CN114032510A - Growth method of tellurium nanowire vertical array - Google Patents
Growth method of tellurium nanowire vertical array Download PDFInfo
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- CN114032510A CN114032510A CN202111363651.3A CN202111363651A CN114032510A CN 114032510 A CN114032510 A CN 114032510A CN 202111363651 A CN202111363651 A CN 202111363651A CN 114032510 A CN114032510 A CN 114032510A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
Abstract
The invention discloses a growth method of a tellurium nanowire vertical array, which comprises the following steps: placing tellurium powder in a quartz tube to be used as a precursor source; placing the quartz tube in a tube furnace, wherein the tellurium powder is positioned in a heating area of the tube furnace; cleaning and drying the substrate, fixing the cleaned and dried substrate in the quartz tube as a deposition material, wherein the substrate is positioned in a cooling area of the tube furnace; pumping the vacuum degree in the tubular furnace to 10-20Pa, introducing inert gas, and removing residual oxygen in the tubular furnace; opening a plasma source to excite the inert gas to generate ionization, forming plasma, and exciting the tellurium powder to be converted into small-particle tellurium powder by the plasma; heating the tube furnace, transferring the small-particle tellurium powder positioned in the temperature rising area of the tube furnace to the temperature reduction area of the tube furnace by heating and gasifying, and depositing at the substrate to grow the tellurium nanowire vertical array.
Description
Technical Field
The invention belongs to the field of low-dimensional nano material preparation, and particularly relates to a growth method of a tellurium nanowire vertical array.
Background
With the progress of science and technology and the development of times, people have higher and higher requirements on electronic devices, and in order to adapt to the requirements of people and further develop the potential of electronic devices, the further development and improvement of the performance of micro-nano materials become research hotspots nowadays. Common micro-nano materials include zero-dimensional quantum dots, one-dimensional nanowires, two-dimensional nanosheets and the like. Due to the special size structure of the micro-nano material, the micro-nano material derives some special quantum effects, and is suitable for the application of micro-nano devices.
The nano-wire is used as an important part of nano-materials and widely applied to research on force, heat, sound, light and electricity. The tellurium nanowires are formed by combining ternary spiral chains of tellurium atoms in parallel by virtue of Van der Waals force, the acting force between the spiral chains in a tellurium crystal structure is small, the energy required by lattice vibration is small, the spiral chains are combined in the chains to form covalent bonds, and the transmission obstruction of electrons in the chains is small. The structure enables the tellurium nanowire to have excellent mechanical, thermal, acoustic and electrical properties, and meanwhile, the band gap of the tellurium nanowire correspondingly absorbs near-infrared waves, so that the tellurium nanowire can be applied to the field of optical communication. However, the tellurium nanowires are small in size and poor in stability, and most of tellurium nanowire preparation processes are not matched with the conventional CMOS process and are difficult to be applied in an integrated manner, so that the tellurium nanowires are frequently required to be self-assembled to obtain a thin film and then subjected to subsequent processing, and the application of the tellurium nanowires is limited.
Disclosure of Invention
In view of the above, in order to solve the above problems, the invention provides a method for growing a tellurium nanowire vertical array, which can directly grow a tellurium nanowire array in situ on a substrate, thereby improving the stability of the tellurium nanowire.
In order to achieve the above object, the present invention provides a method for growing a vertical array of tellurium nanowires, comprising:
placing tellurium powder in a quartz tube to be used as a precursor source;
placing the quartz tube in a tube furnace, wherein tellurium powder is positioned in an elevated temperature zone of the tube furnace;
cleaning and drying the substrate, fixing the cleaned and dried substrate in a quartz tube as a deposition material, wherein the substrate is positioned in a cooling area of the tube furnace;
pumping the vacuum degree in the tube furnace to 10-20Pa, introducing inert gas, and removing residual oxygen in the tube furnace;
opening a plasma source to excite the inert gas to generate ionization, forming plasma, and exciting tellurium powder by the plasma to convert into small-particle tellurium powder;
heating the tube furnace, transferring the small-particle tellurium powder in the heating area of the tube furnace to the cooling area of the tube furnace by heating and gasifying, and depositing on the substrate to grow the tellurium nanowire vertical array.
