CN103496675A - Tellurium nanowire array with field emission characteristic and preparation method as well as application thereof - Google Patents
Tellurium nanowire array with field emission characteristic and preparation method as well as application thereof Download PDFInfo
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Abstract
The invention discloses a tellurium nanowire array with field emission characteristic and a preparation method as well as application thereof. The tellurium nanowire array is provided with a sharp port, and the field emission starting electric field intensity of the tellurium nanowire array is low. According to the preparation method, tellurium is used as an evaporation source and tellurium nanowires are deposited on silicon wafers to obtain the tellurium nanowire array through a physical vapor deposition method. The preparation method has the characteristics of simple experimental equipment and steps, environmental friendliness and the like and does not involve complicated chemical reactions. The tellurium nanowire array has superior stability and can be widely applied to cold cathodes of field emission devices, field emission flat panel displays and/or vacuum microelectronic devices.
Description
Technical field
The present invention relates to the nano-wire array technical field, relate in particular to a kind of tellurium nano-wire array, its preparation method and application with field emission characteristic.
Background technology
Field emmision material has very important purposes in fields such as field emission planar demonstration, electron radiation device and vacuum microelectronic devices.Conductor nano tube/linear array has larger length-to-diameter ratio, higher electric conductivity and less work function, thereby is considered to a kind of field emmision material of excellence.
At present, the preparation that investigators are successful SiO
2(Chinese invention patent application publication No. CN102856141A), ZnO(Adv.Funct.Mater.2009,19,3165-3172), ZnS(Nanoscale2012,4,2658) and CdS(ACS Nano2009,3, the conductor nano tube/linear array such as 949-959), and studied their field emission characteristic.
The disclosed in-situ oxidation of Chinese invention patent application publication No. CN 102856141 A improves the method for silicon nanowire array field emission performance, employing prepares the Si nano-wire array without electrochemical erosion method, then adopts the original position partial oxidation process that the Si nano-wire array is converted into to SiO
xthe Si nanowire core shell structure array coated, due to SiO
xthere is lower electron affinity (0.6-0.8eV), thus the field emission performance of Si nano-wire array can effectively be strengthened, and SiO
xalso can be used as the protective layer of Si nano-wire array, improve the field emission stability of Si nano-wire array.Strength of electric field general 4.0～7.6 is opened in the field emission of the silicon nanowire array that the method makes.
Chinese invention patent application publication No. CN 102476787 A disclose a kind of preparation method of ZnO nanowire array, comprise the steps: to clean substrate; Prepare one deck Zn rete on the surface of cleaning substrate later; The substrate that is prepared with the Zn rete is placed in to 400～800 ℃ of lower thermal treatment 15min～24h, cooling, make ZnO nanowire array.The field emission of the ZnO nanowire array that the method makes is opened strength of electric field probably 3.2～3.5.
Although this area can provide the low nano-wire array of opening strength of electric field at present, the raw material for preparing at present nano-wire array is also more limited, and this area expects that multipotency more enough is applied to prepare the research of the raw material of nano-wire array.
Chinese invention patent application publication No. CN 102910595 A disclose a kind of preparation in macroscopic quantity method of ultra-fine tellurium nano-wire, comprise the following steps: sodium tellurite and reductive agent react under the effect of polyvinylpyrrolidone pH value conditioning agent, obtain reaction mixture; With cold water rapidly cooling described reaction mixture obtain the tellurium nano-wire mother liquor, obtain tellurium nano-wire after solubilizing agent extracts.Tellurium nano-wire quality homogeneous prepared by the method, the tellurium nano-wire diameter is 7～10nm, length is microns up to a hundred, but one time to produce obtains the tellurium nano-wire of 50g.But this application does not specifically disclose its tellurium nano-wire prepared and is obvious array structure, and strength of electric field is opened in unexposed corresponding emission.And the method is Wet Method Reaction, the technique relative complex.
Chinese invention patent application publication No. CN 101435067 A disclose a kind of preparation method of the tellurium nano-wire array based on physical vapor deposition, by the size of adjusting AC power output voltage and the distance of glass substrate and tungsten boat, in vacuum chamber, by thermal evaporation tellurium raw material, directly deposit the film with tellurium nano-wire array structure on glass substrate, the method can guarantee being uniformly distributed of nanophase.But the information such as strength of electric field are opened in the field emission of this application unexposed tellurium nano-wire array.
