CN102299058B - Method for manufacturing micro-electronic part by using nanometer materials with multilevel heterostructure - Google Patents
Method for manufacturing micro-electronic part by using nanometer materials with multilevel heterostructure Download PDFInfo
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Abstract
The invention relates to the technical field of semiconductor micro-electronic parts, and in particular relates to nanometer semiconductor materials with a multilevel heterostructure manufactured by combining an electrospinning technology with a hydrothermal synthesis technology and a method for manufacturing a micro-electronic part with stable performances by using the nanometer semiconductor materials. In the method, inorganic oxide nanofibers obtained by adopting the electrospinning technology to sinter is takend as a core. The method comprises the following steps: depositing and growing inorganic oxide nanorods on fiber surfaces sequentially by the hydrothermal reaction to obtain single-dimensional arborescent nanometer materials with the multilevel heterostructure; and assembling an FET (field-effect transistor). The FET has higher electron mobility and exceeds the vast majority of FETs in the long service life and the high stability. The maximum electron mobility of anatase titanium dioxide nanofiber/ titanic schorl titanium dioxide nanorod FETs with the multilevel heterostructure can be above 10cm<2>/Vs, and the performances do not attenuate hardly with the increment of the time and the humidity.
Description
Technical field
The invention belongs to the Nano semiconductor technical field of microelectronic devices, be specifically related to a kind ofly utilize Electrospinning and have the nano semiconductor material of multistage heterogeneous structure in conjunction with Hydrothermal Synthesis technology preparation, and be used for constructing the method that high-performance is stablized microelectronic component.
Background technology
Microelectronic component is owing to have that volume is little, lightweight, reliability is high, operating rate is fast, read and write the density advantages of higher, and the development of information age is had tremendous influence.Field-effect transistor be the simplest in the current semi-conductor electronic device also be most important construction unit, be present studied the most deep a kind of device.Can be divided into inorganic field effect transistor and organic field effect tube according to material category, although organic field effect tube is compared the inorganic field effect transistor in price, flexibility and element manufacturing with operation very large advantage is arranged, lower electron mobility is (generally at 0.01cm
2/ Vs is following) become and limit its real application and the bottleneck that develops.In addition, existing organic and inorganic field effect transistor also is to satisfy current electronics industry demand on life-span and stability, still needs and will further improve.And method in the past needs complicated processing procedure sometimes, and this can increase the technique degree, and price also can raise and be unfavorable for promoting.
Summary of the invention
The purpose of this invention is to provide and a kind ofly utilize Electrospinning and have the nano semiconductor material of multistage heterogeneous structure in conjunction with Hydrothermal Synthesis technology preparation, and be used for constructing the method that high-performance is stablized microelectronic component.
Accurate one-dimensional micro-nanometer structure is owing to have large specific area and draw ratio, thereby possessed excellent characteristic electron, receives much concern in recent years.And electrostatic spinning technique is a kind of method of can the production overlength continuous one-dimensional micro-nanometer material, and it is simple that this technology has equipment, production cost is low, the use material is extensive and the output fiber size is even, the advantages such as specific area is large have been proved to be a kind of new method of assembling effectively, easily electronic device.Therefore in the present invention, we provide a kind of and have utilized electrostatic spinning technique and have the nano semiconductor material of multistage heterogeneous structure in conjunction with the preparation of Hydrothermal Synthesis technology, and are used for constructing the method that high-performance is stablized microelectronic component.
The nano material of this multistage heterogeneous structure be the inorganic oxide nanofiber that obtains take the electrospinning sintering as trunk, follow-up in fiber surface deposition growing inorganic oxide nanometer rods by hydro-thermal reaction, obtain the nano material of accurate one dimension dendroid multistage heterogeneous structure.Be assembled into afterwards field-effect transistor, field-effect transistor has the electron mobility of superelevation, and long-life and high stability are considerably beyond other most of field-effect transistors.Field-effect transistor maximum electron mobility such as anatase titania nanofiber/rutile titanium dioxide nanometer rods multilevel hierarchy can reach 10cm
2More than/the Vs, along with the increase of time lengthening and humidity, decay does not almost appear in performance.
The method of the invention technique is simple, and is with low cost, and good reproducibility can be prepared long-acting, stable and high performance inorganic field effect transistor, can be the development and application developing thinking of electronic applications high performance field effect transistors.