According to the embodiment of the invention, the normal direction of one surface of the substrate points to the center of the quartz tube, and the growth direction of the tellurium nanowire vertical array points to the center of the quartz tube.
According to an embodiment of the present invention, cleaning a substrate includes: sequentially cleaning with acetone for 20min, absolute ethanol for 20min, and deionized water for 20 min.
According to an embodiment of the invention, the substrate is resistant to temperatures greater than 300 c,
preferably, the substrate material comprises: silicon, silicon dioxide, mica, polyacetimide, carbon fiber.
According to an embodiment of the invention, the tube furnace is a plasma enhanced chemical vapor deposition furnace.
According to an embodiment of the invention, the inert gas comprises: one or more of nitrogen, argon, helium, and neon,
preferably, the inert gas flow rate is 0-50 sccm.
According to the embodiment of the invention, the power of the plasma source is adjusted to be 50W, and the reflected power is less than 20W.
According to the embodiment of the invention, the growth temperature of the tellurium nanowire vertical array is 500-650 ℃.
According to the embodiment of the invention, the temperature rise time of the tube furnace is 30-40min, and the heat preservation time is 30-60 min.
According to an embodiment of the present invention, the above growing method further comprises:
after the vertical tellurium nanowire array is grown, naturally cooling the tube furnace to below 60 ℃;
and placing the grown tellurium nanowire vertical array in a dry environment for storage.
According to the growth method of the tellurium nanowire vertical array, provided by the embodiment of the invention, the tellurium nanowire array can be directly grown in situ on the substrate to obtain the tellurium nanowire film, so that the stability of the tellurium nanowire is improved.
Drawings
Fig. 1 schematically shows a schematic view of a growth apparatus implementing a method of growing arrays of tellurium nanowires in accordance with an embodiment of the invention;
FIG. 2 is a schematic view showing a position where a substrate is placed in a quartz tube according to an embodiment of the present invention;
FIG. 3 schematically shows an SEM image of an array of tellurium nanowires grown on a silicon dioxide rigid substrate in accordance with an embodiment of the invention;
FIG. 4 schematically shows an SEM image of an array of tellurium nanowires grown on a polyimide flexible substrate in accordance with an embodiment of the invention;
FIG. 5 schematically shows an SEM image of an array of tellurium nanowires grown on a carbon fiber flexible substrate, in accordance with an embodiment of the invention; and
FIG. 6 schematically shows an SEM image after laser direct writing of tellurium nanowire arrays grown on a polyimide flexible substrate according to an embodiment of the invention;
[ reference numerals ]
1-a plasma source; 2-heating area of tube furnace; 3-a cooling zone of the tube furnace; 4-a quartz tube; 5-tellurium powder; 6-substrate.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The tellurium nanowires have excellent mechanical, thermal, acoustic and electrical properties, and band gaps of the tellurium nanowires correspondingly absorb near-infrared waves, so that the tellurium nanowires can be applied to the field of optical communication and are wide in application range. If the tellurium nanowire is directly grown in situ, redundant steps can be omitted, and deep research on the vertical structure of the tellurium nanowire can be carried out.
According to the above inventive concept, the present invention provides a method for growing a tellurium nanowire vertical array, comprising:
placing tellurium powder in a quartz tube to be used as a precursor source;
placing the quartz tube in a tube furnace, wherein tellurium powder is positioned in an elevated temperature zone of the tube furnace;
cleaning and drying the substrate, fixing the cleaned and dried substrate in a quartz tube as a deposition material, wherein the substrate is positioned in a cooling area of the tube furnace;
pumping the vacuum degree in the tube furnace to 10-20Pa, introducing inert gas, and removing residual oxygen in the tube furnace;
opening a plasma source to excite the inert gas to generate ionization, forming plasma, and exciting tellurium powder by the plasma to convert into small-particle tellurium powder; and
heating the tube furnace, transferring the small-particle tellurium powder in the heating area of the tube furnace to the cooling area of the tube furnace by heating and gasifying, and depositing on the substrate to grow the tellurium nanowire vertical array.
