CN113278933B - Patterned silicon carbide nanowire and silicon nanowire one-dimensional composite material and preparation method thereof - Google Patents
Patterned silicon carbide nanowire and silicon nanowire one-dimensional composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a patterned silicon carbide nanowire and a silicon nanowire one-dimensional composite material, which comprise a silicon carbide nanowire, a silicon nanowire growing in situ in a silicon carbide nanowire array and metal particles distributed at the growing ends of the silicon carbide nanowire and the silicon nanowire, wherein the silicon nanowire is distributed in at least one region of the silicon carbide nanowire in a patterned manner; the functional design of different materials and different areas on the same substrate can be realized, the controllable preparation of the patterned silicon carbide nanowire and silicon nanowire composite material is realized, and the composite film of the silicon carbide nanowire and the silicon nanowire presents an obvious patterned boundary.
Description
Technical Field
The invention relates to the field of one-dimensional nano materials, in particular to a patterned silicon carbide nanowire, a silicon nanowire one-dimensional composite material and a preparation method thereof.
Background
The one-dimensional nano material has large surface area and unique optical, electric and magnetic properties different from those of a block material, so that the one-dimensional nano material has great application prospect in the aspects of microcosmic physics and production of nano devices. While most of the preparation methods produce only a single homogeneous product. With the development of nano devices, one-dimensional nano materials of a single product cannot meet the requirements of the nano devices, and customization of different areas on the same substrate according to the functional requirements cannot be realized.
Disclosure of Invention
In view of the above, the present invention is to provide a patterned silicon carbide nanowire, a patterned silicon nanowire one-dimensional composite material, and a method for preparing the same, which can realize functional designs of different materials and different regions on the same substrate, and the preparation process is controllable.
The patterned silicon carbide nanowire and silicon nanowire one-dimensional composite material comprises a silicon carbide nanowire, a silicon nanowire growing in a silicon carbide nanowire array in situ and metal particles distributed at the growing ends of the silicon carbide nanowire and the silicon nanowire, wherein the silicon nanowire is distributed in at least one region of the silicon carbide nanowire in a patterned manner;
further, the silicon carbide nanowire is formed by catalytic growth of a silicon substrate and carbon deposited on the silicon substrate;
further, the metal particles are formed of a catalyst that catalyzes the growth of silicon carbide nanowires and silicon nanowires;
further, the metal particles are nickel.
The invention relates to a preparation method of a patterned silicon carbide nanowire and a silicon nanowire one-dimensional composite material, which comprises the following steps:
a. depositing a carbon film on the silicon substrate with the drawn mask pattern by using a magnetron sputtering system to prepare a silicon/carbon composite film layer;
b. removing the mask pattern of the silicon/carbon composite film layer in the step a, and depositing a metal film layer on the surface of the silicon/carbon composite film layer to obtain a silicon/carbon/nickel composite film layer;
c. b, performing heat treatment on the composite film layer in the step b to prepare a patterned silicon carbide nanowire and a composite film of the silicon nanowire;
further, in the step a, drawing a mask pattern on the silicon substrate by adopting a direct writing method;
further, in the step a, firstly, a magnetron sputtering system is utilized to carry out back-sputtering cleaning on the surface of the silicon substrate, and then the magnetron sputtering system is utilized to deposit a carbon film on the substrate through a carbon target;
further, in the step b, a magnetron sputtering system is utilized to carry out pre-sputtering treatment on the metal target, and then a nickel film is deposited on the substrate through the nickel target;
further, in step a, the vacuum degree is 8-12X 10 -5 When the pressure is 4-6Pa, carrying out back-splash cleaning on the surface of the silicon substrate for 15-25min under the Ar gas environment; after the back-sputtering cleaning is finished, pre-sputtering the carbon target for 3-7min under the conditions that the sputtering power is 90-110W and the gas flow is 90-110sccm, then adjusting the air pressure to 0.8-1.2Pa, adding 25-35V pulse negative bias on the substrate, and depositing a carbon film on the substrate through the carbon target for 25-35 min;
in step b, the vacuum degree is 8-12X 10 -5 Pa, the pressure is 4-6Pa, under the Ar gas environment, pre-sputtering the nickel target for 3-7min under the sputtering power of 140-160W and the gas flow of 90-110sccm, adjusting the gas pressure to 0.8-1.2Pa, applying 70-90V pulse negative bias on the substrate, and depositing a nickel film on the substrate through the nickel target for 8-15 s;
further, in the step c, annealing the composite film layer in a vacuum tube furnace at the annealing temperature of 900-1100 ℃, and naturally cooling to room temperature after heat preservation for 1-3 h.
