CN111217320A - Method for growing cadmium sulfide nanowire array on surface of silicon wafer - Google Patents
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- CN111217320A CN111217320A CN202010040193.9A CN202010040193A CN111217320A CN 111217320 A CN111217320 A CN 111217320A CN 202010040193 A CN202010040193 A CN 202010040193A CN 111217320 A CN111217320 A CN 111217320A
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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; the silicon pyramid structure is used for increasing the adhesion between 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 using deionized water. The growth of cadmium sulfide nanowires on the surface of a silicon wafer is realized by introducing a pyramid structure and combining a hydrothermal growth method for the first time; the pyramid is introduced, so that the adhesion between the silicon surface and the cadmium sulfide seed layer is increased, and compared with the method for introducing the silicon pillar structure on the silicon surface, the method is simple, low in cost and easy to operate.
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, photoresistors and the like. Due to the development of nanotechnology, scientists find that nanotopography has more excellent performance on materials, such as reflection reduction and the like. Scientists have increasingly prepared nanometer morphologies such as cadmium sulfide nanospheres, nanowires, nanoflowers and the like by using a hydrothermal method, a chemical vapor deposition method, a template method and the like. However, most of the cadmium sulfide nanostructures prepared by the method are nanopowder, that is, the cadmium sulfide nanostructures cannot be directly grown on a required substrate, which is unfavorable for the application of the cadmium sulfide nanomaterials on devices. Recent studies have shown that scientists have also succeeded in hydrothermally growing cadmium sulfide nanostructures on ITO-covered glass surfaces, alumina (ceramic surfaces). However, as a commonly used semiconductor substrate, there are few reports of growing cadmium sulfide nanostructures on the surface of a silicon wafer.
In the previous work of the invention, cadmium sulfide nano-structures and nano-rod structures with the aspect ratio less than 2 are successfully prepared on the surfaces of silicon wafers. The Method comprises the steps of firstly preparing a silicon columnar structure on the surface of a silicon wafer by a cesium chloride nano-island self-assembly Method, then wrapping a seed layer by magnetron sputtering, and finally growing cadmium sulfide nano-columns (J.Liu, X.X.Liang, Y.T.Wang, B.Wang, T.C.Zhang, F.T.Yi, Preparation CdS of nanoparticles on silicon nanoparticles by hydrothermal Method, mater.Res.Bull.120(2019) 110591) by a hydrothermal Method. In the method, by means of the surface of the columnar silicon structure, cadmium sulfide nanorods are grown on the surface of a silicon wafer, but the preparation of the columnar silicon structure by the cesium chloride nano island self-assembly method is high in cost and needs to use an ICP dry etching machine. Meanwhile, the cadmium sulfide nanorod growing on the surface of the silicon nanorod has the height-width ratio smaller than 2, the cadmium sulfide on the side wall of the silicon nanorod is poor in appearance, and the nanorod is uneven in appearance.
The prior art is difficult to prepare a nanowire structure on the surface of a silicon wafer.
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. According to the invention, 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 can not fall off in the process of preparing the cadmium sulfide nano array. On the other hand, the pyramid structure does not have side walls as the silicon pillar array, so the grown nanowires are relatively uniform. Meanwhile, the invention discloses a process condition for growing the cadmium sulfide nanowire aiming at the shape of the pyramid.
The invention is mainly characterized in that:
1. the invention realizes the growth of the structure for preparing the cadmium sulfide nanowire with the height-width ratio more than 3 on the surface of the silicon wafer for the first time.
2. 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, so that the adhesiveness of the silicon surface and the cadmium sulfide seed layer is increased, and the seed layer cannot fall off in the hydrothermal reaction process. The pyramid structure is a common reflection reducing structure on the surface of a silicon wafer, 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 pyramid appearance.
3. The use of the seed layer leads cadmium sulfide nanowires to grow on the surface of the silicon pyramid, and experimental results show that the thickness of the seed layer is about 75-85 nanometers and is the optimal value, if the thickness is more than 120 micrometers, the cadmium sulfide nanowires obviously fall off in the hydrothermal reaction process, and if the thickness is less than 50 micrometers, the growth speed of the cadmium sulfide nanowires becomes slow and uneven, which is not beneficial to the growth of the cadmium sulfide nanowires and influences the appearance of the cadmium sulfide nanowires.