Fig. 1 schematically shows a schematic view of a growth apparatus implementing a growth method of tellurium nanowire arrays according to an embodiment of the present invention. The method for growing the vertical tellurium nanowire array is described in detail with reference to fig. 1, and the method for growing the tellurium nanowire array comprises steps S01 to S09.
In operation S01, the tellurium powder 5 is placed in the quartz tube 4 as a precursor source.
In operation S02, the quartz tube 4 is placed in a tube furnace with tellurium powder in the elevated temperature zone 2 of the tube furnace.
According to an embodiment of the invention, the tube furnace is a plasma Enhanced Chemical Vapor deposition PECVD (plasma Enhanced Chemical Vapor deposition) furnace.
According to the embodiment of the invention, the growth method adopts an additional plasma-assisted vapor deposition process and adopts a tube furnace, so that the preparation equipment requirement is lower, and the mass production of tellurium nanowires is ensured.
According to the embodiment of the invention, the tellurium powder is positioned at the position deviated from the substrate in the temperature rising region of the tube furnace, so that the tellurium powder is conveniently transferred to the substrate, and the loss is reduced.
In operation S03, the substrate 6 is cleaned and dried.
According to an embodiment of the invention, the substrate has a withstand temperature of more than 300 ℃. Specifically, the substrate is subjected to a high temperature of 300 degrees celsius for at least 30 minutes without decomposition and deterioration.
According to an embodiment of the invention, the substrate material comprises: silicon, silicon dioxide, mica, polyimide pi (polyacetyl imide), carbon fiber.
According to the embodiment of the invention, the substrate can be made of silicon or silicon dioxide, which means that the preparation process of the tellurium nanowire can be directly integrated into the CMOS process without a complex transfer sequencing process, and the application and processing are more convenient.
According to the embodiment of the invention, the substrate can be a flexible substrate such as PI, carbon fiber and the like, and the application prospect of the tellurium nanowire growth method in the field of flexible electronics is also shown.
According to an embodiment of the present invention, cleaning a substrate includes: sequentially cleaning with acetone for 20min, absolute ethanol for 20min, and deionized water for 20 min.
The cleaned and dried substrate 6 is fixed in the quartz tube 4 as a deposition material in operation S04, and the substrate is located in the cooling zone 3 of the tube furnace.
According to the embodiment of the invention, the substrate is fixed in the quartz tube in a manner of pasting and fixing the substrate by using the double-sided carbon adhesive tape.
Fig. 2 is a schematic diagram illustrating the placement position of the substrate in the quartz tube according to the embodiment of the invention, and as shown in fig. 2, the placement position of the substrate is ensured that the normal direction of one surface of the substrate is directed to the center of the quartz tube, so as to ensure that the growth direction of the tellurium nanowire vertical array is directed to the center of the quartz tube.
In operation S05, the vacuum degree in the tube furnace is pumped to 10-20Pa, and inert gas is introduced to remove the residual oxygen in the tube furnace.
According to the embodiment of the invention, the air pressure is pumped to be below 20Pa by using a vacuum pump, and meanwhile, inert gas is introduced for 10-15min at the flow rate of 50sccm, so that the inert gas is ensured to replace the air in the equipment cavity.
According to an embodiment of the invention, the inert gas comprises: one or more of nitrogen, argon, helium, and neon.
For example, the inert gas flow rate is 0 to 50 sccm.
