CN111217320B - Method for growing cadmium sulfide nanowire array on surface of silicon wafer - Google Patents
Method for growing cadmium sulfide nanowire array on surface of silicon wafer Download PDFInfo
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- CN111217320B CN111217320B CN202010040193.9A CN202010040193A CN111217320B CN 111217320 B CN111217320 B CN 111217320B CN 202010040193 A CN202010040193 A CN 202010040193A CN 111217320 B CN111217320 B CN 111217320B
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Abstract
The invention discloses a method for growing a cadmium sulfide nanowire array on the surface of a silicon wafer, which comprises the following steps: 1) Preparing a silicon pyramid structure on the surface of a silicon wafer, and then preparing a cadmium sulfide seed layer on the surface of the silicon pyramid; wherein the silicon pyramid structure is used for increasing the adhesiveness of the silicon surface and the cadmium sulfide seed layer; 2) Growing cadmium sulfide nanowires on the cadmium sulfide seed layer by a hydrothermal method to obtain a cadmium sulfide nanowire array; 3) Rinsing and airing the cadmium sulfide nanowire array obtained in the step 2) by deionized water. According to the invention, the growth of the cadmium sulfide nanowire on the surface of the silicon wafer is realized by introducing a pyramid structure and combining a hydrothermal growth method for the first time; the pyramid is introduced to increase the adhesiveness between the silicon surface and the cadmium sulfide seed layer, so that the method is simple, the cost is low, and the operation is easy compared with the method for introducing a silicon column structure on the surface of a silicon wafer.
Description
Technical Field
The invention relates to a method for growing a cadmium sulfide nanowire array, in particular to a method for growing a cadmium sulfide nanowire array on the surface of a silicon wafer.
Background
Cadmium sulfide is an important semiconductor material and is widely applied to photosensitive devices such as solar cells and photoresistors. Due to the development of nanotechnology, scientists have found that nanotopography has more excellent properties on materials, such as reduced reflection, etc. The nano morphology of cadmium sulfide nanospheres, nanowires, nanoflower and the like is prepared by a hydrothermal method, a chemical vapor deposition method, a template method and the like in a profound manner by the scientists. However, most of the methods produce cadmium sulfide nanostructures as nanopowders, i.e., cannot be grown directly on a desired substrate, which is detrimental to the application of the cadmium sulfide nanomaterial to devices. Recent studies have shown that scientists have also successfully grown cadmium sulfide nanostructures on ITO-coated glass surfaces, alumina (ceramic surfaces) using hydrothermal methods. However, silicon wafers are commonly used as semiconductor substrates, and few reports of growing cadmium sulfide nanostructures on the surface of silicon wafers are available.
In the previous work of the invention, the cadmium sulfide nano structure, the nanorod structure and the aspect ratio of less than 2 are prepared on the surface of the silicon wafer. The preparation method comprises the steps of firstly preparing a silicon columnar structure on the surface of a silicon wafer by using a cesium chloride nanometer island self-assembly method, then wrapping a seed layer by using magnetron sputtering, and finally growing cadmium sulfide nanometer columns (J.Liu, X.X.Liang, Y.T.Wang, B.Wang, T.C.Zhang, F.T.Yi, preparation of CdS nanorods on silicon nanopillars surface by hydrothermal Method, mater.Res.Bull.120 (2019) 110591) by using a hydrothermal method. According to the method, the cadmium sulfide nanorods are grown on the surface of the silicon wafer by means of the surface of the columnar structure of silicon, but the cost for preparing the columnar structure of the silicon by using the cesium chloride nanometer island self-assembly method is high, and an ICP dry etching machine is needed. Meanwhile, the cadmium sulfide nanorods grown on the surface of the silicon nanorods have the aspect ratio smaller than 2, the cadmium sulfide on the side wall of the silicon nanorods has poor appearance and uneven appearance.
