CN102953113A - Method for preparing silicon-based nano-scale ordered porous silicon - Google Patents
Method for preparing silicon-based nano-scale ordered porous silicon Download PDFInfo
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- CN102953113A CN102953113A CN2012104008501A CN201210400850A CN102953113A CN 102953113 A CN102953113 A CN 102953113A CN 2012104008501 A CN2012104008501 A CN 2012104008501A CN 201210400850 A CN201210400850 A CN 201210400850A CN 102953113 A CN102953113 A CN 102953113A
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Abstract
The invention discloses a method for preparing silicon-based nano-scale ordered porous silicon, comprising the following steps of: (1) ultrasonically washing an n-shaped one-side polished monocrystalline silicon piece in an acetone solvent, absolute ethyl alcohol and de-ionized water sequentially; and (2) preparing a porous silicon layer on the polished surface of the silicon piece by a double-tank electrochemical corrosion method, taking the aqueous solution of hydrofluoric acid having the mass fraction of 5-9% as corrosive liquid, and applying corrosion current, wherein the density of the corrosion current is 75-155 mA/cm<2>, and the corrosion time is 5-30 min; and the process is performed at the room temperature without illumination. The method disclosed by the invention is simple, quick, effective and practicable, and high in operability; and the bore diameter of the obtained porous silicon is at hundred-nanometer scale, and has the characteristics of high porosity and highly ordered pore canals. The method is capable of achieving the purpose of the silicon-based nano-scale ordered porous silicon by controlling the concentration of the hydrofluoric acid, the corrosion current density and the corrosion time; and the silicon-based nano-scale ordered porous silicon is an ideal material for preparing biological and chemical sensor elements.
Description
Technical field
The invention relates to silica-based porous silicon, relate in particular to a kind of preparation method who utilizes the double flute electrochemical erosion method to prepare the ordered porous silicon of silicon-based nano size.
Background technology
Find first porous silicon when Uhlir carried out electrochemical etching in hydrofluoric acid aqueous solution in 1956.Silica-based porous silicon is formed by etching at silicon chip surface, though still consisted of by Siliciumatom, because its special porousness microstructure shows many physics-chem characteristics that are different from single crystal silicon material.As utilize the photoluminescence property of porous silicon to make opto-electronic device; Utilize the low thermal conductivity of porous silicon to prepare the thermal insulation layer material; Utilize the porous silicon specific surface area large, the characteristics that chemical mobility of the surface is high prepare the reduce power consumption biological and chemical sensor of working and room temperature.Especially in recent years along with the develop rapidly of micromachined manufacturing system, make to be easy to demonstrate huge development prospect with the integrated porous silicon of silicon circuit.
At present the classification of silica-based porous silicon is obtained the common recognition of scientific research circle, generally according to its aperture size it has been divided into macropore silicon (aperture〉50nm), mesoporous silicon (aperture 2-50nm) and microporous silicon (aperture＜2nm).Mesoporous silicon and microporous silicon are less because of aperture size, and the duct is comparatively coarse, present the randomness structure of " dendroid " and " spongy "; Macropore silicon has unified hole shape, aperture and straight smooth pore passage structure, the cycle order that presents height is arranged, has good permeability, easily the realization molecule is inhaled/desorption and transport process rapidly, has broad application prospects in various fields such as molecular adsorption, separation, filtration, catalytic carrier and electrode materialss.And macropore silicon hole internal cause is easy to load other low-dimensional nano-functional materials, form novel nano composite heterogenous junction structure, have the specific surface area larger than general nano material, can bring into play better Nanosurface effect and coupling synergistic effect, significantly promote the performance of biological and chemical sensor.But since the aperture in micron-sized macropore silicon porosity far below mesoporous silicon and microporous silicon, the quantity of absorption position can reduce greatly, causes its application at aspects such as sensor, device chipization are integrated to be restricted.Silica-based porous silicon for existing preparation remains in some shortcomings, and research preparation aperture is at hundred nano-scale, and the silica-based porous silicon that has simultaneously the arrangement of high porosity and duct high-sequential is expected to obtain widely practical application.
