CN116463627B - Indium phosphide nanowire and preparation method thereof - Google Patents
Indium phosphide nanowire and preparation method thereof Download PDFInfo
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- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 239000002070 nanowire Substances 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 99
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000002105 nanoparticle Substances 0.000 claims abstract description 26
- 239000002120 nanofilm Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000012159 carrier gas Substances 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 19
- 238000000137 annealing Methods 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 230000009471 action Effects 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 34
- 229910052710 silicon Inorganic materials 0.000 claims description 34
- 239000010703 silicon Substances 0.000 claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 17
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 238000007740 vapor deposition Methods 0.000 claims description 6
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 12
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000010931 gold Substances 0.000 description 51
- 239000010410 layer Substances 0.000 description 30
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 26
- 235000012239 silicon dioxide Nutrition 0.000 description 22
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
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- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
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- 238000000151 deposition Methods 0.000 description 3
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- 239000010408 film Substances 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical group [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
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- 239000000126 substance Substances 0.000 description 3
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- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
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- 239000004065 semiconductor Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
The invention belongs to the technical field of nano material preparation, and discloses an indium phosphide nanowire and a preparation method thereof, wherein the method comprises the following steps: evaporating a layer of Au nano film on the substrate A by adopting an evaporation method, and then carrying out annealing treatment to enable the Au nano film to be fused and agglomerated and form Au nano particles, so as to obtain a substrate C; cleaning the chemical vapor deposition reaction chamber to remove oxygen; then placing the substrate C in a cleaned chemical vapor deposition reaction chamber; setting the air pressure in the cleaned chemical vapor deposition reaction chamber as a preset air pressure, introducing carrier gas and InP source, heating to 750-950 ℃, and enabling the InP source to contact and react with Au nano-particles in the substrate C under the action of the carrier gas to form InP nanowires. The InP nanowires prepared by the method are very dense, smooth in surface, and uniform in distribution, and the diameter range of the nanowires is 10-100 nm, and the length of the nanowires can reach tens of micrometers.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to an indium phosphide nanowire and a preparation method thereof.
Background
Indium phosphide (InP) as a semiconductor material has excellent characteristics, such as high saturated electron drift velocity, proper light-emitting wavelength, low-loss optical fiber communication, strong radiation resistance, good thermal conductivity, high photoelectric conversion efficiency, high forbidden bandwidth and the like, so that the indium phosphide substrate can be widely applied to manufacturing optical module devices, sensing devices, high-end radio-frequency devices and the like. Nanowires of various forms and structures, such as porous nanowires, nanowires of coaxial core-shell structure, heterostructure nanowires, can be prepared based on a single nanowire; nanowire arrays, nanowire meshes, and nanowire bundles can be prepared according to different combinations of individual nanowires. Thus, the nanowire can be provided with the performance meeting the requirements of different devices by designing the morphology and the structure of the nanowire. The one-dimensional nano-structure has small size, high flexibility and good compatibility with the existing semiconductor integrated circuit technology, so that the one-dimensional nano-material is beneficial to the research of high integration and micro devices, which is important to the development of high-performance integrated circuit systems.
Compared with other nanostructures, the one-dimensional nanowire has excellent light absorption capacity, excellent carrier separation and collection capacity, excellent mechanical flexibility, rich surface state regulation and control functions and good compatibility, and has unique advantages in researching the dependence of the electrical, photoelectric and mechanical properties of the device on the dimension. InP, a very important group iii-v compound, has a high electron mobility, an ultra-small surface recombination rate, and a direct optical bandgap, and thus has wide applicability in solar cells, optical fiber communication, high-speed electronic devices, and infrared laser fields. Compared with InP nano particles, the one-dimensional InP structure has higher separation efficiency of electrons and holes and carrier transport capability, and has higher specific surface area and smaller volume compared with InP block and film materials, so the one-dimensional InP nano structure is widely regarded as the main development direction of InP material preparation.