It is difficult to prepare nanowire structures on the surface of a silicon wafer in the prior art.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a method for growing a cadmium sulfide nanowire array on the surface of a silicon wafer. The pyramid structure is prepared on the surface of the silicon wafer by a wet etching method, and the pyramid structure can effectively increase the adhesion between the seed layer and the silicon wafer, so that the seed layer cannot fall off in the process of preparing the cadmium sulfide nano array. On the other hand, the pyramid structure does not have sidewalls as does the silicon pillar array, so the grown nanowires are relatively uniform. Meanwhile, the invention discloses the technological conditions for growing the cadmium sulfide nanowire aiming at the pyramid shape.
The invention is mainly characterized in that:
1. the invention realizes the growth of the structure for preparing the cadmium sulfide nanowire with the aspect ratio larger than 3 on the surface of the silicon wafer for the first time.
2. The invention realizes the growth of the cadmium sulfide nanowire on the surface of the silicon wafer by introducing the pyramid structure and combining a hydrothermal growth method for the first time. The pyramid is introduced to increase the adhesiveness between the silicon surface and the cadmium sulfide seed layer, so that the seed layer cannot fall off in the hydrothermal reaction process. The pyramid structure is a structure which is commonly used on the surface of a silicon wafer and used for reducing reflection, but is used for the first time in the process of preparing the cadmium sulfide nanowire on the surface of the silicon wafer, and the growth of the cadmium sulfide nanowire on the surface of the silicon wafer is successfully realized by means of the appearance of the pyramid.
3. The use of the seed layer, the growth of cadmium sulfide nanowires on the surface of the silicon pyramid, the experimental result shows that the thickness of the seed layer is about 75-85 nanometers as the optimal value, if the thickness is more than 120 micrometers, obvious falling off occurs in the hydrothermal reaction process, the thickness is less than 50 micrometers, the growth speed of the cadmium sulfide nanowires can be slowed down, and the growth of the cadmium sulfide nanowires is uneven, which is unfavorable for the growth of the cadmium sulfide nanowires, and affects the appearance of the cadmium sulfide nanowires.
4. The specific conditions of the hydrothermal reaction are correspondingly optimized, and the growth conditions of the hydrothermal method are as follows:
the molar ratio of cadmium nitrate to thiourea is 1:3. glutathione is an important complexing agent, and if glutathione is not added, cadmium sulfide nanowires cannot grow on the surface of the gold tower. If the molar ratio of glutathione is less than 0.2, the growth speed of the nanowire is slow and uneven, and when the molar ratio is more than 0.4, the optimal molar ratio is 0.2-0.3, the corrosion phenomenon occurs.
The technical scheme of the invention is as follows:
a method for growing a cadmium sulfide nanowire array on the surface of a silicon wafer comprises the following steps:
1) Preparing a silicon pyramid structure on the surface of a silicon wafer, and then preparing a cadmium sulfide seed layer on the surface of the silicon pyramid; wherein the silicon pyramid structure is used for increasing the adhesiveness of the silicon surface and the cadmium sulfide seed layer;
2) Growing cadmium sulfide nanowires on the cadmium sulfide seed layer by a hydrothermal method to obtain a cadmium sulfide nanowire array;
3) Rinsing and airing the cadmium sulfide nanowire array obtained in the step 2) by deionized water.
Further, in the step 1), the silicon wafer is subjected to wet etching, and the silicon pyramid structure is obtained on the surface of the silicon wafer after the silicon wafer is kept in an alkaline solution for 20-30 minutes at 80 ℃.
Further, the mass fraction of sodium hydroxide in the alkaline solution is 1.5%, the mass fraction of sodium silicate is 1.5%, and the volume fraction of isopropanol is 6.5%.
Further, growing cadmium sulfide nanowires on the cadmium sulfide seed layer by a hydrothermal method; the growth conditions of the hydrothermal method comprise a solution consisting of deionized water, cadmium nitrate, thiourea and glutathione, wherein the growth temperature is 195-205 ℃ and the growth time is 1.5-2 hours; wherein deionized water: cadmium nitrate: thiourea: the molar ratio of glutathione is 80:1:3:0.2 to 0.3.
Further, the thickness of the seed layer is 75-85 nanometers.