Preparing the most frequently used method of silica-based porous silicon is the galvanic corrosion preparation method, and it has fast and convenient, parameter and is easy to control, the advantage of good reproducibility.And the porous silicon layer that utilizes the double flute electrochemical erosion method to form on silicon substrate surface is more even, and preparation process needn't be considered in advance further to have simplified technique at silicon base back side extraction electrode simultaneously.
Summary of the invention
Purpose of the present invention, it is the shortcoming that the porous silicon that overcomes prior art can not satisfy high-specific surface area and duct high-sequential simultaneously, provide a kind of simple to operate, with low cost, the preparation method of the ordered porous silicon of silicon-based nano size that technical maturity, duct pattern and pore size can flexible.
The present invention is achieved by following technical solution.
The preparation method of the ordered porous silicon of a kind of silicon-based nano size has following steps:
(1) cleaning silicon chip:
The monocrystalline silicon piece of N-shaped single-sided polishing is put into acetone solvent successively, and the difference ultrasonic cleaning is 20 minutes in dehydrated alcohol, the deionized water, removes surface and oil contaminant; Put into subsequently massfraction and be 5% hydrofluoric acid aqueous solution and soaked 15 minutes, remove the zone of oxidation on surface; Clean with deionized water again, at last silicon chip is put into dehydrated alcohol for subsequent use;
(2) prepare silica-based porous silicon
Utilize the double flute electrochemical erosion method to prepare porous silicon layer at the glazed surface of silicon chip, be first that 5 ~ 9% hydrofluoric acid aqueous solution adds in the etching tank as corrosive fluid with massfraction, insert respectively a pair of platinum electrode as negative electrode and anode to two and half grooves again, then silicon chip is assemblied in the anchor clamps, the anchor clamps two sides offers corrosion window; For guaranteeing stopping property, twine with sealant tape around the anchor clamps, closely be fixed in the slot at etching tank middle part; With DC voltage-stabilizing constant current source jointed anode and negative electrode, making current is corroded; Applying corrosion electric current density is 75 ~ 155mA/cm
2, etching time is 5 ~ 30min, preparation condition is room temperature and need not by illumination;
Corrosion process is extracted clamping plate after finishing, and makes silica-based porous silicon.
The resistivity of the silicon chip of described step (1) is 0.01 ~ 0.02 Ω cm, and thickness is 350 ~ 500 μ m.
The die size of described step (1) is the rectangular silicon substrate of 2.2cm * 0.8cm.
The invention has the beneficial effects as follows, the aperture of novel silica-based porous silicon is at hundred nano-scale, have the characteristics of the large and duct high-sequential of specific surface area concurrently, effectively improved the deficiency of traditional silicon base porous silicon, be expected to make silica-based Porous Silicon Sensors element to obtain more excellent performance, can greatly expand the Application Areas of silica-based porous silicon aspect the biological and chemical sensor.
Secondly, the present invention has improved traditional electrical chemical corrosion preparation condition, utilizes the making method of double flute electrochemical erosion method to have a prepared porous silicon layer of the present invention more even.Can realize the purpose of the ordered porous silicon of silicon-based nano size of the present invention by control hydrofluoric acid concentration, corrosion electric current density and etching time.
Description of drawings
Fig. 1 is double flute electrochemical erosion method apparatus structure schematic diagram;
Reference numeral among Fig. 1 is: 1 is etching tank, and 2 is the DC voltage-stabilizing constant current source, and 3 is platinum electrode, and 4 is stationary fixture, and 5 is corrosive fluid, and 6 is corrosion window, and 7 is silicon chip, and 8 is fixed slot;
Fig. 2 is the electron scanning micrograph of the ordered porous silicon face of silicon-based nano size that is parallel to substrate surface of example 1 preparation;
Fig. 3 is the electron scanning micrograph perpendicular to the ordered porous silicon of the silicon-based nano size cross section of substrate surface of example 1 preparation;
Fig. 4 is the electron scanning micrograph of the silica-based porous silicon surface of example 2 preparations;
Fig. 5 is the electron scanning micrograph in the silica-based porous silicon cross section of example 2 preparations;
Fig. 6 is the electron scanning micrograph of the silica-based porous silicon surface of example 3 preparations;
Fig. 7 is the electron scanning micrograph in the silica-based porous silicon cross section of example 3 preparations.