The current preparation methods of InP nanowires mainly include Chemical Vapor Deposition (CVD), metal Organic Chemical Vapor Deposition (MOCVD), molecular Beam Epitaxy (MBE), chemical Beam Epitaxy (CBE), and the like. However, growing nanowires on a substrate using Metal Organic Chemical Vapor Deposition (MOCVD) and an epitaxial method has problems of complicated equipment, high price, long period of growing crystals, and the like. Therefore, the existing technology mainly adopts a liquid phase method to prepare one-dimensional InP nano materials, can prepare a large amount of one-dimensional InP nano structures through a growth method (such as a hydrothermal method, a solvothermal method and the like) at low temperature, has the advantages of strong operability, good repeatability and the like, but is difficult to prepare one-dimensional InP nano structures with smooth surfaces and high crystallinity, which also limits the electron-hole separation efficiency and the internal carrier transport capacity of the materials, and further reduces the working efficiency of photon, electron and photoelectric devices constructed based on the one-dimensional InP nano materials.
Therefore, there is a need to develop a method for preparing group iii-v nano materials with excellent properties, which is simple to operate and has low cost, so the present invention provides an indium phosphide nanowire and a preparation method thereof.
Disclosure of Invention
The invention provides an indium phosphide nanowire and a preparation method thereof, which aims to solve the problems that in the prior art, the nanowire grows on a substrate by utilizing a Metal Organic Chemical Vapor Deposition (MOCVD) and an epitaxial method, equipment is complex, the price is high, the period of growing crystals is long and the like, and a one-dimensional InP nano structure with smooth surface and high crystallinity is difficult to obtain by a liquid phase method. According to the invention, the InP nanowire is prepared by a simple, efficient and low-cost Chemical Vapor Deposition (CVD), the InP nanowire with high crystal quality and low defect is prepared by regulating and controlling the particle size of Au catalytic particles, the substrate temperature, the heat preservation time, the type of quartz tube, the opening direction and other technological parameters, the rule of growing InP nanowires with different shapes and sizes on a Si substrate by the CVD method is explored, and the growth mechanism of the InP nanowire is revealed.
The invention relates to an indium phosphide nanowire and a preparation method thereof, which are realized by the following technical scheme:
the first object of the invention is to provide a preparation method of indium phosphide nanowires, comprising the following steps:
step 1, evaporating a layer of Au nano film on a substrate A by adopting an evaporation method to obtain a substrate B with the Au nano film;
wherein, the substrate A is any one of a silicon substrate, a sapphire substrate and a gallium arsenide substrate with an oxide layer;
step 2, annealing the substrate B to enable the Au nano-film to be fused and agglomerated and form Au nano-particles, so as to obtain a substrate C with the Au nano-particles;
step 3, cleaning the chemical vapor deposition reaction chamber to remove oxygen; subsequently placing the substrate C in the cleaned chemical vapor deposition reaction chamber;
wherein the included angle between the substrate C and the horizontal plane is 14-16 degrees;
and 4, setting the air pressure in the chemical vapor deposition reaction chamber after cleaning as preset air pressure, introducing carrier gas and InP source, heating to 750-950 ℃, and enabling the InP source to contact and react with Au nano-particles in the substrate C under the action of the carrier gas to form InP nanowires.
Further, the InP source is InP powder, and the purity of the InP powder is more than or equal to 99.99%.
Further, the carrier gas is any one of argon, a mixed gas of argon and hydrogen, a mixed gas of argon and carbon dioxide, and a mixed gas of argon and carbon monoxide.
Further, the substrate A is provided with SiO 2 And (3) a silicon wafer of a layer.
Further, in the step 4, the predetermined air pressure is 45 to 55Pa.
Further, in the process of heating to 750-950 ℃, when the temperature is increased to less than or equal to 300 ℃, the feeding rate of the carrier gas is 180-220 SCCM, and the carrier gas is continuously fed for 0.8-1.2 h at the temperature of 300 ℃ at the rate of 180-220 SCCM; then, when the temperature is raised from 300 ℃ to 750-950 ℃, the feeding rate of the carrier gas is 48-52 SCCM, and the temperature is kept for 0.5-2 h at the temperature of 750-950 ℃.
Further, in the step 2, the annealing treatment temperature is 550-650 ℃ and the annealing time is 10-30 min.
Further, in step 1, the vapor deposition current is 75 to 85A, and the vapor deposition time is 50 to 70s.
