CN100411063C - A kind of tin dioxide/tin coaxial nano cable and its preparation method and application - Google Patents

Abstract

The invention discloses a tin dioxide/tin coaxial nano-cable and its preparation method and application. The inner core of the cable is a tin nano-wire, the outer shell of the cable is a tin dioxide nano-tube, the inner core and the outer shell are coaxial structures, and the cable The diameter is 20-30nm and the length is 500-900 microns. The preparation method is as follows: put the reaction source in the high-temperature-resistant inner tube, place a single-crystal silicon wafer near the reaction source, place the single-crystal silicon wafer on the high-temperature-resistant material, put the high-temperature-resistant inner tube into the high-temperature-resistant outer tube, and then Put it into a heating furnace, vacuumize it, and then pass in an inert gas to raise the temperature of the furnace to 550-750°C, keep it warm and then cool it down to obtain a tin dioxide/tin coaxial nano-cable. The invention can be applied in the fields of biomedicine, micro-device preparation and circuit connection, micro-device communication and the like. The preparation process of the invention is simple, the cost is low, and mass production can be realized.

Description

A kind of tin dioxide/tin coaxial nano cable and its preparation method and application

technical field

The invention relates to nano-cable technology, in particular to a tin dioxide/tin coaxial nano-cable and its preparation method and application.

Background technique

Since the advent of the first human transistor, its size has shrunk by two times every 18 months, and today's "Penten 4" is only more than 100 nanometers; What connection is used between the components of the high-density integrated circuit? This is a difficult problem faced by the world's scientific community. At this stage, it is difficult for technology to break through the ultrafine limit, and scientists from all over the world are pinning their hopes on the application of nanotechnology. Scientists now claim to have the ability to create nanocables thinner than the tiniest of human blood vessels. This means that scientists can make nano-cables travel freely in human blood vessels and reach any designated location without hindering the normal flow of blood, oxygen and nutrients in blood vessels. Scientists also observed that the transport of electrons in nanocables is different from that of ordinary conductors, with faster transport and less energy consumption. Its birth may also lay the foundation for the generation of next-generation optical fibers.

Nano-cable refers to the nano-wire whose core is a semiconductor or conductor, and is coated with a heterogeneous nano-shell (conductor or non-conductor), and the outer shell and core are coaxial, so it is called a coaxial nano-cable. Due to the special properties of this type of material, it will play an important role in future nanostructure devices, especially in biomedicine, micro-device preparation and circuit connection, and micro-communication device manufacturing. At present, polyvinyl alcohol/silver nano-cables and zinc sulfide-zinc oxide nano-cables have been prepared in China, but the synthesis methods often require harsh conditions such as high temperature, laser, and solution synthesis.

Contents of the invention

In order to solve the disadvantages of the above-mentioned prior art, the primary purpose of the present invention is to provide a tin dioxide/tin coaxial nano-cable with simple preparation process and wide application range.

Another object of the present invention is to provide a preparation method for synthesizing the above-mentioned tin dioxide/tin coaxial nano-cable by thermal evaporation, which has the advantages of simple operation, low cost, less time-consuming and suitable for mass production.

Another object of the present invention is to provide the application of the above-mentioned tin dioxide/tin coaxial nano-cable.

The object of the present invention is achieved through the following technical solutions: a tin dioxide/tin coaxial nano-cable, the inner core of which is a tin nanowire with a diameter of 10-15 nm, and the outer shell is a tin dioxide nano-wire with a thickness of 5-7.5 nm. The tube, the inner core and the outer shell are coaxial structures, which together constitute a tin dioxide/tin coaxial nanocable, and the inner core and the outer shell are tightly combined, and there is no gap between the two; the entire tin dioxide/tin coaxial nanocable The diameter is 20-30nm and the length is 500-900 microns.