It is still too high that strength of electric field is opened in the field emission of conductor nano tube/linear array prepared by prior art, and part nano-wire array building-up process relates to complicated chemical reaction process.Research shows that the top pattern of one-dimensional nano line array has very important impact to its field emission characteristic, such as due to most advanced and sophisticated local fields effect, the conical tip nano-wire array can reduce the intensity (Nanotechnology2010,21,225707) of opening electric field significantly.Therefore, developing the one-dimensional nano line array with special tip is of great significance for improving its field emission performance tool.
Summary of the invention
One of purpose of the present invention is to provide a kind of tellurium nano-wire array with field emission characteristic, and its emission unlatching strength of electric field is lower, has excellent stability.
Tellurium nano-wire array with field emission characteristic provided by the invention has sharp-pointed port.Preferably, it is conical or cylindrical that the top of described tellurium nano-wire array is, perhaps described tellurium nano-wire array is comprised of conical tellurium nano-wire that (it is conical to be that every tellurium nano-wire is as a whole, numerous such tellurium nano-wires rearrange tellurium nano-wire array, the top of this tellurium nano-wire array is very sharp-pointed, can be called " needle point shape tip ", therefore this tellurium nano-wire array also can be called " tellurium nano-wire array that top is needle point shape ").Above-mentioned is only three kinds of forms of sharp-pointed port, and sharp-pointed port of the present invention is not limited to these three kinds, such as top can also be to be sexangle.
Preferably, the unlatching strength of electric field of described tellurium nano-wire array is 3.27～6.67V/ μ m, preferably 3.27～3.71V/ μ m.
As preferably, described tellurium nano-wire array by the physical vapor precipitator method, take tellurium as evaporation source and on silicon chip the deposition tellurium nano-wire obtain.
Two of purpose of the present invention is to provide the above-mentioned preparation method with tellurium nano-wire array of field emission characteristic, and its experimental installation and step are simple, and does not relate to complex chemical reaction.
Preparation method provided by the invention, for by the physical vapor precipitator method, be take tellurium as evaporation source, and the deposition tellurium nano-wire obtains described tellurium nano-wire array on silicon chip.
In preparation method of the present invention, by controlling temperature, base reservoir temperature and the depositing time of tellurium evaporation source in the physical vapor precipitation process, can obtain the tellurium nano-wire array with sharp-pointed port; Particularly, it is conical or cylindrical that the top of described tellurium nano-wire array is, or described tellurium nano-wire array is comprised of conical tellurium nano-wire.Preparation method of the present invention has experimental installation and step is simple, does not relate to complex chemical reaction, has the characteristics such as environment friendly.The field emission unlatching strength of electric field of the tellurium nano-wire array that preparation method of the present invention makes is lower, has excellent stability.
Preparation method of the present invention can comprise the steps:
(1) the tellurium powder is placed in to tube furnace central authorities as evaporation source, clean silicon chip is placed in to the tube furnace downstream as deposition substrate;
(2) heated Tube-furnace, to the evaporation source temperature, at 700～800 ℃, the deposition substrate temperature, at 300～450 ℃, under the mixed gas atmosphere of rare gas element and hydrogen, is carried out 60～70min, grows described tellurium nano-wire array.
In preparation method of the present invention, described silicon chip can be p-type silicon chip or N-shaped silicon chip.
Preferably, the surface that described silicon chip exposes is (111) crystal face, (100) crystal face or (110) crystal face, preferably (111) crystal face.
Preferably, described silicon chip is the silicon chip of removing surface silica dioxide.
Preferably, the method for described silicon chip removal surface silica dioxide is to use the hydrofluoric acid pickling.Hydrofluoric acid be unique can with the acid of silicon dioxde reaction, in its cleaning to heavily doped silicon, important application is arranged.Heavily doped silicon refers to and mixes the more semiconductor silicon single crystal of impurity level, can effectively remove the impurity such as silicon-dioxide by the hydrofluoric acid pickling.The concentration of hydrofluoric acid solution used is not particularly limited, but the hydrofluoric acid solution that preferred mass concentration is 47～51% is cleaned.
Preferably, after the pickling of described use hydrofluoric acid, described silicon chip is placed in to spirituous solution and carries out supersound process, then with distilled water, clean, and dry up and obtain clean silicon chip with nitrogen, standby.
