CN109989101B - Preparation method of indium antimonide nanowire - Google Patents
Preparation method of indium antimonide nanowire Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 93
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000015654 memory Effects 0.000 claims abstract description 23
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
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- 238000000034 method Methods 0.000 claims abstract description 20
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
- B22D17/14—Machines with evacuated die cavity
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- B22D19/00—Casting in, on, or around objects which form part of the product
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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
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Abstract
The invention discloses a method for preparing indium antimonide nanowires, which comprises the steps of preparing InSb bulk metal, melting the InSb bulk metal, preparing an anodic aluminum oxide template containing the indium antimonide nanowires by using the anodic aluminum oxide template, soaking the anodic aluminum oxide template containing the indium antimonide nanowires in a mixed solution of chromic acid and phosphoric acid for 24 hours, removing the anodic aluminum oxide template, and filtering by using ethanol to obtain the indium antimonide nanowires. Meanwhile, a method for preparing the organic field effect transistor type memory by using the prepared indium antimonide nanowire is also provided. The indium antimonide nanowire prepared by the method is applied to the charge storage layer of the organic field effect transistor, and the power of the transistor can be reduced.
Description
Technical Field
The invention belongs to the technical field of self-preparation of nano materials, and particularly relates to a preparation method of an indium antimonide nanowire.
Background
In recent years, the information technology has been developed vigorously, and electronic products have become an indispensable part of people's life. Data storage devices are currently classified into volatile and non-volatile memories. Volatile memory devices are memories that need to be maintained by current, and when the supply current is interrupted, the stored data completely disappears, and most volatile memory devices are manufactured as random access memories, which are mainly used as storage media for temporary data of computer applications. The non-volatile memory is not required to be maintained by current, and the stored data can be rewritten by passing current, and is generally applied to read-only memories and flash memories. The volatile memory causes a large amount of energy loss due to electric leakage, and the non-volatile memory can improve the problem of electric leakage, so that the non-volatile memory is gradually paid attention to.
The organic non-volatile memory has low cost and can be used for wearable electronic products, thereby arousing great research interest of scientific researchers. The organic non-volatile memory has a structure similar to that of a floating gate component, except that the organic non-volatile memory mainly comprises a semiconductor layer, a charge storage layer and a dielectric layer. The memory effect is achieved by applying a bias voltage to the charge storage layer to generate a corresponding hysteresis behavior. The charge storage layer mainly uses nano floating gate dielectric or high molecular polymer as the charge storage layer material, and the material can be influenced by the shape and uniformity of the internal nano particles and the intensity of the loading electric field in the tunneling layer.
Typical nanowires are defined as one-dimensional structural materials with aspect ratio of over 1000, and can be divided into three major categories, namely pure metal nanowires, semiconductor nanowires and insulator nanowires. In the field of nano material research, semiconductor nanowires have the advantages of good semiconductor characteristics, high electron mobility, few internal structure defects and the like, and are the research objects of numerous scholars.
The disadvantages of the chemical vapor deposition and the metal organic chemical vapor deposition for fabricating nanowires are that the size of the wire diameter and the uniformity of the nanowire components are not controllable, and the application is limited. The method is different from chemical vapor deposition and organic metal chemical vapor deposition. The component proportion of the nano wire is ensured to be uniform by controlling the component proportion of the mother material, and the diameter of the nano wire can be controlled by controlling the size of a nano hole on the anodic alumina template.
In the global scope, the previous research does not utilize the copolymer/nanowire as the charge storage layer to prepare the data storage element, and the invention utilizes the copolymer/nanowire as the charge storage layer to prepare the data storage element, thereby being beneficial to improving the storage capacity of the data storage element.
Disclosure of Invention
The invention aims to provide a method for preparing indium antimonide nanowires, which is characterized in that the indium antimonide nanowires are prepared in a mode of vacuum die casting assisted by an aluminum oxide template, and then a nonvolatile data storage element is prepared by taking an indium antimonide nanowire/PMAA mixture as a charge storage layer.