The method for preparing the above-mentioned tin dioxide/tin coaxial nano-cable includes the following steps: putting a reaction source in a high-temperature-resistant inner tube, and placing a single crystal silicon wafer as a lining in the inner tube at a place 0.5 to 2.0 cm away from the reaction source At the bottom, place the monocrystalline silicon wafer on the high-temperature resistant material, then put the high-temperature-resistant inner tube into the high-temperature-resistant outer tube, put the high-temperature-resistant outer tube into the heating furnace, and then vacuumize the heating furnace for 15 to 60 minutes. Then pass in an inert gas of 25-60 sccm (standard milliliters per minute), so that the vacuum degree in the furnace reaches 100-500 Torr (1Torr=1/760 standard atmospheric pressure=133Pa), the furnace temperature rises to 550-750°C, and the temperature is kept at 550-500°C. After continuing at 750°C for 2-4 hours, stop the heating, and cool the furnace down to room temperature to obtain a tin dioxide/tin coaxial nano-cable.

In order to better realize the present invention, the reaction source is stannous oxide powder with a purity of 99.99%; the inner diameter of the high-temperature-resistant inner tube is 1-3 cm, and the inner diameter of the high-temperature-resistant outer tube is 5-10 cm; The high-temperature material is a ceramic sheet, and the surface of the single crystal silicon sheet is sprayed with a gold-silver alloy with a thickness of about 10 to 50 nanometers; the area of the single crystal silicon sheet is (2×2) to (6×6) mm ² ; Both the high temperature resistant inner tube and the high temperature resistant outer tube can be quartz tubes. The position of the thermocouple of the heating furnace and the position of the reaction source are on a vertical line, and the inert gas can be argon, helium, neon, krypton or xenon.

The tin dioxide/tin coaxial nano cable prepared by the above method can be widely used in the fields of biomedicine, micro-device preparation and circuit connection, micro-device communication and the like.

Compared with the prior art, the present invention has the following advantages and beneficial effects: for the first time, the present invention synthesizes tin dioxide/tin coaxial nano-cables by thermal evaporation, and the method is simple and reliable in operation, low in cost and less time-consuming. The tin dioxide/tin coaxial nano-cable synthesized by the invention has a diameter of about 20-30 nanometers and a length of 500-900 microns, which is sufficient for many circuit connections or communication roles in the field of micro-device preparation. Compared with cables such as polyvinyl alcohol/silver nano-cables (300 nanometers thick) and zinc sulfide-zinc oxide nano-cables (460 nanometers thick) that have been prepared in China, the scale of the cable of the present invention is smaller and the applicability is better; and The synthesis process is simple, does not require harsh conditions such as high temperature, laser, and solution synthesis, and is more conducive to integrated mass production.

Description of drawings

Fig. 1 is the apparatus figure of the present invention to prepare tin dioxide/tin coaxial nano-cable by thermal evaporation method.

Fig. 2 is a photo of the field emission electric field of the tin dioxide/tin coaxial nano-cable of the present invention.

Fig. 3 is an X-ray diffraction analysis spectrum of the tin dioxide/tin coaxial nano-cable of the present invention.

Fig. 4 is a Raman spectrum of the tin dioxide/tin coaxial nanocable of the present invention at room temperature.

Fig. 5 (a) is the transmission electron micrograph of the cable of the present invention, and Fig. 5 (b) is the high-resolution photo of inner core and shell junction; Fig. 5 (c) is the electron diffraction photo of shell; Fig. 5 (d) An electron diffraction photo of the inner core.

Detailed ways

The present invention will be further described in detail below with reference to the examples and drawings, but the implementation of the present invention is not limited thereto.