Embodiment
The present invention is raw materials used all to adopt commercially available chemically pure reagent.
Embodiment 1
(1) Wafer Cleaning:
Be that 0.015 Ω cm, thickness are the monocrystalline silicon piece of single-sided polishing of the N-shaped (100) of 400 ± 10 μ m with resistivity, cut into the rectangular silicon substrate that is of a size of 2.2cm * 0.8cm, put into successively acetone solvent, the difference ultrasonic cleaning is 20 minutes in dehydrated alcohol, the deionized water, put into subsequently massfraction and be 5% hydrofluoric acid aqueous solution and soaked 15 minutes, clean for subsequent use with deionized water again.
(2) prepare silica-based porous silicon:
Utilize the double flute electrochemical erosion method to prepare porous silicon layer at the glazed surface of silicon chip.Be massfraction that 7% hydrofluoric acid aqueous solution adds in the galvanic corrosion groove as corrosive fluid first, need not to add tensio-active agent and oxygenant; Insert respectively a pair of platinum electrode as negative electrode and anode to two and half grooves again, then silicon chip is assemblied in the anchor clamps, the anchor clamps two sides offers parallel rectangle corrosion window, is of a size of 1.6cm * 0.4cm.For guaranteeing stopping property, twine with sealant tape around the anchor clamps, closely be fixed in the slot at etching tank middle part.With DC voltage-stabilizing constant current source jointed anode and negative electrode, making current is corroded, and the electrochemical corrosion device structural representation as shown in Figure 1.The corrosion electric current density that wherein applies is 125mA/cm
2, etching time is 20min, under the room temperature preparation and need not by illumination.Corrosion process is extracted clamping plate after finishing, and takes out the silicon chip after corroding, and makes silica-based porous silicon.Reference numeral among Fig. 1 is: 1 is etching tank, and 2 is the DC voltage-stabilizing constant current source, and 3 is platinum electrode, and 4 is stationary fixture, and 5 is corrosive fluid, and 6 is corrosion window, and 7 is silicon chip, and 8 is fixed slot.
The electron scanning micrograph of the ordered porous silicon face pattern of prepared silicon-based nano size and cross-section structure as shown in Figures 2 and 3, the mean pore size of the porous silicon parameter of preparation is 170.28nm, layer thickness is 68.78 μ m, porosity reaches 75.73%, surface topography is the polynuclear plane that polygonal hole forms, Cross Section Morphology is that straight columniform duct high-sequential is arranged, and hole wall is comparatively coarse.
Embodiment 2
The present embodiment is similar to embodiment 1, and difference is, used corrosive fluid is that massfraction is 6% hydrofluoric acid aqueous solution in the step (2), and the corrosion electric current density that applies is 120mA/cm
2, etching time is 20min.Prepared silica-based porous silicon surface pattern and the electron scanning micrograph of cross-section structure are as shown in Figure 4 and Figure 5.The mean pore size of the porous silicon parameter of preparation is 227.81nm, and layer thickness is 33.39 μ m, and porosity is 66%, and surface topography is the polynuclear plane that polygonal hole forms, and Cross Section Morphology is that straight columniform duct high-sequential is arranged, and hole wall is comparatively smooth.
Embodiment 3
The present embodiment is similar to embodiment 1, and difference is, used corrosive fluid is that massfraction is 7% hydrofluoric acid aqueous solution in the step (2), and the corrosion electric current density that applies is 125mA/cm
2, etching time is 15min.Prepared silica-based porous silicon surface pattern and the electron scanning micrograph of cross-section structure are as shown in Figure 6 and Figure 7, the mean pore size of the porous silicon parameter of preparation is 112.25nm, layer thickness is 53.42 μ m, porosity is 68.75%, surface topography is the polynuclear plane that polygonal hole forms, Cross Section Morphology is that straight columniform duct high-sequential is arranged, and hole wall is very coarse and have side opening to occur.