Preferably, the described supersound process time is 1～10min, for example 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, preferably 10min.
In preparation method of the present invention, the purity of described tellurium powder is more than 99%, for example 99.01%, 99.10%, 99.20%, 99.50%, 99.90%, 99.95%, 99.98%, 99.99%, 99.991%, 99.995% or 99.999%, preferably more than 99.9%, more preferably more than 99.99%.
Preferably, before heating, tube furnace is evacuated, makes intraductal pressure remain on 1～4pa.
Preferably, after vacuumizing, continue to pass into rare gas element, thoroughly to remove residual oxygen in pipe.
Preferably, described rare gas element is one or more the mixing in nitrogen, argon gas, helium and neon.Described mixing typical case but the example of indefiniteness comprise: the mixing of nitrogen and argon gas, the mixing of argon gas and helium, the mixing of helium and neon, the mixing of nitrogen and helium, the mixing of nitrogen and neon, the mixing of nitrogen, argon gas and helium, the mixing of argon gas, helium and neon, the mixing of nitrogen, argon gas, helium and neon.
Preferably, continue to pass into rare gas element 5～60min, for example 6min, 9min, 10min, 15min, 20min, 25min, 30min, 40min, 50min, 55min or 59min, preferably 15～30min.
Preferably, the flow velocity of described rare gas element is 50～150sccm(standard-state cubic centimeter per minute, mark condition milliliter per minute), for example 60sccm, 70sccm, 80sccm, 90sccm, 110sccm, 120sccm, 130sccm or 140sccm, preferably 100sccm.
In preparation method of the present invention, the heating rate of described step (2) is 5～30 ℃/min, for example 6 ℃/min, 9 ℃/min, 11 ℃/min, 15 ℃/min, 18 ℃/min, 21 ℃/min, 25 ℃/min or 29 ℃/min, preferably 15 ℃/min.
Preferably, 700～800 ℃ of the evaporation source temperature of described step (2), for example 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃, 760 ℃, 770 ℃, 780 ℃ or 790 ℃, preferably 700 ℃ or 800 ℃.
Preferably, 300～450 ℃ of the deposition substrate temperature of described step (2), for example 310 ℃, 320 ℃, 330 ℃, 340 ℃, 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃, 420 ℃, 430 ℃ or 440 ℃, preferably 360 ℃ or 400 ℃.
Preferably, the growth time 60～70min of described step (2), for example, 61min, 62min, 63min, 64min, 65min, 66min, 67min, 68min or 69min.
Preferably, the rare gas element of described step (2) is one or more the mixing in nitrogen, argon gas, helium and neon.Described mixing typical case but the example of indefiniteness comprise: the mixing of nitrogen and argon gas, the mixing of argon gas and helium, the mixing of helium and neon, the mixing of nitrogen and helium, the mixing of nitrogen and neon, the mixing of nitrogen, argon gas and helium, the mixing of argon gas, helium and neon, the mixing of nitrogen, argon gas, helium and neon.
Preferably, the rare gas element of described step (2) and the airshed of hydrogen ratio are 10:1～2:2, for example 10:1,9:1,8:1,7:1,6:1,5:1,4:1,3:1 or 2:1, preferably 4:1.
Preferably, the rare gas element of described step (2) and the flow velocity of hydrogen are 10～40sccm, for example 15sccm, 20sccm, 25sccm, 30sccm, 35sccm or 40sccm, preferably 25sccm.
Preferably, described step (2) afterwards, is cooled to room temperature.
Preferably, the described naturally cooling that is cooled to.
In preparation method of the present invention, when the temperature of tellurium evaporation source is 690～710 ℃, preferably 700 ℃, base reservoir temperature is 350～370 ℃, preferably 360 ℃, and growth time is 60～80min, preferably during 70min, and it is conical that gained tellurium nano-wire array top is.
In preparation method of the present invention, when the temperature of tellurium evaporation source is 790～810 ℃, preferably 800 ℃, base reservoir temperature is 390～410 ℃, preferably 400 ℃, and when growth time is 50～70min, preferred 60min, the gained tellurium nano-wire array is comprised of conical tellurium nano-wire.
