CN103950889B - The excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance - Google Patents
The excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance Download PDFInfo
- Publication number
- CN103950889B CN103950889B CN201410193257.3A CN201410193257A CN103950889B CN 103950889 B CN103950889 B CN 103950889B CN 201410193257 A CN201410193257 A CN 201410193257A CN 103950889 B CN103950889 B CN 103950889B
- Authority
- CN
- China
- Prior art keywords
- silicon
- bead
- nanowire array
- silver
- silicon nanowire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 78
- 239000010703 silicon Substances 0.000 title claims abstract description 78
- 239000002070 nanowire Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011324 bead Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 239000002356 single layer Substances 0.000 claims abstract description 11
- 238000005260 corrosion Methods 0.000 claims abstract description 9
- 230000007797 corrosion Effects 0.000 claims abstract description 9
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 238000001020 plasma etching Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000005566 electron beam evaporation Methods 0.000 claims abstract description 6
- 239000005357 flat glass Substances 0.000 claims description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000010410 layer Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 230000003247 decreasing effect Effects 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000010365 information processing Effects 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Cold Cathode And The Manufacture (AREA)
Abstract
The invention discloses the excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance belonging to Flied emission technical field.The method arrange first on a silicon substrate packed mono-layer PS bead and reactive ion etching process is carried out to it, then adopt electron beam evaporation silver-plated, after removing PS bead, then silver-colored catalyzed corrosion carried out in substrate, obtain the silicon nanowire array that diameter is larger; By dry oxidation process, silicon nanowires is become cutting-edge structure again, and reduce silicon nanowires diameter further, increase nano wire spacing.The cuspidated silicon nanowire array of tool prepared by the inventive method, has excellent field emission performance; Its cut-in voltage is 1.8V/ μm, and current stability is better; Meanwhile, silicon nanowires monocrystalline is functional, can at larger area rule solid matter, and draw ratio controllability is stronger.This method cost is low, productive rate is high, Modulatory character is good, thus can be applied in the production of silica-based field electron transmitting device.
Description
Technical field
The invention belongs to Flied emission technical field, particularly the excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance.
Background technology
Silicon is the of paramount importance semiconductor of electronic information technical field; The oxide of silicon and silicon and nitride are due to rich content in the earth, and low in raw material price, mature preparation process, obtains and apply very widely in electrical interconnection integrated circuit.Since half a century, microelectronic technology obtains deep development, has become the core technology of calculating, communication, the automatically field such as control and information processing.Silicon nanowires, as the important One, Dimensional Semiconductor Nano Materials of a class, has good application prospect in nano-device.Meanwhile, silicon nanowires has stable semiconducting behavior, and can be mutually compatible with modern semiconductor technology.Because nano material has unique character such as small-size effect, skin effect, quantum size effect and quantum tunneling effect, thus make it have the excellent physical and chemical performance that bulk material do not have.
Silicon nanowires has excellent field emission characteristic, has broad application prospects in microelectronic vacuum and feds field; Can be used for the nano electron devices such as preparation high performance field effect transistors (FET), single electron detector and Field Emission Display.The nano wire of regular arrangement that obtains of directly etching, has higher field enhancement factor, and is convenient to follow-up assembling, have potential application prospect in structural unit and nano electron device, have higher using value in feds on a silicon substrate.
Along with silicon nanowires synthesis, assembling and the continuous maturation of measuring technique, its large-scale integrated at nano-device will be realized.But should see, silicon nanowires the aspect such as to be prepared from macroscopic view preparation, electrical performance stability, assembling and performance test, device and also be there is still an open question simultaneously.At present, silicon nanowires nano electron device rests on the laboratory research stage mostly, and its repeatability is poor, and the large-scale integrated from nano-device also has sizable distance.
Summary of the invention
The object of this invention is to provide that a kind of field emission performance is excellent, the preparation method of the bulk silicon nano-wire array with cutting-edge structure.