A second object of the present invention is to provide an indium phosphide nanowire prepared by the above-mentioned preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses indium phosphide powder as raw material, silicon dioxide film as insertion layer, au as catalyst, improves the preparation process to build reaction environment with sufficient oxygen insulation, and grows InP nanowire with excellent performance by Chemical Vapor Deposition (CVD).
The invention adopts a low-pressure vapor deposition method, indium phosphide powder is used as a raw material, the temperature exceeds the melting point when heating, the raw material sublimates, and Au is used as a catalyst. On the basis of depositing the Au nano-film on the substrate, a small vacuum rapid annealing furnace is used, and the Au nano-film is heated to be fused and agglomerated to form the Au nano-particles. The prepared Au nano-particles are mainly used as catalysts for preparing InP nanowires. In the process of preparing the InP nanowire by using the CVD method, indium atoms generated by the thermally decomposed InP powder firstly react with Au nano-particles In a molten state to generate Au-In solid solution alloy, and then InP is generated by the supersaturation precipitation of In the Au-In solid solution alloy and the reaction of P In the atmosphere, so that the InP can preferentially grow to form the InP nanowire due to the anisotropism of InP crystals.
The invention regulates and controls the components and the morphology of the InP nanowire by regulating and controlling the decomposition temperature of the raw materials, the heating temperature of the substrate and the particle size of the gold catalytic particles, so that the raw materials are fully decomposed, and then the raw materials are transported and deposited on a silicon wafer by combining with a special atmosphere to prepare the InP nanowire, thereby improving the crystal quality and the photoelectric property of the InP nanowire.
The diameter of the InP nanowire prepared by the method reaches tens to hundreds of nanometers, and the length of the InP nanowire can reach tens to tens of micrometers. The raman spectrum test results were almost free of drift compared to a defect-free bulk InP single crystal. In a scanning electron microscope photograph, inP nanowires are very dense, have smooth surfaces, have diameters ranging from 10nm to 100nm, have lengths of tens of micrometers, and are uniformly distributed. The sample in the spherical electron microscope photograph is an InP nanowire on a Si/SiO2/Au (under the anaerobic condition) substrate, wherein the lattice d distance of the InP nanowire (111) is 0.34nm and is the same as that of a bulk InP body monocrystal, which shows that the prepared nanowire is a pure InP nanowire, and the low-defect InP nanowire is obtained.
Drawings
FIG. 1 is a Raman spectrum of a sample obtained in example 1;
FIG. 2 is a Raman spectrum of the sample obtained in comparative example 1;
FIG. 3 is an electron scanning microscope photograph of the sample obtained in example 1;
FIG. 4 is an electron scanning microscope photograph of the sample obtained in comparative example 1;
FIG. 5 is a spherical electron micrograph of InP nanowires on the sample obtained by the treatment of example 1; fig. 5 (a) is a spherical aberration electron micrograph at a scale of 50nm, and fig. 5 (b) is a spherical aberration electron micrograph at a scale of 10 nm.
Detailed Description
The inventor considers that the InP nanowires with high quality and low defects are the basic conditions for preparing high-performance photodetectors. However, in the process of preparing the InP nanowire by the CVD method, sufficient oxygen insulation cannot be achieved, other substances are easy to generate, and the prepared sample is impure, so the invention provides the method for introducing high-speed hydrogen-argon mixed gas at the initial stage of the reaction and preserving the temperature for one hour at 300 ℃, and then vacuumizing again, so that the reaction process is insulated as much as possible. And the technical solutions in the embodiments of the present invention will be clearly and completely described below.
The invention provides an indium phosphide nanowire, and a preparation method thereof is as follows:
step 1, evaporating a layer of Au nano film on a substrate A by adopting an evaporation method to obtain a substrate B with the Au nano film;
the substrate A used in the present invention is any one of a silicon substrate with an oxide layer, a sapphire substrate and a gallium arsenide substrate, and is preferably a silicon substrate with an oxide layer, that is, a silicon substrate with SiO 2 Silicon wafer of layer and with SiO 2 The layer serves as an interposed layer, and the silicon dioxide layer can prevent the substrate from being contaminated by the outside, i.e., serves as a surface passivation layer.
