CN102126724A - Method for preparing silicon nanowire array with smooth surface - Google Patents
Method for preparing silicon nanowire array with smooth surface Download PDFInfo
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- CN102126724A CN102126724A CN2011100803726A CN201110080372A CN102126724A CN 102126724 A CN102126724 A CN 102126724A CN 2011100803726 A CN2011100803726 A CN 2011100803726A CN 201110080372 A CN201110080372 A CN 201110080372A CN 102126724 A CN102126724 A CN 102126724A
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Abstract
The invention relates to a method for preparing a length-controlled silicon nanowire array with a smooth surface, and belongs to the technology of the preparation of nanometer materials. The method comprises the following steps of: firstly, performing wet chemical cleaning on a silicon wafer; secondly, depositing a silver nanometer granular layer on the surface of the silicon wafer in mixed solution containing hydrofluoric acid and silver nitrate by an electroless chemical deposition method; thirdly, performing chemical etching by mixed solution containing the hydrofluoric acid and hydrogen peroxide; and finally, removing silver nanometer granules by using nitric acid to obtain the silicon nanowire array. In the method, length-controlled silicon nanowires with the smooth surfaces are prepared by regulating the concentration and etching time of the hydrogen peroxide serving as an oxidant simply in a chemical etch system, so the technical problem of preparing the silicon nanowires with fewer surface defects in metal-assisted chemical etching is solved.
Description
Technical field
What the present invention relates to is a kind of method of nano material preparation technical field, specifically is a kind of preparation method of smooth surface silicon nanowire array of length controlled.
Background technology
At present, large-scale development is the photoelectric transformation efficiency that reduces the production cost of solar cell and improve battery with the core place that utilizes solar energy power generating.Silicon nanowires since can with photoabsorption and current carrier separate perpendicular quadratureization (be photoabsorption along silicon nanowires axially and current carrier in the radial separation of nano wire), compare the collection effciency that has not only strengthened photoabsorption but also improved current carrier with the classic flat-plate silion cell, thereby just might in short, the with low cost silicon materials of current carrier diffusion length, realize the solar cell of greater efficiency.So silicon nanowires has important application prospects aspect reduction solar cell cost, the raising photoelectric transformation efficiency.At present, the preparation method of silicon nanowires mainly comprises gas-liquid-solid trichotomy, reactive ion etching method and metal assistant chemical etching method etc.; In these methods, metal assistant chemical etching method is the preparation method of minimum, the simple possible of cost, and it will have important effect in following silicon nanowires preparation and photovoltaic application.
Find through the retrieval that existing silicon nanowires is prepared the aspect document, people such as Peng were " advanced material " (Advanced Materials) 2002,14 volumes, having reported a kind of on the 1164-1167 page or leaf is the chemical process of preparation silicon nanowires in 50 ℃ of following hydrofluoric acid and the silver nitrate aqueous solution in temperature, and is metal aided nano electrochemical method with this method summary.Up to the present, by this method being prepared the big quantity research of silicon nanowires, people have realized utilizing the method for metal assistant chemical etching to prepare silicon nanowire array.Yet utilize the surface of silicon nanowires of metal assistant chemical lithographic technique preparation to have a large amount of defectives, simultaneously neither be very clear and definite to the concrete mechanism and the oxygenant effect understanding of its metal catalytic.Surface imperfection has increased the recombination losses of current carrier on the surface and has also seriously limited the photoelectric transformation efficiency of silicon nanowires solar cell and the application in photovoltaic.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of preparation method of smooth surface silicon nanowire array of length controlled is provided, the preparation of the smooth surface silicon nanowires of having realized length controlled by the concentration and the etching time of simple adjustment oxidant hydrogen peroxide in the chemical etching system, thus the technical barrier of the less silicon nanowires of preparation surface imperfection in metal assistant chemical etching solved.
The present invention is achieved by the following technical solutions, the present invention is by at first carrying out wet chemical cleans to silicon chip, in the mixing solutions that contains hydrofluoric acid and Silver Nitrate, utilize no electrochemical deposition method at silicon chip surface depositing silver nano-particle layer then, mixing solutions through containing hydrofluoric acid and hydrogen peroxide carries out chemical etching, removes silver nano-grain with nitric acid at last and obtains silicon nanowire array.
Described silicon chip is meant: resistivity is p type (100) the crystal orientation electronic-grade silicon chip of 0.01-0.03 Ω cm;
Described wet chemical cleans is meant: silicon chip was used earlier acetone, dehydrated alcohol, deionized water ultrasonic cleaning respectively 15 minutes successively, be 1: 1: 5 ammoniacal liquor then successively with volume ratio: hydrogen peroxide: water boiled under 85 ℃ 15 minutes, at massfraction is to soak 1 minute in 3% the hydrofluoric acid, be 1: 1: 5 hydrochloric acid again in volume ratio: hydrogen peroxide: boiled 15 minutes under 85 ℃ in the water, wash the silicon chip that obtains hydrophobic surface with deionized water and dilute hydrofluoric acid solution successively at last.