In preparation method of the present invention, when the temperature of tellurium evaporation source is 690～710 ℃, preferably 700 ℃, base reservoir temperature is 390～410 ℃, preferably 400 ℃, and growth time is 50～70min, preferably during 60min, and gained tellurium nano-wire array top is cylindrical.
A kind of preferred version of preparation method of the present invention comprises the steps:
(1 ') is placed in the hydrofluoric acid solution pickling by heavily doped p-type silicon chip, to remove surperficial silicon-dioxide;
(2 ') is placed in spirituous solution by the silicon chip after cleaning in step (1 ') and carries out supersound process 1～10min, then with distilled water, cleans, and dries up standby with nitrogen;
(3 ') is that tellurium powder more than 99.99% is placed in the tube furnace middle section as evaporation source using purity, the silicon chip after clean in step (2 ') is placed in to the tube furnace downstream area, as deposition substrate;
Before (4 ') heating, tube furnace is evacuated, intraductal pressure remains on 1～4pa;
(5 ') flow velocity with 50～150sccm passes into argon gas 15～30min, thoroughly to remove residual oxygen in pipe;
(6 ') is heated to 700～800 ℃ by the tube furnace middle section, and heating rate is 5～30 ℃/min, and the temperature at the bottom of silicon wafer-based remains on 300～450 ℃, passes into the mixed gas of argon gas and hydrogen simultaneously;
(7 ') keeps step (6 ') middle heat-up time of 60～70min, then closes well heater, naturally cools to room temperature, obtains described tellurium nano-wire array.
Three of purpose of the present invention is to provide the above-mentioned application of the tellurium nano-wire array of field emission characteristic in cold cathode, field emission displays and/or the vacuum microelectronic device of feds that have.
With other field emmision material and preparation method thereof, compare, the present invention has following beneficial effect:
(1) the physical vapor precipitator method that the present invention uses have experimental installation and step is simple, do not relate to complex chemical reaction, have the characteristics such as environment friendly;
(2) the field emission characteristic excellence of tellurium nano-wire array provided by the invention; Open electric field ratio ZnO, SnO
2, GeSe and Bi
2se
3little Deng conductor nano tube/linear array;
(3) method for preparing tellurium nano-wire array provided by the invention, can regulate and control by temperature, base reservoir temperature (depositing temperature) and the depositing time of regulation and control tellurium evaporation source the port pattern of tellurium nano-wire array, thus accurate controlling field emission characteristic (opening strength of electric field and enhancement factorβ);
(4) tellurium nano-wire array provided by the invention has excellent stability, can be widely used in cold cathode, field emission displays and/or the vacuum microelectronic device of feds.
The accompanying drawing explanation
Fig. 1 is that in the embodiment of the present invention 1, top is conical tellurium nano-wire array Electronic Speculum figure;
Fig. 2 is the tellurium nano-wire array Electronic Speculum figure be comprised of conical tellurium nano-wire in the embodiment of the present invention 2;
Fig. 3 is that in the embodiment of the present invention 3, top is columniform tellurium nano-wire array Electronic Speculum figure;
Fig. 4 is that in the embodiment of the present invention 4, top has the more tellurium nano-wire array Electronic Speculum figure of dense circular cylinder shape;
Fig. 5 is that in the embodiment of the present invention 5, top is hexagonal tellurium nano-wire array Electronic Speculum figure;
Fig. 6 be in the embodiment of the present invention 1,2 and 3 top be conical tellurium nano-wire array (1), the tellurium nano-wire array (2) that formed by conical tellurium nano-wire and the top field emission J that is columniform tellurium nano-wire array (3) and the graph of relation of electric field strength E;
Fig. 7 be in the embodiment of the present invention 1,2 and 3 top be conical tellurium nano-wire array (1), the tellurium nano-wire array (2) that formed by conical tellurium nano-wire and the top field emission FN graphic representation that is columniform tellurium nano-wire array (3);
Fig. 8 is the field emission stability graphic representation that in the embodiment of the present invention 1 and 2, top is conical tellurium nano-wire array (1) and the tellurium nano-wire array (2) that is comprised of conical tellurium nano-wire.
Embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail.It will be understood to those of skill in the art that following examples are only the preferred embodiments of the present invention, so that understand better the present invention, thereby should not be considered as limiting scope of the present invention.For a person skilled in the art, the present invention can have various modifications and variations, within the spirit and principles in the present invention all, any modification of doing, is equal to and replaces or improvement etc., within all should being included in protection scope of the present invention.