Technical scheme of the present invention is as follows:
The excellent preparation method with the silicon nanowire array of cutting-edge structure of field emission performance, comprises the following steps:
(1) clean silicon base and carry out hydrophilic treated;
(2) diameter of packed mono-layer of arranging on a silicon substrate is the PS bead of 960-1000nm;
(3) using the oxygen of flow 40-60SCCM as reacting gas, at pressure 2Pa, under the condition of power 30-50W, the little ball array of PS of preparation in step 2 is carried out to the reactive ion etching process of 300-320s, the diameter of PS bead is decreased to about 480-580nm;
(4) silver-plated by electron beam evaporation on a silicon substrate, plated film speed is 3 dusts per second, and the plated film time is 4min, then is placed on ultrasonic dissolution PS bead in toluene, thus obtains porous silverskin;
(5) silicon base is placed in the H of HF and 0.3M of 4.8M
2o
2mixed solution in insulation within 8 minutes, carry out silver-colored catalyzed corrosion process, then be placed in mass fraction be 50% nitric acid remove remaining silver;
(6) by the silicon nanowire array that obtains in step (5) at O
2in atmosphere, be incubated 60-80 minute at 900-1000 DEG C and carry out dry oxidation, take out the oxide layer being placed in the HF aqueous solution of mass fraction 1-5% and removing surface, obtain silicon nanowire array.
The method of PS bead arrangement is: sheet glass is placed in surface plate central authorities, adds deionized water to a little higher than glass sheet surface of the water surface in surface plate; Be that the PS bead solution of 0.5-3% slowly drops on sheet glass by mass fraction, bead spreads at liquid level, sodium dodecyl sulfate solution is instilled from surface plate edge after stopping dropping, silicon chip is put into surface plate side, tweezers are utilized to push it to PS bead solid matter side, take out after the moisture in silicon base evaporates completely, namely it be placed with the little ball array of PS of packed mono-layer.
Beneficial effect of the present invention is:
1) method of the present invention is by simplifying the preparation technology improving PS bead template, improves the individual layer of preparation PS bead template, solid matter, success rate and efficiency; And adopt the ultrasonic removal bead of toluene solution, overcome obstacle silicon base being difficult to totally remove PS bead, ensure that the carrying out of subsequent step;
2) silver-colored catalyzed corrosion is combined with dry oxidation technique by method of the present invention, thus achieves the large area preparation with cutting-edge structure silicon nanowire array, and the diameter of silicon nanowires is decreased to most advanced and sophisticated 180nm, and root is about 380nm; This cutting-edge structure and the performance of Flied emission can be significantly improved compared with Large space.The cut-in voltage of the silicon nanowire array that the method prepares far below additive method prepare silicon nanowire array, cutting-edge structure greatly improves field enhancement factor; Simultaneously because spacing is comparatively large, thus avoid mutual screen effect, substantially increase field emission performance.
3) silicon nanowire array that the present invention prepares can not only obtain good field emission performance, and monocrystalline is functional, can larger area rule solid matter, nano wire has tip, spacing and draw ratio controllability stronger.In addition, this method cost is low, productive rate is high, Modulatory character is good, is thus expected to obtain practical application very much in the production of silica-based feds.Prepared nano wire field emission performance is cut-in voltage 1.8V/ μm, and field enhancement factor is 5785; Current stability test shows that it is under the voltage of 2.3V/ μm, and current density is stabilized in about 300 μ A/cm
2, stability bandwidth is 8%.
Accompanying drawing explanation
Fig. 1 is the flow chart of large scale silicon nanowire array preparation process; Wherein (a) is arrangement PS bead, b () is reactive ion etching, (c) is the silver-plated result of magnetron sputtering, and (d) removes bead for ultrasonic, e () is silver-colored catalyzed corrosion, (f) is dry oxidation.
Fig. 2 is the stereoscan photograph of preparation large scale silicon nanowire array process; Wherein (a) is reactive ion etching result, and (b) goes bead result for the silver-plated result of magnetron sputtering, (c) for ultrasonic, and (d) is silver-colored catalyzed corrosion result.
Fig. 3 is the stereoscan photograph after dry oxidation.
Fig. 4 is the transmission electron microscope photo with the silicon nanowires of cutting-edge structure of preparation;
Wherein (a) is low power picture, and (b) is nano wire side pattern, and (c) is nano wire top pattern.
Fig. 5 is the field emission performance test curve of silicon nanowire array, i.e. current-voltage curve; Illustration is F-N curve.
Fig. 6 is the field emission performance stable testing type curve of silicon nanowire array.
Detailed description of the invention
Below will the present invention is further illustrated by accompanying drawing and instantiation.