Of the present inventionly construct high-performance by multistage heterogeneous structure and stablize microelectronic component, it comprises the steps:
One: accurate one dimension dendroid multistage heterogeneous structure preparations of nanomaterials
A. 0.3～1g soluble high-molecular compound is joined in 5～10ml solvent 1 (one or more in DMF, the second alcohol and water), under ℃ condition of room temperature～100, be stirred to solution and clarify fully, then be cooled to room temperature;
B. 0.2～2.0g soluble inorganic salt or solubility inorganic oxide precursor body are joined in 3～6ml solvent 2 (one or more in DMF, ethanol, acetic acid and the water), vigorous stirring mixes it under the drying condition; Then the solution that obtains is joined in the solution of steps A fast, stirring mixes two kinds of solution;
C. the mixed solution that step B is obtained is put into the glass spray fiber tube of electrospinning device, the tube head internal diameter of glass spray fiber tube is 0.5～3mm, take the aluminium cover as anode, be that two parallel aluminum strips or the stainless steel strip of 2～3cm accepted product as minus plate with spacing, the distance of two interpolars is 10～30cm, the voltage that applies 6～30KV at two interpolars carries out Electrospun, thereby obtains the nanofiber that contains macromolecular compound be arranged in parallel at negative electrode;
D. with the quartz plate that cleans up the nanofiber that contains macromolecular compound between minus plate is collected, in air, placed 10～20 hours, then under 400～700 ℃ of temperature sintering 3～5 hours to remove macromolecular compound; Or directly minus plate and the nanofiber that contains macromolecular compound sintering under 400～700 ℃ of temperature are collected oxide fibre with the quartz plate that cleans up or polytetrafluoroethylsubstrate substrate after 3～5 hours again; Thereby obtain the inorganic oxide nanofiber that is arranged in parallel of diameter 50～300nm in quartz plate or polytetrafluoroethylsubstrate substrate;
E. get in addition the solvent 3 (ethanol of 0.1～2.0g soluble inorganic salt or solubility inorganic oxide precursor body and 10～40ml, in hydrochloric acid and the water one or more) mix, in the system that the quartz plate that obtains among this solution and the step D or polytetrafluoroethylsubstrate substrate are transferred to hydrothermal reaction kettle, carry out hydro-thermal reaction, thereby a large amount of inorganic oxide nanometer rods of inorganic oxide nanofiber surface hydrothermal growth at step D, then it is dry to take out the substrate washing, namely obtains having the inorganic oxide nano material of accurate one dimension dendroid multistage heterogeneous structure at quartz plate or polytetrafluoroethylsubstrate substrate surface;
Further, when the inorganic oxide nanometer rods of the inorganic oxide nanofiber surface of step D hydrothermal growth is zinc oxide, the substrate quartz plate, hydrothermal system is the mixed solution of soluble zinc salt, hexamethylenetetramine and water, wherein zinc salt concentration is 0.01～0.04mol/L, hexamethylenetetramine concentration is about 0.005～0.01mol/L, and hydrothermal condition is 80～100 ℃ of reactions 1～8 hour; When the inorganic oxide nanometer rods of the inorganic oxide nanofiber surface of step D hydrothermal growth is tin ash, the substrate polytetrafluoroethylene, hydrothermal system is the mixed solution of solubility pink salt, NaOH, water, ethanol (or ethylenediamine), wherein water mixes with ethanol (or ethylenediamine) equal-volume, pink salt concentration is 0.04～0.07mol/L, naoh concentration is 0.31～0.44mol/L, and hydrothermal condition is 180～250 ℃ of reactions 1～48 hour; When the inorganic oxide nanometer rods of the inorganic oxide nanofiber surface of step D hydrothermal growth is titanium dioxide, the substrate quartz plate, hydrothermal system is soluble titanium dioxide presoma, water and hydrochloric acid (concentration is about 12mol/L), wherein water mixes with the hydrochloric acid equal-volume, and TiO 2 precursor concentration is that 0.01～0.05mol/L hydrothermal condition is 100～200 ℃ of reactions 1～5 hour.
Soluble high-molecular compound described in the inventive method is polyvinyl alcohol, polyvinylpyrrolidone or polyacrylonitrile; Described soluble inorganic salt is soluble zinc salt, such as zinc acetate, zinc nitrate or zinc chloride; The solubility pink salt is such as butter of tin or stannous chloride; Solubility inorganic oxide precursor body is the soluble titanium dioxide presoma, such as butyl titanate, isopropyl titanate or titanium tetrachloride.
Two: the assembling of field-effect transistor, field-effect transistor adopts top grid top contact structure.
F. the making of source, drain electrode: send quartz plate or polytetrafluoroethylsubstrate substrate that step e obtains to vacuum coating equipment, by with the mask plate aluminium electrode that evaporation 50～100nm is thick on the inorganic oxide nano material of the accurate one dimension dendroid multistage heterogeneous structure of substrate surface of source, drain electrode complementary structure, thereby formation source, drain electrode structure, distance between source, drain electrode is that channel width is 60～100 μ m, and the line of source, drain electrode is consistent with the direction of inorganic oxide nanofiber;
G. the preparation of gate electrode and gate insulation layer: select N-shaped＜100〉silicon chip, thickness is 1～2mm, resistivity is 3～5M Ω cm, adopts dry-oxygen oxidation method at this silicon chip SiO that grows
2Gate insulation layer, growth temperature are 900～1200 ℃, SiO
2The thickness of gate insulation layer is 1500～2000nm, then the surface is had SiO
2The wafer dicing of gate insulation layer is the strip structure of wide 1～2mm, long 1～3cm, cleans and oven dry;
H. polyvinylpyrrolidone is mixed with into viscous fluid with deionized water, getting two droplet viscous fluids with the needle point of cleaning places evaporation that the quartz plate of aluminium electrode one side or the two ends of polytetrafluoroethylsubstrate substrate are arranged, line between two thickness drops and the direction of inorganic oxide nanofiber are perpendicular, the silicon chip of the strip structure for preparing among the step G is placed thickness drop top, and firmly it is compacted to SiO
2Or nitride gate insulating barrier and aluminium electrode securement, after the viscous fluid drying is solidified, prepare long-acting, stable and high performance inorganic semiconductor field-effect transistor; In this device architecture, air can be filled in the raceway groove between source, the drain electrode, so it and SiO
2The layer while is as the insulating barrier of this device.
Test macro adopts Keithley 4200 Sourcemeter and the shielding harness supporting with it, test is to carry out under the condition of 5%RH～20%RH in room temperature, relative humidity, stability test is to carry out under the condition of 11%RH～85%RH in room temperature, relative humidity, among the present invention gate insulation layer also available silicon nitride layer replace SiO
2Layer.
Three: the calculating of transistor mobility among the present invention
There is the calculating of the field-effect transistor mobility of saturation region to adopt formula I
DS=(C
iμ W/2L) (V
GS-V
T)
2, I wherein
DSBe leakage current, V
GSGrid voltage, V
TBe cut-in voltage, W is the diameter of quasi-one-dimensional nanometer material and the product of material quantity (single device W is exactly the diameter of material), and L is that raceway groove is wide, C
iThat (1600nm silicon dioxide and dry air be C during together as insulating barrier for the insulating barrier unit-area capacitance
i=2.16*10
-5F/m
2200nm silicon nitride and dry air C together as insulating barrier the time
i=3.45*10
-4F/m
2, computational methods can be with reference to small 2011,7, No.5,597～600).
The computing formula of the transistor mobility of linear zone adopts I
DS=μ C
i/ L[(V
GS-V
T) V
DS-1/2V
DS 2], every representative meaning is the same, V
DSBe source-drain voltage.
