of annealing figure, (c) is 500 DEG C of annealing figure.
Embodiment
Embodiment 1
Because the beam intensity of the negative ion of drawing can directly have influence on ion implantation efficiency, so necessary optimization sputtering line.Common planar shaped target is comparatively strong to the scattering process of the negative ion of sputtering, causes the beam intensity of extraction more weak.If the Front-end Design of target become cone angle to be 45-60
oconcave cone shape (see accompanying drawing 3), then the scattering process in sputter procedure is weakened, and focussing force is greatly enhanced, thus increases negative ion line.Experiment proves, when other conditions are identical, adopt the concave cone shape sputtering target designed in the present invention, the beam intensity of drawing in deposition target chamber will exceed about order of magnitude than with common planar targets, this will significantly promote ion implantation efficiency, especially atomicity is greater than to the cluster negative ion injection of 4.
Present method obtains Si
1-Si
7cluster, the relation of its line and cluster size as shown in Figure 4, wherein Si
2line reach 3.5 microamperes, Si
7reach 3nA, all can meet the requirement of silene deposition to amount of ions.
Be the Si of 10keV by energy
2 -ion cluster is injected on monocrystalline Ag (111) substrate, and implantation dosage is 2 × 10
15atoms/cm
2, this dosage is equivalent to the silene rete of two layers of thickness.Previous experiments proves, if inject the atom dosage (1 × 10 corresponding to individual layer silene thickness
15atoms/cm
2), because the Siliciumatom injected has certain depth profile, and the diffusion of Siliciumatom can be carried out to substrate surface on the one hand in annealing process, then carry out to the direction deviating from surface on the other hand, so the Siliciumatom number deficiency arriving Ag (111) surface can be caused to form individual layer silene, thus we have selected larger implantation dosage.
After cluster ion implantation completes, the sample of injection is put into the chamber of scanning tunnel microscope (STM) device systems, with the Ar of 600eV
+carry out sputter process to sample surfaces, to remove pollutent and the adsorptive on surface, during sputtering, the vacuum tightness of chamber is 4 × 10
-3pa.In this chamber, anneal is carried out to sample immediately, annealing temperature is 400-500 DEG C, the main purpose of this annealing process is: make the Siliciumatom of injection be diffused into substrate surface on the one hand, nearly surface is made on the other hand to reconstruct because of the silver atoms upset by ion implantation bombardment, be restored to Ag (111) structure, promote that silene produces on its surface.
While annealing process is carried out, we have carried out the measurement of x-ray photoelectron power spectrum (XPS) and low-energy electron diffraction spectrum (LEED) to sample, the results are shown in accompanying drawing 5 and Fig. 6.As can be seen from LEED collection of illustrative plates, the point diffraction in figure is less, and show that the anneal of 400 DEG C fails to form silene, surface tissue still locates confusion.When annealing temperature rises to 450 DEG C, point diffraction obviously increases, and shows that this temperature is conducive to silver atoms greatly at surface reconstruction.When annealing temperature continues to rise to 500, point diffraction has no and continues to increase, and infers 450 thus
oc is the optimum temps that reconstruct occurs Ag (111) substrate, is beneficial to the growth of silene.Corresponding Si-Si bond and Ag-Si key is also been observed in XPS spectrum.
Claims (8)
1. a preparation method for silene, is characterized in that, comprises the steps:
The preparation of silicon target:
(1) by purity be 99.9% silico briquette be processed into silicon target through workshop, the shape of silicon target is concave cone shape;
Draw silicon clusters ionic fluid:
(2) above-mentioned silicon target is arranged on the sputtering target of caesium sputter negative ion source, sputters silicon target with cesium ion, the Si that sputtering produces
2 -cluster negative ion beam is drawn by extraction electrode fairlead;
Cluster ion implantation:
(3) monocrystalline Ag (111) substrate is placed in the sample table in deposition target chamber, Si
2 -cluster negative ion is deposited on Ag (111) substrate through overscanning electric fields uniform after accelerating through probe voltage;
(4) sputtering and anneal:
The sample injected is put under scanning tunnel microscope, in control 2 × 10
-3-5 × 10
-3vacuum chamber in, with the Ar of 600eV
+ion pair surface sputters, to remove surface contaminant, then 8 × 10
-9-2 × 10
-8carry out anneal to sample under the ultrahigh vacuum(HHV) of Pa, annealing temperature is 400-500 DEG C, can complete the preparation of silene.