According to the invention, after the substrate A is cleaned, a preferred evaporation mode is adopted, a single-layer or multi-layer Au film can be deposited on the surface of the cleaned substrate A according to actual requirements, the evaporation current is 75-85A, and the Au nano film with the required thickness can be obtained according to the adjustment of the evaporation time.
Step 2, annealing the substrate B to enable the Au nano-film to be fused and agglomerated and form Au nano-particles, so as to obtain a substrate C with the Au nano-particles;
it should be noted that, in the invention, the catalyst is also an important factor in controlling the growth of the nanowire, and different catalyst metals are selected because of different eutectic temperatures of the alloy with the source material, so that different growth mechanisms of the nanowire can be realized, and the growth direction of the nanowire is further effectively controlled. In the VLS growth process, the diameter and the growth direction of the nanowire can be regulated by adopting catalysts with different thicknesses, because the thicker catalyst has larger droplet size after annealing, and the source material forms the nanowire with larger diameter when supersaturated in the catalyst alloy is separated out. Therefore, the Au nano film is preferably evaporated on the substrate A and then annealed, so that the diameter and the growth direction of the nano wire can be conveniently and effectively regulated and controlled by regulating and controlling the form of the Au catalyst, and the Au serving as the catalyst for growing the nano wire is grown by catalyzing and growing by Auin alloy according to a gas-liquid-solid (VLS) mechanism. And the substrate B is annealed at 550-650 ℃ for 10-30 min, so that the Au nano-films are fused and agglomerated to form Au nano-particles, and the formed Au nano-particles are tightly contacted with the substrate, thereby being beneficial to catalyzing an InP source material to form InP nanowires on the substrate C.
Step 3, cleaning the chemical vapor deposition reaction chamber to remove oxygen; subsequently placing the substrate C in the cleaned chemical vapor deposition reaction chamber;
it should be noted that, in the present invention, the group III-V compound is highly susceptible to oxidation, which results in a grown nanowire structure having many defects, and thus seriously affects the performance of the nanowire device. Therefore, before chemical vapor deposition treatment is carried out, the chemical vapor deposition reaction chamber is cleaned to remove oxygen in the chemical vapor deposition reaction chamber, so that defects can be effectively reduced, and the InP nanowire with low defects and even no defects can be obtained. The inert gas is adopted to purge the chemical vapor deposition reaction chamber so as to remove oxygen or air in the chemical vapor deposition reaction chamber, so that the chemical vapor deposition reaction chamber is cleaned; the substrate C is then placed therein in preparation for subsequent deposition to form InP nanowires.
In order to enable the InP nanowire to be better deposited on the substrate C, the substrate C is obliquely placed in the chemical vapor deposition reaction chamber, and the included angle between the substrate C and the horizontal plane is 14-16 degrees, so that the contact area between the substrate C and the carrier gas flow is increased, and the InP nanowire is better deposited on the substrate C.
Step 4, setting the air pressure in the chemical vapor deposition reaction chamber after cleaning as preset air pressure, introducing carrier gas and InP source, heating to 750-950 ℃, and enabling the InP source to contact and react with Au nano-particles in the substrate C under the action of the carrier gas, so as to form InP nanowires;
it should be noted that, the predetermined air pressure is 45-55 Pa, so that the vacuum is pumped to a lower vacuum state, the reaction device is in a low vacuum state, and more air is exhausted, so as to avoid the influence of oxygen in the air on the quality of InP nanowire deposition.
According to the invention, the InP powder with the purity of 99.99% is preferably used as an InP source, the InP powder is simple in reaction raw material, the raw material is an inorganic substance with low cost and low toxicity, the use of organic substances is avoided, and the InP powder is not easy to contact with inflammable and extremely toxic organic solvents. Meanwhile, compared with other reactants, the pure indium phosphide powder can grow samples with better crystal quality. And the carrier gas is selected from any one of argon, argon and hydrogen mixed gas, argon and carbon dioxide mixed gas and argon and carbon monoxide mixed gas.
