CN108689432A - A method of growing rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer - Google Patents
A method of growing rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer Download PDFInfo
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- CN108689432A CN108689432A CN201810580833.8A CN201810580833A CN108689432A CN 108689432 A CN108689432 A CN 108689432A CN 201810580833 A CN201810580833 A CN 201810580833A CN 108689432 A CN108689432 A CN 108689432A
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- C01G47/00—Compounds of rhenium
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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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of in the silicon base of non-oxidation layer grows the method for rhenium disulfide nanometer sheet.Described method includes following steps:S1. it cleans silicon base and is pre-processed;S2. in multi-temperature zone tube furnace, in two neighboring warm area, respectively there are one aluminium oxide boats;Wherein, the spacing distance of two aluminium oxide boats is 20~30cm, and sulphur source is placed in the center of upstream warm area aluminium oxide boat, and rhenium source is placed in the downstream edge of downstream warm area aluminium oxide boat, silicon base growth is face-down, is 0~1cm at a distance from the downstream edge of downstream warm area aluminium oxide boat;S3. inert gas is then passed through into double temperature-area tubular furnaces, heating is reacted, you can rhenium disulfide nanometer sheet is grown in the silicon base of non-oxidation layer.The present invention is rhenium source by sulphur source, rhenium trioxide of sublimed sulfur, with chemical vapor infiltration, by adjusting the position in rhenium source and silicon base in the distance and downstream warm area in sulphur source and rhenium source, you can directly grow rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer.
Description
Technical field
The present invention relates to technical field of nanometer material preparation more particularly to a kind of growing two in the silicon base of non-oxidation layer
The method of sulfuration rhenium nanometer sheet.
Background technology
Two-dimentional transient metal chalcogenide compound(TMDs)With graphene similar structures, possess excellent electricity, optics, magnetic
The performances such as, mechanics become one of the hot spot of current material science research.Rhenium disulfide(ReS2)It is this material man in recent years
One " nova " in race, with most of studied same type of material with high lattice symmetry(Such as MoS2,WS2Deng)Performance
Go out isotropism difference, due to the presence for sending Butterworth to distort, ReS2The asymmetry degree higher in structure has unique torsion
Bent 1T phases, to make it that there is anisotropic in electrical properties and optical property.And ReS2Make with very weak layer coupling
With so that no matter single layer or multilayer ReS2It is direct band gap, the influence of the variation of the number of plies to its band structure is little.These
Unique feature allows it to have huge potential application value in the fields such as photoelectric device and catalysis production hydrogen.
All the time, the silicon semi-conducting material one of most abundant as earth content, with good band gap width,
Electrical properties and optical property are excellent, are often combined with other compounds and are used in the fields such as photoelectric device and catalysis production hydrogen,
And achieve some all well and good achievements.And currently, ReS2Nanometer sheet is only capable of in silica, mica, goldleaf, graphene etc.
It is synthesized on material, to the ReS that will synthesize on these substrates2Photoelectric device or catalysis production hydrogen applied to silicon substrate
Etc., it is required to be transferred to target substrate by various means, this unquestionable process can be to its pattern, structure etc.
It can damage, while bring some unnecessary troubles.Therefore, ReS2Application in these areas has received a degree of
Limitation.If a large amount of biology ReS can directly be grown in non-oxidation layer silicon base2Material, and preparation method is easy to operate, stream
Journey is few, efficient, reproducible, will be to ReS2Application have broad prospects.
Invention content
The purpose of the present invention is to provide a kind of in the silicon base of non-oxidation layer grows the method for rhenium disulfide nanometer sheet.
The method of the invention is with chemical vapor infiltration, by adjusting the position in rhenium source and silicon base in the second warm area, i.e., by rhenium source
Position be adjusted to the downstream edge of aluminium oxide boat, and silicon base is placed in the downstream edge of the aluminium oxide boat in rhenium source, ensures silicon
Substrate is at a distance from the seamless contact of downstream edge of aluminium oxide boat or 0.4 times only no more than silicon base bond length, you can
Rhenium disulfide nanometer sheet is grown in the silicon base of non-oxidation layer, is overcome rhenium disulfide nanometer sheet and is difficult in non-oxidation layer(Two
Silica)Silicon base on the problem that directly grows, the application for developing rhenium disulfide nanometer sheet has great importance.