Embodiment 1
(1) by the ultrasonic cleaning be immersed in dense H one by one of silicon base and sheet glass acetone, alcohol, deionized water
2sO
4and H
2o
2volume ratio is carry out hydrophilic treated in the mixed solution of 4:1;
(2) arrange on a silicon substrate the PS bead of one deck packed mono-layer, method is as follows: dried up by sheet glass and be placed on surface plate central authorities, adds deionized water to a little higher than glass sheet surface of the water surface in surface plate; Mass fraction dilution obtained is 0.5%, and diameter is that the aqueous solution of the PS bead of 960nm slowly drops on sheet glass, and bead spreads at liquid level, covers after individual layer bead stop dripping until most of liquid level; Instilling 1mL mass fraction from surface plate edge is the sodium dodecyl sulfate solution of 1%, by silicon chip from putting into surface plate, utilize tweezers to push it to PS bead solid matter side, take out after the moisture in silicon base evaporates completely, namely it be placed with the little ball array of PS of packed mono-layer; As shown in accompanying drawing 1 (a) He 2 (a).
(3) using the oxygen of flow 40SCCM as reacting gas, at pressure 2Pa, under the condition of power 30W, the little ball array of PS of preparation in step 2 is carried out to the reactive ion etching process of 300s, the diameter of PS bead is decreased to about 580nm; As shown in accompanying drawing 1 (b) He 2 (b).
(4) silver-plated by electron beam evaporation on a silicon substrate, plated film speed is 3 dusts per second, and the plated film time is 4min, as shown in accompanying drawing 1 (c) He 2 (c); Be placed on ultrasonic dissolution PS bead in toluene again, thus obtain porous silverskin; As shown in accompanying drawing 1 (d) He 2 (d).
(5) silicon base is placed in the H of HF and 0.3M of 4.8M
2o
2mixed solution in insulation within 8 minutes, carry out silver-colored catalyzed corrosion process, then be placed in mass fraction be 50% nitric acid remove remaining silver; Process is as shown in accompanying drawing 1 (e).
(6) by the silicon nanowire array that obtains in step (5) at O
2in atmosphere, at 900 DEG C, insulation carries out dry oxidation in 70 minutes, takes out the oxide layer that the HF aqueous solution being placed on mass fraction 1% removes surface for 60 minutes; Process is as shown in accompanying drawing 1 (f); The silicon nanowires length prepared is 3.2 μm, and tip diameter is 180nm, and root diameter (RD) is the silicon nanowire array of 380nm, and result as shown in figures 3 and 4.
(7) sample obtained in step (6) is connected wire as negative electrode at its back side by conductive silver glue, and be fixed on sheet glass central authorities; Using being coated with the ITO electro-conductive glass of fluorescence coating as anode, between anode and cathode, adding a sheet glass (0.5mm) and with tweezers, three is fixed.The wire at negative and positive the two poles of the earth is connected to the electrode place of field emission performance testing equipment, system is evacuated down to 10
-6pa, cathode and anode spacing is 500nm, tests its electric current and obtains current-voltage curve, as depicted in figures 5 and 6 at 0-1100V making alive.
Utilize the silicon nanowire array length that a process for preparing to be 3.2 μm, tip diameter is 180nm, and root diameter (RD) is 380nm.This array has excellent field emission performance; (electric current reaches 10 μ A/cm to its cut-in voltage
2required voltage value) can 1.8V/ μm be reached, because cutting-edge structure causes its field enhancement factor up to 5785; Under the voltage of 2.3V/ μm, current density is stabilized in about 300 μ A/cm
2, stability bandwidth is 8%.Current stability is better.
Embodiment 2
(1) by the ultrasonic cleaning be immersed in dense H one by one of silicon base and sheet glass acetone, alcohol, deionized water
2sO
4and H
2o
2volume ratio is carry out hydrophilic treated in the mixed solution of 4:1;
(2) utilize the method for self assembly to arrange on a silicon substrate the PS bead of one deck packed mono-layer, method is as follows: dried up by sheet glass and be placed on surface plate central authorities, adds deionized water to a little higher than glass sheet surface of the water surface in surface plate; Mass fraction dilution obtained is 0.5%, and diameter is that the PS bead aqueous solution of 980nm slowly drops on sheet glass, and bead spreads at liquid level, covers after individual layer bead stop dripping until most of liquid level; Instilling 1mL mass fraction from surface plate edge is the sodium dodecyl sulfate solution of 1%, by silicon chip from putting into surface plate, utilize tweezers to push it to PS bead solid matter side, take out after the moisture in silicon base evaporates completely, namely it be placed with the little ball array of PS of packed mono-layer; As shown in accompanying drawing 1 (a) He 2 (a).