In the chemical vapor deposition process, in the process of heating to 750-950 ℃, when the temperature is increased to less than or equal to 300 ℃, the carrier gas is introduced at the rate of 180-220 SCCM, and is continuously introduced at the rate of 180-220 SCCM for 0.8-1.2 h at the temperature of 300 ℃ so as to ensure that oxygen in the chemical vapor deposition reaction chamber is removed and the chemical vapor deposition reaction chamber is insulated from oxygen; then, when the temperature is raised to 750-950 ℃ from 300 ℃, the introducing rate of carrier gas is 48-52 SCCM, and the temperature is kept for 0.5-2 h at 750-950 ℃, so that InP powder is thermally decomposed at high temperature of 750-950 ℃ to generate an indium source and a P source, in atoms In the generated indium source are firstly contacted with Au nano particles In a molten state to form Au-In solid solution alloy, and In the Au-In solid solution alloy is supersaturated and separated out to react with P In the atmosphere to generate InP, and the InP preferentially grows to form InP nanowires due to the anisotropism of InP crystals, so that InP nanowires are formed on a substrate.
In the following examples, inP nanowires were prepared using a single temperature zone vacuum tube furnace system. The single-temperature-zone tube furnace is provided with a heat preservation zone and a transition zone, the temperature of the heat preservation zone is set at a set temperature, and the temperature of a part of the transition zone, which is far from the heat preservation zone, is lower. Firstly, measuring the temperature distribution of the tube furnace from a heat preservation area to a tube orifice by using a thermocouple when the temperature of the heat preservation area of the tube furnace is 800 ℃ through an empty burning tube furnace. By utilizing the law, the raw materials and the substrate can be at different temperatures by adjusting the positions of the raw materials and the substrate in the tube furnace, so that the raw materials are thermally decomposed at a higher temperature, and InP nanowires are grown on the substrate at a lower temperature. The influence of the substrate temperature and the growth time on the appearance of the InP nanowire prepared by the CVD method is explored. In addition, the type and the placement direction of the small quartz tube can also influence the growth of the InP nanowires, and the single-opening quartz tube is selected to prepare the InP nanowires for the quartz tube with the opening facing the ventilation direction and the exhaust direction and the double-opening quartz tube respectively in the following embodiments, and finally, the proper quartz tube and the opening direction are determined.
Example 1
The embodiment provides an indium phosphide nanowire, and the preparation method thereof is as follows:
1) Preparing an Au nano film:
SiO with 300nm thickness on surface 2 Cutting the silicon wafer into 5mm×10mm pieces, respectively ultrasonic cleaning in acetone, deionized water and ethanol for 10min, and drying to obtain cleaned SiO-containing silicon wafer 2 A silicon wafer of a layer; then using a small thermal evaporation evaporator to make the cleaned surface have SiO 2 Evaporating the silicon wafer surface of the layer under the current of 80A for 60s to obtain SiO on the silicon wafer 2 And evaporating a layer of Au nano film on the layer to obtain the substrate B.
2) Preparing Au nano-particles:
and (3) placing the obtained substrate B in a small vacuum rapid annealing furnace, and annealing for 15min at 600 ℃ to enable the Au thin film to be annealed at high temperature to form Au nano particles, thus obtaining the substrate C.
3) InP nanowire formation
About 0.1g of InP powder having a purity of 99.99% was weighed into the bottom of a single-opening thin quartz tube having a length of 30cm, a diameter of 9mm and a wall thickness of 1 mm.
The substrate C is placed in the thin quartz tube 25cm away from the tube bottom by using graphite paper as a carrier, and the substrate C is kept at an inclination angle of about 15 degrees, so that the substrate C is in full contact with steam generated by thermal decomposition of InP powder.
Then placing the fine quartz tube filled with InP powder and a substrate C in a tube furnace, enabling the InP powder at the bottom of the tube to be positioned at the center of a heat preservation area of the tube furnace, setting 800 ℃ as a thermal decomposition temperature of raw materials, keeping the heat preservation time for 0.5H, setting the heat preservation time for 1H at 300 ℃ simultaneously, connecting a gas path of the tube furnace, enabling the pressure in the tube to be kept at 50Pa through a mechanical pump and vacuum pumping at a gas outlet end, and introducing hydrogen-argon mixed gas (H) of 200SCCM at a gas inlet end through a gas flowmeter 2 5 percent of the equipment is installed, and then the tube furnace is started to openAnd (3) starting a heating program, carrying out vacuumizing operation on the device after the temperature is increased to 300 ℃ and the temperature is kept for 1h, fully insulating oxygen in the device, changing the gas flow into 50SCCM, continuing the heating program, and taking out the sample after the temperature program of the tubular furnace is finished and the tubular furnace is cooled to the room temperature. And obtaining the silicon chip with the InP nanowires.
