CN105529242A - Method for preparing bead-shaped monocrystalline silicon nanowire - Google Patents
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- 239000002070 nanowire Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 229910021417 amorphous silicon Inorganic materials 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052718 tin Inorganic materials 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 6
- 229910052738 indium Inorganic materials 0.000 claims abstract description 6
- 230000003197 catalytic effect Effects 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 239000002923 metal particle Substances 0.000 claims abstract description 5
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 238000012545 processing Methods 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 11
- 239000004065 semiconductor Substances 0.000 claims description 10
- 230000001939 inductive effect Effects 0.000 claims description 9
- 238000001259 photo etching Methods 0.000 claims description 5
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- 238000010521 absorption reaction Methods 0.000 claims description 2
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- 238000004049 embossing Methods 0.000 claims description 2
- 238000009832 plasma treatment Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 230000002269 spontaneous effect Effects 0.000 claims description 2
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- 230000003213 activating effect Effects 0.000 abstract 1
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- 239000002243 precursor Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 17
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- 239000003054 catalyst Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001338 self-assembly Methods 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
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- 238000002474 experimental method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
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- 238000004377 microelectronic Methods 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 230000032258 transport Effects 0.000 description 2
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- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention discloses a method for preparing a bead-shaped monocrystalline silicon nanowire. The method comprises the following steps: (1) evaporating an induced metal film of In, Sn or Bi in a position area as an initial position for nanowire growth on a flat substrate; (2) putting the substrate into a PECVD system cavity, processing a sample with hydrogen plasmas at 200-500 DEG C for 5-30 minutes, and forming a lot of quasi-nano catalytic metal particles from dozens of nanometers to several microns by the metal film; (3) covering an amorphous silicon layer (from several nanometers to hundreds of nanometers) with a proper thickness as a precursor dielectric layer in the PECVD system; and (4) annealing the product in vacuum or non-oxidizing atmospheres of hydrogen, nitrogen and the like, activating the catalytic metal particles, spontaneously absorbing the amorphous silicon, separating out monocrystalline silicon, and simultaneously periodically changing the diameters to grow the bead-shaped nanowire.
Description
One, technical field
The present invention relates generally to field of semiconductor devices, particularly single electron quantum device preparation and application field.
Two, technical background
Semiconductor nano line structure, due to the optics of its uniqueness and electrical properties, has boundless application prospect in electronic device, photodetection, biomedicine, sensor.Silicon materials are most crucial in current semi-conducting material, most widely used material.Over half a century in the past, microelectronic every generation huge advance is all carried out round silicon materials.Improving and including many new materials in through decades, the core technology platform of traditional counting is still based on silicon.Meanwhile, along with going deep into of research, day by day obviously be sure of that silicon can prepare the device with quantum charge and spin properties of all new generation as a kind of outstanding host material.This comprises from quantum computer to spintronics application widely.Silicon materials due to the existence of its weak SO coupling and isotope and zero nuclear spin be the ecotopia of spinning electron.Quantum device based on silicon has possessed on the basis of the manufacturing technology of classic computer exquisiteness will have huge application prospect in Quantum Spin control combination.
The microelectronics of existing industrialization and semiconductor technology take to have developed over half a century very ripe (Top-down) from top to bottom technology, namely the fine machining methods such as chemical wet etching are adopted, large material is cut little, form structure or device, and integrated with circuit, realize system microminiaturization.And having arrived nanometer and quantum device epoch, yardstick will reach even a few nanometer of hundred nanometers, and the technology thereupon produced and Cost Problems are by highly significant.And Bottom-up technology, it is the way of molecule, atom packaging technology, namely functional molecular, the atom with specific physicochemical property, by molecule, intraatomic active force, form the molecular line of nanoscale, film and other structure subtly, then be integrated into micro-system by nanostructure and functional unit.This manufacturing technology reflects a kind of theory of nanometer technology, namely from the level design of atom and molecule, assembled material, device and system, is the very promising manufacturing technology of one.
VLS (gas-liquid-solid) growth mechanism is the ripe growth mechanism preparing nano wire based on Bottom-up technology.The General Requirements of VLS growth mechanism must have the existence of catalyst, first growth material is evaporated into gaseous state, at suitable temperature, catalyst can form liquid eutectic with the constituent element of growth material is molten mutually, the constituent element of growth material constantly obtains from gas phase, after matter constituent element molten in liquid state reaches supersaturation, whisker will be separated out along solid-liquid interface one preferential direction, grow up to linear crystal.The size of catalyst will control the size of grown whisker to a great extent obviously.Experiment proves that this growth mechanism can be used for preparing the even more complicated monocrystalline of a large amount of simple substance, binary compound, and the essentially no dislocation of monocrystalline of the method growth, fast growth.A large amount of quasi-one-dimensional nanometer materials can be prepared by the size controlling catalyst.
Three, summary of the invention
For the problems referred to above, the object of this invention is to provide a kind of method preparing high-quality pearl string shape silicon nanowires.
Technical solution of the present invention is: a kind of method preparing pearl string shape monocrystalline silicon nano line, adopt the method for self-align growth and integrated planar semiconductor nanowires, step is as follows, 1) on smooth substrate, coordinate the technology such as photoetching or other pattern generation techniques, accurately control at films such as selected region evaporation inducing metal In, Sn or Bi, thickness in several nanometer to tens nanometers; 2) above-mentioned substrate is put into PECVD system chamber, utilize the plasma of hydrogen to process metallic film when temperature 200 DEG C-500 DEG C, power 2W-50W, make it to become the discrete accurate catalyzing nano-particles of diameter between tens nanometers are to several microns; The change such as temperature, power, time by the difference and process that regulate and control thickness of metal film can control to be formed the size of catalyticing metal particle; 3) in a pecvd system, substrate covers the amorphous silicon layer of one deck suitable thickness (a few nanometer to tens nanometer); 4) (temperature is at 350 DEG C-400 DEG C) are annealed in a vacuum or in the non-oxidizing atmosphere such as hydrogen, nitrogen; the catalyticing metal particle that is activated meeting spontaneous absorption amorphous silicon; crystallize out silicon, diameter generating period change simultaneously, grows pearl string shape nano wire.
The present invention program can regulate and control the growth of pearl string shape nano wire by parameters such as the temperature conditions of plasma treatment time power and temperature in adjustment growth course, covering amorphous silicon thickness and growth, annealing temperature and times, obtain the silicon nanowires that diameter, Cycle Length etc. are adjustable.
Selected inducing metal both can be Sn, Bi or In, also can be the metal that other can be induced plane nano line and grow.
Further, the pearl string shape nano wire of planar growth both can be silicon nanowires, also can be the semiconductor nanowires such as germanium, and nano wire both can be intrinsic nano wire also can be doped nanowire.
Mask plate both can be used in the location of inducing metal, also can utilize photoetching technique, nanometer embossing obtains.
The substrate of growth pearl string shape silicon nanowires is planar semiconductor substrate, or organic resistance to 350 DEG C of high-temperature material substrates.
Gu plane solid-liquid-(IP-SLS) growth mechanism that the present invention adopts is similar to VLS mechanism, is with the difference of VLS mechanism, in VLS mechanism growth course, required raw material are provided by gas phase; And in SLS mechanism growth course, required raw material provides from solid-state non-crystalline material, in general, in the method, conventional low-melting-point metal (as In, Sn or Bi etc.) is as cosolvent, is equivalent to the catalyst in VLS mechanism.
Beneficial effect of the present invention, the present invention adopts IP-SLS method to grow pearl string shape semiconductor nanowires in a pecvd system.The advantage of IP-SLS method is, the self-align nano-wire array of primary reconstruction can be realized, pearl string shape Silicon nanowire growth technology is based on IP-SLS method, by regulating and controlling the thickness of metal catalytic drop and amorphous silicon, by interaction inherent between metal catalytic drop and nano wire, original position autonomous growth goes out the nano wire of diameter mechanical periodicity, proves after transmission electron microscope characterizes, it only has diameter to change, and nano wire itself keeps high quality single crystal.In conjunction with the position of the technological orientation catalysed particulates such as photoetching, the plane high-quality pearl string shape silicon nanowire array that self assembly is self-align just can be obtained.Because the selection of this type of nanowire growth and substrate has nothing to do, except common nano wire transfer techniques, its still can at the bottom of part high temperature-resistant liner on to realize primary reconstruction self-align.Again owing to itself being exactly monocrystalline silicon, can merge mutually with existing silicon technology easily, be convenient to integra-tion application.The special coulomb island structure that the nano wire grown due to the present invention has, will transport regulation and control to realizing single electron, prepare single-electron device and have revolutionary breakthrough.Again because its growth is completely by the determining positions of catalysis inducing metal, the self-align array growth of self assembly can be realized, by single electron quantum device integrated in there is huge applications prospect.The self assembly self-align single electron quantum device preparation that the technology is (Button-up) technology based on from bottom to top and integratedly provide key technology basis.Therefore, the technology that the self-align preparation of IPSLS growth mechanism self assembly that the present invention takes grows pearl string shape silicon nanowires has broad application prospects in single electron quantum device is prepared and be integrated.
Four, accompanying drawing explanation
Fig. 1: the manufacturing flow chart of a kind of high-quality pearl string shape monocrystalline silicon nano line provided by the invention.
In Fig. 2, (a) is the SEM shape appearance figure of pearl string shape monocrystalline silicon nano line.B TEM image that ()-(d) is nano wire, wherein (b) is low power TEM image, and (c) and (d) is the high-resolution TEM image of A and B point (region) in (b).
Fig. 3. (a), under Coulomb blockade effect, pearl string shape nano wire realizes the schematic diagram that single electron transports, and (b) prepares schematic diagram for single electron quantum device.
Five, embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, the present invention is described in more detail.
Embodiment 1, Sn (tin) induced growth diameter is in about 100nm/300nm periodically variable pearl string shape monocrystalline silicon nanometer
Line
1) general thickness 500 μm and front is adopted with the N-shaped heavy doping monocrystalline silicon piece of the silicon dioxide layer of 300nm dry-oxygen oxidation as experiment substrate.And adopt RCA standard cleaning method to clean substrate, obtain totally smooth substrate.
2) adopt conventional lithographic techniques, substrate is produced stripe array pattern, and the width of bar shaped is 10 μm, spacing 100 μm.Adopt the method for thermal evaporation at the inducing metal Sn with evaporation 100nm on the substrate of photoengraving pattern.After removing photoresist with acetone, leave the stripe array pattern of metal Sn.
3) sample is put into PECVD system, after vacuumizing, temperature 320 DEG C, under the atmosphere of hydrogen of pressure 80Pa, open the radio frequency of PECVD system, power is 20W, utilize the hydrogen gas plasma processing sample 10min formed, form the metal Sn drop of about 500-800nm.
4) be cooled to 120 DEG C in a pecvd system, pump the hydrogen in system, pass into silane, pressure maintains 18Pa, under radio-frequency power 2W, substrate covers the amorphous silicon membrane that one deck is about 60nm.
5) PECVD system is warming up to 400 DEG C, and anneal 30min in the atmosphere of hydrogen of 130Pa.The Sn drop be activated will absorb the amorphous silicon of surrounding, and autonomous induction grows diameter at about 100nm/300nm periodically variable pearl string shape monocrystalline silicon nano line.
Embodiment 2, Sn (tin) induced growth diameter is at about 30nm/80nm periodically variable pearl string shape monocrystalline silicon nano line
1) general thickness 500 μm and front is adopted with the N-shaped heavy doping monocrystalline silicon piece of the silicon dioxide layer of 300nm dry-oxygen oxidation as experiment substrate.And adopt RCA standard cleaning method to clean substrate, obtain totally smooth substrate.
2) adopt conventional lithographic techniques, substrate is produced stripe array pattern, and the width of bar shaped is 10 μm, spacing 100 μm.Adopt the method for thermal evaporation at the inducing metal Sn with evaporation 100nm on the substrate of photoengraving pattern.After removing photoresist with acetone, leave the stripe array pattern of metal Sn.
3) sample is put into PECVD system, after vacuumizing, temperature 320 DEG C, under the atmosphere of hydrogen of pressure 80Pa, open the radio frequency of PECVD system, power is 20W, utilize the hydrogen gas plasma processing sample 10min formed, form the metal Sn drop of about 500-800nm.
4) be cooled to 120 DEG C in a pecvd system, pump the hydrogen in system, pass into silane, pressure maintains 18Pa, under radio-frequency power 2W, substrate covers the amorphous silicon membrane that one deck is about 30nm.
5) PECVD system is warming up to 400 DEG C, and anneal 30min in the atmosphere of hydrogen of 130Pa.The Sn drop be activated will absorb the amorphous silicon of surrounding, and autonomous induction grows diameter at about 30nm/80nm periodically variable pearl string shape monocrystalline silicon nano line.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. prepare the method for plane bead string shape monocrystalline silicon nano line for one kind, it is characterized in that step is as follows, 1) on smooth substrate, coordinate photoetching or other pattern generation techniques, at locating area evaporation In, Sn or Bi inducing metal film, be the initial position of nanowire growth, thickness of metal film in several nanometer to tens nanometers; 2) above-mentioned substrate is put into PECVD system chamber, after temperature 200 DEG C-500 DEG C, hydrogen gas plasma processing sample 5-30 minute, metal film can form the accurate nano-catalytic metallic particles of a large amount of tens nanometers to different size between several microns; 3) amorphous silicon layer of one deck suitable thickness (a few nanometer is to hundreds of nanometer) in a pecvd system, is covered as presoma dielectric layer; 4) annealing, temperature are at 350-400 DEG C in a vacuum or in the non-oxidizing atmosphere such as hydrogen, nitrogen, and catalyticing metal particle can be activated, spontaneous absorption amorphous silicon, separate out monocrystalline silicon, and diameter generating period change simultaneously, grows pearl string shape nano wire.
2. method according to claim 1, is characterized in that: step 2) middle plasma power 2-20W.
3. method according to claim 1, is characterized in that: step 4) in a vacuum or in the non-oxidizing atmosphere such as hydrogen, nitrogen annealing time be 30-60min.
4. method according to claim 1, it is characterized in that: the growth being regulated and controled pearl string shape nano wire by the temperature conditions of plasma treatment time power and temperature in adjustment growth course, covering amorphous silicon thickness and growth, annealing temperature and time parameter, obtains the silicon nanowires that diameter, Cycle Length etc. are adjustable.
5. method according to claim 1, it is characterized in that the adjusting and controlling growth of the size of pearl string shape nano wire refers to the size by regulation and control metal catalytic drop, amorphous silicon thickness, annealing temperature and time parameter realize.
6. method according to claim 1, is characterized in that described inducing metal both can be Sn, Bi or In, or other can the metal of induced growth plane nano line.
7. method according to claim 1, it is characterized in that the pearl string shape nano wire of planar growth both can be silicon nanowires, Ge semiconductor nano wire, nano wire is intrinsic nano wire or doped nanowire.
8. method according to claim 1, is characterized in that the location mask plate of inducing metal, or utilizes photoetching technique, nanometer embossing.
9. method according to claim 1, is characterized in that the substrate growing pearl string shape silicon nanowires is planar semiconductor substrate, or organic resistance to 350 DEG C of high-temperature material substrates.
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Cited By (2)
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| CN107640741A (en) * | 2017-03-15 | 2018-01-30 | 南京大学 | A kind of plane germanium silicon based on the supply of heterogeneous lamination noncrystal membrane and related nanowire growth pattern and the method for component regulation and control |
| CN108231542A (en) * | 2018-01-09 | 2018-06-29 | 南京大学 | A kind of plane germanium silicon based on heterogeneous lamination noncrystal membrane and related nanowire growth method |
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| CN101891145A (en) * | 2009-05-22 | 2010-11-24 | 熊长宏 | Silicon nanowire preparation by gas-liquid-solid phase method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107640741A (en) * | 2017-03-15 | 2018-01-30 | 南京大学 | A kind of plane germanium silicon based on the supply of heterogeneous lamination noncrystal membrane and related nanowire growth pattern and the method for component regulation and control |
| CN107640741B (en) * | 2017-03-15 | 2019-11-15 | 南京大学 | A method of plane germanium silicon and related nanowire growth pattern and component regulation based on the supply of heterogeneous lamination noncrystal membrane |
| CN108231542A (en) * | 2018-01-09 | 2018-06-29 | 南京大学 | A kind of plane germanium silicon based on heterogeneous lamination noncrystal membrane and related nanowire growth method |
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