CN104649273A - Preparation method of low-doped porous P-type silicon nanowire - Google Patents
Preparation method of low-doped porous P-type silicon nanowire Download PDFInfo
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- CN104649273A CN104649273A CN201310602511.6A CN201310602511A CN104649273A CN 104649273 A CN104649273 A CN 104649273A CN 201310602511 A CN201310602511 A CN 201310602511A CN 104649273 A CN104649273 A CN 104649273A
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Abstract
The invention relates to technical field of a nanomaterial, and particularly relates to a preparation method of a low-doped porous P-type silicon nanowire. The preparation method comprises the following steps: soaking the low-doped porous P-type silicon material into a concentrated sulfuric acid and hydrogen peroxide mixed solution, taking out the low-doped porous P-type silicon material after soaking, and then soaking the low-doped porous P-type silicon material in a hydrofluoric acid solution to obtain a first prepared material; transferring the first prepared material into a 5-15mmol/L metal nitrate solution, and soaking for 30-120 seconds to obtain a second prepared material, wherein the solvent of the metal nitrate solution is a 2-10wt% hydrofluoric acid water solution; washing the second prepared material with water; placing the washed second prepared material into a 0.1-0.6mol/L hydrogen peroxide solution, corroding for 2-60 minutes at room temperature and taking out, to obtain a third prepared material, wherein the solvent of the hydrofluoric acid solution is a 2-10wt% hydrofluoric acid water solution; and placing the third prepared material into a nitrate acid solution and soaking for 1-5 hours, to obtain the low-doped porous P-type silicon nanowire.
Description
Technical field
The invention belongs to technical field prepared by nano material, refer in particular to low-doped porous P-type silicon nano wire normal temperature preparation method.
Background technology
Monocrystalline porous silicon nano wire has unique semiconductor property, photoelectric property and good mechanical properties, biocompatibility, huge specific surface area, and surface is easily modified, in photochemical catalysis, biosensor and photoelectric device etc., there is significant application value.Current scholar's The book of Changes works out the multiple method preparing monocrystalline porous silicon nano wire, wherein metal assistant chemical etch mainly through methods such as in-situ reducing at silicon materials surface deposition layer of metal nano particle, again through the corrosion treatment of corrosive fluid different time, finally obtain monocrystalline porous silicon nano wire with the metallic particles of acid fluid dissolves removal surface attachment.Metal assistant chemical etch easy handling, equipment is simple, and the reaction times is short, and the aperture of monocrystalline porous silicon nano wire and length are easy to regulation and control.
Metal assistant chemical etch prepares the direct effective means of monocrystalline porous silicon nano wire.But during by metal assistant chemical etch, the doping level of single crystal silicon material can affect the surfaceness of the silicon nanowires obtained, and even determines and whether can produce aperture structure.Research shows, generally with expensive highly doped type silicon materials (N-type silicon chip resistance: be less than 0.02 Ω cm; P-type silicon sheet resistivity: be less than 0.005 Ω cm) silicon nanowires (J.Am.Chem.Soc., 2009,9,3550 with vesicular structure could be made by metal assistant chemical etch as starting material; Nano Lett., 2009,9,4539).In this preparation process, production cost is higher, seriously constrain porous silicon nano wire practical application.
A small amount of report is had to provide the method being prepared low-doped porous silicon nano wire with low-doped silicon chip by metal assistant chemical etch at present, but this method is generally limited to the low-doped silicon of N-type as starting material, and preparation process requires heating (J.Mater.Chem., 2011,21,801), the waste of the energy and the production means is caused, and the aperture of sample and the more difficult regulation and control of length.
Summary of the invention
For solving the problem, the invention provides a kind of preparation method of low-doped porous P-type silicon nano wire, comprising the steps:
Step 1: immersed by low-doped P-type silicon material in the mixed solution of the vitriol oil and hydrogen peroxide, soaks after 5 ~ 10 minutes and takes out, then the hydrofluoric acid solution immersion of putting into 2 ~ 10wt% obtained the first saw lumber after 1 ~ 10 minute;
Wherein, in the mixed solution of the described vitriol oil and hydrogen peroxide, the ratio of the vitriol oil and hydrogen peroxide is 3:1 ~ 4:1;
Step 2: it is in the metal nitrate salt brine solution of 5 ~ 15mmol/L that described first saw lumber is moved into concentration, soaks 30 ~ 120 seconds, makes described first saw lumber obtains the second saw lumber after depositing metallic nanoparticles;
Wherein, the solvent of described metal-nitrate solutions is 2 ~ 10wt% hydrofluoric acid aqueous solution;
Step 3: with described second saw lumber of water cleaning;
Step 4: the superoxol that concentration is 0.1 ~ 0.6mol/L is put in the second saw lumber after step 3 is cleaned, corrodes under normal temperature after 2 ~ 60 minutes and takes out, obtain the 3rd saw lumber;
Wherein, the solvent of described superoxol is 2 ~ 10wt% hydrofluoric acid aqueous solution;
Step 5: described 3rd saw lumber is put into aqueous nitric acid and soak 1 ~ 5 hour, namely obtain described low-doped porous P-type silicon nano wire.