Described utilization does not have electrochemical deposition method and is meant at silicon chip surface depositing silver nano-particle layer: with silicon chip putting into hydrofluoric acid that concentration under the room temperature is 4.0 mol and 15.0 mmoles/liter the aqueous solution 60-120 of Silver Nitrate take out rapidly after second, make silicon chip surface uniform deposition one deck silver nano-grain.
Described chemical etching is meant: the silicon chip that will deposit the silver nano-grain layer embathes in deionized water earlier, immerse in the mixing solutions that contains hydrofluoric acid and hydrogen peroxide then and carry out etching, wherein: the concentration of hydrofluoric acid is 5.0 mol, the concentration of hydrogen peroxide is 0.02 to 8.0 mol, and entire reaction is carried out at ambient temperature and utilize wavelength in the sign of photoluminescence is that the laser of 514.5 nanometers is as exciting light.
Describedly remove silver nano-grain with nitric acid and be meant: be 65% salpeter solution drip washing silicon chip removing its surperficial silver nano-grain with massfraction earlier, and then with deionized water rinsing and 60 ℃ of oven dry in baking oven.
The present invention passes through no electrochemical process at silicon chip surface depositing silver nano-particle layer, with this as catalytic templating etching in the hydrofluoric acid solution that hydrogen peroxide oxidation is handled, control the surface topography and the luminosity of silicon nanowires by the concentration of regulating hydrogen peroxide, observe the hydrogen peroxide that obtains suitable concn in conjunction with high resolution electron microscopy and photoluminescence, successfully prepare smooth surface, the less silicon nanowire array of defective.Because the preparation silicon nanowires is just can realize by simple chemical reaction at ambient temperature, and the length of silicon nanowires can be controlled by the reaction times, this method is applicable to the nano-wire array preparation of bulk silicon chip level simultaneously, so this has improved important reference for low-cost, mass preparation high quality silicon nano wire, has great importance in material preparation and photovoltaic application.
Description of drawings
Fig. 1 is an embodiment effect synoptic diagram 1;
Among the figure: (a c) is the low power transmission electron microscope picture of the sample for preparing under the hydrogen peroxide concentration of 0.4 and 0.1 mol; (b is corresponding to (a, c) the high power transmission electron microscope picture at middle frame of broken lines place d); (e) luminescent spectrum of silicon nanowires under the different hydrogen peroxide concentrations.
Fig. 2 is an embodiment effect synoptic diagram 2;
Among the figure: (a-c) under the hydrogen peroxide concentration of 0.1 mol, the reaction times is respectively the sem photograph of 10,30 and 60 minutes smooth surface silicon nanowire array; (d) silicon nanowires length is with the variation relation of etching time.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Utilize p type (100) the crystal orientation electronic-grade silicon chip of resistivity,, will carry out etching under the room temperature in its hydrofluoric acid mixed aqueous solution under different hydrogen peroxide concentrations then by the depositing silver nano particle for 0.01-0.03 Ω cm; After etching finishes silicon chip is characterized (surface condition that mainly is the research silicon nanowires) with carrying out high resolving power transmission electron microscope pattern after nitric acid and deionized water rinsing and the oven dry respectively, utilize the micro-Raman of Jobin Yvon LabRAM HR 800UV/luminescent spectrum instrument to carry out the photoluminescence test simultaneously, exciting light is that wavelength is the Ar of 514.5 nanometers
+Laser apparatus.Concrete implementation step is as follows:
(1) silicon chip is used earlier successively acetone, dehydrated alcohol, deionized water ultrasonic cleaning respectively 15 minutes, it is 1: 1: 5 ammoniacal liquor then with volume ratio: hydrogen peroxide: water, boiling under 85 ℃ 15 minutes, is to soak in 3% the hydrofluoric acid to remove silicon oxide layer in 1 minute with massfraction again; Be 1: 1: 5 hydrochloric acid then with volume ratio: hydrogen peroxide: water, boiled the last silicon chip that obtains fluorine terminated surface hydrophobicity successively with deionized water and dilute hydrofluoric acid solution flushing 15 minutes under 85 ℃.
(2) cleaned silicon slice placed being gone under the room temperature concentration is 4.0 mol hydrofluoric acid and 15.0 mmoles/rise in the aqueous solution of Silver Nitrate, and Immersion time 80 seconds takes out rapidly then, and silicon chip surface has deposited one deck silver nano-grain equably.