According to the embodiment of the invention, in the tellurium nanowire growth process, the vacuum pump is in an open state, and meanwhile, the flow rate of the inert gas is adjusted as required to obtain nanowires with different diameters, wherein the larger the flow rate is, the thicker the nanowires are.
In operation S06, the plasma source 1 is turned on to excite the inert gas to ionize and form plasma, and the plasma excites the tellurium powder 5 to transform into small particles of the tellurium powder.
According to the embodiment of the invention, the power of the plasma source is adjusted to be 50W, and the reflected power is less than 20W.
In operation S07, the tube furnace is heated, and the small-particle tellurium powder in the temperature rising region of the tube furnace is heated, gasified, transferred to the temperature lowering region of the tube furnace, and deposited on the substrate 6, so as to grow the tellurium nanowire vertical array.
According to the embodiment of the invention, the growth temperature of the tellurium nanowire vertical array is 500-650 ℃.
According to the embodiment of the invention, the temperature rise time of the tube furnace is 30-40min, and the heat preservation time is 30-60 min.
According to the embodiment of the invention, the lower the growth temperature of the tellurium nanowire is set, the slower the tellurium powder is transferred, the more obvious the dominant orientation of the tellurium nanowire is grown, and the thinner the tellurium nanowire is.
According to the embodiment of the invention, the temperature rise time, the growth temperature and the growth time need to be reasonably controlled according to the quality of the tellurium powder, the growth time needs to be long enough to ensure that the tellurium powder is transferred and deposited completely, but cannot be too long enough to avoid the loss of the prepared nanowire along with the transfer of airflow,
according to the embodiment of the invention, the actual growth process needs to be controlled by matching with the mass of the tellurium powder, and when the mass of the tellurium powder is 50mg, the growth time is 30-60 min.
In an exemplary embodiment, after the growth of the tellurium nanowire vertical array is completed, the tube furnace is naturally cooled to be below 60 ℃, and the tellurium nanowire vertical array after the growth is completed is placed in a dry environment for storage.
According to the embodiment of the invention, the tellurium nanowire array is directly grown on the substrate in situ by the method for growing the tellurium nanowire vertical array, the manufacturing process is simple, a large amount of uniform nanowires can be obtained, and the self-assembly process is omitted; the more ordered tellurium nanowire film is directly obtained, the problems of poor stability of a single tellurium nanowire and the like are solved, the application range of the tellurium nanowire is expanded, and the requirements of scientific research and production can be met; furthermore, the tellurium nanowire array film obtained by the invention can be subjected to laser direct writing for patterning, and the film can be further designed to meet the requirements of different electronic device structures.
The growth method of the tellurium nanowire vertical array is explained by the embodiment of taking silicon dioxide as the substrate. It should be noted that the examples are only specific embodiments of the present invention, and are not intended to limit the present invention.
Weighing about 50mg of tellurium elementary substance powder, and putting the powder into the bottom of a quartz test tube with the specification of phi 20 multiplied by 200 mm.
And sequentially cleaning the silicon dioxide sheet with acetone for 20min, absolute ethyl alcohol for 20min and deionized water for 20min, drying, and adhering a clean substrate to the opening of the test tube by using a double-sided carbon adhesive tape, wherein the surface of the substrate deposition material faces to the center of the interface of the test tube.
And (3) placing the quartz test tube into a PECVD furnace, wherein the tellurium simple substance in the quartz test tube is in an increasing temperature area in the furnace, and the substrate is in a decreasing temperature area.
The vacuum degree in the tube is pumped to 20Pa, and Ar gas is introduced for cleaning for 10 min.
The Ar gas is turned off. And turning on the plasma source, setting the power to be 50W, and adjusting the reflected power to be less than 20W.
And heating the PECVD furnace to enable the temperature rise region to be heated to 550 ℃ after 35min, preserving the temperature for 30min, and then naturally cooling to be below 60 ℃.
And placing the obtained tellurium nanowire vertical array in a dry environment for storage.