Mechanism of the present invention can be done following understanding: the laggard horizontal high voltage blending of soluble inorganic salt or inorganic oxide precursor body and macromolecule mixed dissolution obtains the composite fibre take macromolecule as template.According to selected metal precursor and macromolecule, select suitable sintering temperature and heating schedule, at high temperature with the macromolecule template burn off in the composite fibre, make simultaneously at high temperature oxidation of slaine and crystallization, form ceramic semiconductors metal oxide based nano-fiber.Then place the hydrothermal reaction kettle of HTHP, be deposited on uniformly the trunk fiber surface through newly-generated after a while inorganic oxide nanometer rods, and continuous elongated chap.In the material of dendroid multistage heterogeneous structure, these peripheral monocrystalline oxide nanometer rods have higher crystallinity, in addition the formation between they and the trunk oxide fibre countless interfaces, all these has improved the characteristic of device greatly, such as the appearance of saturation region, the increase of on-off ratio and the raising of electron mobility etc.The nanorod surfaces carrier concentration changes when countless nanometer rods is exposed in the air of different humidity; but because the existence of interface; this variation can't be delivered in the trunk fiber, thereby device is had certain protective effect, and the life-span of device and stability are obviously improved.
First passage hydro-thermal reaction of the present invention is made the characteristic that accurate one dimension dendroid multistage heterogeneous structure nano material improves the inorganic, metal oxide field-effect transistor at oxide surface depositing nano rod, and obtained surprising result, except the raising of on-off ratio and electron mobility, life-span and the stability of device also are greatly improved.It is simple that the method has preparation technology, and convenient operation and the advantage such as repeat, and production equipment is simple and convenient requires lowlyer to working condition, and low production cost has wide market application foreground, is easy to promotion and application.
Description of drawings
Fig. 1: be process schematic diagram and the section structure schematic diagram of anatase nanofiber superficial growth rutile nano-stick in thermal and hydric environment of example for the embodiment of the invention 1,2 and 3;
Fig. 2: obtained accurate one dimension dendroid multistage heterogeneous structure nano material is assembled into the structural representation of device in the various embodiments of the present invention;
Fig. 3: embodiment 1 prepared anatase crystal titanium dioxide nanofiber transmission electron microscope photo; Illustration is its electron diffraction pattern, picture scale: 100nm;
Fig. 4: embodiment 1 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the ESEM sheet of rutile crystal type titanium dioxide nanofiber as the accurate one dimension dendroid multilevel hierarchy nano material of branch, picture scale: 5 μ m;
Fig. 5: embodiment 1 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the ESEM sheet of rutile crystal type titanium dioxide nanofiber as the accurate one dimension dendroid multilevel hierarchy nano material of branch, picture scale: 500nm;
Fig. 6: embodiment 1 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transistorized output characteristic curve of rutile crystal type titanium dioxide nanofiber as branch, illustration is the photo of transistor ESEM;
Fig. 7: embodiment 1 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transistorized transfer characteristic curve of rutile crystal type titanium dioxide nanofiber as branch;
Fig. 8: embodiment 1 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transistorized time stability test result of rutile crystal type titanium dioxide nanofiber as branch;
Fig. 9: embodiment 1 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transistorized humidity stability test result of rutile crystal type titanium dioxide nanofiber as branch;
Figure 10: embodiment 2 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transmission electron microscope photo of rutile crystal type titanium dioxide nanofiber as branch, picture scale: 200nm;
Figure 11: embodiment 2 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transistorized output characteristic curve of rutile crystal type titanium dioxide nanofiber as branch, illustration is the photo of transistor ESEM;
Figure 12: embodiment 3 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transmission electron microscope photo of rutile crystal type titanium dioxide nanofiber as branch, picture scale: 100nm;
Figure 13: embodiment 3 is prepared take the anatase crystal titanium dioxide nanofiber as trunk, take the accurate one dimension dendroid multilevel hierarchy nano material transistorized output characteristic curve of rutile crystal type titanium dioxide nanofiber as branch, illustration is the photo of transistor ESEM;
As shown in Figure 1, the inorganic oxide nanofiber that sintering is obtained places the hydro-thermal reaction environment, after beginning to react very short time, some sparse oxide nano-particles begin in the fiber surface deposition, prolong the continuous growth of reaction time nano particle and become sparse nanometer rods, continue to prolong the hydro-thermal reaction time, nanometer rods is elongated chap gradually, until reaction finishes, fiber surface deposits countless closely nanometer rods, and the nanometer rods orientation is perpendicular to the outer surface of fiber.
As shown in Figure 2,1 is that grid N-shaped Si, 2 is SiO
2Gate insulation layer, 3 be quartz plate or teflon plate substrate, 4 for as the aluminium lamination of source-drain electrode, 5 for the oxidate nano fiber after the sintering, 6 for after the hydro-thermal reaction at the oxide nano-rod of fiber surface deposition growing.
As shown in Figure 3, embodiment 1 prepared titanium dioxide nanofiber transmission electron microscope photo and electronic diffraction result, the nanofiber surface that can find out the titanium dioxide that the present invention makes is coarse, and diameter homogeneous, fibre diameter are distributed between 80～200 nanometers substantially.Can find out that from the electronic diffraction ring titanium dioxide is the anatase structured of polycrystalline.
As shown in Figure 4, embodiment 1 is prepared take the anatase titania nanofiber as trunk, take the nano material stereoscan photograph of rutile titanium dioxide nanometer rods as the accurate one dimension dendroid multilevel hierarchy of branch, can find out that the material pattern that the present invention makes is good, diameter homogeneous, rutile nano-stick closely and uniformly are arranged in the surface of anatase nanofiber.
As shown in Figure 5, embodiment 1 is prepared take the anatase titania nanofiber as trunk, take the nano material transmission electron microscope photo of rutile titanium dioxide nanometer rods as the accurate one dimension dendroid multilevel hierarchy of branch, what illustration provided is the electron diffraction diagram of surface titanium dioxide nanometer rods.The titanium dioxide that can find out the hydro-thermal reaction deposition is the rutile structure of monocrystalline.
As shown in Figure 6, the transistorized output characteristic curve of embodiment 1 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano material, this transistor has showed the N-shaped characteristic of standard.Leakage current is linear under small voltage increases, and leakage current reaches capacity under large voltage.What illustration provided is the ESEM picture of transistor channel, and this transistor is five nano material transistors.