(3) silicon chip that will deposit the silver nano-grain layer embathes in deionized water earlier, immerse lightly then in the aqueous solution of hydrofluoric acid, hydrogen peroxide and carry out etching, wherein the concentration of hydrofluoric acid is 5.0 mol, and the concentration of hydrogen peroxide is then adjustable in 0.02 to 8.0 mol scope; Entire reaction is to carry out under 30 ℃ the condition in temperature.
(4) reaction was that 65% nitric acid drip washing is to remove silver nano-grain with the silicon chip massfraction after 30 minutes; And then with a large amount of deionized water rinsings and 60 ℃ of oven dry in baking oven.
(5) (Fig. 1 (e) determines the surface topography of silicon nanowires under different hydrogen peroxide concentrations to pass through the observation of high resolving power transmission electron microscope pattern sign (as Fig. 1 (a-d)) and photoluminescence.Discovery can obtain smooth surface under the hydrogen peroxide condition of about 0.1 mol of concentration (Fig. 1 (c, d)), do not have the silicon nanowire array of luminous signal (Fig. 1 (e)) at visible-range; Very coarse (Fig. 1 (a, b)) and show the very strong characteristics of luminescence of porous silicon (Fig. 1 (e)) in the surface of silicon nanowires when being higher than this concentration at visible-range; The speed of growth of silicon nanowires is then very slow when being lower than this concentration; Obtained in the system of hydrofluoric acid, hydrogen peroxide and water, preparing as catalyzer the reaction conditions of smooth surface silicon nanowire array thus with silver nano-grain.
Hydrogen peroxide concentration prepares big area, ganoid silicon nanowire array provides a kind of new way of studying metal assistant chemical etching mechanism simultaneously by regulating, understood the effect of oxidant hydrogen peroxide in the preparation silicon nanowires to a certain extent, this simple and effective preparation method will make silicon nanowires play an important role in efficient, the low-cost photovoltaic application in future.
Embodiment 2
(1) silicon chip is used earlier successively acetone, dehydrated alcohol, deionized water ultrasonic cleaning respectively 15 minutes, it is 1: 1: 5 ammoniacal liquor then with volume ratio: hydrogen peroxide: water, boiling under 85 ℃ 15 minutes, is to soak in 3% the hydrofluoric acid to remove silicon oxide layer in 1 minute with massfraction again; Be 1: 1: 5 hydrochloric acid then with volume ratio: hydrogen peroxide: water, boiled the last silicon chip that obtains fluorine terminated surface hydrophobicity successively with deionized water and dilute hydrofluoric acid solution flushing 15 minutes under 85 ℃.
(2) cleaned silicon slice placed being gone under the room temperature concentration is 4.0 mol hydrofluoric acid and 10.0 mmoles/rise in the aqueous solution of Silver Nitrate, and Immersion time is extended for 100 seconds, takes out rapidly then, and silicon chip surface has deposited one deck silver nano-grain equably.
(3) silicon chip that will deposit the silver nano-grain layer embathes in deionized water earlier, immerses then in the aqueous solution of the hydrofluoric acid that hydrogen peroxide oxidation handles to carry out etching, and wherein the concentration of hydrofluoric acid is 5.0 mol, and the concentration of hydrogen peroxide is 0.1 mol; Entire reaction is to carry out under 35 ℃ the condition in temperature.
(4) reaction times took out silicon chip then and is that 65% nitric acid drip washing is to remove silver nano-grain with massfraction between 5-60 minute; And then with a large amount of deionized water rinsings and 60 ℃ of oven dry in baking oven.
(5) by sem observation under the differential responses time length of smooth silicon nanowire array (Fig. 2 (a-c)), the growth velocity of discovery under this condition is 0.5 micron/minute, the length of silicon nanowires then shows good linear relationship (Fig. 2 (d)) with etching time, thereby has realized the controllable growth of smooth surface silicon nanowires length.
Provide a kind of new way of studying metal assistant chemical etching mechanism simultaneously by under suitable hydrogen peroxide concentration, preparing big area, length controlled, ganoid silicon nanowire array, understood the effect of oxidant hydrogen peroxide in the preparation silicon nanowires to a certain extent, this simple and effective preparation method will make silicon nanowires play an important role in efficient, the low-cost photovoltaic application in future.
Embodiment 3
(1) silicon chip is used earlier successively acetone, dehydrated alcohol, deionized water ultrasonic cleaning respectively 15 minutes, it is 1: 1: 5 ammoniacal liquor then with volume ratio: hydrogen peroxide: water, boiling under 85 ℃ 15 minutes, is to soak in 3% the hydrofluoric acid to remove silicon oxide layer in 1 minute with massfraction again; Be 1: 1: 5 hydrochloric acid then with volume ratio: hydrogen peroxide: water, boiled the last silicon chip that obtains fluorine terminated surface hydrophobicity successively with deionized water and dilute hydrofluoric acid solution flushing 15 minutes under 85 ℃.