Further, the cadmium sulfide seed layer is covered on the surface of the pyramid by adopting a magnetron sputtering method; wherein the target material is 99.99% purity cadmium sulfide, the working temperature is room temperature, the working pressure is 0.2 Pa, the sputtering power is 20 watts, and the sputtering time is 4 minutes.
Further, the silicon wafer is a P-type silicon wafer with the thickness of 0.2-0.5 mm and the resistivity of 1-10Ω & cm.
FIG. 5 is an effect of different molar ratios of glutathione on the growth of cadmium sulfide nanowires on the pyramid surface (SEM front view), at 200℃for 1.5 hours.
The growth temperature is an important parameter for growing the cadmium sulfide nanowire, and experiments show that the cadmium sulfide nanowire can not grow basically at 160 ℃, the nanowire grows slowly at 180 ℃, the nanowire has the best morphology at 200 ℃, and the nanowire becomes thin at 220 ℃ so as to generate corrosion. The growth temperature should be controlled between 195-205 degrees celsius. The temperature is low, the growth speed is too slow, the temperature is too high, and the cadmium sulfide nanowire is corroded.
FIG. 6 is a graph of growth conditions (SEM front view) of cadmium sulfide nanowires at different growth temperatures, wherein the molar ratio of cadmium nitrate, thiourea and glutathione is 1:3:0.3, and the growth time is 1.5 hours.
The appearance of the cadmium sulfide nanowire grown in the growth time is also greatly influenced, and experiments show that: the longer the growth time, the thicker the cadmium sulfide nanowires, but when the growth time exceeds 2 hours, the nanowires at the top of the pyramid are gradually adhered together to form a lump shape, and are obviously uneven. The growth time is 1.5-2 hours, the appearance of the cadmium sulfide nanowire is the best, and the cadmium sulfide nanowire is relatively uniform.
FIG. 7 is a graph of growth of cadmium sulfide nanowires at various times (SEM side view), with a molar ratio of cadmium nitrate, thiourea, glutathione of 1:3:0.3, growth temperature 200 ℃. (a) 0 hours, (b) 0.5 hours, (c) 1 hour, (d) 1.5 hours, (e) 2 hours, and (f) 2.5 hours.
Compared with the prior art, the invention has the following positive effects:
the invention realizes the growth of the cadmium sulfide nanowire on the surface of the silicon wafer by introducing the pyramid structure and combining a hydrothermal growth method for the first time. The pyramid is introduced to increase the adhesiveness between the silicon surface and the cadmium sulfide seed layer. Compared with the method for introducing the silicon column structure on the surface of the silicon wafer, the method is simple, low in cost and easy to operate. The cadmium sulfide nanorods can only be grown on the surface of the silicon column, namely, the aspect ratio is smaller than 2, and the growth of the nanorods is not good enough on the side surface of the silicon column structure, so that the growth of the cadmium sulfide nanorods is not uniform. On the surface of the pyramid, the uniform growth of the cadmium sulfide nanowire is realized, the diameter of the nanowire is 100-150 nanometers, the height is 400-500 nanometers, the aspect ratio is greater than 3, and the top end is in a hexagonal shape, as shown in figure 8. If the pyramid structure is not used on the polished silicon wafer surface, the seed layer is fallen off in the hydrothermal reaction process, and the growth of the cadmium sulfide nanowire on the silicon wafer surface is impossible. Meanwhile, if a seed layer with proper thickness is not provided, the cadmium sulfide nanowire can not grow on the surface of the silicon wafer.
For hydrothermal reaction growth conditions, chen Fei et al (F.Chen, R.Zhou, L.Yang, M.Shi, G.Wu, M.Wang, H.Chen, one-Step Fabrication of CdS Nanorod Arrays via Solution Chemistry, j. Phys. Chem. C112 (2008) 13457-13462) also grown cadmium sulfide nanorods with similar hydrothermal reaction conditions, the hydrothermal method they applied was: 80 ml of deionized water, 1 mmol of cadmium nitrate, 3 mmol of thiourea, 0.6 mmol of glutathione, and the reaction temperature is 200 ℃ for 3.5 hours; the diameter of the grown nano rod is 100 nanometers, and the length is about 300-400 nanometers, but the method of the document is to realize the growth of the cadmium sulfide nano wire on ITO glass, but not on the surface of a silicon wafer.