4. The hydrothermal reaction, the specific conditions of which are correspondingly optimized, the growth conditions of the hydrothermal method are as follows:
the molar ratio of the cadmium nitrate to the 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 the glutathione is lower than 0.2, the growth speed of the nanowire is slow and uneven, the molar ratio is 0.2-0.3, and if the molar ratio is higher than 0.4, the corrosion phenomenon occurs.
The technical scheme of the invention is as follows:
a method for growing cadmium sulfide nanowire arrays 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; the silicon pyramid structure is used for increasing the adhesion between 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 using deionized water.
Further, in the step 1), the silicon wafer is subjected to wet etching, and is kept in an alkaline solution at 80 ℃ for 20-30 minutes, so that the silicon pyramid structure is obtained on the surface of the silicon wafer.
Further, the alkaline solution contains 1.5% by mass of sodium hydroxide, 1.5% by mass of sodium silicate and 6.5% by volume of isopropanol.
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, the growth temperature is 195-205 ℃, and the growth time is 1.5-2 hours; wherein the deionized water: cadmium nitrate: thiourea: the molar ratio of the glutathione is 80: 1: 3: 0.2 to 0.3.
Furthermore, the thickness of the seed layer is 75-85 nanometers.
Further, covering the cadmium sulfide seed layer on the surface of the pyramid by adopting a magnetron sputtering method; wherein the target material is cadmium sulfide with the purity of 99.99 percent, 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.
Furthermore, the silicon wafer is a P-type silicon wafer with the thickness of 0.2-0.5 mm and the resistivity of 1-10 omega cm.
FIG. 5 is an SEM (scanning electron microscope) front view showing the effect of different molar ratios of glutathione on the growth of cadmium sulfide nanowires on the pyramid surface, wherein the growth temperature is 200 ℃, and the growth time is 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 the temperature of 160 ℃, the growth of the nanowire is slow at the temperature of 180 ℃, the shape of the nanowire is best at the temperature of 200 ℃, and the nanowire becomes thin and is corroded at the temperature of 220 ℃. Therefore, the growth temperature should be controlled between 195-205 ℃. The temperature is low, the growth speed is too slow, the temperature is too high, and the cadmium sulfide nanowires are corroded.
FIG. 6 is a diagram (SEM front view) of growth conditions 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.
The growth time of the cadmium sulfide nanowire has great influence on the appearance, and experiments show that: the longer the growth time is, the thicker the cadmium sulfide nanowire is, 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, which is obviously uneven. The growth time is 1.5-2 hours, and the cadmium sulfide nanowires have the best appearance and are relatively uniform.
FIG. 7 is a graph (SEM side view) showing growth of cadmium sulfide nanowires at different times, wherein the molar ratio of cadmium nitrate, thiourea and glutathione is 1: 3: 0.3, and the growth temperature is 200 ℃. (a)0 hour, (b)0.5 hour, (c)1 hour, (d)1.5 hour, (e)2 hours, and (f)2.5 hours.
Compared with the prior art, the invention has the following positive effects:
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 adhesion of the silicon surface to 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 nano-rod can only be grown on the surface of the silicon column, namely the height-to-width ratio is less than 2, and the growth of the nano-rod is not good enough on the side surface of the silicon column structure, so that the growth of the cadmium sulfide nano-rod is not uniform. On the pyramid surface, the growth of uniform cadmium sulfide nanowires is realized, the diameter of the nanowires is 100-150 nm, the height is 400-500 nm, the aspect ratio is greater than 3, and the top ends are in a hexagonal shape, as shown in fig. 8. If the pyramid structure is not used on the polished surface of the silicon wafer, the seed layer falls off early in the hydrothermal reaction process, and the growth of the cadmium sulfide nanowire on the surface of the silicon wafer cannot be realized. Meanwhile, if a seed layer with proper thickness is not available, the cadmium sulfide nanowire can not grow on the surface of the silicon wafer.
For the growth conditions of the hydrothermal reaction, Chengfei et al (F.Chen, R.Zhou, L.Yang, M.Shi, G.Wu, M.Wang, H.Chen, One-Step Fabrication of CdS Nanoprod Array solution chemistry, J.Phys.chem.C 112(2008) 13457-: 80 ml of deionized water, 1 mmol of cadmium nitrate, 3 mmol of thiourea and 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 disclosed by the document realizes the growth of the cadmium sulfide nano wire on the ITO glass, and does not realize the growth 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 according to the present invention.
FIG. 2 illustrates the preparation of a pyramid structure on a silicon wafer.
FIG. 3 shows the fabrication of a seed layer on the pyramid structure.
