CN112458539A - Porous silicon nanowire and preparation method thereof - Google Patents
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Abstract
The invention discloses a porous silicon nanowire and a preparation method thereof. The invention aims to develop a novel preparation method of porous silicon nanowires, which utilizes a centimeter-sized silicon wafer to prepare thousands of nanowires through high oxidation etching, thereby greatly reducing the material cost; simultaneously prepared silicon nanowire surface is covered with SiO2The layer has hydrophilicity, porosity and one-dimensional characteristics, is favorable for improving the interaction between the micromolecule metabolite and increasing the specific surface area, can be used as a unique matrix, is used for matrix-assisted laser desorption ionization time-of-flight mass spectrometry, highly sensitively carries out quantitative analysis and detection on the micromolecule metabolite in serum, and realizes accurate diagnosis and classification of cancer clinically.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a porous silicon nanowire and a preparation method thereof.
Background
The Silicon Nano-wire (SiNW) detection unit is the most common biochip basic unit at present, and is widely applied to the field of biological detection, the main working principle of the SiNW detection unit is similar to that of a Metal Oxide Semiconductor Field Effect Transistor (MOSFET), a Silicon dioxide layer on polycrystalline Silicon (polysilicon) or Silicon (Silicon) is used as gate oxygen, and since biomolecules adsorbed on the Silicon Nano-wire in the Silicon Nano-wire detection unit generally carry charges, the charges can regulate the potential of the Silicon Nano-wire similarly to that of the MOSFET, and further influence the conductive characteristic of the Silicon Nano-wire. Thus, specific biomolecules can be identified by monitoring such conductive properties.
In the silicon nanowire detection unit, a source region and a drain region are connected through a silicon nanowire, and the shape of the silicon nanowire can be a cuboid shape or a bent pipe shape. Of course, the shape of the silicon nanowire can be set to other shapes according to actual conditions. In the SiNW detection unit manufacturing process, since the silicon nanowire is a very thin polysilicon line, generally several nanometers to several tens of nanometers, the requirement on the photolithography process is very high, and the best photolithography base station in the industry at present needs to be used, which greatly increases the manufacturing cost of the SiNW detection unit.
Disclosure of Invention
Aiming at the prior art, the invention provides a porous silicon nanowire and a preparation method thereof, which aim to solve the technical problem of difficulty in preparation of the silicon nanowire.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the porous silicon nanowire is characterized by comprising the following steps:
s1: soaking the N-type silicon wafer in a cleaning agent for 1-4 min to remove a surface oxide layer and particle impurities;
s2: transferring the N-type silicon wafer processed by S1 into Ag deposition solution to be soaked for 0.5-2 min, then fishing out, and washing away Ag attached to the surface by deionized water3+(ii) a The Ag deposition solution is HF and AgNO3The concentration of HF in the mixed solution is 3-5M, and AgNO3The concentration of (A) is 0.001-0.01M;
s3: transferring the N-type silicon wafer processed by the S2 into etching liquid, and soaking and etching for 55-65 min; the etching solution is HF and H2O2The concentration of HF in the mixed solution is 4-5M, H2O2The concentration of (A) is 0.5-1M;
s4: and transferring the N-type silicon wafer processed by the S3 into concentrated nitric acid to be soaked for 1-1.5 h to obtain the silicon wafer.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the N-type silicon wafer has a diameter of 2 to 6cm and a resistivity of 0.008 to 0.02 Ω · cm.
Further, the solute of the cleaning agent solution comprises the following components in parts by mass:
15-25 parts of a surfactant, 3-5 parts of a suspending agent and 1-3 parts of a buffer etching liquid; the surfactant is sodium dodecyl sulfate or sodium fatty alcohol-polyoxyethylene ether sulfate; the suspending agent is maleic acid-acrylic acid copolymer or sodium carboxymethyl cellulose; the buffer etching liquid is HF and NH4F, mixing the mixed solution according to the volume ratio of 1: 5-7.
Further, the solute of the cleaning agent solution comprises the following components in parts by mass:
20 parts of sodium dodecyl sulfate, 4 parts of maleic acid-acrylic acid copolymer and 2 parts of buffer etching liquid; the buffer etching solution is HF solution with the concentration of 49 percent and NH with the concentration of 40 percent4And F solution is mixed according to the volume ratio of 1:6 to obtain a mixed solution.