Further, the concentration of described metal nitrate salt brine solution is 5 ~ 12.5mmol/L.
Further, described metal nitrate is Silver Nitrate or iron nitrate.
Further, the concentration of described hydrofluoric acid aqueous solution is 5 ~ 10wt%.
Further, the impedance of described P-type silicon nano wire is 0.005 ~ 1 Ω cm.
Further, described aqueous nitric acid concentration is 6.5 ~ 10wt%.
Beneficial effect:
The normal temperature preparation of porous silicon nano wire provided by the invention and regulation and control length and the method in aperture, achieve uniform pore diameter, the normal temperature preparation of low-doped monocrystalline porous P-type silicon nano wire that Absorbable organic halogens stores.By the factor such as concentration and reaction times of modified hydrogen oxide corrosive fluid, the pore size of low-doped P type porous silicon nano wire can be regulated and controled in 5 ~ 20 nanometer range, and in 1 ~ 50 micrometer range, regulate and control length; The concentration of hydrogen peroxide is larger, and aperture is larger, and the reaction times of hydrogen peroxide is longer, and the length of nano wire is longer.And the starting material used are cheap low-doped silicon materials, considerably reduce the preparation cost of porous silicon nano wire.The present invention has potential using value in photoelectric device, has good Social benefit and economic benefit.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 low-doped porous P-type silicon nano wire.
Fig. 2 is the transmission electron microscope picture of the embodiment of the present invention 1 low-doped porous P-type silicon nano wire.
Fig. 3 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 2 low-doped porous P-type silicon nano wire.
Fig. 4 is the transmission electron microscope picture of the embodiment of the present invention 2 low-doped porous P-type silicon nano wire.
Fig. 5 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 3 low-doped porous P-type silicon nano wire.
Fig. 6 is the transmission electron microscope picture of the embodiment of the present invention 3 low-doped porous P-type silicon nano wire.
Fig. 7 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 4 low-doped porous P-type silicon nano wire.
Fig. 8 is the transmission electron microscope picture of the embodiment of the present invention 4 low-doped porous P-type silicon nano wire.
Fig. 9 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 5 low-doped porous P-type silicon nano wire.
Figure 10 is the transmission electron microscope picture of the embodiment of the present invention 5 low-doped porous P-type silicon nano wire.
Embodiment
Below in conjunction with accompanying drawing, each embodiment of invention is elaborated.
Embodiment 1
First, various solution is prepared.
Prepare hydrofluoric acid (HF) aqueous solution of 5wt% and 10wt% respectively, for subsequent use.
Get the HF aqueous solution of the above-mentioned 5wt% of 10ml, then add 14.1mg Silver Nitrate (AgNO
3), stirring and dissolving is made into the AgNO of 8.3mmol/L
3solution.
Get the hydrogen peroxide (H of a certain amount of commercially available 30wt%
2o
2), add the HF aqueous solution of a certain amount of above-mentioned 10wt%, after mixing, be made into H
2o
2substance withdrawl syndrome is the H of 0.27mol/L
2o
2-HF solution.
Getting the vitriol oil of commercially available 98wt% and the hydrogen peroxide of 30wt%, is that 3:1 prepares mixing solutions according to volume ratio, for subsequent use;
Get the concentrated nitric acid of commercially available 65wt%, the salpeter solution of adding distil water preparation 10wt%, for subsequent use;
The starting material of the present embodiment adopt the silicon chip being of a size of 1x2cm, and doping type is P type, and material impedance is 0.005 ~ 1 Ω cm.
Introduce the concrete preparation process of this low-doped porous P-type silicon nano wire below.
Step 1: immerse in the mixed solution of the above-mentioned vitriol oil and hydrogen peroxide by low-doped P-type silicon material, soaks after 10 minutes and takes out, then the HF solution putting into 5wt% soaks after 10 minutes, removes the organic impurity of aforementioned p-type silicon materials surface attachment, obtains the first saw lumber.
