CN105499601B - Preparation method of silver nanocluster - Google Patents
Preparation method of silver nanocluster Download PDFInfo
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- CN105499601B CN105499601B CN201510964206.0A CN201510964206A CN105499601B CN 105499601 B CN105499601 B CN 105499601B CN 201510964206 A CN201510964206 A CN 201510964206A CN 105499601 B CN105499601 B CN 105499601B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title abstract description 7
- 229910052709 silver Inorganic materials 0.000 title abstract description 7
- 239000004332 silver Substances 0.000 title abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 79
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 79
- 239000010703 silicon Substances 0.000 claims abstract description 79
- 239000002070 nanowire Substances 0.000 claims abstract description 47
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 27
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007853 buffer solution Substances 0.000 claims abstract description 23
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 108020004414 DNA Proteins 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000007654 immersion Methods 0.000 claims description 11
- 238000011010 flushing procedure Methods 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000008363 phosphate buffer Substances 0.000 claims description 3
- 108091028043 Nucleic acid sequence Proteins 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 230000001934 delay Effects 0.000 claims description 2
- 239000011435 rock Substances 0.000 claims description 2
- 150000001805 chlorine compounds Chemical group 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 240000007594 Oryza sativa Species 0.000 abstract 1
- 235000007164 Oryza sativa Nutrition 0.000 abstract 1
- 235000009566 rice Nutrition 0.000 abstract 1
- 239000000725 suspension Substances 0.000 description 8
- 101710134784 Agnoprotein Proteins 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 5
- 239000012279 sodium borohydride Substances 0.000 description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 description 4
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010249 in-situ analysis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of silver nanoclusters, which comprises the following steps: 1) mixing AgNO3Solution and DNA solution according to AgNO3Mixing the DNA with the DNA at a molar ratio of 6:1-16:1, adding a certain volume of first buffer solution, quickly shaking for 30s-2min, and standing for 10-30 min; 2) placing the silicon nanowire array in 2-8% hydrofluoric acid (HF) solution for 10-40min, cleaning with deoxygenated water, and ultrasonically treating to obtain silicon nanowire solution with silicon-hydrogen bonds on the surface; 3) adding the silicon nanowire with the surface having the silicon-hydrogen bond into the mixed solution in the step 1), quickly shaking for 30s-3min, standing for 5-10 h, discarding the silicon nanowire at the lower layer to obtain the silver nanowireAnd (5) clustering rice. The invention uses the silicon-hydrogen bond on the surface of the silicon nanowire as a reducing agent to prepare the silver nanocluster, the silicon nanowire can be removed by standing, and the obtained silver nanocluster can be directly used for subsequent biological application and is not influenced by a small amount of NaBH in a common method4Or reaction products thereof.
Description
Technical field
The invention belongs to the preparing technical field of the preparation field of nanocluster, more particularly to noble metal nano cluster.
Background technology
The molecular noble metal nano cluster of a small amount of metal raw, due to making it be passed in chemistry with unique photoluminescent property
There is important potential application in sense, bio-imaging and biological in-situ analysis.Therefore, in recent years, many has been developed on noble metal
The preparation method of cluster, mainly including template, monolayer Protection Code, etching method etc..Wherein using DNA as the silver nanoparticle of template
The features such as preparation method of cluster is simple, emission wavelength easily regulates and controls, hypotoxicity, bio-compatibility are good and light is stable makes with DNA
For template ag nano-cluster have in terms of bio-imaging, chemical detection many outstanding work (J.H.Yu, S.Choi,
R.M.Dickson,Angew.Chem.Int.Ed.2009,48,318–320；S.Choi, R.M.Dicksonc, J.H.Yu,
Chem.Soc.Rev.,2012,41,1867–1891).However, this method generally uses NaBH4Reducing process, obtained Yin Na
Rice cluster contains a small amount of NaBH4Or its reaction product, it is unfavorable for the application that ag nano-cluster is analyzed in biological in-situ.