As shown in Figure 7, the transistorized transfer characteristic curve of embodiment 1 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano material.This transistorized cut-in voltage is-55 volts, and the field effect electron mobility surpasses 10cm
2/ Vs.
As shown in Figure 8, embodiment 1 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano material transistor was placed two months in air at room temperature, it is 40 volts that follow-on test is found at source-drain voltage, when grid voltage is 20 volts, the electric current of device is not decay almost, shows that the good life-span of transistor stability of our this structure is longer.
As shown in Figure 9, in the environment of different humidity, test under the embodiment 1 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano material transistor room temperature, it is 40 volts at source-drain voltage, when grid voltage is 20 volts, the electric current of device does not almost change with the rising of humidity, shows that the transistor of our this structure has good humidity stability.
As shown in figure 10, the transmission photo of embodiment 2 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano materials, relatively can find out with Fig. 5, the nanometer rods of 3 hours fiber surface depositions of hydro-thermal reaction is obviously than 4 hours weak point of hydro-thermal reaction and thin, and nanometer rods is arranged also comparatively sparse.
As shown in figure 11, the transistorized output characteristic curve of embodiment 2 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano materials, this transistor has still showed the N-shaped characteristic of standard.Leakage current is linear under small voltage increases, and leakage current reaches capacity under large voltage.But compare with Fig. 6, the source-drain voltage when leakage current reaches capacity obviously increases.What illustration provided is the ESEM picture of transistor channel, and this transistor is two nano material transistors.
As shown in figure 12, the transmission photo of embodiment 3 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano materials, relatively can find out with Fig. 5 and Figure 10, hydro-thermal reaction 2 hours, the nanometer rods of fiber surface deposition is shorter thinner, arrange also more sparsely, these change the growth course schematic diagram of giving with Fig. 1 and also match.
As shown in figure 13, the transistorized output characteristic curve of embodiment 3 prepared accurate one dimension anatase/rutile dendroid multilevel hierarchy nano materials, this transistor has still showed the N-shaped characteristic of standard.But compare with Fig. 6 and Figure 11, leakage current does not still go out to reach capacity when source-drain voltage is increased to 70 volts.What illustration provided is the ESEM picture of transistor channel, and this transistor is four nano material transistors.
Embodiment
1, utilizes the field-effect transistor of the dendroid multistage heterogeneous structure material of electrical spinning method and Hydrothermal Synthesis preparation take titanium dioxide nanofiber as trunk
Embodiment 1:
In the 50ml conical flask, 0.45g polyvinylpyrrolidone (PVP) is added in the 7.5ml ethanol, stirring at room 8h clarifies fully to solution.
Other gets a 10ml conical flask, adds successively the 1.5g butyl titanate, 3ml ethanol and 3ml acetic acid, and room temperature vigorous stirring 10min is to fully dissolving.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.
The solution that mixes is put into the spray fiber tube of Electrospun equipment, the internal diameter of spray fiber tube head is 1mm, and as anode, (spacing 2.2cm) accepts product as negative electrode with parallel aluminum strip with the aluminium cover, two anode-cathode distances are 20cm, and applying voltage is that 10kV carries out Electrospun.The nanofiber that contains polyvinylpyrrolidone that will between two parallel aluminum strips of negative electrode, obtain like this to be arranged in parallel (the method can list of references Appl.Phys.Lett.2006,89,133125).
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, placing in the air allowed butyl titanate slowly be hydrolyzed in 12 hours, then put into Muffle furnace, slowly be warming up to 450 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, thereby obtained titanium dioxide nanofiber.The control Electrospun spray silk time just can be controlled fiber arranged quantity.Gained titanium dioxide nanofiber diameter is about 80～200nm, and fiber is anatase crystal.
Get the 50ml beaker, add successively 15ml water, 15ml concentrated hydrochloric acid (concentration is about 12mol/L) and 0.5g butyl titanate, the solution that stirs clarification, transfer to together with the quartz plate that is attached with parallel anatase titania nanofiber in the hydrothermal reaction kettle of 40ml, in 150 ℃ of constant temperature ovens, placed 4 hours, it is dry to take out the quartz plate washing, countless titanium dioxide nano-rods are deposited on fiber surface and continuous elongated chap during this time, nanometer rods is perpendicular to the fiber surface close-packed arrays, and these nanometer rods present rutile crystal type.Thereby obtain take the anatase titania nanofiber as trunk at the quartz plate substrate, take the nano material of rutile titanium dioxide nanometer rods as the accurate one dimension dendroid multilevel hierarchy of branch;
The making of source, drain electrode: the quartz plate substrate that will be loaded with dendroid multilevel hierarchy nano material places vacuum coating equipment, will and the source that forms of needs, the mask plate of drain electrode complementary structure place between vapor deposition source and the nano material, the thickness of AM aluminum metallization electrode is 100nm on nano material, thereby the source, the drain electrode structure that have raceway groove between formation source, drain electrode, adjust the position of mask plate, making line between source, drain electrode is that the direction of raceway groove is consistent with the direction of nanofiber;
The preparation of gate electrode and gate insulation layer: the surface is had SiO
2Then the strip that the Si sheet of gate insulation layer is divided into that 2mm is wide, 2cm is long used in ethanol, acetone, the deionized water each ultrasonic cleaning 15 minutes successively, and dry for standby;
The making of field-effect transistor (FET) device: with PVP and deionized water hybrid modulation viscous fluid (PVP mass fraction 3～5wt%), get the two ends (line between two PVP drops and the direction of nanofiber are perpendicular) that two droplet thickness fluid injections place the quartz plate substrate with the cleaning needle point, above-mentioned strip Si sheet is placed the viscous fluid top at once, and firmly it is compacted to SiO
2With the Al electrode securement, treat that the PVP viscous fluid solidifies, just obtained rutile/anatase dendroid multilevel hierarchy nano material field-effect transistor.This transistor field-effect mobility maximum surpasses 10cm
2/ Vs, and in the different humidity environment test component, electric current does not have to change substantially, through bimestrial follow-on test, device is intact and almost not decay of electric current still, these excellent performances are rare in the transistor that other has been reported.