Fig. 3 schematically shows an SEM image of a tellurium nanowire array grown on a silicon dioxide rigid substrate according to an embodiment of the present invention, and scanning the tellurium nanowire vertical array to obtain the SEM image shown in fig. 3 clearly shows that the tellurium nanowire vertical array has good uniformity in the process.
Fig. 4 schematically shows an SEM image of the tellurium nanowire array grown on the polyacetimide flexible substrate according to the embodiment of the present invention, the substrate material in the above embodiment is changed to polyacetimide, and the rest conditions are unchanged, so as to obtain the tellurium nanowire vertical array for scanning, thereby obtaining the SEM image shown in fig. 4.
Fig. 5 schematically shows an SEM image of the tellurium nanowire array grown on the carbon fiber flexible substrate according to the embodiment of the present invention, the substrate material in the above embodiment is changed into carbon fiber, and the rest conditions are not changed, so as to obtain the tellurium nanowire vertical array for scanning, thereby obtaining the SEM image shown in fig. 5.
The above three SEM charts shown in FIGS. 3 to 5 show that the growth method of the present invention has low requirement on the substrate, good compatibility, and good uniformity of the obtained vertical tellurium nanowire array.
Fig. 6 schematically shows an SEM image of the tellurium nanowire array grown on the polyimide flexible substrate after laser direct writing, as shown in fig. 6, the tellurium nanowire array film can be further designed to meet the requirements of different electronic device structures, and also shows that the process has high compatibility with the mature CMOS process.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method of growing a vertical array of tellurium nanowires, comprising:
placing tellurium powder in a quartz tube to be used as a precursor source;
placing the quartz tube in a tube furnace, wherein the tellurium powder is positioned in a heating area of the tube furnace;
cleaning and drying the substrate, fixing the cleaned and dried substrate in the quartz tube as a deposition material, wherein the substrate is positioned in a cooling area of the tube furnace;
pumping the vacuum degree in the tubular furnace to 10-20Pa, introducing inert gas, and removing residual oxygen in the tubular furnace;
opening a plasma source to excite the inert gas to generate ionization, forming plasma, and exciting the tellurium powder to be converted into small-particle tellurium powder by the plasma; and
heating the tube furnace, transferring the small-particle tellurium powder positioned in the temperature rising area of the tube furnace to the temperature reduction area of the tube furnace by heating and gasifying, and depositing at the substrate to grow the tellurium nanowire vertical array.
2. The growth method according to claim 1, wherein a normal direction of one surface of the substrate points to a center of the quartz tube, and a growth direction of the tellurium nanowire vertical array points to the center of the quartz tube.
3. The growth method of claim 1, wherein cleaning the substrate comprises: sequentially cleaning with acetone for 20min, absolute ethanol for 20min, and deionized water for 20 min.
4. The growth method of claim 1, wherein the substrate has a withstand temperature of greater than 300 ℃,
preferably, the substrate material comprises: silicon, silicon dioxide, mica, polyacetimide, carbon fiber.
5. The growth method of any one of claims 1-4, wherein the tube furnace is a plasma enhanced chemical vapor deposition furnace.
6. The growth method of any one of claims 1-4, wherein the inert gas comprises: one or more of nitrogen, argon, helium, and neon,
preferably, the inert gas flow rate is 0 to 50 sccm.
7. The growth method according to any one of claims 1 to 4, wherein the power of the plasma source 1 is adjusted to 50W and the reflected power is less than 20W.
8. The growth method as claimed in claim 1, wherein the growth temperature of the tellurium nanowire vertical array is 500-650 ℃.
9. The growth method according to any one of claims 1 to 4, wherein the tube furnace has a temperature rise time of 30 to 40min and a temperature hold time of 30 to 60 min.
10. The growth method of any one of claims 1-4, further comprising:
after the growth of the tellurium nanowire vertical array is finished, naturally cooling the tube furnace to below 60 ℃;
and placing the vertical tellurium nanowire array after the growth in a dry environment for storage.
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