The invention is realized by the following technical scheme:
a preparation method of indium antimonide nanowires comprises the following steps:
1) mixing indium particles and antimony powder, heating the mixture in a vacuum environment, melting the mixture, continuously heating the mixture until the mixture is uniformly mixed, and cooling the mixture to form InSb bulk metal;
2) putting the InSb bulk metal in a vacuum environment, heating to 400 ℃, preserving heat for 24 hours, and cooling;
3) preparing an anodic aluminum oxide template by using a pure aluminum sheet as an anodic aluminum oxide substrate, wherein the anodic aluminum oxide is provided with nano holes with uniform size;
4) putting the InSb bulk metal prepared in the step (1) on an anodic alumina template in mold extrusion, heating until the InSb bulk metal becomes molten state, pressurizing to enable the molten indium antimonide to enter into nanopores of the anodic alumina template, and cooling to obtain the anodic alumina template containing indium antimonide nanowires;
5) and carrying out heat treatment on the anodic aluminum oxide template containing the indium antimonide nanowire, soaking the anodic aluminum oxide template in a mixed solution of chromic acid and phosphoric acid, and filtering the anodic aluminum oxide template with ethanol to obtain the indium antimonide nanowire.
Further, the vacuum environment in the step (1) and the step (2) is that the air pressure is less than 10-3mm Hg。
Further, the cooling in the step (2) is specifically cooling to room temperature at a speed of 50 ℃/H.
Further, the heating in the step (4) is specifically heating to 530 ℃ and keeping the temperature for 10 minutes.
Further, the pressurizing in the step (4) is specifically that the pressure of the hydraulic press is 50kg/cm2For a duration of 1 minute.
Further, the heat treatment in the step (5) is specifically as follows: the temperature was maintained at 400 ℃ for 1 hour and then cooled to room temperature at a rate of 50 ℃ per hour.
Further, the mixed solution of chromic acid and phosphoric acid in the step (5) is as follows: 1.8 wt% CrO3+6vol.％H3PO4+92vol.％H2O。
In another aspect of the present invention, there is also provided a method for manufacturing an organic field effect transistor type memory using an indium antimonide nanowire, comprising the steps of:
mixing indium antimonide nanowire with polymethacrylic acid (PMAA), and placing in methanol (CH)3OH), preparing a nanowire suspension by ultrasonic vibration, and coating the nanowire suspension on SiO (1.5 cm multiplied by 300 nm) by using a spin coater2A substrate;
pentacene (C)22H14) Plating on the indium antimonide nanowire layer, plating a gold electrode, wherein the length and width of the electrode are 1000 mu m and 50 mu m respectively, and the deposition thickness is 80nm, thus obtaining the organic field effect transistor type memory.
The invention has the beneficial effects that:
(1) the anode alumina template is used for assisting in manufacturing the nanowires by utilizing a vacuum die-casting mode, the components of the nanowires can be controlled by adjusting the component proportion of raw materials, and the nanowires with uniform element component proportion can be formed;
(2) the nano-wire has a larger length-diameter ratio reaching 1000, and is used as a charge storage layer to prepare a data storage element, thereby being beneficial to improving the critical voltage offset and the switching current ratio of the data storage element.
(3) Indium antimonide has a higher electron mobility of about 7.7 x 10 at room temperature than group III-V semiconductor materials4cm2/(Vs), the band gap is small, about 0.18eV, and the hole mobility is 850cm2/(Vs), high speed low power field effect materialThe ideal selection of materials, so indium antimonide is applied to the charge storage layer of the organic field effect transistor, and the power of the transistor can be reduced.
Drawings
FIG. 1 is a structure of an organic field effect transistor type storage element;
FIG. 2 is an anodized aluminum template having an aperture of 86.12 + -5.44 nm;
FIG. 3 is a SEM topography for nanowires with an average diameter of about 83 nm;
FIG. 4 is a SEM topography for nanowires with an average diameter of about 102 nm;
FIG. 5 is a nanowire SEM topography with an average diameter of about 382 nm;
figure 6 is a nanowire composition analysis of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Step 1: indium antimonide (InSb) bulk metal was vacuum melted.
5g of indium (In) particles having a purity of 99.99% and antimony (Sb) powder having a purity of 99.99% were weighed on an electronic balance, respectively, and mixed and placed In a quartz test tube having an inner diameter of 1 inch. Vacuumizing to make the air pressure in the quartz test tube less than 10-3mmhg, prevents the metal powder from reacting with oxygen in the air to form oxides when heated. The quartz tube was then heated with a gas torch to melt the metal particles in the tube and then heated for 10 minutes to prevent the two metals from mixing unevenly. Then the mixed molten metal is naturally cooled to room temperature to form indium antimonide (InSb) bulk metal, and the vacuum state is kept in the cooling process.
Putting the InSb bulk metal into a 4-inch quartz test tube, and vacuumizing until the air pressure is less than 10 DEG-3mm Hg, prevented from being excessively heat-treatedThe metal oxide is generated, the metal oxide is heated by a hyperbolic tube furnace, the heat treatment temperature is set to 400 ℃, the heat preservation is carried out for 24 hours, and then the metal oxide is cooled to the room temperature at the speed of 50 ℃/H.