Embodiment 2:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 450 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained titanium dioxide nanofiber.Get the 50ml beaker, add successively 15ml water, 15ml concentrated hydrochloric acid and 0.5g butyl titanate, the solution that stirs clarification, transfer to together with the quartz plate that is attached with parallel anatase titania nanofiber in the hydrothermal reaction kettle of 40ml, in 150 ℃ of constant temperature ovens, placed 3 hours, take out quartz plate washing drying.The rutile nano-stick of fiber surface is obviously than the weak point among the embodiment 1 and thin.
The device assembling process is consistent with embodiment 1.The field-effect mobility maximum is greater than 3cm
2/ Vs, stability descends to some extent with humidity.
Embodiment 3:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 450 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained titanium dioxide nanofiber.Get the 50ml beaker, add successively 15ml water, 15ml concentrated hydrochloric acid and 0.5g butyl titanate, the solution that stirs clarification, transfer to together with the quartz plate that is attached with parallel anatase titania nanofiber in the hydrothermal reaction kettle of 40ml, in 150 ℃ of constant temperature ovens, placed 2 hours, take out quartz plate washing drying.The rutile nano-stick of fiber surface is arranged more sparse, obviously than the also weak point among the embodiment 2 and thin.
The device assembling process is consistent with embodiment 1.The field-effect mobility maximum is about 0.2cm
2/ Vs, electric current is with the vary stable variation of humidity.
Embodiment 4:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 450 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained titanium dioxide nanofiber.Get the 50ml beaker, add successively 35ml deionized water, 0.104g zinc nitrate and 0.0522g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take the anatase titania nanofiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8.7cm
2/ Vs, stability slightly descends with embodiment 1.
Embodiment 5:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 450 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained titanium dioxide nanofiber.Get the 50ml beaker, add successively 35ml deionized water, 0.2195g zinc acetate and 0.028g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take the anatase titania nanofiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8.7cm
2/ Vs, stability test result such as embodiment 4 are similar.
Embodiment 6:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 500 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained titanium dioxide nanofiber.This moment, fiber presented the crystal formation that mixes of anatase and rutile.Get the 50ml beaker, add successively 15ml water, 15ml concentrated hydrochloric acid and 0.5g butyl titanate, the solution that stirs clarification, transfer to together with the quartz plate that is attached with parallel titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 150 ℃ of constant temperature ovens, placed 4 hours, take out quartz plate washing drying.Thereby obtain mixing the crystal formation titanium dioxide nanofiber as trunk take anatase/rutile at the quartz plate substrate, take the nano material of rutile titanium dioxide nanometer rods as the accurate one dimension dendroid multilevel hierarchy of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 10cm
2/ Vs has good stability equally, and is similar such as embodiment 1.
Embodiment 7:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 500 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained the titanium dioxide nanofiber of anatase and rutile mixing crystal formation.Get the 50ml beaker, add successively 35ml deionized water, 0.104g zinc nitrate and 0.0522g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtaining mixing the crystal formation titanium dioxide nanofiber at the quartz plate substrate is trunk, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is about 8.92cm
2/ Vs has preferably stability.
Embodiment 8:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 500 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained the titanium dioxide nanofiber of anatase and rutile mixing crystal formation.Get the 50ml beaker, add successively 35ml deionized water, 0.2195g zinc acetate and 0.028g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtaining mixing the crystal formation titanium dioxide nanofiber at the quartz plate substrate is trunk, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8cm
2/ Vs has preferably stability equally, and is similar such as embodiment 7.
Embodiment 9:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 700 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained titanium dioxide nanofiber.This moment, titania fiber presented pure Rutile Type.Get the 50ml beaker, add successively 15ml water, 15ml concentrated hydrochloric acid and 0.5g butyl titanate, the solution that stirs clarification, transfer to together with the quartz plate that is attached with parallel rutile titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 150 ℃ of constant temperature ovens, placed 2 hours, take out quartz plate washing drying.Thereby obtain take the rutile titanium dioxide nanofiber as trunk at the quartz plate substrate, take the nano material of rutile titanium dioxide nanometer rods as the accurate one dimension dendroid multilevel hierarchy of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 5cm
2/ Vs has good stability equally.
Embodiment 10:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 700 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained the rutile titanium dioxide nanofiber.Get the 50ml beaker, add successively 35ml deionized water, 0.104g zinc nitrate and 0.0522g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take the rutile titanium dioxide nanofiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8.33cm
2/ Vs has preferably stability equally.
Embodiment 11:
The solution outfit is consistent with spinning process and embodiment 1.
The quartz plate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting fiber arranged between two aluminum strips, place after 12 hours in the air and put into Muffle furnace, slowly be warming up to 700 ℃ of constant temperature sintering and Macromolecule PVP all removed in 5 hours, just obtained the rutile titanium dioxide nanofiber.Get the 50ml beaker, add successively 35ml deionized water, 0.2195g zinc acetate and 0.028g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel titanium dioxide nanofiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take the rutile titanium dioxide nanofiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8.33cm
2/ Vs, stability is similar to Example 10.
2, utilize the field-effect transistor of the dendroid multistage heterogeneous structure material of electrical spinning method and Hydrothermal Synthesis preparation take tin dioxide nano fiber as trunk
Embodiment 12:
In the 50ml conical flask, 0.8g polyvinylpyrrolidone (PVP) is added 2.2ml ethanol and 4.4mlN, in the dinethylformamide, stirring at room 8h clarifies fully to solution.
Other gets a 10ml conical flask, and the 0.4g stannous chloride is added in the 2.2ml ethanol, and room temperature vigorous stirring 10min is to fully dissolving.Polymer Solution is mixed with inorganic salt solution, continue at room temperature to stir 1 hour.