The invention has the beneficial effects that: the patterned silicon carbide nanowire and silicon nanowire one-dimensional composite material and the preparation method thereof disclosed by the invention can realize the functional design of different materials and different areas on the same substrate, realize the controllable preparation of the patterned silicon carbide nanowire and silicon nanowire composite material, and the composite film of the silicon carbide nanowire and the silicon nanowire presents an obvious patterned boundary.
Drawings
The invention is further described below with reference to the following figures and examples:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The patterned silicon carbide nanowire and silicon nanowire one-dimensional composite material of the embodiment comprises a silicon carbide nanowire, a silicon nanowire grown in situ in a silicon carbide nanowire array, and metal particles distributed at the growing ends of the silicon carbide nanowire and the silicon nanowire, wherein the silicon nanowire is distributed in at least one region of the silicon carbide nanowire in a patterned manner; the silicon carbide nanowire is formed by the catalytic growth of a silicon substrate and carbon deposited on the silicon substrate; the metal particles are formed from a catalyst that catalyzes the growth of silicon carbide nanowires and silicon nanowires; the silicon nanowires are distributed in the array region of the silicon carbide nanowires in a pattern mode to form a one-dimensional composite structure, and the silicon nanowires can be distributed in a plurality of regions of the silicon carbide nanowires. The metal particles are in granular distribution at growing ends of the silicon carbide nanowires and the silicon nanowires after the carbon/silicon material and the silicon material are grown into the silicon carbide nanowires and the silicon nanowires by catalysis of the catalyst. The patterning of the formed silicon carbide nanowire and the silicon nanowire one-dimensional composite material is clearer and more obvious. The functional design of different materials and different areas on the same substrate can be realized.
In this embodiment, the metal particles are nickel. The nickel catalytic effect is better.
The invention relates to a preparation method of a patterned silicon carbide nanowire and a silicon nanowire one-dimensional composite material, which comprises the following steps:
a. depositing a carbon film 3 on the silicon substrate 1 with the drawn mask pattern 2 by using a magnetron sputtering system to prepare a silicon/carbon composite film layer;
b. removing the mask pattern 2 from the silicon/carbon composite film layer in the step a, and depositing a metal film layer on the surface of the silicon/carbon composite film layer to obtain a silicon/carbon/nickel composite film layer;
c. b, performing heat treatment on the composite film layer in the step b to prepare a patterned silicon carbide nanowire and a composite film of the silicon nanowire; the preparation method has good repeatability and controllable process.
In this embodiment, in step a, a mask pattern 2 is drawn on a silicon substrate 1 by a direct writing method; the mask pattern 2 can be drawn on the silicon substrate 1 by a pen capable of drawing patterns, and the method is simple and controllable and can draw various patterns according to actual requirements.
In the embodiment, in the step a, firstly, a magnetron sputtering system is utilized to carry out back-sputtering cleaning on the surface of a silicon substrate 1, and then the magnetron sputtering system is utilized to deposit a carbon film 3 on the substrate through a carbon target; after the back-sputtering cleaning, the carbon film 3 is convenient to deposit on the substrate, and the film forming property of the carbon film 3 and the film firmness are ensured.
In the embodiment, in the step b, a magnetron sputtering system is used for carrying out pre-sputtering treatment on a metal target, and then a nickel film 4 is deposited on a substrate through a nickel target; the film forming property of the carbon film 3 and the film firmness are ensured.