Example 1

As shown in Figure 1 (wherein 4 is heating element), put into the stannous oxide powder 6 that purity is 99.99% as reaction source in the small quartz tube (high temperature resistance inner pipe) 7 of 2cm in the internal diameter of an opening at one end, these A ceramic sheet 9 is placed near the reaction source, and a ^single crystal silicon sheet 8 sprayed with a gold-silver alloy with a thickness of about 20 nanometers and an area of 5 × 5 mm is placed as a substrate at a place 1.0 cm away from the reaction source on the ceramic sheet 9 , then put this small quartz tube (high temperature resistant inner tube) 7 into the inside of the large quartz tube (high temperature resistant outer tube) 3 with an internal diameter of 8cm, then put this large quartz tube (high temperature resistant outer tube) 3 into the heating In the furnace 2, make the thermocouple 1 (thermocouple position) of the heating furnace 2 and the position of the reaction source on a vertical line. The whole system (i.e. heating furnace 2) starts vacuuming for 20 minutes, and argon gas 5 is introduced to 30 sccm, so that the vacuum degree in the heating furnace reaches 200 Torr, and the furnace temperature (temperature at the thermocouple) rises rapidly from room temperature (25°C) to 650 ℃, keep warm at 650℃ for 2.5 hours, stop heating, let the furnace temperature cool down to room temperature (25℃), take out the substrate, and observe that there are tin dioxide/tin coaxial nano Cable generation.

As shown in Fig. 2, it is a photo of the field emission electric field of the tin dioxide/tin coaxial nano-cable of the present invention. The whole tin dioxide/tin coaxial nano-cable has a diameter of 20-30nm and a length of 500-900 microns.

As shown in Fig. 3 and Fig. 4, the X-ray diffraction analysis spectrum and the Raman spectrum at normal temperature (25° C.) of the tin dioxide/tin coaxial nano-cable of the present invention are respectively shown. According to these two test methods, it can be confirmed that the coaxial nano-cable is composed of tin dioxide and tin.

The transmission electron microscope photo of the cable of the present invention, the high-resolution photo of the junction between the inner core and the outer shell, the electron diffraction photo of the outer shell, and the electron diffraction photo of the inner core as shown in (a), (b), (c), ( d) as shown. By analysis, it can be seen that the inner core of the synthesized tin dioxide/tin coaxial nano-cable of the present invention is a tin nanowire with a diameter of 10～15nm, and the outer shell is a thick tin dioxide nanotube with a thickness of 5～7.5nm. It is a coaxial structure, tightly combined, without any gap between the inner core and the outer shell.

Through the above characterization means, it can be seen that the outer shell of the material of the coaxial nanocable synthesized by the present invention is composed of tin dioxide nanotubes, and the inner core is composed of tin nanowires. Its overall size, inner core size, and shell size are also clear at a glance.

Example 2

Put the stannous oxide powder that purity is 99.99% as reaction source in the small quartz tube (high temperature resistant inner tube) of 3cm in the internal diameter of an end opening, place ceramic sheets near these reaction sources, on this ceramic sheet from reaction source Place a single crystal silicon wafer sprayed with a gold-silver alloy with a thickness of about 50 nanometers and an area of 6× ^6mm2 at a place of 2.0cm as a substrate, and then put this small quartz tube (high temperature resistant inner tube) into a 10cm inner diameter The inside of the large quartz tube (high temperature resistant outer tube), then put this large quartz tube (high temperature resistant outer tube) into the heating furnace, so that the thermocouple (thermocouple position) of the heating furnace and the position of the reaction source are in the on a vertical line. The whole system (i.e. heating furnace) starts to vacuumize for 15 minutes, and feeds helium gas at 25 sccm (standard milliliter per minute), so that the vacuum in the furnace reaches 100 Torr (1 Torr=1/760 standard atmospheric pressure=133Pa), and the temperature of the furnace (thermoelectric Occasional temperature) rises rapidly from room temperature (25°C) to 550°C, and after holding at 550°C for 4 hours, stop heating, let the furnace temperature cool down to room temperature (25°C), take out the substrate, and magnify it with a field emission electron microscope The formation of tin dioxide/tin coaxial nanocables on the substrate was observed.