Adopt the method for scales/electronic balance weighing sample among the present invention, and calculate porosity and the thickness that obtains silica-based porous silicon by formula.Porosity p can pass through (m
1-m
2)/(m
1-m
3) calculate; The porous silicon layer thickness d can be passed through (m
1-m
3)/ρ S calculates, wherein m
1Be uncorroded Si wafer quality, m
2Be the Si wafer quality after the corrosion, m
3For being remaining Si wafer quality behind 1% the KOH aqueous solution dissolving porous silicon layer with massfraction, ρ is the density of silicon, and S is the area that porous silicon forms the zone.
The ordered porous silicon of novel silicon base nano-scale of the present invention, the aperture has the characteristics of high porosity and duct high-sequential concurrently at hundred nano-scale, is the ideal material for the preparation of the biological and chemical sensor element.
Claims (3)
1. the preparation method of the ordered porous silicon of silicon-based nano size has following steps:
(1) cleaning silicon chip:
The monocrystalline silicon piece of N-shaped single-sided polishing is put into acetone solvent successively, and the difference ultrasonic cleaning is 20 minutes in dehydrated alcohol, the deionized water, removes surface and oil contaminant; Put into subsequently massfraction and be 5% hydrofluoric acid aqueous solution and soaked 15 minutes, remove the zone of oxidation on surface; Clean with deionized water again, at last silicon chip is put into dehydrated alcohol for subsequent use;
(2) prepare silica-based porous silicon
Utilize the double flute electrochemical erosion method to prepare porous silicon layer at the glazed surface of silicon chip, be first that 5 ~ 9% hydrofluoric acid aqueous solution adds in the etching tank as corrosive fluid with massfraction, insert respectively a pair of platinum electrode as negative electrode and anode to two and half grooves again, then silicon chip is assemblied in the anchor clamps, the anchor clamps two sides offers corrosion window; For guaranteeing stopping property, twine with sealant tape around the anchor clamps, closely be fixed in the slot at etching tank middle part; With DC voltage-stabilizing constant current source jointed anode and negative electrode, making current is corroded; Applying corrosion electric current density is 75 ~ 155mA/cm
2, etching time is 5 ~ 30min, preparation condition is room temperature and need not by illumination;
Corrosion process is extracted clamping plate after finishing, and makes silica-based porous silicon.
2. according to claim 1 the preparation method of the ordered porous silicon of a kind of silicon-based nano size is characterized in that, the resistivity of the silicon chip of described step (1) is 0.01 ~ 0.02 Ω cm, and thickness is 350 ~ 500 μ m.
3. according to claim 1 the preparation method of the ordered porous silicon of a kind of silicon-based nano size is characterized in that, the die size of described step (1) is the rectangular silicon substrate of 2.2cm * 0.8cm.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103245696A (en) * | 2013-05-11 | 2013-08-14 | 天津大学 | Method for preparing porous silicon-based one-dimensional nanowire gas sensitive element |
| CN103276436A (en) * | 2013-06-17 | 2013-09-04 | 天津大学 | Preparation method of novel ordered nano-porous silicon |
| CN104466117A (en) * | 2014-11-05 | 2015-03-25 | 昆明理工大学 | Preparation method of three-dimensional porous silica powder |
| CN104952947A (en) * | 2015-05-14 | 2015-09-30 | 陕西师范大学 | Current-aided aluminum-doped zinc oxide film chemical texturing method |
| CN105518871A (en) * | 2013-09-27 | 2016-04-20 | 太阳能公司 | Enhanced porosification |
| CN106568828A (en) * | 2016-10-26 | 2017-04-19 | 华南农业大学 | Electrochemical immunosensor based on DNA functionalized nano composite material |
| CN108847383A (en) * | 2018-05-29 | 2018-11-20 | 昆明理工大学 | A kind of preparation method of porous silicon nanowire array |