(1) heavily doped p-type Si sheet (1cm * 1cm) is placed in to hydrofluoric acid solution (mass concentration 47～51%) pickling, to remove surperficial silicon-dioxide.
(2) the Si sheet after cleaning in step (1) is positioned in spirituous solution, ultrasonic clean with distilled water afterwards, and with nitrogen, dry up standbyly, ultrasonic time is chosen for 5min.
(3) the tellurium powder that is 99.99% using purity is placed on the tube furnace middle section as evaporation source, the Si sheet after clean in step (2) is placed in to the downstream area of tube furnace.
(4) before the heating, tube furnace is evacuated, intraductal pressure remains on 1pa.
(5) step (4) and then, pass into the argon gas 30min of 100sccm, thoroughly to remove residual oxygen in pipe.
(6) the tube furnace central zone is heated to 700 ℃, 15 ℃/min of heating rate, the temperature of Si substrate remains on 360 ℃; Pass into argon gas and hydrogen gas mixture 25sccm, the airshed of argon gas and hydrogen is than being 4:1 simultaneously.
(7) keeping step (6) heat-up time is 70min, closes subsequently well heater, naturally cools to room temperature.The tellurium nano-wire array top now obtained is conical, as shown in Figure 1.
(8) be that conical tellurium nano-wire array carries out the field emission characteristic test to the top obtained in step (7), can see that by the J-E curve its unlatching strength of electric field is 3.27V/ μ m, as shown in Fig. 6 curve (1); Fig. 7 curve (1) shows that the field emission characteristic that top is conical tellurium nano-wire array meets the FN curve, and calculating enhancement factorβ is 3270; Fig. 8 curve (1) shows that the field emission performance that top is conical tellurium nano-wire array is stable.
The calculating of enhancement factorβ belongs to general knowledge known in this field.Particularly, enhancement factorβ can calculate by following formula:
ln(J/E
2)＝ln(Aβ
2/φ)-Bφ
-3/2/βE；
Wherein, J is current density, and E is the strength of electric field applied, and A and B are constant, and its value is respectively 1.56 * 10
-10a V
-2eV and 6.83 * 10
3v eV
-3/2μ m
-1, the work function that Φ is material, the work function of tellurium is 4.95eV, β is enhancement factor.
The tellurium nano-wire array that embodiment 2 preparations are comprised of conical tellurium nano-wire
The difference of the present embodiment and embodiment 1 is: in step (6), the tube furnace central zone is heated to 800 ℃, the temperature of Si substrate remains on 400 ℃; In step (7), be 60min heat-up time.Now obtain the tellurium nano-wire array formed by conical tellurium nano-wire, as shown in Figure 2; In step (8), the unlatching electric field that records the tellurium nano-wire array be comprised of conical tellurium nano-wire is 3.71V/ μ m, as shown in Fig. 6 curve (2); Fig. 7 curve (2) shows that the field emission characteristic of the tellurium nano-wire array that is comprised of conical tellurium nano-wire meets the FN curve, and calculating enhancement factorβ is 2785; Fig. 8 curve (2) shows that the field emission performance of the tellurium nano-wire array that is comprised of conical tellurium nano-wire is stable.
The difference of the present embodiment and embodiment 1 is: in step (6), the tube furnace central zone is heated to 700 ℃, the temperature of Si substrate remains on 400 ℃; In step (7), be 60min heat-up time.Now obtaining top is columniform tellurium nano-wire array, as shown in Figure 3; In step (8), the unlatching electric field that to record top be columniform tellurium nano-wire array is 6.67V/ μ m, as shown in Fig. 6 curve (3); Fig. 7 curve (3) shows that the field emission characteristic that top is columniform tellurium nano-wire array meets the FN curve, and calculating enhancement factorβ is 1446.
By the field emission characteristic (opening strength of electric field and enhancement factorβ) of comparing embodiment 1,2 and 3 three kinds of tellurium nano-wire arrays that obtain, can find out that the field emission characteristic that top is conical tellurium nano-wire array is best.