Example 2
The embodiment provides an indium phosphide nanowire, and the preparation method thereof is as follows:
1) Preparing an Au nano film:
SiO with 300nm thickness on surface 2 Cutting the silicon wafer into 5mm×10mm pieces, respectively ultrasonic cleaning in acetone, deionized water and ethanol for 10min, and drying to obtain cleaned SiO-containing silicon wafer 2 A silicon wafer of a layer; then using a small thermal evaporation evaporator to make the cleaned surface have SiO 2 Evaporating the silicon wafer surface of the layer for 70s under 75A current to obtain SiO on the silicon wafer 2 And evaporating a layer of Au nano film on the layer to obtain the substrate B.
2) Preparing Au nano-particles:
and (3) placing the obtained substrate B in a small vacuum rapid annealing furnace, and annealing for 30min at 550 ℃ to enable the Au thin film to be annealed at high temperature to form Au nano particles, thus obtaining the substrate C.
3) InP nanowire formation
About 0.1g of InP powder having a purity of 99.99% was weighed into the bottom of a single-opening thin quartz tube having a length of 30cm, a diameter of 9mm and a wall thickness of 1 mm.
The substrate C is placed in the thin quartz tube 25cm away from the tube bottom by using graphite paper as a carrier, and the substrate C is kept at an inclination angle of about 15 degrees, so that the substrate C is in full contact with steam generated by thermal decomposition of InP powder.
Then placing the fine quartz tube filled with InP powder and the substrate C in a tube furnace, enabling the InP powder at the bottom of the tube to be positioned at the center of a heat preservation area of the tube furnace, setting 750 ℃ as a thermal decomposition temperature of raw materials, keeping the heat for 2 hours, setting the heat preservation time at 300 ℃ for 0.8 hours, connecting a gas path of the tube furnace, and enabling the pressure in the tube to be kept by a mechanical pump at a gas outlet end through vacuum pumpingAt 45Pa, the air inlet end is introduced with hydrogen-argon mixture (H) of 180SCCM through a gas flowmeter 2 5 percent of equipment is installed, the tube furnace is started, a heating program starts to run, when the temperature is raised to 300 ℃ and kept for 0.8h, the device is vacuumized, the device is fully insulated from oxygen, then the gas flow is changed into 45SCCM, the heating program is continued, and after the temperature program of the tube furnace is finished, the sample is taken out after the temperature of the tube furnace is cooled to the room temperature. And obtaining the silicon chip with the InP nanowires.
Example 3
The embodiment provides an indium phosphide nanowire, and the preparation method thereof is as follows:
1) Preparing an Au nano film:
SiO with 300nm thickness on surface 2 Cutting the silicon wafer into 5mm×10mm pieces, respectively ultrasonic cleaning in acetone, deionized water and ethanol for 10min, and drying to obtain cleaned SiO-containing silicon wafer 2 A silicon wafer of a layer; then using a small thermal evaporation evaporator to make the cleaned surface have SiO 2 Evaporating the silicon wafer surface of the layer for 50s under the current of 85A to obtain SiO (silicon dioxide) on the silicon wafer 2 And evaporating a layer of Au nano film on the layer to obtain the substrate B.
2) Preparing Au nano-particles:
and (3) placing the obtained substrate B in a small vacuum rapid annealing furnace, and annealing for 10min at the temperature of 650 ℃ to enable the Au thin film to be annealed at high temperature to form Au nano particles, thus obtaining the substrate C.
3) InP nanowire formation
About 0.1g of InP powder having a purity of 99.99% was weighed into the bottom of a single-opening thin quartz tube having a length of 30cm, a diameter of 9mm and a wall thickness of 1 mm.
The substrate C is placed in the thin quartz tube 25cm away from the tube bottom by using graphite paper as a carrier, and the substrate C is kept at an inclination angle of about 15 degrees, so that the substrate C is in full contact with steam generated by thermal decomposition of InP powder.