The cleaning solution comprises a surfactant, a suspending agent and a buffer etching solution. The surface active agent can reduce the surface tension of the silicon wafer, so that useful components in the cleaning solution can better act on the surface of the silicon wafer to improve the cleaning effect. The suspending agent can ensure that the cleaned fine particles such as silicon carbide, silicon powder and the like and surface oxides are stably transferred and taken in the cleaning liquid, and secondary pollution caused by re-adsorption on the surface of the silicon wafer is avoided. The buffer etching liquid can have a flourishing effect with fine particles and oxides attached to the surface of the silicon wafer, so that the buffer etching liquid is separated from the silicon wafer, and the aim of cleaning is fulfilled. The cleaning agent disclosed by the invention has the advantages that the three components interact with each other, so that the surface of the silicon wafer is not seriously corroded, the excellent cleaning effect is realized, and particularly, the cleaning agent has the excellent cleaning effect on oxides and micro particles attached to the silicon wafer.
Further, the N-type silicon wafer is soaked in the Ag deposition solution for 1min in S2.
Further, the concentration of HF in the Ag deposition solution is 4M, AgNO3The concentration of (D) is 0.005M.
Further, in S3, the immersion time of the N-type silicon wafer in the etching solution is 60 min.
Further, the concentration of HF in the etching solution was 4.8M, H2O2The concentration of (3) was 0.8M.
The invention has the beneficial effects that: the invention aims to innovate a preparation method of porous silicon nanowires (SiNWs), thousands of nanowires are prepared by utilizing a centimeter-sized silicon wafer and performing high oxidation etching, and the material cost is greatly reduced; simultaneously surface coated with SiO2A layer having hydrophilicity. The porosity and one-dimensional characteristics of the material are favorable for improving the interaction between the micromolecular metabolites and increasing the specific surface area, and the material can be used as a unique matrix for matrix-assisted laser desorption ionization time-of-flight mass spectrometry to highly sensitively perform quantitative analysis and detection on the micromolecular metabolites in serum, thereby realizing accurate diagnosis and classification of cancers clinically.
Drawings
FIG. 1 shows the UV-visible spectrophotometer scanning spectrum of SiNWs solution;
FIG. 2 is a view of an SiNWs scanning electron microscope;
FIG. 3 shows the transmission electron microscope results of SiNWs at 200 nm;
FIG. 4 shows the transmission electron microscopy results of SiNWs at 10nm scale.
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention.
Example 1
A porous silicon nanowire, prepared by the following steps:
s1: soaking an N-type silicon wafer with the diameter of 5cm and the resistivity of 0.01 omega cm in a cleaning agent solution for 2min to remove a surface oxide layer; the solute of the cleaning agent solution comprises the following components in parts by mass:
20 parts of sodium dodecyl sulfate, 4 parts of maleic acid-acrylic acid copolymer and 2 parts of buffer etching solution, wherein the buffer etching solution is HF solution with the concentration of 49% and NH with the concentration of 40%4Mixing the solution F with a mixed solution according to the volume ratio of 1: 6; when a cleaning agent solution is prepared, mixing a solute and water according to a mass ratio of 1:4, and uniformly stirring to obtain the cleaning agent;
s2: transferring the N-type silicon wafer processed by S1 into Ag deposition solution, soaking for 1min, taking out, and washing off Ag attached to the surface with deionized water3+(ii) a The Ag deposition solution is HF and AgNO3The concentration of HF in the mixed solution is 4M, AgNO3Is 0.005M;
s3: transferring the N-type silicon wafer processed by the S2 into etching liquid, and soaking and etching for 60 min; the etching solution is HF and H2O2The concentration of HF in the mixed solution is 4.8M, H2O2The concentration of (A) is 0.8M;
s4: transferring the N-type silicon wafer processed by the S3 into concentrated nitric acid to be soaked for 1h, and dissolving Ag particles covered on the surface by the nitric acid; then, washing with deionized water to thoroughly remove residual Ag and HF to obtain pure silicon nanowires;
s5: and (3) putting the etched silicon wafer into deionized water, and simply performing ultrasonic treatment to collect a silicon nanowire solution (SiNWs solution).
