CN104118843B - Nano-structure array material and preparation method thereof - Google Patents
Nano-structure array material and preparation method thereof Download PDFInfo
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- CN104118843B CN104118843B CN201410356646.3A CN201410356646A CN104118843B CN 104118843 B CN104118843 B CN 104118843B CN 201410356646 A CN201410356646 A CN 201410356646A CN 104118843 B CN104118843 B CN 104118843B
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Abstract
Nano-structure array material of the present invention and preparation method thereof, a kind of high temperature resistant, wide bandgap semiconductor 4H crystal formation carbofrax materials that are anticorrosive, possessing nano-wire array and preparation method thereof are referred specifically to, is related to nano-structure array field of material technology.The present invention includes the SiC nanowire of different crystal forms, such as the SiC nanowire of 3C, 4H and 6H crystal formation, such as it is based on n-type heavy doping 4H SiC substrates, even mesoporous array is obtained by selecting appropriate pulse frequency and residence time to apply permanent pulse current to the two poles of the earth, then suitably increase electric current forward direction accounts for width than causing base apertures to depart from substrate with current density, and the nano-wire array is obtained by stripping means.It has the advantages that simple and reliable, repetitive rate is high, and nano-wire array density is high, and saving prepares cost.For power electronics and field of aerospace, using high carrier mobility, thermal conductivity is anticorrosive, it is high pressure resistant the advantages that silicon carbide products, there is provided solid technology material base.
Description
Technical field
The present invention relates to nano-structure array field of material technology, refer specifically to a kind of high temperature resistant, it is anticorrosive, possess nano wire
Wide bandgap semiconductor 4H crystal formation carbofrax materials of array and preparation method thereof.
Background technology
As the carbofrax material of third generation semiconductor, possesses high carrier mobility, thermal conductivity is anticorrosive, high pressure resistant
Etc. the multinomial advantage better than first generation semiconductor, the carborundum of same nanostructured also possesses above advantage, makes it be expected to challenge
Status of the first generation nanostructured silicon materials on sensor, feds and energy storage device.At present, 3C-SiC and 6H-SiC
Nano wire can be prepared by vapor phase method, liquid phase method, solid phase method, but the carborundum of this kind of crystal formation is in most performances
It is difficult to obtained 4H crystal formations, high quality, silicon carbide nanometer line not as good as 4H-SiC, and by such method.4H- is prepared so exploring
The method of SiC nanowire has great importance.Such method is also applied to the preparation of other materials nano-structure array material,
The especially preparation of the SiC nanowire of different crystal forms, such as the SiC nanowire of 3C, 4H and 6H crystal formation.
The content of the invention
It is an object of the invention to overcome in the prior art 4H crystal formations SiC nanowire array be difficult to the present situation prepared, propose
A kind of method being combined by electrochemical etching and simple stripping means obtains 4H crystal formation SiC nanowire arrays.The method
It is equally applicable to the preparation of the nano-structure array material of other materials.
A kind of nano-structure array material of the present invention, its feature, received comprising means are peeled off again through nanostructured modulation
Rice material structure array.Such as a kind of 4H crystal formations SiC nanowire array material, its feature, comprising based on n-type heavy doping 4H-SiC linings
Bottom, thickness are 300~500 μm, twin polishing, the 4H crystal formation SiC nanowires for peeling off to obtain in C faces are prepared into through electrochemical etching
Array.
Wherein, the nano wire wire range is 10-20nm, and nanometer length scope is 3-5 μm, and single nano-wire structure is
Calabash shaped nano thread structure, it is 5nm often to tie cucurbit structure longitudinal length, and nano-wire array area is 1cm2Circular array.
The n-type heavy doping 4H-SiC wafers are that the crystal ingot by the growth of PVT methods is oriented, cut, twin polishing, double
The industrialization chip that face CMP planarization obtains, area 100cm2。
The n-type heavy doping 4H-SiC substrate thickness is 320 μm, and optimal nano wire line footpath often ties cucurbit in 15nm or so
For the nanowire length of shape part in 5nm or so, nanowire length is about 5 μm, etching area about 1cm2Circular etched surface.
The preparation method of nano-array material of the present invention, embodiment comprise the following steps：
Step 1, highly doped n-type 4H-SiC samples are prepared.
Step 2, by it is double lead copper foil and be cut into area be slightly less than the square of sample, then uniform adhesion is in sample Si faces.Will
Sample is fixed on etching cell body anode position, by platinum guaze negative electrode as 2cm directly over anode at.Configure hydrofluoric acid 49%：Ethanol
99%：Hydrogen peroxide 30%=3：6：The mixed liquor of 1 volume ratio is as electrolyte.Setpoint frequency is 2500Hz forward current, just
To electric current 100%, current density 40mA/cm2, forward direction accounts for the wide constant-current pulse than for 50%, and power-on, the time is
3min, then forward direction accounted for wide than being promoted to 100% or current density being promoted into 80mA/cm2, time 30s.
Step 3, take out sample and be soaked in 2min in the solution of ethanol 99%, be then placed into air and treat that ethanol is waved completely
Hair, skin layer is peeled off by peeling off means, the present embodiment leads copper foil to peel off the layer using double, that is, obtains described 4H crystal formations
SiC nanowire array.