The solution that mixes is put into the spray fiber tube, the internal diameter of spinning head is 1mm, (spacing 2.2cm) accepts product as negative electrode with parallel stainless steel substrates, two anode-cathode distances are 20cm, applying voltage is that 12kV carries out Electrospun, will obtain so fiber arranged between two parallel stainless steel substrates of negative electrode.The control Electrospun spray silk time just can be controlled fiber arranged quantity.The parallel fibers that obtains is put into Muffle furnace together with stainless steel substrates, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained tin dioxide nano fiber diameter is about 130～200nm.
Polytetrafluoroethylsubstrate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting the tin dioxide nano fiber of arranging between two stainless steel substrates.Get the 50ml beaker, add successively 15ml ethylenediamine, 15ml deionized water, 0.5g butter of tin and 0.5g NaOH.After ultrasonic 15 minutes, this mixed solution is transferred in the reactor of 40ml with the polytetrafluoroethylene slice, thin piece that is attached with parallel tin dioxide nano fiber, placed 24 hours at 220 ℃, both obtained take tin dioxide nano fiber as trunk, take the material of nanometer tin dioxide rod as the accurate one dimension dendroid multilevel hierarchy of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is about 9.5cm
2/ Vs has good stability, and is similar to Example 1.
Embodiment 13:
Solution outfit, spinning process and sintering process are all consistent with embodiment 12.
Polytetrafluoroethylsubstrate substrate is cleaned up in ethanol, acetone and deionized water for ultrasonic successively, be used for collecting the tin dioxide nano fiber of arranging between two stainless steel substrates.Get the 50ml beaker, add successively 0.5g butter of tin, 0.7g NaOH, 20ml deionized water and 20ml ethanol, and ultrasonic 15 minutes.This mixed solution is transferred in the reactor of 40ml with the polytetrafluoroethylene slice, thin piece that is attached with parallel tin dioxide nano fiber, placed 24 hours at 180 ℃, namely obtain take tin dioxide nano fiber as trunk, take the material of nanometer tin dioxide rod as the accurate one dimension dendroid multilevel hierarchy of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 9cm
2/ Vs has good stability equally, and is similar to Example 1.
Embodiment 14:
The solution outfit is consistent with embodiment 12 with spinning process.Collect fiber arranged between two aluminium flakes with the quartz plate substrate that cleans up, and transfer in the Muffle furnace, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.
Get the 50ml beaker, add successively 15ml water, 15ml concentrated hydrochloric acid and 0.5g butyl titanate, the solution that stirs clarification, transfer to together with the quartz plate that is attached with parallel tin dioxide nano fiber in the hydrothermal reaction kettle of 40ml, in 150 ℃ of constant temperature ovens, placed 4 hours, take out quartz plate washing drying.Thereby obtain take tin dioxide nano fiber as trunk at the quartz plate substrate, take the nano material of rutile titanium dioxide nanometer rods as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 6.8cm
2/ Vs, the stability test result is similar to Example 1.
Embodiment 15:
Solution outfit, spinning process and sintering process are all consistent with embodiment 14.
Get the 50ml beaker, add successively 35ml deionized water, 0.104g zinc nitrate and 0.0522g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel tin dioxide nano fiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take tin dioxide nano fiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8cm
2/ Vs, stability better, and is similar to embodiment 8.
Embodiment 16:
Solution outfit, spinning process and sintering process are all consistent with embodiment 14.
Get the 50ml beaker, add successively 35ml deionized water, 0.2195g zinc acetate and 0.028g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel tin dioxide nano fiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take tin dioxide nano fiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8cm
2/ Vs, the stability of device better.
Embodiment 17:
In the 50ml conical flask, 0.8g polyvinylpyrrolidone (PVP) is added 2.2ml ethanol and 4.4mlN, in the dinethylformamide, stirring at room 8h clarifies fully to solution.
Other gets a 50ml conical flask, and the 0.4g butter of tin is added in the 2.2ml ethanol, and room temperature vigorous stirring 10min is to fully dissolving.Polymer Solution is mixed with inorganic salt solution, continue at room temperature to stir 1 hour.
Spinning process, sintering process and hydrothermal reaction process are consistent with embodiment 12.Thereby obtain take tin dioxide nano fiber as trunk at the teflon plate substrate, take the material of nanometer tin dioxide rod as the accurate one dimension dendroid multilevel hierarchy of branch.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is about 9.5cm
2/ Vs has good stability.
Embodiment 18:
In the 50ml conical flask, 0.8g polyvinylpyrrolidone (PVP) is added 2.2ml ethanol and 4.4mlN, in the dinethylformamide, stirring at room 8h clarifies fully to solution.
Other gets a 50ml conical flask, and the 0.4g butter of tin is added in the 2.2ml ethanol, and room temperature vigorous stirring 10min is to fully dissolving.Polymer Solution is mixed with inorganic salt solution, continue at room temperature to stir 1 hour.
Spinning process, spinning process and hydrothermal reaction process are consistent with embodiment 13.Thereby obtain take tin dioxide nano fiber as trunk at the teflon plate substrate, take the material of nanometer tin dioxide rod as the accurate one dimension dendroid multilevel hierarchy of branch.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 9cm
2/ Vs.
Embodiment 19:
In the 50ml conical flask, 0.8g polyvinylpyrrolidone (PVP) is added 2.2ml ethanol and 4.4mlN, in the dinethylformamide, stirring at room 8h clarifies fully to solution.
Other gets a 50ml conical flask, and the 0.4g butter of tin is added in the 2.2ml ethanol, and room temperature vigorous stirring 10min is to fully dissolving.Polymer Solution is mixed with inorganic salt solution, continue at room temperature to stir 1 hour.
Spinning process, spinning process and hydrothermal reaction process are consistent with embodiment 14.Thereby obtain take tin dioxide nano fiber as trunk at the quartz plate substrate, take the nano material of rutile titanium dioxide nanometer rods as the accurate one dimension dendroid multistage heterogeneous structure of branch.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 6.8cm
2/ Vs has good stability equally, and is similar such as embodiment 1.
Embodiment 20:
In the 50ml conical flask, 0.8g polyvinylpyrrolidone (PVP) is added 2.2ml ethanol and 4.4mlN, in the dinethylformamide, stirring at room 8h clarifies fully to solution.