The content of the invention
The technical problem to be solved in the present invention is a kind of method for preparing ag nano-cluster of offer, and this method does not have
NaBH4Residual or its reaction product.
For the above-mentioned technical problem of solution, the present invention uses following technical proposals：
A kind of preparation method of ag nano-cluster, it comprises the following steps：
1) by AgNO3Solution and DNA solution press AgNO3With DNA mol ratio 6:1-16:1 mixing, adds certain volume
First buffer solution, quickly rocks 30s-2min, stands 10-30min；
2) silicon nanowire array is placed in 10-40min in 2-8% hydrofluoric acid (HF) solution, cleaned with deaerated water, ultrasonic
There is the silicon nanowires solution of si-h bond to surface；
3) by the surface have si-h bond silicon nanowires add step 1) in mixed solution in, Quick shaking 30s-
3min, stands 5-10 hours, takes supernatant liquor, obtain ag nano-cluster.
Step 1) described in AgNO3Solution is 1-2mM AgNO3The aqueous solution.
First buffer solution is that can generate ag nano-cluster and keep the stable buffer solutions of DNA, it is therefore preferable to, described the
One buffer solution is pH7.0 buffer solution, it is highly preferred that first buffer solution delays for the phosphate of pH7.0 not chloride ion-containing
Fliud flushing.
Preferably, step 1) in AgNO3Stood with DNA mixed liquor in frozen water.
Described DNA sequence dna is：a)5’-AATTCCCCCCCCCCCCTTAA-3’；b)5’-CCCACCCACCCTCCCA-
3’；Or c) 5 '-CCCCCCCCCCCC-3 '.
The deaerated water is the water for removing oxygen, it is therefore preferable to which logical nitrogen half an hour removes the water of oxygen.
Preferably, there is the silicon nanowires of si-h bond to be added immediately after preparing in mixed solution 1) surface.
Step 1) DNA solution is 50-150 μM of DNA solution, it is preferable that and the DNA solution pH value is pH7.4.
The DNA solution is the phosphate buffer of not chloride ion-containing.
Preferably, step 3) described in dwell temperature be 4 DEG C standing.
The silicon nanowire array preparation method is：Various sizes of silicon chip is taken, is entered successively with acetone, ethanol, distilled water
Row is cleaned by ultrasonic, it is preferable that the time of ultrasonic cleaning is 10~30 minutes；By the silicon chip after cleaning be placed in containing concentration be 3~
8mmol/L AgNO3Soaked with 2~7mol/L HF mixed aqueous solution, it is preferable that the time of immersion is 5~10
Minute；The H containing concentration for 2~7mol/L HF and 0.05~0.4mol/L will be immersed after silicon chip extracting2O2Mixed aqueous solution
In, and be incubated in 40~60 DEG C of water-bath, silicon chip is taken out after 15~45 minutes, mass concentration is put into for 36% concentrated hydrochloric acid and matter
Amount concentration be 36% concentrated nitric acid volume ratio be 3: 1 mixed liquor in, immersion 0.5~2.5 hour after take out silicon chip；Use distilled water
Dried naturally after flushing, obtain a diameter of 200- of the silicon nanowire array being made up of silicon nanowires, wherein silicon nanowires
350nm, length is 10-30 μm of silicon nanowires.
Beneficial effects of the present invention are as follows：
The present invention is as reducing agent to prepare ag nano-cluster by the use of the si-h bond of surface of silicon nanowires, passes through standing
Silicon nanowires is removed, obtained ag nano-cluster can be directly used for follow-up biologic applications, not by a small amount of in common method
NaBH4Or the influence of its reaction product.
Brief description of the drawings
The embodiment to the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the fluorescence spectrum for the ag nano-cluster that the embodiment of the present invention 1 is obtained.
Fig. 2 shows the TEM photos for the ag nano-cluster that the embodiment of the present invention 1 is obtained.