Example 2
A porous silicon nanowire, prepared by the following steps:
s1: soaking an N-type silicon wafer with the diameter of 5cm and the resistivity of 0.02 omega cm in a cleaning agent solution for 2min to remove a surface oxide layer; the solute of the cleaning agent solution comprises the following components in parts by mass:
15 parts of fatty alcohol-polyoxyethylene ether sodium sulfate; 5 parts of sodium carboxymethylcellulose and 3 parts of buffer etching solution, wherein the buffer etching solution is 49% of HF solution and 40% of NH4Mixing the solution F with a mixed solution according to the volume ratio of 1: 7; when a cleaning agent solution is prepared, mixing a solute and water according to a mass ratio of 1:4, and uniformly stirring to obtain the cleaning agent;
s2: transferring the N-type silicon wafer processed by S1 into Ag deposition solution, soaking for 2min, taking out, and washing off Ag attached to the surface with deionized water3+(ii) a The Ag deposition solution is HF and AgNO3The concentration of HF in the mixed solution is 3M, AgNO3The concentration of (A) is 0.01M;
s3: transferring the N-type silicon wafer processed by the S2 into etching liquid, and soaking and etching for 55 min; the etching solution is HF and H2O2The concentration of HF in the mixed solution is 5M, H2O2The concentration of (A) is 0.5M;
s4: transferring the N-type silicon wafer processed by the S3 into concentrated nitric acid to be soaked for 1h, and dissolving Ag particles covered on the surface by the nitric acid; then, washing with deionized water to thoroughly remove residual Ag and HF to obtain pure silicon nanowires;
s5: and (3) putting the etched silicon wafer into deionized water, and simply performing ultrasonic treatment to collect a silicon nanowire solution (SiNWs solution).
Example 3
A porous silicon nanowire, prepared by the following steps:
s1: soaking an N-type silicon wafer with the diameter of 2cm and the resistivity of 0.0008 omega cm in a cleaning agent solution for 1min to remove a surface oxide layer; the solute of the cleaning agent solution comprises the following components in parts by mass:
25 parts of sodium dodecyl sulfate; 3 portions of sodium carboxymethylcellulose and 1 portion of buffer etching solution, wherein the buffer etching solution is HF solution with the concentration of 49 percent and NH with the concentration of 40 percent4Mixing the solution F with a mixed solution according to the volume ratio of 1: 5; when preparing the cleaning agent solution, the solute is addedMixing with water at a mass ratio of 1:4, and stirring;
s2: transferring the N-type silicon wafer processed by S1 into Ag deposition solution, soaking for 0.5min, taking out, and washing off Ag attached to the surface with deionized water3+(ii) a The Ag deposition solution is HF and AgNO3The concentration of HF in the mixed solution is 5M, AgNO3The concentration of (A) is 0.002M;
s3: transferring the N-type silicon wafer processed by the S2 into etching liquid, and soaking and etching for 65 min; the etching solution is HF and H2O2The concentration of HF in the mixed solution is 4M, H2O2The concentration of (A) is 1M;
s4: transferring the N-type silicon wafer processed by the S3 into concentrated nitric acid to be soaked for 1h, and dissolving Ag particles covered on the surface by the nitric acid; then, washing with deionized water to thoroughly remove residual Ag and HF to obtain pure silicon nanowires;
s5: and (3) putting the etched silicon wafer into deionized water, and simply performing ultrasonic treatment to collect a silicon nanowire solution (SiNWs solution).
Examples of the experiments
The SiNWs solution was ultrasonically homogenized and the spectrum was scanned using an ultraviolet visible spectrophotometer to obtain the result figure 1 showing a broad absorption peak in the ultraviolet region.
The SiNWs solution with uniform ultrasound is respectively dripped on the smooth surface of a silicon wafer and the surface of a copper mesh, vacuum drying is carried out, characterization is carried out through a scanning electron microscope and a transmission electron microscope, the SiNWs solution under the scanning electron microscope is shown in the figure 2, the transmission electron microscope result of a 200nm visual field of a scale is shown in the figure 3, and the fact that the nanowire has the porous characteristic of irregular holes is verified. FIG. 4 is a transmission electron microscope result with a 10nm field of view on a scale showing porosity and thin oxide on the surface.