Step 2: and (4) preparing an anodic aluminum oxide template.
A pure aluminum sheet with the purity of 99.99 percent is selected as an anodic alumina substrate, and is cut into a wafer with the diameter of 2.6cm and the thickness of 0.1cm, and then the following steps are carried out.
(a) Physically grinding and polishing the cut high-purity aluminum sheet, and then putting the aluminum sheet into electrolyte for electrolytic polishing, wherein the electrolyte is HClO (15 vol.% of)4+15vol.％CH3(CH2)3OCH2CH2OH)+70vol.％C2H6And O, and introducing a voltage of 40V for 15 minutes to obtain the smooth surface of the aluminum sheet.
(b) Place the electropolished aluminum flake in 6 vol.% H3PO4In the solution, a voltage of 125V was applied for the first anodic treatment, which lasted for 2 hours. And a cooling system is required to be used for cooling in the anode treatment process, so that the aluminum sheet is prevented from being burnt through due to overheating in the anode treatment process.
(c) Placing the aluminum sheet after primary anode treatment into a mixed solution of chromic acid and phosphoric acid (1.8 wt% CrO)3+6vol.％H3PO4+92vol.％H2O) and heated to 70 ℃, for a soaking time of 40 minutes, removing the alumina after the first anodic treatment. The surface of the aluminum substrate can present a concave and uneven surface, and the concave part on the surface is nucleated preferentially during secondary anodic treatment to become a starting point for the growth of the nano holes, so that the nano holes arranged in order are formed.
(d) Aluminum flake charged with 6 vol.% H3PO4And (3) introducing 125V voltage into the solution to carry out secondary anodic treatment, wherein the anodic treatment time is prolonged to 48 hours, which is favorable for increasing the thickness of the anodic oxidation film. And a cooling system is required to be used for cooling in the anode treatment process, so that the aluminum sheet is prevented from being burnt through due to overheating in the anode treatment process.
(e) The twice anodized aluminum sheet was placed in a solution of copper chloride and hydrochloric acid (8 wt% CuCl)2+5vol.％HCl+85vol.％H2O), soaking in 1After 0 min, residual aluminum was removed and re-soaked in 6 vol.% phosphoric acid (H)3PO4) Removing the barrier layer from the solution to obtain the semitransparent anodized aluminum.
(f) The prepared translucent anodized aluminum was soaked in 10 vol.% of H2SO4The solution was applied with 18V for 40 minutes to obtain an anodic alumina template with a pore size of 86.12 + -5.44 nm, as shown in FIG. 2.
And step 3: and (4) vacuum pressure casting.
And (3) preparing the nanowire by taking the anodic aluminum oxide obtained in the step (2) as a template in a vacuum pressure casting manner.
And (3) placing the indium antimonide blocky metal prepared in the step (1) on an anodic aluminum oxide template in die extrusion. And putting the mould into a closed space, vacuumizing, heating to 530 ℃, and preserving heat for 10 minutes to ensure that the indium antimonide in the mould becomes molten. The indium antimonide in a molten state enters the nano holes of the anodic aluminum oxide template by utilizing the pressurization of a hydraulic press, and the pressure of the hydraulic press is about 50kg/cm2And the duration is 1 minute, then the aluminum oxide template and the indium antimonide are naturally cooled to the room temperature at the room temperature to obtain the anode aluminum oxide template containing the indium antimonide nanowire, then the anode aluminum oxide template is put into a hyperbolic tube furnace for heat treatment, the heat treatment temperature is 400 ℃, the heat preservation time is 1 hour, and then the anode aluminum oxide template is cooled to the room temperature at the speed of 50 ℃/hour. Finally, the anodic aluminum oxide template containing the indium antimonide nanowire is soaked in a mixed solution of chromic acid and phosphoric acid (1.8 wt% CrO)3+6vol.％H3PO4+92vol.％H2O), removing the anodic aluminum oxide template, and filtering with ethanol to obtain the indium antimonide nanowire with the average diameter of about 83nm, as shown in figure 3.
And 4, step 4: and preparing an organic field effect transistor type memory.
Mixing the 2mg nanowire obtained in step 3 with 5mg polymethacrylic acid (PMAA), and adding 1 ml of methanol (CH)3OH), preparing nanowire suspensions with different concentrations by ultrasonic vibration. The nanowire suspension was coated on 1.5cm × 1.5cm × 300nm SiO using a spin coater2On the substrate, the spin coater speed was set at 2000r/min for 60 seconds.