Step 2: described first saw lumber is moved into the AgNO that above-mentioned concentration is 8.3mmol/L
3in solution, soak 60 seconds, make described first saw lumber obtains the second saw lumber after depositing silver nano particle.
Step 3: with the second saw lumber described in a large amount of washed with de-ionized water.
Step 4: the H that concentration is 0.27mol/L is put in the second saw lumber after step 3 is cleaned
2o
2in solution, under normal temperature, corrosion reaction was taken out after 30 minutes, obtained the 3rd saw lumber.
Step 5: the salpeter solution described 3rd saw lumber being put into 10wt% soaks 2 hours, namely obtains described low-doped porous P-type silicon nano wire product.As shown in Figure 1 and Figure 2, the low-doped porous P-type silicon nano wire aperture that the present embodiment obtains, uniform length, its surface presentation single crystal structure, pore size is about 20nm, and length is about 10 μm.
Embodiment 2
With reference to the method for embodiment 1, prepare the HF aqueous solution of 5wt%, 10wt%, the AgNO of 8.3mmol/L respectively
3the H of solution, 0.27mol/L
2o
2the mixed solution of-HF solution, the vitriol oil and hydrogen peroxide (volume ratio 3:1), the salpeter solution of 10wt%.The starting material of the present embodiment are consistent with embodiment 1.
Concrete preparation process is:
Step 1: immerse in the mixed solution of the above-mentioned vitriol oil and hydrogen peroxide by low-doped P-type silicon material, soaks after 10 minutes and takes out, then the HF solution putting into 5wt% soaked after 10 minutes, obtained the first saw lumber;
Step 2: described first saw lumber is moved into the AgNO that above-mentioned concentration is 8.3mmol/L
3in solution, soak 60 seconds, make described first saw lumber obtains the second saw lumber after depositing silver nano particle;
Step 3: with the second saw lumber described in a large amount of washed with de-ionized water;
Step 4: the H that concentration is 0.27mol/L is put in the second saw lumber after step 3 is cleaned
2o
2in solution, under normal temperature, corrosion reaction was taken out after 5 minutes, obtained the 3rd saw lumber.
Step 5: the salpeter solution described 3rd saw lumber being put into 10wt% soaks 5 hours, namely obtains described low-doped porous P-type silicon nano wire product.As shown in Figure 3, Figure 4, the low-doped porous P-type silicon nano wire aperture that the present embodiment obtains, uniform length, its surface presentation single crystal structure, pore size is about 20nm, and length is about 2.8 μm.
Embodiment 3
With reference to the method for embodiment 1, prepare the mixed solution of the HF aqueous solution of 5wt%, 10wt%, the vitriol oil and hydrogen peroxide (volume ratio 2:1) respectively, the salpeter solution of 6.5wt%, for subsequent use.
Get the HF aqueous solution of the above-mentioned 10wt% of 10ml, then add 33.5mg iron nitrate (Fe (NO
3)
3), stirring and dissolving is made into the Fe (NO of 8.3mmol/L
3)
3solution.
Get the hydrogen peroxide (H of a certain amount of commercially available 30wt%
2o
2), add the HF aqueous solution of a certain amount of above-mentioned 5wt%, after mixing, be made into H
2o
2substance withdrawl syndrome is the H of 0.27mol/L
2o
2-HF solution.
Concrete preparation process is:
Step 1: immerse in the mixed solution of the above-mentioned vitriol oil and hydrogen peroxide by low-doped P-type silicon material, soaks after 5 minutes and takes out, then the HF solution putting into 10wt% soaked after 5 minutes, obtained the first saw lumber;
Step 2: described first saw lumber is moved into the Fe (NO that above-mentioned concentration is 8.3mmol/L
3)
3in solution, soak 60 seconds, make described first saw lumber obtains the second saw lumber after depositing silver nano particle;
Step 3: with the second saw lumber described in a large amount of washed with de-ionized water;
Step 4: the H that concentration is 0.27mol/L is put in the second saw lumber after step 3 is cleaned
2o
2in solution, under normal temperature, corrosion reaction was taken out after 60 minutes, obtained the 3rd saw lumber.
Step 5: the salpeter solution described 3rd saw lumber being put into 6.5wt% soaks 2 hours, namely obtains described low-doped porous P-type silicon nano wire product.As shown in Figure 5, Figure 6, the low-doped porous P-type silicon nano wire aperture that the present embodiment obtains, uniform length, its surface presentation single crystal structure, pore size is about 20nm, and length is about 17 μm.