Then placing the fine quartz tube filled with InP powder and substrate C in a tube furnace, placing InP powder at the bottom of the tube at the center of the heat preservation zone of the tube furnace, setting 800 deg.C as thermal decomposition temperature of raw material, and preserving heatThe time is 0.5H, the heat preservation time is 1.2H at 300 ℃, the gas path of the tube furnace is connected, the pressure in the tube is kept at 55Pa by the evacuation of a mechanical pump at the gas outlet end, and the hydrogen-argon mixed gas (H) of 220SCCM is introduced into the gas inlet end through a gas flowmeter 2 5 percent of equipment is installed, the tube furnace is started, a heating program starts to run, when the temperature is raised to 300 ℃ and kept for 1 hour, the device is vacuumized, the device is fully insulated from oxygen, then the gas flow is changed into 55SCCM, the heating program is continued, and after the temperature program of the tube furnace is finished, the sample is taken out after the temperature of the tube furnace is cooled to room temperature. And obtaining the silicon chip with the InP nanowires.
Example 4
This example provides an indium phosphide nanowire, and the preparation method differs from example 1 only in that:
in this example, when preparing the Au nanofilm:
with 300nm thick SiO on the surface 2 The gallium arsenide substrate of the layer serves as substrate a.
Comparative example 1
The comparative example provides an indium phosphide nanowire, and its preparation method is as follows:
1) Preparing an Au nano film:
SiO with 300nm thickness on surface 2 Cutting the silicon wafer into 5mm×10mm pieces, respectively ultrasonic cleaning in acetone, deionized water and ethanol for 10min, and drying to obtain cleaned SiO-containing silicon wafer 2 A silicon wafer of a layer; then using a small thermal evaporation evaporator to make the cleaned surface have SiO 2 Evaporating the silicon wafer surface of the layer under the current of 80A for 60s to obtain SiO on the silicon wafer 2 And evaporating a layer of Au nano film on the layer to obtain the substrate B.
2) Preparing Au nano-particles:
and (3) placing the obtained substrate B in a small vacuum rapid annealing furnace, and annealing for 15min at 600 ℃ to enable the Au thin film to be annealed at high temperature to form Au nano particles, thus obtaining the substrate C.
3) InP nanowire formation
About 0.1g of InP powder having a purity of 99.99% was weighed into the bottom of a single-opening thin quartz tube having a length of 30cm, a diameter of 9mm and a wall thickness of 1 mm.
The substrate C is placed in the thin quartz tube 25cm away from the tube bottom by using graphite paper as a carrier, and the substrate C is kept at an inclination angle of about 15 degrees, so that the substrate C is in full contact with steam generated by thermal decomposition of InP powder.
Then placing the fine quartz tube filled with InP powder and the substrate C in a tube furnace, positioning the InP powder at the bottom of the tube at the center of a heat preservation area of the tube furnace, setting 800 ℃ as the thermal decomposition temperature of the raw material, keeping the heat preservation time for 0.5H, connecting the gas path of the tube furnace, vacuumizing the gas outlet end through a mechanical pump to keep the pressure in the tube at about 50Pa, and introducing 200SCCM hydrogen-argon mixed gas (H) into the gas inlet end through a gas flowmeter 2 5 percent of the equipment is installed, the tube furnace is started, a heating program is started to run, the gas flow is changed into 50SCCM when the temperature is increased to 300 ℃, then the heating program is continued, after the temperature program of the tube furnace is finished, the sample is taken out after the temperature program of the tube furnace is cooled to the room temperature, and the silicon chip with the InP nanowires growing is not obtained.
Test section
Raman spectroscopy (one)
The present invention is exemplified by example 1 and comparative example 1, and raman spectrum tests were performed on samples treated in example 1 and comparative example 1, respectively, and the test results are shown in fig. 1 and 2, respectively.
Wherein, fig. 1 is a raman spectrum of the sample obtained in example 1, fig. 2 is a raman spectrum of the sample obtained in comparative example 1, and as can be seen by comparing fig. 1 and fig. 2, example 1 reduces the oxygen content in the sample grown by chemical vapor deposition under a sufficient oxygen-free condition, and the raman spectrum of the sample has no frequency shift compared with bulk InP single crystal. In contrast, the InP nanowires are not obtained in the aerobic condition in comparative example 1, and the raman spectrum measurement shows that the InP nanowires are not contained in the sample, and the raman spectrum measurement shows that the InP nanowires are characteristic peaks of the silicon wafer of the substrate.