(3) using the oxygen of flow 50SCCM as reacting gas, at pressure 2Pa, under the condition of power 30W, the little ball array of PS of preparation in step 2 is carried out to the reactive ion etching process of 310s, the diameter of PS bead is decreased to about 510nm; As shown in accompanying drawing 1 (b) He 2 (b).
(4) silver-plated by electron beam evaporation on a silicon substrate, plated film speed is 3 dusts per second, and the plated film time is 4min, as shown in accompanying drawing 1 (c) He 2 (c); Be placed on ultrasonic dissolution PS bead in toluene again, thus obtain porous silverskin; As shown in accompanying drawing 1 (d) He 2 (d).
(5) silicon base is placed in the H of HF and 0.3M of 4.8M
2o
2mixed solution in insulation within 8 minutes, carry out silver-colored catalyzed corrosion process, then be placed in mass fraction be 50% nitric acid remove remaining silver; Process is as shown in accompanying drawing 1 (e).
(6) by the silicon nanowire array that obtains in step (5) at O
2in atmosphere, at 1000 DEG C, insulation carries out dry oxidation in 70 minutes, takes out the oxide layer that the HF aqueous solution being placed on mass fraction 3% removes surface for 50 minutes; Process is as shown in accompanying drawing 1 (f); The silicon nanowires length prepared is 3.2 μm, and tip diameter is 180nm, and root diameter (RD) is the silicon nanowire array of 380nm, and result as shown in figures 3 and 4.
(7) sample obtained in step (6) is connected wire as negative electrode at its back side by conductive silver glue, and be fixed on sheet glass central authorities; Using being coated with the ITO electro-conductive glass of fluorescence coating as anode, between anode and cathode, adding a sheet glass (0.5mm) and with tweezers, three is fixed.The wire at negative and positive the two poles of the earth is connected to the electrode place of field emission performance testing equipment, system is evacuated down to 10
-6pa, cathode and anode spacing is 500nm, tests its electric current and obtains current-voltage curve, as depicted in figures 5 and 6 at 0-1100V making alive.
Embodiment 3
(1) by the ultrasonic cleaning be immersed in dense H one by one of silicon base and sheet glass acetone, alcohol, deionized water
2sO
4and H
2o
2volume ratio is carry out hydrophilic treated in the mixed solution of 4:1;
(2) utilize the method for self assembly to arrange on a silicon substrate the PS bead of one deck packed mono-layer, method is as follows: dried up by sheet glass and be placed on surface plate central authorities, adds deionized water to a little higher than glass sheet surface of the water surface in surface plate; Mass fraction dilution obtained is 0.5%, and diameter is that the PS bead aqueous solution of 1000nm slowly drops on sheet glass, and bead spreads at liquid level, covers after individual layer bead stop dripping until most of liquid level; Instilling 1mL mass fraction from surface plate edge is the sodium dodecyl sulfate solution of 1%, by silicon chip from putting into surface plate, utilize tweezers to push it to PS bead solid matter side, take out after the moisture in silicon base evaporates completely, namely it be placed with the little ball array of PS of packed mono-layer; As shown in accompanying drawing 1 (a) He 2 (a).
(3) using the oxygen of flow 60SCCM as reacting gas, at pressure 2Pa, under the condition of power 30W, the little ball array of PS of preparation in step 2 is carried out to the reactive ion etching process of 320s, the diameter of PS bead is decreased to about 480nm; As shown in accompanying drawing 1 (b) He 2 (b).
(4) silver-plated by electron beam evaporation on a silicon substrate, plated film speed is 3 dusts per second, and the plated film time is 4min, as shown in accompanying drawing 1 (c) He 2 (c); Be placed on ultrasonic dissolution PS bead in toluene again, thus obtain porous silverskin; As shown in accompanying drawing 1 (d) He 2 (d).