2. the preparation method of silene according to claim 1, is characterized in that, the angle of the bevel angle of the concave cone shape of sputtering silicon target is 45-60
°, sputtering silicon target length is 15mm, and diameter is 7mm.
3. the preparation method of silene according to claim 1, is characterized in that, in step (2), the heating current of the tantalum wire in ion source controls as 20-24A, and the sputtering voltage of sputtering silicon target is 5-6kV, and probe voltage is under the condition of 10-20kV.
4. the preparation method of silene according to claim 1, is characterized in that, in step (2), and the Si sputtered
2 -the energy of cluster negative ion beam is 5-20keV.
5. the preparation method of silene according to claim 1, is characterized in that, in step (3), the size of monocrystalline Ag (111) substrate is 5 × 5mm
2.
6. the preparation method of silene according to claim 1, is characterized in that, in step (3), and Si
2 -cluster negative ion beam implantation dosage is 2 × 10
15atoms/cm
2.
7. the preparation method of silene according to claim 1, is characterized in that, in step (4), the vacuum tightness of sputtering is 4 × 10
-3; The vacuum tightness of annealing is 10
-8pa; Annealing temperature is 450 DEG C.
8. the preparation method of silene according to claim 1, is characterized in that, Si
2 -cluster negative ion beam is Si
1-Si
7cluster Beam.
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| CN201510793100.9A CN105439148B (en) | 2015-11-18 | 2015-11-18 | A kind of preparation method of silene |
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| CN105439148B CN105439148B (en) | 2018-01-05 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105841852A (en) * | 2016-05-30 | 2016-08-10 | 华中科技大学 | Doping silylene based MEMS piezoresistive pressure sensor and manufacturing method thereof |
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| CN102732834A (en) * | 2012-06-18 | 2012-10-17 | 徐明生 | Apparatus for preparing two-dimensional nanometer film |
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-
2015
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Patent Citations (3)
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| CN102373433A (en) * | 2011-11-21 | 2012-03-14 | 武汉大学 | Method for preparing ultrathin carbon film by using carbon cluster ion beam |
| CN102732834A (en) * | 2012-06-18 | 2012-10-17 | 徐明生 | Apparatus for preparing two-dimensional nanometer film |
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Non-Patent Citations (4)
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|---|
| BAOJIE FENG ET AL.: "observation of dirac cone warping and chirality effects in silicene", 《ACSNANO》 * |
| X.M.WANG ET AL.: "small cluster ions from source of negative ions by cesium sputtering", 《NUCLEAR INSTRUMENTS AND METHOD IN PHYSICS RESEARCH B》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105841852A (en) * | 2016-05-30 | 2016-08-10 | 华中科技大学 | Doping silylene based MEMS piezoresistive pressure sensor and manufacturing method thereof |
| CN105841852B (en) * | 2016-05-30 | 2018-08-03 | 华中科技大学 | A kind of MEMS piezoresistive pressure sensor and its manufacturing method based on doping silene |
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| CN105439148B (en) | 2018-01-05 |
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Effective date of registration: 20211116 Address after: 430070 room 1-102, special zone, building 1, Wuhan Putian Science Park, No. 20, University Park Road, Donghu New Technology Development Zone, Wuhan, Hubei Province Patentee after: Wuhan newfeige Nano Technology Co.,Ltd. Address before: 443500 Changyang Innovation Industrial Park, Yichang City, Hubei Province Patentee before: YICHANG HOUHUANG VACUUM TECHNOLOGY Co.,Ltd. |
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