The above-mentioned purpose of the present invention is achieved by following scheme:
A method of it growing rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer, is prepared using chemical vapor infiltration,
Include the following steps:
S1. it cleans silicon base and is pre-processed;
S2. in multi-temperature zone tube furnace, the aluminium oxide boat for holding sublimed sulfur is placed in upstream warm area, holds the oxidation of rhenium trioxide
Aluminium boat is placed in the center of downstream warm area, and the spacing distance of two aluminium oxide boats is 20~30cm, and rhenium trioxide is located at oxidation
The downstream edge of aluminium boat, silicon base are placed in the upper edge of rhenium trioxide warm area aluminium oxide boat, and silicon base growth is face-down, silicon base with
Distance between the downstream edge of rhenium trioxide warm area aluminium oxide boat is no more than 0.4 times of silicon base bond length;
S3. inert gas is then passed through into double temperature-area tubular furnaces, heating is reacted, you can in the silicon base of non-oxidation layer
Upper growth rhenium disulfide nanometer sheet.
The present invention is rhenium source by sulphur source, rhenium trioxide of sublimed sulfur, by adjusting the relative position of sulphur source and rhenium source, and
The position in rhenium source and silicon base in the warm area of downstream grows rhenium disulfide with chemical vapor infiltration in the silicon base of non-oxidation layer
Nanometer sheet.Inventor chances on the distance by controlling sulphur source and rhenium source, and by the position tune in rhenium source by multiple experiment
The whole downstream edge for aluminium oxide boat, silicon base are placed in the downstream edge of the aluminium oxide boat in rhenium source, ensure silicon base and aluminium oxide
The seamless contact of downstream edge of boat or 0.4 times of distance for being only no more than silicon base bond length, you can in non-oxidation layer
Rhenium disulfide nanometer sheet is grown in silicon base, is overcome rhenium disulfide nanometer sheet and is difficult in the silicon base of non-oxidation layer directly give birth to
Long problem.
The silicon base of non-oxidation layer of the present invention, which refers to silicon substrate surface, does not have the presence of silica.The silicon base
Generally rectangular, short side refers to the shorter one side of length, is typically referred to after silicon base is positioned on the aluminium oxide boat in rhenium source, with
The parallel side of the axis of aluminium oxide boat.
The downstream of the aluminium oxide boat refers to distinguishing upstream and downstream using the flow direction of inert protective gas as standard, three
Rheium oxide is located at the downstream edge of aluminium oxide boat, refers to one end that rhenium trioxide is located remotely from sulphur source;The silicon base and three oxygen
Change 0.4 times that the distance between the downstream edge of rhenium warm area aluminium oxide boat is no more than silicon base bond length, refers to that silicon base is located at
The one end of rhenium source aluminium oxide boat far from sulphur source, and between its one end of one side far from sulphur source and rhenium source aluminium oxide boat far from sulphur source
Vertical range is no more than 0.4 times of silicon base bond length.
Preferably, in step S2 the mole dosage of sublimed sulfur far more than rhenium trioxide.So that rhenium disulfide nanometer sheet is in nothing
What is grown in the silicon base of oxide layer is more preferable.
Preferably, the inert gas in step S3 is argon gas or nitrogen;The heating process is:The temperature of upstream warm area is
10~50 DEG C, keep 0~20 min;Then 180~300 DEG C are warming up to through 0~10min and keep 30~70min;Downstream warm area
Temperature be 10~50 DEG C through 20~40min be warming up to 600~900 DEG C and keep 5~50min
Preferably, heating process described in step S3 is:The temperature of upstream warm area is 30 DEG C, keeps 10min;Then it heats up through 3min
To 180 DEG C and keep 50min;The temperature of downstream warm area is 30 DEG C and is warming up to 700 DEG C through 23min and keeps 40min.
Preferably, the air-flow of inert gas is 0~200sccm in step S3.
Preferably, the air-flow of inert gas is 50sccm in step S3.
Preferably, silicon base process is cleaned in step S1 is:Silicon base is each according to the sequence of acetone, ethyl alcohol, deionized water
It is cleaned by ultrasonic 5~60min, 150~300W of ultrasonic power, 10~60KHz of frequency.
Preferably, silicon base process is cleaned in step S1 is:Silicon base is each according to the sequence of acetone, ethyl alcohol, deionized water
It is cleaned by ultrasonic 10min, ultrasonic power 180W, frequency 40KHz.
Preferably, the process of pretreatment silicon base is in step S1:Cleaned silicon chip is impregnated in etching solution and is removed
The oxide layer on surface is gone, then deionized water is rinsed, and inert gas is used in combination to dry up.
Preferably, the etching solution is hydrofluoric acid solution, potassium hydroxide solution or sodium hydroxide solution.