Other gets a 50ml conical flask, and the 0.4g butter of tin is added in the 2.2ml ethanol, and room temperature vigorous stirring 10min is to fully dissolving.Polymer Solution is mixed with inorganic salt solution, continue at room temperature to stir 1 hour.
Spinning process, spinning process and hydrothermal reaction process are consistent with embodiment 15.Thereby obtain take tin dioxide nano fiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8cm
2/ Vs, stability better.
Embodiment 21:
In the 50ml conical flask, 0.8g polyvinylpyrrolidone (PVP) is added 2.2ml ethanol and 4.4mlN, in the dinethylformamide, stirring at room 8h clarifies fully to solution.
Other gets a 50ml conical flask, and the 0.4g butter of tin is added in the 2.2ml ethanol, and room temperature vigorous stirring 10min is to fully dissolving.Polymer Solution is mixed with inorganic salt solution, continue at room temperature to stir 1 hour.
Spinning process, spinning process and hydrothermal reaction process are consistent with embodiment 16.Thereby obtain take tin dioxide nano fiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multistage heterogeneous structure of branch.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 8cm
2/ Vs has preferably stability equally.
3. utilize the field-effect transistor of the dendroid multistage heterogeneous structure material of electrical spinning method and Hydrothermal Synthesis preparation take zinc oxide nano fiber as trunk
Embodiment 22:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 10ml absolute ethyl alcohol, dissolving is 8 hours under the dry room temperature, clarifies fully to solution.Other gets the 10ml conical flask, and the 0.595g zinc nitrate is dissolved in 4mlN, in the dinethylformamide, stirs 10 minutes under the room temperature to fully dissolving.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour to even.
The solution that mixes is put into the spray fiber tube, the internal diameter of spinning head is 1mm, (spacing 2.2cm) accepts product as negative electrode with parallel aluminium flake, two anode-cathode distances are 20cm, applying voltage is that 20kV carries out Electrospun, will obtain so fiber arranged between two parallel stainless steel substrates of negative electrode.The control Electrospun spray silk time just can be controlled fiber arranged quantity.Collect fiber arranged between two aluminium flakes with the quartz plate substrate that cleans up, and transfer in the Muffle furnace, slowly be warming up to 500 ℃ of constant temperature sintering 5 hours.
Get the 50ml beaker, add successively 35ml deionized water, 0.104g zinc nitrate and 0.0522g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel zinc oxide nano fiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take zinc oxide nano fiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multilevel hierarchy of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is about 10.45cm
2/ Vs, stability better.
Embodiment 23:
Solution outfit, spinning process and sintering process are all consistent with embodiment 22.
Get the 50ml beaker, add successively 35ml deionized water, 0.2195g zinc acetate and 0.028g hexamethylenetetramine, be stirred to the solution clarification, transfer to together with the quartz plate that is attached with parallel tin dioxide nano fiber in the hydrothermal reaction kettle of 40ml, in 95 ℃ of constant temperature ovens, placed 8 hours, take out quartz plate washing drying.Thereby obtain take zinc oxide nano fiber as trunk at the quartz plate substrate, take the nano material of zinc oxide nano rod as the accurate one dimension dendroid multilevel hierarchy of branch.
The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 10cm
2/ Vs, stability better.
Embodiment 24:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 10ml absolute ethyl alcohol, dissolving is 8 hours under the dry room temperature, clarifies fully to solution.Other gets the 10ml conical flask, and the 0.2726g zinc chloride is dissolved in 4mlN, in the dinethylformamide, stirs 10 minutes under the room temperature to fully dissolving.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour to even.
Spinning process, sintering process and water-heat process are consistent with embodiment 22.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 10cm
2/ Vs, stability better.
Embodiment 25:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 10ml absolute ethyl alcohol, dissolving is 8 hours under the dry room temperature, clarifies fully to solution.Other gets the 10ml conical flask, and the 0.2726g zinc chloride is dissolved in 4mlN, in the dinethylformamide, stirs 10 minutes under the room temperature to fully dissolving.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour to even.
Spinning process, sintering process and water-heat process are consistent with embodiment 23.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 10cm
2/ Vs, stability better.
Embodiment 26:
The outfit mass fraction is 8% polyvinyl alcohol water solution, and 95 ℃ were refluxed 5 hours, and were cooled to room temperature behind the dissolve complete.Other is equipped with mass fraction is 16.7% zinc acetate aqueous solution, is stirred to fully dissolving.Get this zinc acetate solution of 3g and dropwise add the 7.6g polyvinyl alcohol water solution, it is even to be stirred to solution.
Spinning process, sintering process and water-heat process are consistent with embodiment 22.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 10cm
2/ Vs, stability better.
Embodiment 27:
The outfit mass fraction is 8% polyvinyl alcohol water solution, and 95 ℃ were refluxed 5 hours, and were cooled to room temperature behind the dissolve complete.Other is equipped with mass fraction is 16.7% zinc acetate aqueous solution, is stirred to fully dissolving.Get this zinc acetate solution of 3g and dropwise add the 7.6g polyvinyl alcohol water solution, stir 12 hours even to solution.
Spinning process, sintering process and water-heat process are consistent with embodiment 23.The device assembling process is consistent with embodiment 1.This device maximum electron mobility is greater than 10cm
2/ Vs, stability better.