The difference of the present embodiment and embodiment 1 is: in step (6), the tube furnace central zone is heated to 700 ℃, the temperature of Si substrate remains on 380 ℃; In step (7), be 60min heat-up time.Now obtaining top is columniform tellurium nano-wire array, as shown in Figure 4; In step (8), the unlatching electric field that to record top be columniform tellurium nano-wire array is 7.56V/ μ m; The field emission characteristic that top is columniform tellurium nano-wire array meets the FN curve, and calculating enhancement factorβ is 479.The top that the present embodiment makes is the more encryption that columniform tellurium nano-wire array makes than embodiment 3.
The difference of the present embodiment and embodiment 1 is: in step (6), the tube furnace central zone is heated to 800 ℃, the temperature of Si substrate remains on 300 ℃; In step (7), be 60min heat-up time.Now obtaining top is hexagonal tellurium nano-wire array, as shown in Figure 5; In step (8), the unlatching electric field that to record top be hexagonal tellurium nano-wire array is 9.8V/ μ m; The field emission characteristic that top is hexagonal tellurium nano-wire array meets the FN curve, and calculating enhancement factorβ is 508.
Applicant's statement, the present invention illustrates detailed features of the present invention and detailed method by above-described embodiment, but the present invention is not limited to above-mentioned detailed features and detailed method, do not mean that the present invention must rely on above-mentioned detailed features and detailed method could be implemented.The person of ordinary skill in the field should understand, any improvement in the present invention is selected the interpolation of the equivalence replacement of component and ancillary component, the selection of concrete mode etc. to the present invention, within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. the tellurium nano-wire array with field emission characteristic, is characterized in that, described tellurium nano-wire array has sharp-pointed port;
Preferably, it is conical or cylindrical that the top of described tellurium nano-wire array is, or described tellurium nano-wire array is comprised of conical tellurium nano-wire;
Preferably, the unlatching strength of electric field of described tellurium nano-wire array is 3.27～6.67V/ μ m, preferably 3.27～3.71V/ μ m.
2. tellurium nano-wire array according to claim 1, is characterized in that, described tellurium nano-wire array deposits tellurium nano-wire as evaporation source and on silicon chip and obtains by the physical vapor precipitator method, the tellurium of take.
3. the preparation method of a tellurium nano-wire array as claimed in claim 1 or 2, is characterized in that, described method, for by the physical vapor precipitator method, be take tellurium as evaporation source, and the deposition tellurium nano-wire obtains described tellurium nano-wire array on silicon chip.
4. preparation method according to claim 3, is characterized in that, described method comprises the steps:
(1) the tellurium powder is placed in to tube furnace central authorities as evaporation source, clean silicon chip is placed in to the tube furnace downstream as deposition substrate;
(2) heated Tube-furnace, to the evaporation source temperature, at 700～800 ℃, the deposition substrate temperature, at 300～450 ℃, under the mixed gas atmosphere of rare gas element and hydrogen, is carried out 60～70min, grows described tellurium nano-wire array.
5. preparation method according to claim 4, is characterized in that, described silicon chip is the p-type silicon chip;
Preferably, the surface that described silicon chip exposes is (111) crystal face;
Preferably, described silicon chip is the silicon chip of removing surface silica dioxide;
Preferably, the method for described silicon chip removal surface silica dioxide is to use the hydrofluoric acid pickling;
Preferably, after the pickling of described use hydrofluoric acid, described silicon chip is placed in to spirituous solution and carries out supersound process, then with distilled water, clean, and dry up and obtain clean silicon chip with nitrogen, standby;
Preferably, the described supersound process time is 1～10min, preferred 10min.
6. according to the described preparation method of claim 4 or 5, it is characterized in that, the purity of described tellurium powder is more than 99%, preferably more than 99.9%, more preferably more than 99.99%;
Preferably, before heating, tube furnace is evacuated, makes intraductal pressure remain on 1～4pa;
Preferably, after vacuumizing, continue to pass into rare gas element, thoroughly to remove residual oxygen in pipe;
Preferably, described rare gas element is one or more the mixing in nitrogen, argon gas, helium and neon;
Preferably, continue to pass into rare gas element 5～60min, preferred 15～30min;
Preferably, the flow velocity of described rare gas element is 50～150sccm, preferred 100sccm.