Embodiment 4
With reference to the method for embodiment 1, prepare the mixed solution of the HF aqueous solution of 5wt%, 10wt%, the vitriol oil and hydrogen peroxide (volume ratio 4:1) respectively, the salpeter solution of 6.5wt%, for subsequent use.
Get the HF aqueous solution of the above-mentioned 10wt% of 10ml, then add 8.5mg Silver Nitrate (AgNO
3), stirring and dissolving is made into the AgNO of 5.0mmol/L
3solution.
Get the hydrogen peroxide (H of a certain amount of commercially available 30wt%
2o
2), add the HF aqueous solution of a certain amount of above-mentioned 5wt%, after mixing, be made into H
2o
2substance withdrawl syndrome is the H of 0.15mol/L
2o
2-HF solution.
The starting material of the present embodiment are consistent with embodiment 1.
Concrete preparation process is:
Step 1: immerse in the mixed solution of the above-mentioned vitriol oil and hydrogen peroxide by low-doped P-type silicon material, soaks after 5 minutes and takes out, then the HF solution putting into 10wt% soaked after 3 minutes, obtained the first saw lumber;
Step 2: described first saw lumber is moved into the AgNO that above-mentioned concentration is 5.0mmol/L
3in solution, soak 50 seconds, make described first saw lumber obtains the second saw lumber after depositing silver nano particle;
Step 3: with the second saw lumber described in a large amount of washed with de-ionized water;
Step 4: the H that concentration is 0.15mol/L is put in the second saw lumber after step 3 is cleaned
2o
2in solution, under normal temperature, corrosion reaction was taken out after 30 minutes, obtained the 3rd saw lumber.
Step 5: the salpeter solution described 3rd saw lumber being put into 6.5wt% soaks 1 hour, namely obtains described low-doped porous P-type silicon nano wire product.As shown in Figure 7, Figure 8, the low-doped porous P-type silicon nano wire aperture that the present embodiment obtains, uniform length, its surface presentation single crystal structure, pore size is about 10nm, and length is about 10 μm.
Embodiment 5
With reference to the method for embodiment 1, prepare the mixed solution of the HF aqueous solution of 5wt%, 8wt%, 10wt%, the vitriol oil and hydrogen peroxide (volume ratio 4:1) respectively, the nitric acid of 10%, for subsequent use.
Get the HF aqueous solution of the above-mentioned 10wt% of 10ml, then add 50.5mg iron nitrate (Fe (NO
3)
3), stirring and dissolving is made into the Fe (NO of 8.3mmol/L
3)
3solution.
Get the hydrogen peroxide (H of a certain amount of commercially available 30wt%
2o
2), add the HF aqueous solution of a certain amount of above-mentioned 8wt%, after mixing, be made into H
2o
2substance withdrawl syndrome is the H of 0.6mol/L
2o
2-HF solution.
The starting material of the present embodiment are consistent with embodiment 3.
Concrete preparation process is:
Step 1: immerse in the mixed solution of the above-mentioned vitriol oil and hydrogen peroxide by low-doped P-type silicon material, soaks after 8 minutes and takes out, then the HF solution putting into 5wt% soaked after 3 minutes, obtained the first saw lumber;
Step 2: described first saw lumber is moved into the AgNO that above-mentioned concentration is 12.5mmol/L
3in solution, soak 100 seconds, make described first saw lumber obtains the second saw lumber after depositing silver nano particle;
Step 3: with the second saw lumber described in a large amount of washed with de-ionized water;
Step 4: the H that concentration is 0.6mol/L is put in the second saw lumber after step 3 is cleaned
2o
2in solution, under normal temperature, corrosion reaction was taken out after 30 minutes, obtained the 3rd saw lumber.
Step 5: the salpeter solution described 3rd saw lumber being put into 10% soaks 5 hours, namely obtains described low-doped porous P-type silicon nano wire product.As shown in Figure 9, Figure 10, the low-doped porous P-type silicon nano wire aperture that the present embodiment obtains, uniform length, its surface presentation single crystal structure, pore size is about 25nm, and length is about 10 μm.
Integrated embodiment 1 ~ 5 is known, and the low-doped porous P-type silicon nano wire that the present invention obtains realizes the effective controlled adjustment of size.In metal nitrate of the present invention, HF acid, the isoparametric useful range of hydrogen peroxide, the aperture of P-type silicon nano wire increases with the increase of concentration of hydrogen peroxide in step 4, and its length increases with the prolongation of hydroperoxidation time.