(5) silicon base is placed in the H of HF and 0.3M of 4.8M
2o
2mixed solution in insulation within 8 minutes, carry out silver-colored catalyzed corrosion process, then be placed in mass fraction be 50% nitric acid remove remaining silver, process is as shown in accompanying drawing 1 (e).
(6) by the silicon nanowire array that obtains in step (5) at O
2in atmosphere, at 1000 DEG C, insulation carries out dry oxidation in 80 minutes, takes out the oxide layer that the HF aqueous solution being placed on mass fraction 5% removes surface for 40 minutes.Process is as shown in accompanying drawing 1 (f); The silicon nanowires length prepared is 3.2 μm, and tip diameter is 180nm, and root diameter (RD) is the silicon nanowire array of 380nm, and result as shown in figures 3 and 4.
(7) sample obtained in step (6) is connected wire as negative electrode at its back side by conductive silver glue, and be fixed on sheet glass central authorities; Using being coated with the ITO electro-conductive glass of fluorescence coating as anode, between anode and cathode, adding a sheet glass (0.5mm) and with tweezers, three is fixed.The wire at negative and positive the two poles of the earth is connected to the electrode place of field emission performance testing equipment, system is evacuated down to 10
-6pa, cathode and anode spacing is 500nm, tests its electric current and obtains current-voltage curve, as depicted in figures 5 and 6 at 0-1100V making alive.
Claims (1)
1. the excellent preparation method with the silicon nanowire array of cutting-edge structure of field emission performance, is characterized in that, comprise the following steps:
(1) clean silicon base and carry out hydrophilic treated;
(2) diameter of packed mono-layer of arranging on a silicon substrate is the PS bead of 960-1000nm;
(3) using the oxygen of flow 40-60SCCM as reacting gas, at pressure 2Pa, under the condition of power 30-50W, the little ball array of PS of preparation in step (2) is carried out to the reactive ion etching process of 300-320s, the diameter of PS bead is decreased to 480-580nm;
(4) silver-plated by electron beam evaporation on a silicon substrate, plated film speed is 3 dusts per second, and the plated film time is 4min, then is placed on ultrasonic dissolution PS bead in toluene, thus obtains porous silverskin;
(5) silver-colored catalyzed corrosion process is carried out in mixed solution insulation silicon base being placed in the H2O2 of HF and 0.3M of 4.8M for 8 minutes, then be placed in mass fraction be 50% nitric acid remove remaining silver;
(6) by the silicon nanowire array that obtains in step (5) in O2 atmosphere, be incubated 60-80 minute at 900-1000 DEG C and carry out dry oxidation, take out the oxide layer being placed in the HF aqueous solution of mass fraction 1-5% and removing surface, obtain silicon nanowire array;
In described step (2), the method for PS bead arrangement is: sheet glass is placed in surface plate central authorities, adds deionized water to a little higher than glass sheet surface of the water surface in surface plate; Be that the PS bead solution of 0.5-3% slowly drops on sheet glass by mass fraction, bead spreads at liquid level, sodium dodecyl sulfate solution is instilled from surface plate edge after stopping dropping, silicon chip is put into surface plate side, tweezers are utilized to push it to PS bead solid matter side, take out after the moisture in silicon base evaporates completely, namely it be placed with the little ball array of PS of packed mono-layer.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410193257.3A CN103950889B (en) | 2014-05-08 | 2014-05-08 | The excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410193257.3A CN103950889B (en) | 2014-05-08 | 2014-05-08 | The excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103950889A CN103950889A (en) | 2014-07-30 |
CN103950889B true CN103950889B (en) | 2015-08-19 |
Family
ID=51328282
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201410193257.3A Active CN103950889B (en) | 2014-05-08 | 2014-05-08 | The excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103950889B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108232204A (en) * | 2016-12-10 | 2018-06-29 | 中国科学院大连化学物理研究所 | A kind of silicon base ordered polarizing electrode and its preparation method and application |
CN109853044B (en) * | 2019-01-21 | 2021-06-15 | 南京航空航天大学 | Monocrystalline silicon surface composite microstructure based on full-wave band antireflection and preparation method thereof |