(2) cleaned silicon slice placed being gone under the room temperature concentration is 4.0 mol hydrofluoric acid and 20.0 mmoles/rise in the aqueous solution of Silver Nitrate, and Immersion time is 60 seconds, takes out rapidly then, and silicon chip surface has deposited one deck silver nano-grain equably.
(3) silicon chip that will deposit the silver nano-grain layer embathes in deionized water earlier, immerses then in the aqueous solution of the hydrofluoric acid that hydrogen peroxide oxidation handles to carry out etching, and wherein the concentration of hydrofluoric acid is 5.0 mol, and the concentration of hydrogen peroxide is 0.1 mol; Entire reaction is to carry out under 25 ℃ the condition in temperature.
(4) reaction times took out silicon chip then and is that 65% nitric acid drip washing is to remove silver nano-grain with massfraction between 1-30 minute; And then with a large amount of deionized water rinsings and 60 ℃ of oven dry in baking oven.
(5) by sem observation the length of smooth silicon nanowire array is in the scope of 250-6400 nanometer under the differential responses time, growth velocity is 0.16 micron/minute.The integrated reflection intensity that experiment records this smooth surface silicon nanowire array can reach below 1%, has excellent anti-reflection characteristic.
Provide a kind of new way of studying metal assistant chemical etching mechanism simultaneously by under suitable hydrogen peroxide concentration, preparing big area, length controlled, ganoid silicon nanowire array, understood the effect of oxidant hydrogen peroxide in the preparation silicon nanowires to a certain extent, this simple and effective preparation method will make silicon nanowires have excellent anti-reflection characteristic and light falls into effect, plays an important role in efficient, the low-cost photovoltaic application in future.
Claims (6)
1. the preparation method of the smooth surface silicon nanowire array of a length controlled, it is characterized in that, by at first silicon chip being carried out wet chemical cleans, in the mixing solutions that contains hydrofluoric acid and Silver Nitrate, utilize no electrochemical deposition method at silicon chip surface depositing silver nano-particle layer then, mixing solutions through containing hydrofluoric acid and hydrogen peroxide carries out chemical etching, removes silver nano-grain with nitric acid at last and obtains silicon nanowire array.
2. the preparation method of the smooth surface silicon nanowire array of length controlled according to claim 1 is characterized in that, described silicon chip is meant: resistivity is p type (100) the crystal orientation electronic-grade silicon chip of 0.01-0.03 Ω cm.
3. the preparation method of the smooth surface silicon nanowire array of length controlled according to claim 1, it is characterized in that, described wet chemical cleans is meant: silicon chip is used earlier acetone successively, dehydrated alcohol, deionized water ultrasonic cleaning each 15 minutes, be 1: 1: 5 ammoniacal liquor then successively with volume ratio: hydrogen peroxide: water boiled under 85 ℃ 15 minutes, at massfraction is to soak 1 minute in 3% the hydrofluoric acid, be 1: 1: 5 hydrochloric acid again in volume ratio: hydrogen peroxide: boiled 15 minutes under 85 ℃ in the water, wash the silicon chip that obtains hydrophobic surface with deionized water and dilute hydrofluoric acid solution successively at last.
4. the preparation method of the smooth surface silicon nanowire array of length controlled according to claim 1, it is characterized in that, described utilization does not have electrochemical deposition method and is meant at silicon chip surface depositing silver nano-particle layer: with silicon chip putting into hydrofluoric acid that concentration under the room temperature is 4.0 mol and 15.0 mmoles/liter the aqueous solution 60-120 of Silver Nitrate take out rapidly after second, make silicon chip surface uniform deposition one deck silver nano-grain.
5. the preparation method of the smooth surface silicon nanowire array of length controlled according to claim 1, it is characterized in that, described chemical etching is meant: the silicon chip that will deposit the silver nano-grain layer embathes in deionized water earlier, immerse in the mixing solutions that contains hydrofluoric acid and hydrogen peroxide then and carry out etching, wherein: the concentration of hydrofluoric acid is 5.0 mol, the concentration of hydrogen peroxide is 0.02 to 8.0 mol, and entire reaction is carried out at ambient temperature and utilize wavelength in the sign of photoluminescence is that the laser of 514.5 nanometers is as exciting light.
6. the preparation method of the smooth surface silicon nanowire array of length controlled according to claim 1, it is characterized in that, describedly remove silver nano-grain with nitric acid and be meant: be 65% salpeter solution drip washing silicon chip removing its surperficial silver nano-grain with massfraction earlier, and then with deionized water rinsing and 60 ℃ of oven dry in baking oven.
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