Claims (6)
1. a preparation method for low-doped porous P-type silicon nano wire, is characterized in that, comprise the steps:
Step 1: immersed by low-doped P-type silicon material in the mixed solution of the vitriol oil and hydrogen peroxide, soaks after 5 ~ 10 minutes and takes out, then the hydrofluoric acid solution immersion of putting into 2 ~ 10wt% obtained the first saw lumber after 1 ~ 10 minute;
Wherein, in the mixed solution of the described vitriol oil and hydrogen peroxide, the volume ratio of the vitriol oil and hydrogen peroxide is 3:1 ~ 4:1;
Step 2: it is in the metal nitrate salt brine solution of 5 ~ 15mmol/L that described first saw lumber is moved into concentration, soaks 30 ~ 120 seconds, makes described first saw lumber obtains the second saw lumber after depositing metallic nanoparticles;
Wherein, the solvent of described metal-nitrate solutions is 2 ~ 10wt% hydrofluoric acid aqueous solution;
Step 3: with described second saw lumber of water cleaning;
Step 4: the superoxol that concentration is 0.1 ~ 0.6mol/L is put in the second saw lumber after step 3 is cleaned, corrodes under normal temperature after 2 ~ 60 minutes and takes out, obtain the 3rd saw lumber;
Wherein, the solvent of described superoxol is 2 ~ 10wt% hydrofluoric acid aqueous solution;
Step 5: described 3rd saw lumber is put into aqueous nitric acid and soak 1 ~ 5 hour, namely obtain described low-doped porous P-type silicon nano wire.
2. the preparation method of P-type silicon nano wire according to claim 1, it is characterized in that, the concentration of described metal nitrate salt brine solution is 5 ~ 12.5mmol/L.
3. the preparation method of P-type silicon nano wire according to claim 1 or 2, it is characterized in that, described metal nitrate is Silver Nitrate or iron nitrate.
4. the preparation method of P-type silicon nano wire according to claim 1, it is characterized in that, the concentration of described hydrofluoric acid aqueous solution is 5 ~ 10wt%.
5. the preparation method of P-type silicon nano wire according to claim 1, it is characterized in that, the impedance of described P-type silicon nano wire is 0.005 ~ 1 Ω cm.
6. the preparation method of P-type silicon nano wire according to claim 1, it is characterized in that, described aqueous nitric acid concentration is 6.5 ~ 10wt%.
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Cited By (5)
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| CN105854876A (en) * | 2016-04-22 | 2016-08-17 | 大连理工大学 | Preparation method for silicon photocatalyst with 3D multilevel structure |
| CN107118774A (en) * | 2017-04-11 | 2017-09-01 | 枣庄学院 | A kind of method for preparing constant tilt angle silicon nanowire structure |
| CN108786813A (en) * | 2018-06-01 | 2018-11-13 | 福州大学 | A kind of nucleocapsid silicon nanowires-cobaltosic oxide composite photocatalyst material and its preparation and application |
| CN108996471A (en) * | 2018-07-26 | 2018-12-14 | 深圳清华大学研究院 | The graphical preparation method of silicon nanowires and preparation method thereof, silicon nanowires |
| CN110028038A (en) * | 2018-01-12 | 2019-07-19 | 天津大学 | A kind of silicon nanowires micro-structure regulation method towards different field application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854876A (en) * | 2016-04-22 | 2016-08-17 | 大连理工大学 | Preparation method for silicon photocatalyst with 3D multilevel structure |
| CN107118774A (en) * | 2017-04-11 | 2017-09-01 | 枣庄学院 | A kind of method for preparing constant tilt angle silicon nanowire structure |
| CN110028038A (en) * | 2018-01-12 | 2019-07-19 | 天津大学 | A kind of silicon nanowires micro-structure regulation method towards different field application |
| CN108786813A (en) * | 2018-06-01 | 2018-11-13 | 福州大学 | A kind of nucleocapsid silicon nanowires-cobaltosic oxide composite photocatalyst material and its preparation and application |
| CN108786813B (en) * | 2018-06-01 | 2020-11-10 | 福州大学 | Core-shell structure silicon nanowire-cobaltosic oxide composite photocatalytic material and preparation and application thereof |
| CN108996471A (en) * | 2018-07-26 | 2018-12-14 | 深圳清华大学研究院 | The graphical preparation method of silicon nanowires and preparation method thereof, silicon nanowires |
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