CN113213421B (en) * | 2021-05-12 | 2022-04-15 | 清华大学 | Method and device for preparing large-area array nanoneedle structure |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100491233C (en) * | 2006-07-14 | 2009-05-27 | 清华大学 | Preparation process of nanometer silicon line array |
CN101302118A (en) * | 2008-03-31 | 2008-11-12 | 北京师范大学 | Preparation of silicon nanowire array |
CN101540348B (en) * | 2008-12-12 | 2011-03-16 | 北京师范大学 | Preparation technology of multi-purpose silicon micro-nano structure |
CN101497429B (en) * | 2009-03-06 | 2010-09-15 | 吉林大学 | Method for preparing silicon hollow nano-cone array |
KR101195546B1 (en) * | 2010-05-07 | 2012-10-29 | 국립대학법인 울산과학기술대학교 산학협력단 | Method of making silicon nano wires and method of fabricating rechargeable lithium battery using the same |
TW201302600A (en) * | 2011-07-04 | 2013-01-16 | Univ Nat Taiwan Science Tech | Method for fabricating silicon nanowire arrays |
CN103194740B (en) * | 2012-01-10 | 2015-04-29 | 中国科学院合肥物质科学研究院 | Preparation method of metal silver ordered porous array membrane |
CN103489753B (en) * | 2013-09-27 | 2016-04-06 | 清华大学 | A kind of preparation method of large-area small-size core-shell structure silicon nanowire array |
CN103641059B (en) * | 2013-12-30 | 2016-03-30 | 中国人民解放军国防科学技术大学 | Metal film nano-structure array that silicon post supports and preparation method thereof |
-
2014
- 2014-05-08 CN CN201410193257.3A patent/CN103950889B/en active Active
Also Published As
Publication number | Publication date |
---|---|
CN103950889A (en) | 2014-07-30 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103213933B (en) | A kind of silicon based three-dimensional micro cell nano pole structure | |
CN104638049A (en) | P-type graphene/N-type germanium nanocone array schottky junction infrared photoelectric detector and preparation method thereof | |
CN106198674B (en) | A kind of mesoporous graphene preparation process and it is based on mesoporous graphene field effect transistor biosensor | |
CN101266919A (en) | A method for selectively etching silicon nano line | |
CN107086306A (en) | A kind of use graphene film as negative pole miniature thin-film lithium battery | |
CN103950889B (en) | The excellent preparation method with the silicon nanowire array of cutting-edge structure of a kind of field emission performance | |
CN102556949A (en) | Preparation method of silicon micro/nanometer line array with controllable dimension | |
CN103337449B (en) | Method prepared by the transplanting of silicon nanowire array and simple Devices thereof | |
CN107179337A (en) | A kind of bimodulus humidity sensor and preparation method thereof | |
CN106784332A (en) | A kind of PEDOT:PSS‑MoO3The preparation method of/silicon nanowire array organic inorganic hybridization solar cell | |
CN107863416A (en) | A kind of preparation method of Flexible graphene silicon solar cell | |
CN102270692A (en) | Graphene-cadmium selenide nanoribbon heterojunction, battery, module and preparation method of module | |
CN103681965A (en) | Preparation method of flexible substrate silicon nanowire heterojunction solar cell | |
US20230389431A1 (en) | CORE-SHELL COAXIAL GALLIUM NITRIDE (GaN) PIEZOELECTRIC NANOGENERATOR AND METHOD FOR MANUFACTURING THE SAME | |
CN109648096B (en) | Method for converting random nanocone array into silver nanosheet constructed micro/nano structure array in situ | |
CN105185910A (en) | Method for fabricating monocrystal micro-nano line array of organic semiconductor by using writing brush | |
CN104701020B (en) | Three-dimensional micro-electrode preparation method based on the photoresists of SU 8 | |
CN204529302U (en) | Self-supporting three-dimension device | |
CN103489753B (en) | A kind of preparation method of large-area small-size core-shell structure silicon nanowire array | |
CN114496768A (en) | Preparation method of nano-pillar array | |
CN104037320A (en) | Manufacturing method of large-area zinc oxide nano-micro generator | |
CN104947043A (en) | Preparation method of Si-ITO composite nanowire ordered array | |
CN108493327A (en) | Spiro-MeOTAD/ZnO piezoelectric type nano generators and preparation method thereof | |
CN207866749U (en) | A kind of integrated humidity sensor | |
CN106555207B (en) | The preparation method of field-effect electro-catalysis hydrogen-producing machine part |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant |