CN103147125A - Method for preparing low-cost powdery polycrystalline-silicon base nanowire - Google Patents

Method for preparing low-cost powdery polycrystalline-silicon base nanowire Download PDF

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CN103147125A
CN103147125A CN2013100609994A CN201310060999A CN103147125A CN 103147125 A CN103147125 A CN 103147125A CN 2013100609994 A CN2013100609994 A CN 2013100609994A CN 201310060999 A CN201310060999 A CN 201310060999A CN 103147125 A CN103147125 A CN 103147125A
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powder
polysilicon
base nano
preparation
wire
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CN2013100609994A
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李传波
张春倩
薛春来
成步文
王启明
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Institute of Semiconductors of CAS
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Institute of Semiconductors of CAS
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Abstract

The invention relates to a method for preparing a low-cost powdery polycrystalline-silicon base nanowire. The method comprises the following steps of: (1) taking a substrate, and forming regular meshy air gaps in the interior of the substrate, which is 30 micrometers away from the upper surface of the substrate, by using a laser; (2) growing a nucleation layer, a N-type doped layer, a multiple-quantum-well light-emitting layer, a P-type doped layer and an ITO layer on the substrate in sequence by adopting the MOCVD (metal-organic chemical vapor deposition) method; (3) etching from one side of the ITO layer to the interior of N-type doped layer downwards by adopting a photoetching method to form a mesa; (4) preparing a P-type electrode on the non-etched side of the ITO layer; and (5) preparing a N-type electrode on the mesa. The method provided by the invention is simple in process and low in cost and is suitable for industrial production and application.

Description

The preparation method of cheap powder polysilicon base nano-wire
Technical field
The invention belongs to technical field of semiconductors, particularly a kind of preparation method of cheap powder polysilicon base nano-wire.
Background technology
Scantling will show many specific physiques after dropping to nanometer range, become study hotspot in recent years.As a member of nano material family, the silicon-based nano wire material has shown its wide application prospect (Nature Nanotechnol.3,31,2008 in nanoelectronics, clean energy and sensor field; Nano Lett.8,307,2008; Nature, 451,163,2008; Nature 449,885, and 2007; Nano Lett.4,245,2004), development is cheap, the high quality silicon base nano-wire is of far-reaching significance.
At present Si base nano-wire structure is how by golden catalysis CVD method (Science, 293,1289,2001; .Nature 440,69,2006; Science 313,1100, and 2006) and metal catalytic chemical corrosion method (Angew.Chem., Int.Ed.44,2737,2005) preparation.The nano wire of the former preparation is short, productive rate is low, and can introduce heavy metal, has limited its application.Metal catalytic chemical corrosion method technique is simple, need not main equipment.This method is found for the scholar of Tsing-Hua University the earliest, its silicon nanowires of preparing has that area is large, crystalline phase is consistent, monocrystalline is good, doping content is controlled, silver catalyst can be removed with chemical process, can not produce the advantages such as heavy metal contamination, obtained at present international extensive concern (Appl.Phys.Lett.57,1046,1990; J.Phys.Chem.C 112,4444, and 2008; Nano Lett.9,4539,2009; Adv.Mater.19,744,2007; Adv.Funct.Mater.16,387,2006; Small 1,1062, and 2005).Yet up to the present, this fado is used for the preparation of silicon nanowires as parent material with single crystal silicon material, cost is higher, has limited it in some fields such as the practical application of lithium cell, solar cell, is badly in need of Optimization Technology or preparation method to reduce its cost.And polysilicon sill, the particularly price of polysilicon powder be well below silicon single crystal, if prepare nano wire take it as parent material, cost will significantly reduce, and this will certainly promote the commercial application of silica-based nanowire greatly.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of cheap powder polysilicon base nano-wire, the method manufacture craft is simple, and low price is easy to realize industrialization production and application.
The present invention proposes a kind of preparation method of cheap powder polysilicon base nano-wire, comprise the steps:
Step 1: get a powder polysilicon sill;
Step 2: adopt dilute hydrofluoric acid, rinsing powder polysilicon sill;
Step 3: the powder polysilicon sill of rinsing is placed in corrosive fluid, corrodes, form powder polysilicon base nano-wire;
Step 4: powder polysilicon base nano-wire is separated, cleans;
Step 5: the powder polysilicon base nano-wire that will separate, cleaned is transferred in concentrated nitric acid solution, removes the metal catalyst on powder polysilicon sill;
Step 6: clean, naturally dry, complete preparation.
Description of drawings
For concrete technology contents of the present invention is described, be described in detail as follows below in conjunction with specific examples and Toyota, wherein:
Fig. 1 is preparation method's schema of the present invention;
Fig. 2 is polysilicon nanowire SEM figure of the present invention.
Embodiment
See also shown in Figure 1ly, the invention provides a kind of preparation method of cheap powder polysilicon base nano-wire, comprise the steps:
Step 1: get a powder polysilicon sill, described powder polysilicon sill is polysilicon or polycrystalline silicon germanium, the powder particle size of described polysilicon sill is 50 nanometers-2 millimeter, the particle size uniformity no requirement (NR), the powder of described polysilicon sill can be N-shaped, p-type or intrinsic doping, purity is 2N-8N, and described polycrystalline silicon germanium Ge component is 0.1%-99%;
Step 2: adopt dilute hydrofluoric acid, rinsing powder polysilicon sill is removed the oxide compound on powder polysilicon sill surface, and described hydrofluoric acid concentration is 0.1%-5%, completes under room temperature and agitation condition, and described rinsing time is 1min-15min;
Step 3: the powder polysilicon sill of rinsing is placed in corrosive fluid, corrodes, form powder polysilicon base nano-wire, the temperature of described corrosive fluid is 0-95 ℃, and described corrosive fluid is AgNO3 and HF, is added with H in described corrosive fluid 2O 2, Fe (NO 3) 3Or NH 4NO 3, or and combination, described corrosive fluid additive can be in corrosion process substep add, be intended to control the concentration of corrosion speed and corrosive fluid oxygenant; The etching time of described corrosive fluid can be at 10min-24h, described corrosion process need be placed in stink cupboard, waste liquid need reclaim or do corresponding harmless treatment, such as adding calcium chloride solution to be settled out the heavy metal ion such as fluorion and silver in waste liquid, described corrosion container can add a cover or avoid with corresponding large container the corrosive fluids such as hydrofluoric acid to spill, can add ethanol to assemble to control corrosion speed and nano wire cluster thereof in described corrosive fluid, described corrosion can stirred or rock under condition and carry out, described corrosion container is tetrafluoroethylene or polypropylene material, described corrosive fluid AgNO 3Concentration is that 0.005-0.1mol/l, HF concentration are 3-10mol/l, described additive H 2O 2Concentration is 0.1-3mol/l, NH 4NO 3Concentration is 0.01-1%.
Step 4: powder polysilicon base nano-wire is separated, cleans, and described scavenging solution is deionized water, cleans repeatedly until hydrofluoric acid is cleaned totally;
Step 5: the powder polysilicon base nano-wire that will separate, cleaned is transferred in concentrated nitric acid solution, described concentrated nitric acid concentration is 5-15mol/L, remove the metal catalyst on powder polysilicon sill, it is 5-60min that described concentrated nitric acid is removed the silver catalyst etching time.
Step 6: clean, centrifugation is dried naturally, completes preparation (consult Fig. 2, form cheap powder polysilicon base nano-wire), and described scavenging solution is deionized water, and described wash number is 3-4 time, can adopt the oven dry of heating to accelerate its drying.
The above; only embodiments of the invention; be not that the present invention is done any pro forma restriction; every any simple modification, equivalent variations and modification of above embodiment being done according to the technology of the present invention essence; within all still belonging to the technical solution of the present invention scope, so protection scope of the present invention is when being as the criterion with claims.

Claims (6)

1. the preparation method of a cheap powder polysilicon base nano-wire, comprise the steps:
Step 1: get a powder polysilicon sill;
Step 2: adopt dilute hydrofluoric acid, rinsing powder polysilicon sill;
Step 3: the powder polysilicon sill of rinsing is placed in corrosive fluid, corrodes, form powder polysilicon base nano-wire;
Step 4: powder polysilicon base nano-wire is separated, cleans;
Step 5: the powder polysilicon base nano-wire that will separate, cleaned is transferred in concentrated nitric acid solution, removes the metal catalyst on powder polysilicon sill;
Step 6: clean, naturally dry, complete preparation.
2. the preparation method of cheap powder polysilicon base nano-wire according to claim 1, wherein powder polysilicon sill is polysilicon or polycrystalline silicon germanium.
3. the preparation method of cheap powder polysilicon base nano-wire according to claim 1, wherein the temperature of corrosive fluid is 0-95 ℃.
4. the preparation method of cheap powder polysilicon base nano-wire according to claim 1, wherein corrosive fluid is AgNO3 and HF.
5. the preparation method of cheap powder polysilicon base nano-wire according to claim 1, wherein be added with H in the described corrosive fluid of step 3 2O 2, Fe (NO 3) 3Or NH 4NO 3, or and combination.
6. the preparation method of cheap powder polysilicon base nano-wire according to claim 1, the powder particle size of wherein said polysilicon sill are 50 nanometers-2 millimeter.
CN2013100609994A 2013-02-27 2013-02-27 Method for preparing low-cost powdery polycrystalline-silicon base nanowire Pending CN103147125A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104051791A (en) * 2014-06-23 2014-09-17 中国科学院半导体研究所 Preparation method of polycrystalline silicon-based nano-structure lithium battery
CN114920289A (en) * 2022-05-12 2022-08-19 山东大学 Preparation method of titanium sesquioxide nanowire

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KR101023143B1 (en) * 2004-02-25 2011-03-18 삼성에스디아이 주식회사 Device for texturing silicon wafer for solar cell
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104051791A (en) * 2014-06-23 2014-09-17 中国科学院半导体研究所 Preparation method of polycrystalline silicon-based nano-structure lithium battery
CN114920289A (en) * 2022-05-12 2022-08-19 山东大学 Preparation method of titanium sesquioxide nanowire

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Application publication date: 20130612