7. according to the described preparation method of claim 4 to 6 any one, it is characterized in that, the heating rate of described step (2) is 5～30 ℃/min, preferred 15 ℃/min;
Preferably, the rare gas element of described step (2) is one or more the mixing in nitrogen, argon gas, helium and neon;
Preferably, the airshed of the rare gas element of described step (2) and hydrogen is than being 10:1～2:2, preferred 4:1;
Preferably, the flow velocity of the rare gas element of described step (2) and hydrogen is 10～40sccm, preferred 25sccm;
Preferably, described step (2) afterwards, is cooled to room temperature;
Preferably, the described naturally cooling that is cooled to.
8. according to the described preparation method of claim 4 to 7 any one, it is characterized in that, when the temperature of tellurium evaporation source is 690～710 ℃, preferably 700 ℃, base reservoir temperature is 350～370 ℃, preferably 360 ℃, when growth time is 60～80min, preferred 70min, it is conical that gained tellurium nano-wire array top is; Or
When the temperature of tellurium evaporation source is 790～810 ℃, preferably 800 ℃, base reservoir temperature is 390～410 ℃, preferably 400 ℃, and growth time is 50～70min, preferably during 60min, and the gained tellurium nano-wire array is comprised of conical tellurium nano-wire; Or
When the temperature of tellurium evaporation source is 690～710 ℃, preferably 700 ℃, base reservoir temperature is 390～410 ℃, preferably 400 ℃, and growth time is 50～70min, preferably during 60min, and gained tellurium nano-wire array top is cylindrical.
9. according to the described preparation method of claim 4 to 8 any one, it is characterized in that, described method comprises the steps:
(1 ') is placed in the hydrofluoric acid solution pickling by heavily doped p-type silicon chip, to remove surperficial silicon-dioxide;
(2 ') is placed in spirituous solution by the silicon chip after cleaning in step (1 ') and carries out supersound process 1～10min, then with distilled water, cleans, and dries up standby with nitrogen;
(3 ') is that tellurium powder more than 99.99% is placed in the tube furnace middle section as evaporation source using purity, the silicon chip after clean in step (2 ') is placed in to the tube furnace downstream area, as deposition substrate;
Before (4 ') heating, tube furnace is evacuated, intraductal pressure remains on 1～4pa;
(5 ') flow velocity with 50～150sccm passes into argon gas 15～30min, thoroughly to remove residual oxygen in pipe;
(6 ') is heated to 700～800 ℃ by the tube furnace middle section, and heating rate is 5～30 ℃/min, and the temperature at the bottom of silicon wafer-based remains on 300～450 ℃, passes into the mixed gas of argon gas and hydrogen simultaneously;
(7 ') keeps step (6 ') middle heat-up time of 60～70min, then closes well heater, naturally cools to room temperature, obtains described tellurium nano-wire array.
10. the application of tellurium nano-wire array as claimed in claim 1 or 2 in cold cathode, field emission displays and/or the vacuum microelectronic device of feds.
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|---|---|---|---|
| CN201310436069.4A CN103496675A (en) | 2013-09-23 | 2013-09-23 | Tellurium nanowire array with field emission characteristic and preparation method as well as application thereof |
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Cited By (3)
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| CN109368605A (en) * | 2018-11-01 | 2019-02-22 | 西北大学 | A kind of preparation method of tellurium nano-wire material, tellurium nano-wire material and device |
| CN114032510A (en) * | 2021-11-17 | 2022-02-11 | 中国科学院半导体研究所 | Growth method of tellurium nanowire vertical array |
| CN115465843A (en) * | 2022-10-10 | 2022-12-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tellurium nanoribbon array and preparation method thereof |
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| CN101435067A (en) * | 2008-12-01 | 2009-05-20 | 北京航空航天大学 | Preparation of tellurium nano-wire array based on physical vapour deposition |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109368605A (en) * | 2018-11-01 | 2019-02-22 | 西北大学 | A kind of preparation method of tellurium nano-wire material, tellurium nano-wire material and device |
| CN109368605B (en) * | 2018-11-01 | 2021-10-19 | 西北大学 | Preparation method of tellurium nanowire material, tellurium nanowire material and device |
| CN114032510A (en) * | 2021-11-17 | 2022-02-11 | 中国科学院半导体研究所 | Growth method of tellurium nanowire vertical array |
| CN115465843A (en) * | 2022-10-10 | 2022-12-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tellurium nanoribbon array and preparation method thereof |
| CN115465843B (en) * | 2022-10-10 | 2023-11-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tellurium nanoribbon array and preparation method thereof |
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