Fig. 4 shows cadmium sulfide nanowires grown on a seed layer.
FIG. 5 is an SEM front view showing the effect of glutathione with different molar ratios on the growth of cadmium sulfide nanowires on the pyramid surface, wherein the growth temperature is 200 ℃ and the growth time is 1.5 hours;
(a) the molar ratio is 0, (b) the molar ratio is 0.1, (c) the molar ratio is 0.2, (d) the molar ratio is 0.3, (e) the molar ratio is 0.4, and (f) the molar ratio is 0.6.
FIG. 6 is a diagram (SEM front view) of growth conditions 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 (SEM side view) showing growth of cadmium sulfide nanowires at different times, wherein the molar ratio of cadmium nitrate, thiourea and glutathione is 1: 3: 0.3, the growth temperature is 200 ℃;
(a)0 hour, (b)0.5 hour, (c)1 hour, (d)1.5 hour, (e)2 hours, and (f)2.5 hours.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples, but the present application is not limited thereto.
The process flow diagram for preparing the cadmium sulfide nanowire on the surface of the silicon wafer is shown in fig. 2-4, and the steps mainly comprise the steps of firstly adopting alkaline solution to carry out anisotropic corrosion on the surface of the silicon wafer to prepare a pyramid structure. The pyramid structure can effectively increase the adhesive force between the seed layer and the silicon wafer, so that the seed layer can not fall off in the process of preparing the cadmium sulfide nano array. And then covering a seed layer on the pyramid surface by a magnetron sputtering method. And 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, 100-150 nm diameter, 400-500 nm height and more than 3 aspect ratio.
In the invention, the silicon material is a silicon wafer used in the semiconductor industry, the thickness of the silicon wafer is 0.2-0.5 mm, the silicon wafer is P-type, the resistivity of the silicon wafer is 1-10 omega cm, and the surface of the silicon wafer is a polished surface. First, a silicon wafer is subjected to wet etching and kept in an alkaline solution (1.5% by mass of sodium hydroxide, 1.5% by mass of sodium silicate, and 6.5% by volume of isopropyl alcohol) at 80 ℃ for 20 to 30 minutes to obtain a silicon pyramid structure with an average size of 4 μm on the surface of the silicon wafer. Secondly, preparing a cadmium sulfide seed layer on the surface of the silicon pyramid by a magnetron sputtering method, wherein the target material is cadmium sulfide with the purity of 99.99 percent, 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. And then, growing the cadmium sulfide nanowire by a hydrothermal method, wherein the growth conditions of the hydrothermal method are 80 ml of deionized water, 1 mmol of cadmium nitrate, 3 mmol of thiourea and 0.3 mmol of glutathione, wherein the glutathione is a complexing agent. The prepared solution was poured into a reaction vessel having a capacity of 100 ml, and the reaction was maintained at 200 ℃ for 1.5 hours. After the reaction is finished, the temperature is cooled naturally to room temperature, and a sample is taken out. And finally, repeatedly rinsing with deionized water and drying. And finishing the growth process of the cadmium sulfide nanowire on the surface of the silicon wafer.
The above description is further described in detail with reference to specific embodiments, and specific embodiments of the present application are not to be construed as being limited to the description. It will be apparent to those skilled in the art from this disclosure that many more simple derivations or substitutions can be made without departing from the inventive concepts herein.
Claims (7)
1. A method for growing cadmium sulfide nanowire arrays 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; the silicon pyramid structure is used for increasing the adhesion between 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 using deionized water.
2. The method as claimed in claim 1, wherein in the step 1), the silicon wafer is subjected to wet etching, and is kept in an alkaline solution at 80 ℃ for 20-30 minutes to obtain the silicon pyramid structure on the surface of the silicon wafer.
3. The method of 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 nanowires are grown on the cadmium sulfide seed layer using a hydrothermal process; the growth conditions of the hydrothermal method comprise a solution consisting of deionized water, cadmium nitrate, thiourea and glutathione, the growth temperature is 195-205 ℃, and the growth time is 1.5-2 hours; wherein the deionized water: cadmium nitrate: thiourea: the molar ratio of the glutathione is 80: 1: 3: 0.2 to 0.3.
5. The method of claim 1, wherein the seed layer has a thickness of 75 to 85 nm.
6. The method of claim 1 or 5, wherein the cadmium sulfide seed layer is covered on the pyramid surface by a magnetron sputtering method; wherein the target material is cadmium sulfide with the purity of 99.99 percent, 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.
7. The method according to 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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