Example 3

Put the stannous oxide powder that purity is 99.99% in the small quartz tube (high temperature resistant inner tube) of 1cm in the inner diameter of an open end as reaction source, place ceramic sheets near these reaction sources, on this ceramic sheet from reaction source Place a single crystal silicon wafer sprayed with a gold-silver alloy with a thickness of about 10 nanometers and an area of 2× ^2mm2 at a place of 0.5cm as a substrate, and then put this small quartz tube (high temperature resistant inner tube) into a 5cm inner diameter The inside of the large quartz tube (high temperature resistant outer tube), then put this large quartz tube (high temperature resistant outer tube) into the heating furnace, so that the thermocouple (thermocouple position) of the heating furnace and the position of the reaction source are in the on a vertical line. The whole system (that is, the heating furnace) starts to be vacuumed for 60 minutes, and the argon gas is introduced to 60 sccm, so that the vacuum degree in the furnace reaches 500 Torr, and the furnace temperature (the temperature at the thermocouple) rises rapidly from room temperature (25°C) to 750°C, and the heat preservation After 2 hours at 750° C., stop heating, allow the furnace to cool naturally to room temperature (25° C.), take out the substrate, and observe the generation of tin dioxide/tin coaxial nanocables on the substrate through magnification with a field emission electron microscope.

The above-mentioned embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the above-mentioned embodiment, and any other changes, modifications, substitutions, combinations, Simplifications should be equivalent replacement methods, and all are included in the protection scope of the present invention.

Claims (9)

1. tin ash/tin coaxial nano cable, it is characterized in that: its inner core is that diameter is the stannum nanowire of 10～15nm, and its shell is the tin dioxide nanometer tube of the thick 5～7.5nm of being, and inner core and shell are coaxial configuration, do not have the space between the two; The diameter of whole cable is 20～30nm, and length is 500～900 microns.

2. method for preparing the described tin ash of claim 1/tin coaxial nano cable, it is characterized in that: described tin ash/tin coaxial nano cable inner core is that diameter is the stannum nanowire of 10～15nm, its shell is the tin dioxide nanometer tube of the thick 5～7.5nm of being, inner core and shell are coaxial configuration, do not have the space between the two; The diameter of whole cable is 20～30nm, and length is 500～900 microns; The described method for preparing tin ash/tin coaxial nano cable comprises the steps: to put into reaction source in the pipe at one in high temperature resistant, and in interior pipe, place monocrystalline silicon piece as substrate from the place of reaction source 0.5～2.0cm, monocrystalline silicon piece is placed on the exotic material, then pipe in high temperature resistant is put into the inside of high temperature resistant outer tube, high temperature resistant outer tube is put into heating furnace, heating furnace vacuumized 15～60 minutes then, feed inert gas 25～60sccm again, make the interior vacuum degree of stove reach 100～500Torr, make furnace temperature rise to 550～750 ℃, and be incubated 550～750 ℃ and continue after 2～4 hours, stop heating, make furnace temperature be cooled to room temperature, promptly make tin ash/tin coaxial nano cable; Described reaction source is that purity is 99.99% stannous oxide powder.

3. the preparation method of tin ash according to claim 2/tin coaxial nano cable is characterized in that: the internal diameter of described high temperature resistant interior pipe is 1～3cm, and the internal diameter of high temperature resistant outer tube is 5～10cm.

4. the preparation method of tin ash according to claim 2/tin coaxial nano cable is characterized in that: described exotic material is a potsherd.

5. the preparation method of tin ash according to claim 2/tin coaxial nano cable is characterized in that: it is the electrum of 10～50 nanometers that described monocrystalline silicon sheet surface has sprayed thick.

6. the preparation method of tin ash according to claim 2/tin coaxial nano cable is characterized in that: described monocrystalline silicon piece area is (2 * 2)～(6 * 6) mm ²

7. the preparation method of tin ash according to claim 2/tin coaxial nano cable is characterized in that: described high temperature resistant interior pipe and high temperature resistant outer tube are quartz ampoule.

8. the preparation method of tin ash according to claim 2/tin coaxial nano cable is characterized in that: the thermocouple position of described heating furnace and the residing position of reaction source are on a vertical straight line.

9. the preparation method of a kind of tin ash according to claim 2/tin coaxial nano cable is characterized in that: described inert gas is argon gas, helium, neon, krypton gas or xenon.

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