While the present invention has been described in detail with reference to the embodiments, it should not be construed as limited to the scope of the patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (9)
1. A preparation method of porous silicon nanowires is characterized by comprising the following steps:
s1: soaking the N-type silicon wafer in a cleaning agent solution for 1-4 min to remove a surface oxide layer and particle impurities;
s2: transferring the N-type silicon wafer processed by S1 into Ag deposition solution to be soaked for 0.5-2 min, then fishing out, and washing away Ag attached to the surface by deionized water3+(ii) a The Ag deposition solution is HF and AgNO3The concentration of HF in the mixed solution is 3-5M, AgNO3The concentration of (A) is 0.001-0.01M;
s3: transferring the N-type silicon wafer processed by the S2 into etching liquid, and soaking and etching for 55-65 min; the etching liquid is HF and H2O2The concentration of HF in the mixed solution is 4-5M, H2O2The concentration of (A) is 0.5-1M;
s4: and transferring the N-type silicon wafer processed by the S3 into concentrated nitric acid to be soaked for 1-1.5 h to obtain the silicon wafer.
2. The method of preparing porous silicon nanowires of claim 1, wherein: the diameter of the N-type silicon wafer is 2-6 cm, and the resistivity is 0.008-0.02 omega cm.
3. The method of preparing porous silicon nanowires of claim 1, wherein: the solute of the cleaning agent solution comprises the following components in parts by mass:
15-25 parts of a surfactant, 3-5 parts of a suspending agent and 1-3 parts of a buffer etching liquid; the surfactant is sodium dodecyl sulfate or fatty alcohol-polyoxyethylene ether sodium sulfate; the suspending agent is maleic acid-acrylic acid copolymer or sodium carboxymethyl cellulose; the buffer etching liquid is HF and NH4F, mixing the mixed solution according to the volume ratio of 1: 5-7.
4. The method for preparing porous silicon nanowires of claim 3, wherein: the solute of the cleaning agent solution comprises the following components in parts by mass:
20 parts of sodium dodecyl sulfate, 4 parts of maleic acid-acrylic acid copolymer and 2 parts of buffer etching liquid; the buffer etching solution is HF solution with the concentration of 49% and NH with the concentration of 40%4And F solution is mixed according to the volume ratio of 1:6 to obtain a mixed solution.
5. The method of preparing porous silicon nanowires of claim 1, wherein: in S2, the N-type silicon wafer is soaked in the Ag deposition solution for 1 min.
6. The method for preparing porous silicon nanowires according to claim 1 or 5, wherein: the concentration of HF in the Ag deposition solution is 4M, AgNO3The concentration of (D) is 0.005M.
7. The method of preparing porous silicon nanowires of claim 1, wherein: in S3, the N-type silicon wafer is soaked in the etching solution for 60 min.
8. The method for preparing porous silicon nanowires according to claim 1 or 7, wherein: the concentration of HF in the etching solution is 4.8M, H2O2The concentration of (3) was 0.8M.
9. Porous silicon nanowires prepared by the preparation method according to any one of claims 1 to 8.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114639807A (en) * | 2022-03-04 | 2022-06-17 | 东华大学 | Porous silicon nanoparticle/porous carbon nanofiber composite electrode material and preparation method and application thereof |
| CN114975851A (en) * | 2022-01-26 | 2022-08-30 | 昆明理工大学 | Nano porous silicon electrode material, preparation method thereof and application thereof in preparation of silicon-air battery |
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| CN103157620A (en) * | 2011-12-14 | 2013-06-19 | 北大方正集团有限公司 | Cleaning fluid and cleaning method of silicon wafer back before metalization |
| CN103571644A (en) * | 2013-10-31 | 2014-02-12 | 合肥中南光电有限公司 | Water-based silicon wafer cleaning agent and preparation method thereof |
| CN111413395A (en) * | 2020-04-21 | 2020-07-14 | 四川大学 | Application of porous silicon nanowire combined with MA L DI-TOF MS in metabolic small molecule detection |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114975851A (en) * | 2022-01-26 | 2022-08-30 | 昆明理工大学 | Nano porous silicon electrode material, preparation method thereof and application thereof in preparation of silicon-air battery |
| CN114975851B (en) * | 2022-01-26 | 2024-04-12 | 昆明理工大学 | Nano porous silicon electrode material, preparation method thereof and application thereof in preparation of silicon air battery |
| CN114639807A (en) * | 2022-03-04 | 2022-06-17 | 东华大学 | Porous silicon nanoparticle/porous carbon nanofiber composite electrode material and preparation method and application thereof |
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