In this example, in step a, the degree of vacuum was 8 to 12X 10 -5 When the pressure is 4-6Pa, carrying out back-splash cleaning on the surface of the silicon substrate 1 for 15-25min under the Ar gas environment; after the back-sputtering cleaning is finished, pre-sputtering the carbon target for 3-7min under the conditions that the sputtering power is 90-110W and the gas flow is 90-110sccm, then adjusting the air pressure to 0.8-1.2Pa, adding 25-35V pulse negative bias on the substrate, and depositing the carbon film 3 on the substrate through the carbon target for 25-35 min;
in step b, the vacuum degree is 8-12X 10 -5 Pa, the pressure is 4-6Pa, under the Ar gas environment, pre-sputtering the nickel target for 3-7min under the sputtering power of 140-160W and the gas flow of 90-110sccm, adjusting the gas pressure to 0.8-1.2Pa, applying 70-90V pulse negative bias on the substrate, and depositing the nickel film 4 on the substrate through the nickel target for 8-15 s;
in the embodiment, in the step c, the composite film layer is annealed in a vacuum tube furnace at the annealing temperature of 900 ℃ and 1100 ℃, and is naturally cooled to the room temperature after heat preservation for 1-3 hours.
Example one
The preparation method of the patterned silicon carbide nanowire and the silicon nanowire one-dimensional composite material of the embodiment comprises the following steps:
a. ultrasonically cleaning the silicon substrate 1 in alcohol for 15 minutes, then drying the silicon substrate, and ultrasonically cleaning the silicon substrate with acetone for 15 minutes; drawing a mask pattern 2 on a silicon substrate 1 by direct writing under a vacuum degree of 8 × 10 -5 When the pressure is 4Pa, carrying out back splash cleaning on the surface of the silicon substrate 1 for 15min under the Ar gas environment; after the back-sputtering cleaning is finished, pre-sputtering the carbon target for 3min under the conditions that the sputtering power is 90W and the gas flow is 90sccm, adjusting the air pressure to 0.8Pa, adding 25V pulse negative bias on the substrate, and depositing the carbon film 3 on the substrate through the carbon target for 25 min; preparing a silicon/carbon composite film layer;
b. removing the mask pattern 2 of the silicon/carbon composite film layer in the step a, and then keeping the vacuum degree at 8 multiplied by 10 -5 Pa, the pressure is 4Pa, in an Ar gas environment, pre-sputtering a nickel target for 3min under the sputtering power of 140W and the gas flow of 90sccm, adjusting the gas pressure to 0.8Pa, adding 70V pulse negative bias on a substrate, depositing a nickel film 4 on the substrate through the nickel target, and depositing for 8s to prepare a silicon/carbon/nickel composite film layer;
c. and (c) annealing the composite film layer in the step (b) in a vacuum tube furnace at the annealing temperature of 900 ℃, preserving the heat for 1h, and naturally cooling to room temperature to obtain the patterned silicon carbide nanowire and silicon nanowire composite film.
Example two
The preparation method of the patterned silicon carbide nanowire and the silicon nanowire one-dimensional composite material of the embodiment comprises the following steps:
a. ultrasonically cleaning the silicon substrate 1 in alcohol for 13 minutes, then drying the silicon substrate, and ultrasonically cleaning the silicon substrate with acetone for 13 minutes; drawing a mask pattern 2 on a silicon substrate 1 by direct writing under a vacuum of 12 × 10 -5 When the pressure is 6Pa, carrying out back splash cleaning on the surface of the silicon substrate 1 for 25min under the Ar gas environment; after the back-sputtering cleaning is finished, the sputtering power is 110W, and the gas flow is 110sPre-sputtering a carbon target for 7min under ccm, then adjusting the air pressure to 1.2Pa, adding 35V pulse negative bias on a substrate, and depositing a carbon film 3 on the substrate through the carbon target for 35 min; preparing a silicon/carbon composite film layer;
b. removing the mask pattern 2 of the silicon/carbon composite film layer in the step a, and then keeping the vacuum degree at 12 multiplied by 10 -5 Pa, the pressure is 6Pa, in an Ar gas environment, pre-sputtering a nickel target for 7min under the sputtering power of 160W and the gas flow of 110sccm, adjusting the gas pressure to 1.2Pa, adding 90V pulse negative bias on a substrate, depositing a nickel film 4 on the substrate through the nickel target, and depositing for 15s to prepare a silicon/carbon/nickel composite film layer;
c. and c, annealing the composite film layer in the step b in a vacuum tube furnace, keeping the annealing temperature at 1100 ℃, preserving the heat for 3 hours, and naturally cooling to room temperature to obtain the patterned silicon carbide nanowire and silicon nanowire composite film.