| CN109023501A (en) * | 2018-08-16 | 2018-12-18 | 湖南文理学院 | A kind of preparation method of nano-structure porous silicon list concavees lens |
| CN109056050A (en) * | 2018-08-16 | 2018-12-21 | 湖南文理学院 | A kind of preparation method of nano-structure porous silicon biconvex lens |
| CN109056049A (en) * | 2018-08-16 | 2018-12-21 | 湖南文理学院 | A kind of preparation method of nano-structure porous silicon biconcave lens |
| CN109137059A (en) * | 2018-10-12 | 2019-01-04 | 湖南文理学院 | A kind of preparation method of silicon-based nano porous silicon list convex lens |
| CN109234791A (en) * | 2018-10-12 | 2019-01-18 | 湖南文理学院 | A method of preparing nano-structure porous silicon biconvex lens |
| CN109813776A (en) * | 2017-11-20 | 2019-05-28 | 天津师范大学 | Intermediate pore size porous silicon-base zinc oxide films film composite material gas sensor and its preparation method and application |
| CN113403613A (en) * | 2020-03-16 | 2021-09-17 | 上海昱瓴新能源科技有限公司 | Preparation device and preparation method of porous silicon powder |
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Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103245696A (en) * | 2013-05-11 | 2013-08-14 | 天津大学 | Method for preparing porous silicon-based one-dimensional nanowire gas sensitive element |
| CN103276436A (en) * | 2013-06-17 | 2013-09-04 | 天津大学 | Preparation method of novel ordered nano-porous silicon |
| TWI646694B (en) * | 2013-09-27 | 2019-01-01 | 太陽電子公司 | Method for forming porous layer on silicon substrate |
| CN105518871A (en) * | 2013-09-27 | 2016-04-20 | 太阳能公司 | Enhanced porosification |
| CN104466117A (en) * | 2014-11-05 | 2015-03-25 | 昆明理工大学 | Preparation method of three-dimensional porous silica powder |
| CN104466117B (en) * | 2014-11-05 | 2017-11-10 | 昆明理工大学 | A kind of preparation method of three-dimensional porous silica powder |
| CN104952947A (en) * | 2015-05-14 | 2015-09-30 | 陕西师范大学 | Current-aided aluminum-doped zinc oxide film chemical texturing method |
| CN104952947B (en) * | 2015-05-14 | 2017-04-12 | 陕西师范大学 | Current-aided aluminum-doped zinc oxide film chemical texturing method |
| CN106568828B (en) * | 2016-10-26 | 2019-04-09 | 华南农业大学 | A kind of electrochemical immunosensor based on DNA functionalized nano composite material |
| CN106568828A (en) * | 2016-10-26 | 2017-04-19 | 华南农业大学 | Electrochemical immunosensor based on DNA functionalized nano composite material |
| CN109813776A (en) * | 2017-11-20 | 2019-05-28 | 天津师范大学 | Intermediate pore size porous silicon-base zinc oxide films film composite material gas sensor and its preparation method and application |
| CN108847383A (en) * | 2018-05-29 | 2018-11-20 | 昆明理工大学 | A kind of preparation method of porous silicon nanowire array |
| CN109023501A (en) * | 2018-08-16 | 2018-12-18 | 湖南文理学院 | A kind of preparation method of nano-structure porous silicon list concavees lens |
| CN109056049A (en) * | 2018-08-16 | 2018-12-21 | 湖南文理学院 | A kind of preparation method of nano-structure porous silicon biconcave lens |
| CN109056050A (en) * | 2018-08-16 | 2018-12-21 | 湖南文理学院 | A kind of preparation method of nano-structure porous silicon biconvex lens |
| CN109023501B (en) * | 2018-08-16 | 2020-06-02 | 湖南文理学院 | Preparation method of nano porous silicon single concave lens |
| CN109056050B (en) * | 2018-08-16 | 2020-08-04 | 湖南文理学院 | Preparation method of nano porous silicon biconvex lens |
| CN109137059A (en) * | 2018-10-12 | 2019-01-04 | 湖南文理学院 | A kind of preparation method of silicon-based nano porous silicon list convex lens |
| CN109234791A (en) * | 2018-10-12 | 2019-01-18 | 湖南文理学院 | A method of preparing nano-structure porous silicon biconvex lens |
| CN109234791B (en) * | 2018-10-12 | 2020-10-27 | 湖南文理学院 | Method for preparing nano porous silicon biconvex lens |
| CN113403613A (en) * | 2020-03-16 | 2021-09-17 | 上海昱瓴新能源科技有限公司 | Preparation device and preparation method of porous silicon powder |
| CN113403613B (en) * | 2020-03-16 | 2023-02-03 | 上海昱瓴新能源科技有限公司 | Preparation device and preparation method of porous silicon powder |
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Application publication date: 20130306 |