Drawings
FIG. 1 is a flow chart of a method for preparing cadmium sulfide nanowires on the surface of a silicon wafer.
Fig. 2 is a diagram of the preparation of a pyramid structure on a silicon wafer.
Fig. 3 is a diagram of the preparation of a seed layer on a pyramid structure.
FIG. 4 is a diagram of growing cadmium sulfide nanowires on a seed layer.
FIG. 5 is an effect of different molar ratios of glutathione on the growth of cadmium sulfide nanowires on pyramid surfaces (SEM elevation), at 200℃for 1.5 hours;
the molar ratio of (a) was 0, (b) was 0.1, (c) was 0.2, (d) was 0.3, (e) was 0.4, and (f) was 0.6.
FIG. 6 is a graph of growth conditions (SEM front view) of cadmium sulfide nanowires at different growth temperatures, wherein the molar ratio of cadmium nitrate, thiourea and glutathione is 1:3:0.3, the growth time is 1.5 hours;
(a)160℃,(b)180℃,(c)200℃,(d)220℃。
FIG. 7 is a graph of growth of cadmium sulfide nanowires at various times (SEM side view), with a molar ratio of cadmium nitrate, thiourea, glutathione of 1:3:0.3, the growth temperature is 200 ℃;
(a) 0 hours, (b) 0.5 hours, (c) 1 hour, (d) 1.5 hours, (e) 2 hours, and (f) 2.5 hours.
Detailed Description
The present application will now be described in further detail with reference to the accompanying drawings and examples, but is not limited thereto.
The process flow chart of the preparation of the cadmium sulfide nanowire on the surface of the silicon wafer is shown in fig. 2-4, and the preparation method mainly comprises the steps of firstly adopting alkaline solution to anisotropically corrode the surface of the silicon wafer to prepare a pyramid structure. The pyramid structure can effectively increase the adhesion between the seed layer and the silicon wafer, so that the seed layer cannot fall off in the process of preparing the cadmium sulfide nano array. And then covering the pyramid surface with a seed layer by using a magnetron sputtering method. Finally, growing the cadmium sulfide nanowire by a hydrothermal method. The method has the advantages of low cost, uniform size of the grown cadmium sulfide nanowire, diameter of 100-150 nanometers, height of 400-500 nanometers and aspect ratio of more than 3.
In the invention, silicon wafers used in the semiconductor industry are selected as silicon materials, the thickness is 0.2-0.5 mm, the P-type resistivity is 1-10Ω cm, and the surface is a polished surface. First, the silicon wafer was wet etched, and the silicon pyramid structure with an average size of 4 μm was obtained on the surface of the silicon wafer at 80℃for 20 to 30 minutes in an alkaline solution (1.5% sodium hydroxide by mass, 1.5% sodium silicate by mass, and 6.5% isopropyl alcohol by volume). Secondly, preparing a cadmium sulfide seed layer on the surface of the silicon pyramid by using a magnetron sputtering method, wherein the target material is 99.99% pure cadmium sulfide, the working temperature is room temperature, the working pressure is 0.2 Pa, the sputtering power is 20 watts, the sputtering time is 4 minutes, and the thickness of the cadmium sulfide seed layer obtained on the surface of the pyramid is 80 nanometers. Then growing the cadmium sulfide nanowire by a hydrothermal method under the growth conditions of 80 milliliters of deionized water, 1 millimole of cadmium nitrate, 3 millimoles of thiourea and 0.3 millimoles of glutathione, wherein the glutathione is a complexing agent. The prepared solution was poured into a reaction vessel having a volume of 100 ml, and the reaction was maintained at 200℃for 1.5 hours. And after the reaction is finished, naturally cooling the temperature to room temperature, and taking out the sample. And finally, repeatedly rinsing with deionized water and airing. Thus, the growth process of the cadmium sulfide nanowire on the surface of the silicon wafer is completed.