EXAMPLE III
The preparation method of the patterned silicon carbide nanowire and the silicon nanowire one-dimensional composite material of the embodiment comprises the following steps:
a. ultrasonically cleaning the silicon substrate 1 in alcohol for 16 minutes, then drying the silicon substrate, and ultrasonically cleaning the silicon substrate with acetone for 16 minutes; drawing a mask pattern 2 on a silicon substrate 1 by direct writing under a vacuum degree of 8 × 10 -5 When the pressure is 6Pa, carrying out back splash cleaning on the surface of the silicon substrate 1 for 15min under the Ar gas environment; after the back-sputtering cleaning is finished, pre-sputtering the carbon target for 7min under the conditions that the sputtering power is 110W and the gas flow is 90sccm, then adjusting the air pressure to 0.8Pa, adding 35V pulse negative bias on the substrate, and depositing the carbon film 3 on the substrate through the carbon target for 25 min; preparing a silicon/carbon composite film layer;
b. removing the mask pattern 2 of the silicon/carbon composite film layer in the step a, and then keeping the vacuum degree at 8 multiplied by 10 -5 Pa, the pressure is 6Pa, in an Ar gas environment, pre-sputtering a nickel target for 3min under the sputtering power of 140W and the gas flow of 110sccm, adjusting the gas pressure to 1.2Pa, adding 70V pulse negative bias on a substrate, depositing a nickel film 4 on the substrate through the nickel target, and depositing for 15s to prepare a silicon/carbon/nickel composite film layer;
c. and (c) annealing the composite film layer in the step (b) in a vacuum tube furnace at the annealing temperature of 900 ℃, preserving the heat for 3h, and naturally cooling to room temperature to obtain the patterned silicon carbide nanowire and silicon nanowire composite film.
Example four
The preparation method of the patterned silicon carbide nanowire and the silicon nanowire one-dimensional composite material of the embodiment comprises the following steps:
a. ultrasonically cleaning the silicon substrate 1 in alcohol for 14 minutes, then drying the silicon substrate, and ultrasonically cleaning the silicon substrate with acetone for 14 minutes; drawing a mask pattern 2 on a silicon substrate 1 by direct writing under a vacuum of 12 × 10 -5 When the pressure is 4Pa, carrying out back splash cleaning on the surface of the silicon substrate 1 for 25min under the Ar gas environment; after the back-sputtering cleaning is finished, pre-sputtering the carbon target for 3min under the conditions that the sputtering power is 90W and the gas flow is 110sccm, adjusting the gas pressure to 1.2Pa, adding 25V pulse negative bias on the substrate, and depositing the carbon film 3 on the substrate through the carbon target for 35 min; preparing a silicon/carbon composite film layer;
b. removing the mask pattern 2 of the silicon/carbon composite film layer in the step a, and then keeping the vacuum degree at 12 multiplied by 10 -5 Under the environment of Pa, the pressure is 4Pa and Ar gas, after pre-sputtering a nickel target for 7min under the sputtering power of 160W and the gas flow of 90sccm, adjusting the gas pressure to 0.8Pa, adding 90V pulse negative bias on a substrate, depositing a nickel film 4 on the substrate through the nickel target for 8s, and preparing a silicon/carbon/nickel composite film layer;
c. and (c) annealing the composite film layer in the step (b) in a vacuum tube furnace, keeping the annealing temperature at 1100 ℃, keeping the temperature for 1-3h, and naturally cooling to room temperature to obtain the patterned silicon carbide nanowire and the composite film of the silicon nanowire.