Pentacene (C) was evaporated by vacuum evaporation22H14) Plating on the nanowire layer with vacuum degree of 10-7mm Hg with a deposition thickness of 30 nm. Plating gold electrode with length and width of 1000 μm and 50 μm respectively by vacuum evaporation method, and vacuum degree of 10-7mm Hg, and the deposition thickness is 80nm, so that the organic field effect transistor type memory can be obtained, and the structure is shown in figure 1.
Example 2
Example 2 the manufacturing process of indium antimonide nanowires for use in a non-volatile data storage element was substantially the same as in example 1, except that 5mg of nanowires prepared in step 3 were mixed with 5mg of polymethacrylic acid (PMAA) in step 4.
Example 3
Example 3 the manufacturing process of indium antimonide nanowires for use in a non-volatile data storage element was essentially the same as in example 1, except that 9mg of nanowires prepared in step 3 were mixed with 5mg of polymethacrylic acid (PMAA) in step 4.
Example 4
Example 4 the indium antimonide nanowire fabrication process for a non-volatile data storage device was essentially the same as in example 1, except that the prepared translucent anodized aluminum was soaked in 5 wt.% C in step 22H2O4And (3) applying 40V voltage to the solution for 40 minutes to obtain the anodic alumina template with the aperture of 96.23 +/-7.32 nm. The nanowires finally prepared in step 3 have an average diameter of about 102nm, as shown in fig. 4.
Example 5
Example 5 the indium antimonide nanowire fabrication process for a non-volatile data storage device was essentially the same as in example 1, except that the prepared translucent anodized aluminum was soaked in 5 wt.% C in step 22H2O4And (3) applying 40V voltage to the solution for 40 minutes to obtain the anodic alumina template with the aperture of 96.23 +/-7.32 nm. The nanowires finally prepared in step 3 have an average diameter of about 102 nm. 5mg of nanowires was mixed with 5mg of polymethacrylic acid (PMAA) in step 4.
Example 6
Example 6 pairsThe fabrication process of indium antimonide nanowires for non-volatile data storage devices was substantially the same as in example 1, except that the prepared translucent anodized aluminum was soaked in 5 wt.% of C in step 22H2O4And (3) applying 40V voltage to the solution for 40 minutes to obtain the anodic alumina template with the aperture of 96.23 +/-7.32 nm. The nanowires finally prepared in step 3 have an average diameter of about 102 nm. 5mg of nanowires were mixed with 9mg of polymethacrylic acid (PMAA) in step 4.
Example 7
Example 7 the fabrication process of indium antimonide nanowire for non-volatile data storage device was substantially the same as in example 1 except that the prepared translucent anodized aluminum was soaked in 6 vol% of H in step 23PO4The solution is applied with 195V voltage for 40 min to obtain the anodic alumina template with the pore diameter of 420 +/-40 nm. The nanowires finally prepared in step 3 have an average diameter of about 382nm, as shown in fig. 5.
Example 8
Example 8 the fabrication process of indium antimonide nanowire for non-volatile data storage device was substantially the same as in example 1 except that the prepared translucent anodized aluminum was soaked in 6 vol% of H in step 23PO4The solution is applied with 195V voltage for 40 min to obtain the anodic alumina template with the pore diameter of 420 +/-40 nm. The nanowires finally prepared in step 3 have an average diameter of about 382 nm. 5mg of nanowires was mixed with 5mg of polymethacrylic acid (PMAA) in step 4.
Example 9
Example 9 the fabrication process of indium antimonide nanowire for non-volatile data storage device was substantially the same as in example 1 except that the prepared translucent anodized aluminum was soaked in 6 vol% of H in step 23PO4The solution is applied with 195V voltage for 40 min to obtain the anodic alumina template with the pore diameter of 420 +/-40 nm. The nanowires finally prepared in step 3 have an average diameter of about 382 nm. 5mg of nanowires were mixed with 9mg of polymethacrylic acid (PMAA) in step 4.
Analysis results of the indium antimonide nanowires prepared in examples 1 to 9
The nanowire composition was analyzed using XRD, and the analysis results were compared with JCPDS cardNO.06-0208(InSb) and No.05-0562(Sb), as shown in FIG. 6. The comparison results show that all three nanowires have InSb crystal planes as main diffraction peaks, and in example 4 and example 7, an Sb diffraction peak at 28.76 ° is found, and it is confirmed that two phases of Sb/InSb coexist.