Preferably, the process that is passed through of inert gas is in step S3:High purity inert gas 10 is first led to the flow of 500sccm
Min is then evacuated to 1*10-4Pa, then it is logical such as inert gas normal pressure.First lead to the inert gas such as high-purity, to exclude dual temperature
Oxygen in area's tube furnace, then vacuumizes again, further empties the oxygen in stove, to ensure that oxygen is not present in stove, with
Just growing state of the rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer is influenced.
Compared with prior art, the invention has the advantages that:
The present invention is rhenium source by sulphur source, rhenium trioxide of sublimed sulfur, with chemical vapor infiltration, by adjusting sulphur source and rhenium source
The position in rhenium source, i.e., is adjusted to the downstream edge of aluminium oxide boat by the position in rhenium source and silicon base in distance and downstream warm area,
And silicon base is placed in the downstream edge of the aluminium oxide boat in rhenium source, ensure silicon base and the downstream edge of aluminium oxide boat is seamless contacts
Or only no more than 0.4 times of silicon base bond length, you can rhenium disulfide nanometer sheet is grown in the silicon base of non-oxidation layer,
It overcomes rhenium disulfide nanometer sheet and is difficult to the problem directly grown in the silicon base of non-oxidation layer, development rhenium disulfide is received
The application of rice piece has great importance.
Description of the drawings
Fig. 1 is the flow diagram of the method for the present invention that rhenium disulfide nanometer sheet is grown in the silicon base of non-oxidation layer
It is intended to.
Fig. 2 be the method for the invention in sulphur source, rhenium source and silicon base position relationship schematic diagram.
Fig. 3 is the SEM figures of the rhenium disulfide nanometer sheet grown in the silicon base of non-oxidation layer prepared by embodiment 1, is put
Big multiple is 10000 times.
Fig. 4 is the SEM figures of the rhenium disulfide nanometer sheet grown in the silicon base of non-oxidation layer prepared by embodiment 1, is put
Big multiple is 50000 times.
Fig. 5 is the SEM figures of the rhenium disulfide nanometer sheet grown in the silicon base of non-oxidation layer prepared by embodiment 1, is put
Big multiple is 100000 times.
Fig. 6 is the Raman spectrum of the rhenium disulfide nanometer sheet grown in the silicon base of non-oxidation layer prepared by embodiment 1
Figure.
Fig. 7 is the XPS of Re in the rhenium disulfide nanometer sheet grown in the silicon base of non-oxidation layer prepared by embodiment 1
Figure.
The XPS figures that Fig. 8 is S in the rhenium disulfide nanometer sheet grown in the silicon base of non-oxidation layer prepared by embodiment 1.
Fig. 9 is the SEM figures for the rhenium disulfide nanometer sheet that silicon base is prepared when position on aluminium oxide boat is improper.
Specific implementation mode
The present invention is made with reference to specific embodiment and further being elaborated, the embodiment is served only for explaining this
Invention, is not intended to limit the scope of the present invention.Test method used in following embodiments is normal unless otherwise specified
Rule method;Used material, reagent etc., unless otherwise specified, for the reagent and material commercially obtained.
Embodiment 1
1, a kind of method growing rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer, is carried out using chemical vapor infiltration
It prepares, preparation flow is as shown in Figure 1.
Material utilization amount is:500 mg sublimed sulfurs(Aladin, 99.99%), 1.5 mg ReO3(Aladin, 99.9%);Hydrogen fluorine
Acid(Tianjin great Mao chemical reagent factories), three-temperature-zone tube furnace(Hefei Ke Jing Materials Technology Ltd., OTF-1200X- III),
Argon gas(Purity is 99.999%).
Specific preparation process is as follows:
(1)Clean silicon base:The small pieces that the round silicon chip that non-oxidation layer is commercialized is cut into 2.5 cm*2.5 cm, are then pressed
Respectively it is cleaned by ultrasonic 10 min, 180 W of ultrasonic power, 40 KHz of frequency according to the sequence of acetone, ethyl alcohol, deionized water.
(2)The pretreatment of silicon base:In certain density hydrofluoric acid solution(Tianjin great Mao chemical reagent factories)In, it will be clear
Washed silicon chip impregnates 5 min to remove a small amount of surface oxide layer, is then rinsed repeatedly with the sharp mouth bottle equipped with deionized water
Silicon chip for several times, is used in combination elevated pressure nitrogen air gun quickly to dry up.