EXAMPLE five
The preparation method of the patterned silicon carbide nanowire and the silicon nanowire one-dimensional composite material of the embodiment comprises the following steps:
a. ultrasonically cleaning the silicon substrate 1 in alcohol for 15 minutes, then drying the silicon substrate, and ultrasonically cleaning the silicon substrate with acetone for 15 minutes; drawing a mask pattern 2 on a silicon substrate 1 by direct writing under a vacuum degree of 10 × 10 -5 When the pressure is 5Pa, carrying out back splash cleaning on the surface of the silicon substrate 1 for 15min under the Ar gas environment; after the back-sputtering cleaning is finished, the sputtering power is 110W, and the gasPre-sputtering the carbon target for 7min at the volume flow of 100sccm, adjusting the air pressure to 0.8Pa, applying 30V pulse negative bias on the substrate, and depositing the carbon film 3 on the substrate through the carbon target for 30 min; preparing a silicon/carbon composite film layer;
b. removing the mask pattern 2 of the silicon/carbon composite film layer in the step a, and then keeping the vacuum degree at 10 multiplied by 10 -5 Pa, the pressure is 4-6Pa, under the Ar gas environment, pre-sputtering a nickel target for 3-7min under the sputtering power of 140-160W and the gas flow of 90-110sccm, adjusting the gas pressure to 0.8-1.2Pa, applying 70-90V pulse negative bias on the substrate, depositing a nickel film 4 on the substrate through the nickel target for 8-15s, and preparing a silicon/carbon/nickel composite film layer;
c. and (c) annealing the composite film layer in the step (b) in a vacuum tube furnace at the annealing temperature of 900-1100 ℃, and naturally cooling to room temperature after heat preservation for 1-3h to obtain the patterned silicon carbide nanowire and the composite film of the silicon nanowire.
EXAMPLE six
The preparation method of the patterned silicon carbide nanowire and the silicon nanowire one-dimensional composite material of the embodiment comprises the following steps:
a. ultrasonically cleaning the silicon substrate 1 in alcohol for 15 minutes, then drying the silicon substrate, and ultrasonically cleaning the silicon substrate with acetone for 15 minutes; drawing a mask pattern 2 on a silicon substrate 1 by direct writing under a vacuum degree of 10 × 10 -5 When the pressure is 5Pa, carrying out back splash cleaning on the surface of the silicon substrate 1 for 20min under the Ar gas environment; after the back-sputtering cleaning is finished, pre-sputtering the carbon target for 5min under the conditions that the sputtering power is 100W and the gas flow is 100sccm, adjusting the gas pressure to 1.0Pa, adding 30V pulse negative bias to the substrate, and depositing a carbon film 3 on the substrate through the carbon target for 30 min; preparing a silicon/carbon composite film layer;
b. removing the mask pattern 2 of the silicon/carbon composite film layer in the step a, and then keeping the vacuum degree at 10 multiplied by 10 -5 Pa, the pressure is 5Pa, in the Ar gas environment, pre-sputtering a nickel target for 5min under the sputtering power of 150W and the gas flow of 100sccm, adjusting the gas pressure to 1.0Pa, adding 80V pulse negative bias on the substrate, depositing a nickel film 4 on the substrate through the nickel target, and depositing for 10s to prepare a silicon/carbon/nickel composite film layer;
c. and (c) annealing the composite film layer in the step (b) in a vacuum tube furnace, keeping the annealing temperature at 1000 ℃, keeping the temperature for 1h, and naturally cooling to room temperature to obtain the patterned silicon carbide nanowire and silicon nanowire composite film.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A patterned silicon carbide nanowire and a silicon nanowire one-dimensional composite material are characterized in that: the silicon nanowire array comprises silicon carbide nanowires, silicon nanowires growing in situ in the silicon carbide nanowire array and metal particles distributed at the growing ends of the silicon carbide nanowires and the silicon nanowires, wherein the silicon nanowires are distributed in at least one region of the silicon carbide nanowires in a patterned mode.