Performance analysis of nonvolatile memory devices prepared in examples 1 to 3
The performance of the storage elements was analyzed using a semiconductor parameter analyzer (4200A-SCS). Wherein the critical voltage offset (Δ V)th) For determining the ability to store charge, Δ V, for a voltage difference between the write and erase curvesthLarger means that the charge is less easily erased and the charge storage capacity is stronger. In contrast, Δ VthThe smaller the charge the weaker the charge storage capacity is easily erased. The switching current ratio is used for judging the electrical performance, and the larger the switching current ratio is, the more obvious the electronic characteristic display is. Therefore, the component is defined to have a maximum Δ VthAnd a high switching current ratio is a good memory element.
TABLE 1 analysis of non-volatile memory device Performance
As shown in Table 1, the memory element with 2mg nanowire added has the largest Δ Vth(about 25V) and a switching current ratio of 105(ii) a Δ V of non-additive nanowire storage elementth8V only and a current switching ratio of 106. Through comparison of measurement results, the fact that the charge storage characteristic can be effectively improved by adding the nanowire storage element is verified. The added nanowire component has good memory characteristics, and if the added amount of the nanowire is increased, the memory effect can be improved. When 5mg and 9mg of nanowire storage elements Δ Vth were added at 15V and 6V, respectively, it was found that the charge trapping ability of the storage elements increased with the addition amount of the nanowiresFirst increasing and then decreasing. The increase in the amount of the added nanowires tends to make the dispersibility thereof poor and cause aggregation, resulting in charge transfer through the nanowires and failure to be trapped by the nanowires. The storage atmosphere pollution of adding 2mg of nano wire has good charge trapping capacity. When the addition amount exceeds 2mg, the charge trapping capacity is reduced, and the aggregation phenomenon is caused due to poor dispersibility of the nanowires, so that charges are easy to lose and cannot be trapped, and the memory characteristic is reduced
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The preparation method of the indium antimonide nanowire is characterized by comprising the following steps of:
1) mixing indium particles and antimony powder, heating in vacuum environment with pressure less than 10-3mmHg, melting, continuously heating until the mixture is uniformly mixed, and cooling to form InSb bulk metal;
2) placing the InSb bulk metal at a gas pressure of less than 10-3Heating to 400 ℃ in a vacuum environment of mm Hg, preserving heat for 24 hours, and cooling to room temperature at the speed of 50 ℃/H;
3) preparing an anodic aluminum oxide template by using a pure aluminum sheet as an anodic aluminum oxide substrate, wherein the anodic aluminum oxide is provided with nano holes with uniform size;
4) putting the InSb bulk metal prepared in the step 1) on an anodic alumina template extruded by a die, heating to 530 ℃ and preserving the temperature for 10 minutes, so that the InSb bulk metal is molten, pressurizing to enable molten indium antimonide to enter nano holes of the anodic alumina template, and cooling to obtain the anodic alumina template containing indium antimonide nano wires;
5) carrying out heat treatment on the anodic aluminum oxide template containing the indium antimonide nanowire, soaking the anodic aluminum oxide template in a mixed solution of chromic acid and phosphoric acid, and filtering the anodic aluminum oxide template with ethanol to obtain the indium antimonide nanowire; the heat treatment specifically comprises the following steps: the temperature was maintained at 400 ℃ for 1 hour and then cooled to room temperature at a rate of 50 ℃ per hour.
2. The method for preparing indium antimonide nanowires of claim 1, wherein the pressurizing in the step 4) is specifically 50kg/cm of hydraulic press pressure2For a duration of 1 minute.
3. The method for preparing indium antimonide nanowires according to claim 1, wherein the mixed solution of chromic acid and phosphoric acid in step 5) is: 1.8 wt% CrO3+6vol.％H3PO4+92vol.％H2O。
4. A method for preparing an organic field effect transistor type memory by utilizing indium antimonide nanowires is characterized by comprising the following steps:
mixing the indium antimonide nanowire prepared in the claim 1 with polymethacrylic acid, placing the mixture in methanol, preparing nanowire suspension through ultrasonic vibration, and coating the nanowire suspension on SiO (1.5 cm x 300 nm) by using a spin coater2A substrate;
and plating pentacene on the indium antimonide nanowire layer, plating a gold electrode, wherein the length and the width of the electrode are 1000 micrometers and 50 micrometers respectively, and the deposition thickness is 80nm, so as to obtain the organic field effect transistor type memory.
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