Fig. 3 shows that the TEM photos wherein 3a for the silicon nanowires that chemical etching method is obtained in the embodiment of the present invention 1 is side view
Figure, 3b is top view.
Fig. 4 shows the fluorescence spectrum for the ag nano-cluster that the embodiment of the present invention 2 is obtained.
Fig. 5 shows the fluorescence spectrum for the ag nano-cluster that the embodiment of the present invention 2 is obtained.
Embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1.
By 20 μ L 1.5mM AgNO3The aqueous solution with containing 50 μ L 100 μM of DNA (5 '-
AATTCCCCCCCCCCCCTTAA-3 ') 20mM PB7.4 buffer solutions mixing, add 110 μ L 20mM PB7.0 buffer solutions,
30s acutely is swayed, 15min in frozen water is placed in.The PB7.0 buffer solutions of the 20mM delay for the phosphoric acid of pH7.0 not chloride ion-containing
Fliud flushing；PB7.4 buffer solutions are the phosphate buffer of pH7.4 not chloride ion-containing.
Silicon nanowire array is placed in 30min in 4% HF solution, cleaned with deaerated water, ultrasound is obtained with surface silicon
The μ g/mL of silicon nanowires suspension 4 of hydrogen bond.20 μ L this suspension are added to above-mentioned AgNO immediately3In DNA mixed liquors,
30s acutely is swayed, 4 DEG C of refrigerators are placed in 10 hours, supernatant liquor is taken, obtains the ag nano-cluster of 570 nanometers of launch wavelength.Gained
Shown in luminescent spectrum Fig. 1 and TEM Fig. 2 of the ag nano-cluster arrived.
The silicon nanowire array preparation method：Various sizes of n (100) silicon chip is taken, successively with 90% acetone, 90%
Ethanol, distilled water carry out be cleaned by ultrasonic 10 minutes, by the silicon chip after cleaning be placed in containing concentration be 5mmol/L AgNO3With
Immersion 8 minutes is carried out in 4.6mol/L HF mixed aqueous solution, will be immersed after silicon chip extracting containing concentration is 4.6mol/L's
HF and 0.2mol/L H2O2Mixed aqueous solution in, system by temperature for 50 DEG C water-bath be incubated, take out silicon chip after 30 minutes,
It is put into the mixed liquor that the volume ratio for the concentrated nitric acid that concentrated hydrochloric acid that mass concentration is 36% is 36% with mass concentration is 3: 1, leaching
Bubble takes out silicon chip after 1 hour, is dried naturally with after distilled water flushing, obtains the silicon nanowire array being made up of silicon nanowires.Silicon
Shown in SEM photograph Fig. 3 of nano-wire array.
Described 90% acetone is the obtained acetone soln being diluted with water, and following embodiments are identical.
Described 90% ethanol is the obtained ethanol solution being diluted with water, and following embodiments are identical.
Embodiment 2
By 96 μ L 1.5mM AgNO3The aqueous solution and 100 μM of DNA (the 5 '-CCCACCCACCCTCCCA- containing 90 μ L
3 ') 20mM PB7.4 buffer solutions mixing, adds 34 μ L20mM PB7.0 buffer solutions, acutely sways 1min, be placed in frozen water
30min。
Silicon nanowire array is placed in 40min in 2% HF solution, cleaned with deaerated water, ultrasound obtains surface si-h bond
The μ g/mL of silicon nanowires suspension 4.20 μ L this suspension are added to above-mentioned AgNO immediately3In DNA mixed liquors, acutely
1min is swayed, 4 DEG C of refrigerators are placed in 5 hours, supernatant liquor is taken, the silver nanoparticle group that launch wavelength is 625 nanometers and 823 nanometers is obtained
Cluster.Shown in luminescent spectrum Fig. 4 of resulting ag nano-cluster and 5.