2. The patterned silicon carbide nanowires and silicon nanowire one-dimensional composite material of claim 1, wherein: the silicon carbide nanowire is formed by catalytic growth of a silicon substrate and carbon deposited on the silicon substrate.
3. The patterned silicon carbide nanowires and silicon nanowire one-dimensional composite material of claim 2, wherein: the metal particles are formed from a catalyst that catalyzes the growth of silicon carbide nanowires and silicon nanowires.
4. The patterned silicon carbide nanowires and silicon nanowire one-dimensional composite material of claim 3, wherein: the metal particles are nickel.
5. The method of claim 1, wherein the patterned silicon carbide nanowires are formed by a method comprising the steps of: the method comprises the following steps:
a. depositing a carbon film on the silicon substrate with the drawn mask pattern by using a magnetron sputtering system to prepare a silicon/carbon composite film layer;
b. removing the mask pattern of the silicon/carbon composite film layer in the step a, and depositing a metal film layer on the surface of the silicon/carbon composite film layer to obtain a silicon/carbon/nickel composite film layer;
c. and c, carrying out heat treatment on the composite film layer in the step b to prepare the patterned silicon carbide nanowire and the composite film of the silicon nanowire.
6. The method of claim 5, wherein the step of preparing the patterned silicon carbide nanowires or the one-dimensional composite material of silicon nanowires comprises: in the step a, a mask pattern is drawn on the silicon substrate by a direct writing method.
7. The method of claim 6, wherein the step of preparing the patterned silicon carbide nanowires or the one-dimensional composite material of silicon nanowires comprises: in the step a, firstly, a magnetron sputtering system is utilized to carry out back-sputtering cleaning on the surface of the silicon substrate, and then the magnetron sputtering system is utilized to deposit a carbon film on the substrate through a carbon target.
8. The method of claim 7, wherein the step of preparing the patterned silicon carbide nanowires or the one-dimensional composite material of silicon nanowires comprises: in the step b, a magnetron sputtering system is utilized to carry out pre-sputtering treatment on the metal target, and then a nickel film is deposited on the substrate through the nickel target.
9. The method of claim 7, wherein the step of preparing the patterned silicon carbide nanowires or the one-dimensional composite material of silicon nanowires comprises: in step a, the vacuum degree is 8-12X 10 -5 Performing back-sputtering cleaning on the surface of the silicon substrate for 15-25min under the Ar gas environment when the pressure is 4-6 Pa; after the back-sputtering cleaning is finished, pre-sputtering the carbon target for 3-7min under the conditions that the sputtering power is 90-110W and the gas flow is 90-110sccm, then adjusting the air pressure to 0.8-1.2Pa, adding 25-35V pulse negative bias on the substrate, and depositing a carbon film on the substrate through the carbon target for 25-35 min;
in step b, the vacuum degree is 8-12X 10 -5 Pa, the pressure is 4-6Pa, under the Ar gas environment, the nickel target is pre-sputtered for 3-7min under the sputtering power of 140-160W and the gas flow of 90-110sccm, the gas pressure is adjusted to 0.8-1.2Pa, 70-90V pulse negative bias is applied to the substrate, the nickel film is deposited on the substrate through the nickel target, and the deposition time is 8-15 s.
10. The method of claim 8, wherein the step of preparing the patterned silicon carbide nanowires or the one-dimensional composite material of silicon nanowires comprises: in the step c, annealing the composite film layer in a vacuum tube furnace at the annealing temperature of 900-1100 ℃, and naturally cooling to room temperature after heat preservation for 1-3 h.
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