(II) Electron scanning microscope testing
The present invention was carried out by electron scanning microscope test on the samples treated in example 1 and comparative example 1, respectively, using example 1 and comparative example 1, and the test results are shown in fig. 3 and 4, respectively.
Among them, fig. 3 is an electron scanning microscope photograph of the sample obtained in example 1, and fig. 4 is an electron scanning microscope photograph of the sample obtained in comparative example 1. As can be seen from fig. 3 and fig. 4, the sample grown in the anaerobic condition in example 1 contains InP nanowires, the nanowires have better appearance, the nanowires are very dense, the surface is smooth, the diameter of the nanowires is in the range of 10-100 nm, the length can reach tens of micrometers, and the nanowires are uniformly distributed; while comparative example 1 did not grow nanowires on the substrate under aerobic conditions.
(III) spherical aberration Electron microscope test
In the present invention, as example 1, an InP nanowire on a sample obtained by the treatment of example 1 was subjected to a spherical electron microscope test, and the test results are shown in fig. 5.
Fig. 5 (a) is a spherical aberration electron micrograph at a scale of 50nm, and fig. 5 (b) is a spherical aberration electron micrograph at a scale of 10 nm. And as can be seen from fig. 5 (a) and fig. 5 (b), the lattice d-spacing of the InP nanowire (111) of example 1 is 0.34 identical to that of the bulk InP bulk single crystal, indicating that the prepared nanowire is a pure InP nanowire, resulting in a low-defect InP nanowire.
It should be apparent that the embodiments described above are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (7)
1. A method for preparing indium phosphide nanowires, which is characterized by comprising the following steps:
step 1, evaporating a layer of Au nano film on a substrate A by adopting an evaporation method to obtain a substrate B with the Au nano film;
wherein, the substrate A is any one of a silicon substrate, a sapphire substrate and a gallium arsenide substrate with an oxide layer;
step 2, annealing the substrate B to enable the Au nano-film to be fused and agglomerated and form Au nano-particles, so as to obtain a substrate C with the Au nano-particles;
step 3, cleaning the chemical vapor deposition reaction chamber to remove oxygen; subsequently placing the substrate C in the cleaned chemical vapor deposition reaction chamber;
wherein the included angle between the substrate C and the horizontal plane is 14-16 degrees;
step 4, setting the air pressure in the chemical vapor deposition reaction chamber after cleaning as preset air pressure, introducing carrier gas and InP source, heating to 750-950 ℃, and enabling the InP source to contact and react with Au nano-particles in the substrate C under the action of the carrier gas, so as to form InP nanowires;
the InP source is InP powder, and the purity of the InP powder is more than or equal to 99.99%;
in the process of heating to 750-950 ℃, when the temperature is increased to less than or equal to 300 ℃, the feeding rate of carrier gas is 180-220 SCCM, and the carrier gas is continuously fed for 0.8-1.2 h at the rate of 180-220 SCCM at the temperature of 300 ℃; then, when the temperature is raised from 300 ℃ to 750-950 ℃, the feeding rate of the carrier gas is 48-52 SCCM, and the temperature is kept for 0.5-2 h at the temperature of 750-950 ℃.
2. The method according to claim 1, wherein the carrier gas is any one of argon, a mixture of argon and hydrogen, a mixture of argon and carbon dioxide, and a mixture of argon and carbon monoxide.
3. The method of claim 1, wherein the substrate A is a substrate with SiO 2 And (3) a silicon wafer of a layer.
4. The method according to claim 1, wherein the predetermined air pressure in step 4 is 45 to 55Pa.
5. The method according to claim 1, wherein in the step 2, the annealing treatment is performed at 550 to 650 ℃ for 10 to 30 minutes.
6. The method according to claim 1, wherein in step 1, the vapor deposition current for vapor deposition is 75 to 85A and the vapor deposition time is 50 to 70s.
7. An indium phosphide nanowire prepared by the preparation method as claimed in any one of claims 1 to 6.
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