Silicon nanowire array preparation method：Take various sizes of n (100) silicon chip, successively with anhydrous propanone, absolute ethyl alcohol,
Distilled water be cleaned by ultrasonic 30 minutes, and the silicon chip after cleaning is placed in containing the AgNO that concentration is 3mmol/L3With 2mol/L's
Immersion 10 minutes is carried out in HF mixed aqueous solution, will be immersed after silicon chip extracting containing the HF and 0.05mol/ that concentration is 7mol/L
L H2O2Mixed aqueous solution in, system by temperature for 60 DEG C water-bath be incubated, take out silicon chip after 45 minutes, be put into mass concentration
In the mixed liquor that the volume ratio for the concentrated nitric acid that concentrated hydrochloric acid and mass concentration for 36% are 36% is 3: 1, immersion takes after 0.5 hour
Go out silicon chip, dried naturally with after distilled water flushing, obtain the silicon nanowire array being made up of silicon nanowires.
Embodiment 3
By 36 μ L 1.5mM AgNO3The aqueous solution and 100 μM of DNA (5 '-CCCCCCCCCCCC-3 ') containing 90 μ L
20mM PB7.4 buffer solutions are mixed, and are added 34 μ L 20mM PB7.0 buffer solutions, are acutely swayed 2min, be placed in 10min in frozen water.
Silicon nanowire array is placed in 10min in 8% HF solution, cleaned with deaerated water, ultrasound obtains surface si-h bond
The μ g/mL of silicon nanowires suspension 4.20 μ L this suspension are added in above-mentioned AgNO3 and DNA mixed liquors immediately, acutely
3min is swayed, 4 DEG C of refrigerators are placed in 8 hours, supernatant liquor is taken, obtains 630 nanometers of ag nano-clusters of launch wavelength.As a result with Fig. 2
It is similar.
Silicon nanowire array preparation method：Various sizes of n (100) silicon chip is taken, successively with 50% acetone, 60% second
Alcohol, distilled water be cleaned by ultrasonic 15 minutes, and the silicon chip after cleaning is placed in containing the AgNO that concentration is 5mmol/L3And 4mol/
In L HF mixed aqueous solution carry out immersion 5 minutes, will be immersed after silicon chip extracting containing concentration for 2mol/L HF and
0.2mol/L H2O2Mixed aqueous solution in, system by temperature for 40 DEG C water-bath be incubated, take out silicon chip after 15 minutes, be put into
In the mixed liquor that the volume ratio for the concentrated nitric acid that the concentrated hydrochloric acid that mass concentration is 36% is 36% with mass concentration is 3: 1, immersion 2.5
Silicon chip is taken out after hour, is dried naturally with after distilled water flushing, obtains the silicon nanowire array being made up of silicon nanowires.
Embodiment 4
By 24 μ L 1.5mM AgNO3The aqueous solution and 100 μM of DNA (5 '-AATTCCCCCCCCCCCCTTAA- containing 60 μ L
3 ') 20mM PB7.4 buffer solutions mixing, adds 22 μ L20mM PB7.0 buffer solutions, acutely sways 30s, be placed in frozen water
15min。
Silicon nanowire array is placed in 30min in 4% HF solution, cleaned with deaerated water, ultrasound obtains surface si-h bond
The μ g/mL of silicon nanowires suspension 4.20 μ L this suspension are added to above-mentioned AgNO immediately3In DNA mixed liquors, acutely
30s is swayed, 4 DEG C of refrigerators are placed in 10 hours, supernatant liquor is taken, obtains ag nano-cluster.Resulting ag nano-cluster it is luminous
Spectrum is similar to Example 1.