The foregoing is a further detailed description of the present application in connection with the specific embodiments, and it is not intended that the specific implementation of the present application be limited to these descriptions. It will be apparent to those skilled in the art from this disclosure that several simple deductions or substitutions can be made without departing from the inventive concepts of the present application.
Claims (5)
1. A method for growing a cadmium sulfide nanowire array on the surface of a silicon wafer comprises the following steps:
1) Preparing a silicon pyramid structure on the surface of a silicon wafer, and then preparing a cadmium sulfide seed layer on the surface of the silicon pyramid; wherein the silicon pyramid structure is used for increasing the adhesiveness of the silicon surface and the cadmium sulfide seed layer; the thickness of the cadmium sulfide seed layer is 75-85 nanometers;
2) Growing cadmium sulfide nanowires on the cadmium sulfide seed layer by a hydrothermal method to obtain a cadmium sulfide nanowire array; the growth conditions of the hydrothermal method comprise a solution consisting of deionized water, cadmium nitrate, thiourea and glutathione, wherein the growth temperature is 195-205 ℃, and the growth time is 1.5-2 hours; wherein deionized water: cadmium nitrate: thiourea: the molar ratio of glutathione is 80:1:3: 0.2-0.3;
3) Rinsing and airing the cadmium sulfide nanowire array obtained in the step 2) by deionized water; the diameter of the cadmium sulfide nanowire in the cadmium sulfide nanowire array is 100-150 nanometers, the height is 400-500 nanometers, and the aspect ratio is more than 3.
2. The method according to claim 1, wherein in step 1), the silicon wafer is subjected to wet etching, and is maintained in an alkaline solution at 80 ℃ for 20 to 30 minutes, to obtain the silicon pyramid structure on the surface of the silicon wafer.
3. The method according to claim 2, wherein the alkaline solution has a mass fraction of sodium hydroxide of 1.5%, a mass fraction of sodium silicate of 1.5% and a volume fraction of isopropyl alcohol of 6.5%.
4. The method of claim 1, wherein the cadmium sulfide seed layer is coated on the surface of the pyramid by a magnetron sputtering method; wherein the target material is 99.99% purity cadmium sulfide, the working temperature is room temperature, the working pressure is 0.2 Pa, the sputtering power is 20 watts, and the sputtering time is 4 minutes.
5. The method of claim 1, wherein the silicon wafer is a P-type silicon wafer having a thickness of 0.2 to 0.5 mm and a resistivity of 1 to 10 Ω -cm.
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| CN103112816A (en) * | 2013-01-30 | 2013-05-22 | 中国科学院大学 | Method for preparing pyramid array on monocrystalline silicon substrate |
| CN104538283A (en) * | 2014-12-18 | 2015-04-22 | 中国科学院高能物理研究所 | Preparation method for inverted pyramid structure on silicon wafer surface |
| CN107175114A (en) * | 2017-05-12 | 2017-09-19 | 华南理工大学 | A kind of cadmium sulfide nano-stick array outsourcing titanium deoxid film composite and preparation method thereof |
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| WO2010057060A2 (en) * | 2008-11-13 | 2010-05-20 | Solexel, Inc. | Methods and systems for manufacturing thin-film solar cells |
| TW201119935A (en) * | 2009-12-04 | 2011-06-16 | Univ Nat Chiao Tung | Catalytic seeding control method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103112816A (en) * | 2013-01-30 | 2013-05-22 | 中国科学院大学 | Method for preparing pyramid array on monocrystalline silicon substrate |
| CN104538283A (en) * | 2014-12-18 | 2015-04-22 | 中国科学院高能物理研究所 | Preparation method for inverted pyramid structure on silicon wafer surface |
| CN107175114A (en) * | 2017-05-12 | 2017-09-19 | 华南理工大学 | A kind of cadmium sulfide nano-stick array outsourcing titanium deoxid film composite and preparation method thereof |
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| Yejing Daia，et al..Enhanced performances of Si/CdS heterojunction near-infrared photodetector by the piezo-phototronic effect.Nano Energy.2017,(第44期),第311-312页第1-2.1节、第317-318页第4节. * |
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