Claims (7)
1. method of constructing microelectronic component by the multistage heterogeneous structure nano material, it comprises the steps:
A. 0.3～1g soluble high-molecular compound is joined in 5～10ml solvent 1, be stirred to solution and clarify fully under ℃ condition of room temperature～100, then be cooled to room temperature, solvent 1 is one or more in DMF, ethanol, the water;
B. 0.2～2.0g soluble inorganic salt or solubility inorganic oxide precursor body are joined in 3～6ml solvent 2, vigorous stirring mixes it under the drying condition; Then the solution that obtains is joined in the solution of steps A fast, stirring mixes two kinds of solution, and solvent 2 is one or more in DMF, ethanol, acetic acid, the water;
C. the mixed solution that step B is obtained is put into the glass spray fiber tube of electrospinning device, the tube head internal diameter of glass spray fiber tube is 0.5～3mm, take the aluminium cover as anode, be that two parallel aluminum strips or the stainless steel strip of 2～3cm accepted product as minus plate with spacing, the distance of two interpolars is 10～30cm, the voltage that applies 6～30KV at two interpolars carries out Electrospun, thereby obtains the nanofiber that contains macromolecular compound be arranged in parallel at negative electrode;
D. with the quartz plate that cleans up the nanofiber that contains macromolecular compound between minus plate is collected, in air, placed 10～20 hours, then under 400～700 ℃ of temperature sintering 3～5 hours to remove macromolecular compound; Or directly minus plate and the nanofiber that contains macromolecular compound sintering under 400～700 ℃ of temperature are collected the inorganic oxide nanofiber with the quartz plate that cleans up or polytetrafluoroethylsubstrate substrate after 3～5 hours again; Thereby obtain the inorganic oxide nanofiber that is arranged in parallel of diameter 50～300nm in quartz plate or polytetrafluoroethylsubstrate substrate;
E. the solvent 3 of getting in addition 0.1～2.0g soluble inorganic salt or solubility inorganic oxide precursor body and 10～40ml mixes, in the system that the quartz plate that obtains among this solution and the step D or polytetrafluoroethylsubstrate substrate are transferred to hydrothermal reaction kettle, carry out hydro-thermal reaction, thereby a large amount of inorganic oxide nanometer rods of inorganic oxide nanofiber surface hydrothermal growth at step D, then it is dry to take out the substrate washing, namely obtains having the inorganic oxide nano material of accurate one dimension dendroid multistage heterogeneous structure at quartz plate or polytetrafluoroethylsubstrate substrate surface; Solvent 3 is one or more in ethanol, hydrochloric acid, the water;
F. the making of source, drain electrode: send quartz plate or polytetrafluoroethylsubstrate substrate that step e obtains to vacuum coating equipment, by with the mask plate aluminium electrode that evaporation 50～100nm is thick on the inorganic oxide nano material of the accurate one dimension dendroid multistage heterogeneous structure of substrate surface of source, drain electrode complementary structure, thereby formation source, drain electrode structure, distance between source, drain electrode is that channel width is 60～100 μ m, and the line of source, drain electrode is consistent with the direction of inorganic oxide nanofiber;
G. the preparation of gate electrode and gate insulation layer: select N-shaped＜100〉silicon chip, thickness is 1～2mm, resistivity is 3～5M Ω cm, adopts dry-oxygen oxidation method at this silicon chip SiO that grows
2Or the nitride gate insulating barrier, growth temperature is 900～1200 ℃, SiO
2Or the thickness of nitride gate insulating barrier is 1500～2000nm, then the surface had SiO
2Or the wafer dicing of nitride gate insulating barrier is the strip structure of wide 1～2mm and long 1～3cm, cleans also oven dry;
H. polyvinylpyrrolidone is mixed with into viscous fluid with deionized water, getting two droplet viscous fluids with the needle point of cleaning places evaporation that the quartz plate of aluminium electrode one side or the two ends of polytetrafluoroethylsubstrate substrate are arranged, line between two thickness drops and the direction of inorganic oxide nanofiber are perpendicular, the silicon chip of the strip structure for preparing among the step G is placed thickness drop top, and firmly it is compacted to SiO
2Or nitride gate insulating barrier and aluminium electrode securement, after the viscous fluid drying is solidified, prepare the inorganic semiconductor field-effect transistor.
2. a kind of method of constructing microelectronic component by the multistage heterogeneous structure nano material as claimed in claim 1, it is characterized in that: the soluble high-molecular compound is polyvinyl alcohol, polyvinylpyrrolidone or polyacrylonitrile.
3. a kind of method of constructing microelectronic component by the multistage heterogeneous structure nano material as claimed in claim 1, it is characterized in that: soluble inorganic salt is soluble zinc salt or solubility pink salt, and solubility inorganic oxide precursor body is the soluble titanium dioxide presoma.
4. a kind of method of constructing microelectronic component by the multistage heterogeneous structure nano material as claimed in claim 3, it is characterized in that: soluble zinc salt is zinc acetate, zinc nitrate or zinc chloride, the solubility pink salt is butter of tin or stannous chloride, and the soluble titanium dioxide presoma is butyl titanate, isopropyl titanate or titanium tetrachloride.
5. a kind of method of constructing microelectronic component by the multistage heterogeneous structure nano material as claimed in claim 1, it is characterized in that: when the inorganic oxide nanometer rods of the inorganic oxide nanofiber surface of step D hydrothermal growth is zinc oxide, the substrate quartz plate, hydrothermal system is the mixed solution of soluble zinc salt, hexamethylenetetramine and water, wherein zinc salt concentration is 0.01～0.04mol/L, hexamethylenetetramine concentration is 0.005～0.01mol/L, and hydrothermal condition is 80～100 ℃ of reactions 1～8 hour.
6. a kind of method of constructing microelectronic component by the multistage heterogeneous structure nano material as claimed in claim 1, it is characterized in that: when the inorganic oxide nanometer rods of the inorganic oxide nanofiber surface of step D hydrothermal growth is tin ash, the substrate polytetrafluoroethylene; Hydrothermal system is the mixed solution of solubility pink salt, NaOH, water and ethanol, or is the mixed solution of solubility pink salt, NaOH, water and ethylenediamine, and wherein water mixes with the ethylenediamine equal-volume with ethanol or water; Pink salt concentration is 0.04～0.07mol/L, and naoh concentration is 0.31～0.44mol/L, and hydrothermal condition is 180～250 ℃ of reactions 1～48 hour.
7. a kind of method of constructing microelectronic component by the multistage heterogeneous structure nano material as claimed in claim 1, it is characterized in that: when the inorganic oxide nanometer rods at the inorganic oxide nanofiber surface of step D hydrothermal growth is titanium dioxide, the substrate quartz plate, hydrothermal system is soluble titanium dioxide presoma, water and hydrochloric acid, wherein water mixes with the hydrochloric acid equal-volume, TiO 2 precursor concentration is 0.01～0.05mol/L, and hydrothermal condition is 100～200 ℃ of reactions 1～5 hour.
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