Silicon nanowire array preparation method：Various sizes of n (100) silicon chip is taken, successively with 40% acetone, 50% second
Alcohol, distilled water be cleaned by ultrasonic 10 minutes, and the silicon chip after cleaning is placed in containing the AgNO that concentration is 8mmol/L3And 7mol/
In L HF mixed aqueous solution carry out immersion 8 minutes, will be immersed after silicon chip extracting containing concentration for 5mol/L HF and
0.2mol/L H2O2Mixed aqueous solution in, system by temperature for 50 DEG C water-bath be incubated, take out silicon chip after 30 minutes, be put into
In the mixed liquor that the volume ratio for the concentrated nitric acid that the concentrated hydrochloric acid that mass concentration is 36% is 36% with mass concentration is 3: 1, immersion 1 is small
When after take out silicon chip, dried naturally with after distilled water flushing, obtain the silicon nanowire array being made up of silicon nanowires.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (12)
1. a kind of preparation method of ag nano-cluster, it is characterised in that this method comprises the following steps：
1) by AgNO3Solution and DNA solution press AgNO3With DNA mol ratio 6:1-16:1 mixing, adds the first of certain volume
Buffer solution, quickly rocks 30s-2min, stands 10-30min；
2) silicon nanowire array is placed in 10-40min in 2-8% hydrofluoric acid (HF) solution, cleaned with deaerated water, ultrasound obtains table
Face has the silicon nanowires solution of si-h bond；
3) by the surface have si-h bond silicon nanowires add step 1) in mixed solution in, Quick shaking 30s-3min,
5-10 hours are stood, lower floor's silicon nanowires is discarded, obtains ag nano-cluster.
2. preparation method according to claim 1, it is characterised in that step 1) described in AgNO3Solution is 1-2mM
AgNO3The aqueous solution.
3. preparation method according to claim 1, it is characterised in that first buffer solution is that can generate ag nano-cluster
The buffer solution stable with DNA is kept.
4. preparation method according to claim 1, it is characterised in that first buffer solution is pH7.0 buffer solution.
5. preparation method according to claim 1, it is characterised in that first buffer solution for pH7.0 it is not chloride from
The phosphate buffer of son.
6. preparation method according to claim 1, it is characterised in that step 1) in AgNO3Mixed liquor with DNA is in frozen water
It is middle to stand.
7. preparation method according to claim 1, it is characterised in that described DNA sequence dna is：a)5’-
AATTCCCCCCCCCCCCTTAA-3’；b)5’-CCCACCCACCCTCCCA-3’；Or 5 '-CCCCCCCCCCCC-3 ' c).
8. preparation method according to claim 1, it is characterised in that step 1) DNA solution is 50-150 μM of DNA
Solution, pH value 7.4.
9. preparation method according to claim 8, it is characterised in that the DNA solution delays for the phosphoric acid of not chloride ion-containing
Fliud flushing.
10. preparation method according to claim 1, it is characterised in that step 3) described stand be in 4 DEG C of standings.
11. preparation method according to claim 1, it is characterised in that the deaerated water is the water for removing oxygen.
12. preparation method according to claim 1, it is characterised in that the silicon nanowire array preparation method is：Take not
With the silicon chip of size, it is cleaned by ultrasonic successively with acetone, ethanol, distilled water；It is 3 that silicon chip after cleaning, which is placed in containing concentration,
~8mmol/L AgNO3Soaked with 2~7mol/L HF mixed aqueous solution；By immersion after silicon chip extracting containing dense
Spend the H of the HF and 0.05~0.4mol/L for 2~7mol/L2O2Mixed aqueous solution in, and in 40~60 DEG C of water-bath protect
Temperature, silicon chip is taken out after 15~45 minutes, is put into the volume that mass concentration is 36% concentrated hydrochloric acid and mass concentration is 36% concentrated nitric acid
Than in the mixed liquor for 3: 1, immersion takes out silicon chip after 0.5~2.5 hour；Dried, obtained by silicon naturally with after distilled water flushing
A diameter of 200-350nm of silicon nanowire array, wherein silicon nanowires that nano wire is constituted, length is 10-30 μm of silicon nanometer
Line.
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