(3)Chemical vapour deposition reaction:Fill sulphur source aluminium oxide boat be placed on inlet end away from first warm area center at;It contains
There is the aluminium oxide boat in rhenium source to be placed on second warm area center;The distance of two aluminium oxide boats is 30cm;Rhenium source is placed on oxidation
The top of aluminium boat, close to downstream position;Silicon base is placed on above rhenium source, and close to one side position of sulphur source, growth is face-down, silicon base
With the downstream edge of aluminium oxide boat is seamless contacts;
Pressure is normal pressure in growth course, first leads to high-purity argon gas with the flow of 500 sccm(99.999%)10 min are cleaned, then
It is evacuated to 1*10-4Pa, then ventilate to normal pressure;
Two warm area temperature are regulated in growth course:First warm area temperature room temperature(30℃)10 min are kept, using 3 min
180 DEG C are warming up to, 50 min are kept;Second warm area temperature is from room temperature(30℃)700 DEG C are warming up to by 23 min, keeps 40
min;Tube furnace lid is opened after the naturally near room temperature of two warm area temperature.
Step(3)In in the tube furnace of three-temperature-zone, the position relationship schematic diagram of sulphur source, rhenium source and silicon chip is as shown in Figure 2.
Air-flow is in growth course:50 sccm.
After reaction, silicon base is taken out, it is observed and is detected, as a result as shown in Fig. 3~8.
Wherein, Fig. 3~5 are the SEM figures of the rhenium disulfide nanometer sheet grown in silicon base.The amplification factor of Fig. 3 is 10000
Times, the amplification factor of Fig. 4 is 50000 times, and the amplification factor of Fig. 5 is 100000 times.From the enlarged drawing of Fig. 3~5 it is found that this method
The rhenium disulfide nanometer sheet large area of growth is covered in the substrate surface of non-oxidation layer, accumulates, is evenly distributed in stratiform, nanometer sheet
Pattern is uniform, and size is big, up to hundreds of nanometers.
Fig. 6 is the Raman spectrogram of the rhenium disulfide nanometer sheet grown in silicon base.ReS known in Raman spectrogram2's
Raman characteristic peak is apparent, and the Raman shift of wherein its three principal character peaks Eg, Ag and like-Eg are respectively at 150.9
cm-1,212.1 cm-1With 305.1 cm-1.In addition, 520.3 cm-1For the raman characteristic peak of silicon base.
The XPS figures that Fig. 7 is Re in the rhenium disulfide nanometer sheet grown in silicon base.In the XPS figures of Re it may be seen that
The level of energy of Re 4f5/2 and 4f7/2 are respectively 44.83 eV and 42.37 eV
The XPS figures that Fig. 8 is S in the rhenium disulfide nanometer sheet grown in silicon base.It may be seen that S 2p3/2 in the XPS figures of S
Position with 2p1/2 is respectively 164.28 eV and 162.92 eV.
2, above-mentioned preparation process and condition are equally used, continuous set-up procedure is passed through(3)In two aluminium oxide boats away from
At a distance from, silicon base is between the downstream edge of aluminium oxide boat, find the distance when two aluminium oxide boats in 20~30cm, silicon substrate
Bottom between the downstream edge of aluminium oxide boat at a distance from 0~1cm(Silicon base is square, its side length is 2.5cm, the length of side
0.4 times i.e. 1cm)When in range, rhenium disulfide is grown very uniform in non-oxidation layer silicon base.And work as silicon base and aluminium oxide
When distance between the downstream edge of boat is more than 1cm, although rhenium disulfide can also be grown in non-oxidation layer silicon base, growth
Nanometer sheet amount it is few and uneven, without apparent regular shape, as shown in Figure 9.When two aluminium oxide boats distance too closely or too
When remote, equally it is unable to get in non-oxidation layer silicon base and grows uniform rhenium disulfide.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention
The limitation of shield range can also be made on the basis of above description and thinking for those of ordinary skill in the art
Other various forms of variations or variation, there is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
All any modification, equivalent and improvement etc., should be included in the protection of the claims in the present invention made by within spirit and principle
Within the scope of.
Claims (10)
1. a kind of method growing rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer, using chemical vapor infiltration system
It is standby, which is characterized in that include the following steps:
S1. it cleans silicon base and is pre-processed;
S2. in multi-temperature zone tube furnace, the aluminium oxide boat for holding sublimed sulfur is placed in upstream warm area, holds the oxidation of rhenium trioxide
Aluminium boat is placed in the center of downstream warm area, and the spacing distance of two aluminium oxide boats is 20~30cm, and silicon base is placed in three oxidations
The upper edge of rhenium warm area aluminium oxide boat, silicon base growth is face-down, the downstream edge of silicon base and rhenium trioxide warm area aluminium oxide boat
Between distance be no more than 0.4 times of silicon base bond length;
S3. inert gas is then passed through into double temperature-area tubular furnaces, heating is reacted, you can in the silicon base of non-oxidation layer
Upper growth rhenium disulfide nanometer sheet.
2. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 1, feature exists
In the spacing distance of two aluminium oxide boats is 30cm.
3. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 1, feature exists
In the inert gas in step S3 is argon gas or nitrogen;The heating process is:The temperature of upstream warm area is 10~50 DEG C, is protected
Hold 0~20 min;Then 180~300 DEG C are warming up to through 0~10min and keep 30~70min;The temperature of downstream warm area is 10
~50 DEG C are warming up to 600~900 DEG C through 20~40min and keep 5~50min.
4. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 3, feature exists
In heating process is described in step S3:The temperature of upstream warm area is 30 DEG C, keeps 10min;Then 180 DEG C are warming up to through 3min
And keep 50min;The temperature of downstream warm area is 30 DEG C and is warming up to 700 DEG C through 23min and keeps 40min.
5. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 1, feature exists
In the air-flow of inert gas is 0~200sccm in step S3.
6. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 5, feature exists
In the air-flow of inert gas is 50sccm in step S3.
7. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 1, feature exists
In cleaning silicon base process in step S1 is:Silicon base according to acetone, ethyl alcohol, deionized water sequence respectively be cleaned by ultrasonic 5~
60min, 150~300W of ultrasonic power, 10~60KHz of frequency.
8. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 7, feature exists
In cleaning silicon base process in step S1 is:Silicon base is respectively cleaned by ultrasonic according to the sequence of acetone, ethyl alcohol, deionized water
10min, ultrasonic power 180W, frequency 40KHz.
9. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 1, feature exists
In the process for pre-processing silicon base in step S1 is:Cleaned silicon chip is impregnated to the oxidation for removing surface in etching solution
Layer, then deionized water flushing, is used in combination inert gas to dry up.
10. growing the method for rhenium disulfide nanometer sheet in the silicon base of non-oxidation layer according to claim 9, feature exists
In the etching solution is hydrofluoric acid solution, potassium hydroxide solution or sodium hydroxide solution.
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| CN110143616A (en) * | 2019-04-30 | 2019-08-20 | 陕西科技大学 | A kind of preparation method of the rhenium disulfide nanometer sheet of vertical-growth |
| CN110002504B (en) * | 2019-04-30 | 2021-04-27 | 陕西科技大学 | Preparation method of rhenium disulfide nanosheet |
| CN110143616B (en) * | 2019-04-30 | 2021-05-28 | 陕西科技大学 | Preparation method of vertically-grown rhenium disulfide nanosheet |
| CN110002504A (en) * | 2019-04-30 | 2019-07-12 | 陕西科技大学 | A kind of preparation method of rhenium disulfide nanometer sheet |
| CN110467358A (en) * | 2019-07-09 | 2019-11-19 | 广东工业大学 | A kind of rhenium disulfide nanometer sheet and its preparation method and application for evolving hydrogen reaction |
| CN114695581B (en) * | 2022-04-27 | 2024-05-14 | 安徽大学 | Preparation method of bismuth sulfide nanosheet array and heterojunction type photoelectrode based on bismuth sulfide nanosheet array |
| CN114695581A (en) * | 2022-04-27 | 2022-07-01 | 安徽大学 | Preparation method of bismuth sulfide nanosheet array and heterojunction type photoelectrode based on bismuth sulfide nanosheet array |
| CN114959637A (en) * | 2022-05-23 | 2022-08-30 | 西北工业大学 | Two-dimensional material torsional angle MoS 2 Preparation and torsion angle MoS of two-dimensional material 2 |
| CN114990523B (en) * | 2022-05-23 | 2024-04-26 | 西北工业大学 | Two-dimensional material torsion angle WS2Is to be used for preparing and twisting two-dimensional material2 |
| CN114990523A (en) * | 2022-05-23 | 2022-09-02 | 西北工业大学 | Two-dimensional material torsional angle WS 2 Preparation of (A) and torsion Angle WS of two-dimensional Material 2 |
| CN114959637B (en) * | 2022-05-23 | 2024-05-28 | 西北工业大学 | Two-dimensional material torsion angle MoS2Is to prepare and twist angle MoS of two-dimensional material2 |
| CN115058700A (en) * | 2022-06-24 | 2022-09-16 | 电子科技大学中山学院 | Preparation method of molybdenum disulfide film and molybdenum disulfide film |
| CN115058700B (en) * | 2022-06-24 | 2023-07-07 | 电子科技大学中山学院 | Preparation method of molybdenum disulfide film and molybdenum disulfide film |
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