As described above, a kind of preparation method of nano-structure array material of the present invention, is such as served as a contrast based on n-type heavy doping 4H-SiC
The preparation method of bottom nano-wire array, obtained by selecting appropriate pulse frequency and residence time to apply permanent pulse current to the two poles of the earth
To even mesoporous array, then suitably increase electric current forward direction accounts for wide than causing base apertures to depart from substrate with current density, hole wall
As nano wire, then obtain the nano-wire array by stripping means.The characteristics of material, is compared to the material prepared more in the past
For material feature, there is nano-wire array density height, nano wire crystal formation is 4H crystal formations etc., and the array preparation is compared to more conventional
Preparation technology for, there is simple and reliable, the advantages that repetitive rate is high.The preparation for deriving device for its high-performance is brought just
Profit.
Embodiment
The present invention is described in further detail with reference to embodiments
A kind of preparation flow of 4H crystal formations SiC nanowire described in the embodiment of the present invention, comprises the following steps：
Step 1, highly doped n-type 4H-SiC pre-etching samples are prepared.The sample is wafer, size 100cm2, inclined 4 °
Cutting, twin polishing, by strict semiconductor technology clean after obtain and through pre-etching sample by wafer cut into 1.2cm ×
1.2cm square plates, then by volume ratio be 1：1 hydrofluoric acid (49%) and ethanol (99%) solution immersion removes surface oxidation
Layer.
Step 2, to lead copper foil to be cut into area be 1cm by double2Square, then uniform adhesion is in sample Si faces.Sample is consolidated
Due to etching cell body anode position, by gauze platinum electrode (negative electrode) as 2cm directly over anode at.Configure hydrofluoric acid (49%)：Second
Alcohol (99%)：Hydrogen peroxide (30%)=3：6：1 volume ratio mixed liquor is as electrolyte.The forward direction electricity that setpoint frequency is 2500Hz
Stream, forward current 100%, current density 40mA/cm2, it is positive to account for the wide constant-current pulse than for 50%, power-on, time
For 3min, then forward direction accounted for wide than being promoted to 100% or current density being promoted into 80mA/cm2, time 30s.
Step 3, take out sample and be soaked in 2min in the solution of ethanol 99%, be then placed into air and treat that ethanol is waved completely
Hair, skin layer is peeled off by peeling off means, this experiment leads copper foil to peel off the layer using double, that is, obtains described 4H crystal formations
SiC nanowire array.
In summary, a kind of preparation method of nano structural material array of the present invention, refers specifically to 4H crystal formation nanometer silicon carbides
Linear array material and preparation method thereof, overcome 4H crystal formations SiC nanowire in the prior art be difficult to prepare it is close with nano-wire array
The problem of low is spent, the array preparation method is simple and reliable.Preparation technology repeatability is strong, high yield rate, spreads out for its high-performance
The preparation of raw device brings facility.Its more existing vapor phase method, liquid phase method, solid phase method, simplify and prepare utensil, save and prepare
Cost.For power electronics and field of aerospace, using high carrier mobility, thermal conductivity is anticorrosive, it is high pressure resistant the advantages that
Third generation semiconductor silicon carbide products, there is provided solid technology material base.
Claims (4)
1. a kind of preparation method of nano-structure array material, it is characterised in that comprise the following steps：
Step 1, n-type heavy doping 4H-SiC liner oxidations layer and cutting process are cleaned；
Step 2, to lead copper foil to be cut into area be 1cm by double2It is square, then uniform adhesion is in n-type heavy doping 4H-SiC substrate Sis
Face, by n-type heavy doping 4H-SiC substrates, etching cell body anode position is fixed on, by platinum guaze negative electrode as 2cm directly over anode
Place；
Configure hydrofluoric acid 49%：Ethanol 99%：Hydrogen peroxide 30%=3：6：The mixed liquor of 1 volume ratio is as electrolyte；
Setpoint frequency be 2500Hz forward current, forward current 100%, current density 40mA/cm2, forward direction accounts for wide ratio and is
50% constant-current pulse, power-on, time 3min, then forward direction accounted for wide than being promoted to 100% or putting forward current density
Rise to 80mA/cm2, time 30s；
Step 3, n-type heavy doping 4H-SiC substrates are taken out, 2min in the solution of ethanol 99% is soaked in, is then placed into air
Treat that ethanol volatilizees completely, peel off skin layer by peeling off means, that is, obtain 4H crystal formation SiC nanowire arrays.
2. the preparation method of nano-structure array material as claimed in claim 1, it is characterised in that the nano-structure array
Material, n-type heavy doping 4H-SiC substrates, thickness are 300~500 μm, twin polishing, are obtained through electrochemical etching method, stripping means
The 4H crystal formation SiC nanowire arrays arrived.
3. the preparation method of nano-structure array material as claimed in claim 1, it is characterised in that the n-type heavy doping 4H-
SiC substrate, for the crystal ingot by the growth of PVT methods is oriented, cutting, the obtained industrialization chip of two-sided CMP planarization, area is
100㎝2。
4. the preparation method of nano-structure array material as claimed in claim 1, it is characterised in that the nano wire crystal formation is
4H, nano wire wire range are 10-20nm, and nanowire length scope is 3-5 μm, and single nano-wire structure is calabash shaped structure,
Longitudinal length is 5nm, and array area is 1 ㎝2Circular array.
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| CN104876179B (en) * | 2015-04-16 | 2017-01-11 | 华中科技大学 | Large-area assembling method for non-contact type one-dimensional nano material |
| CN105133018B (en) * | 2015-07-08 | 2016-08-24 | 宁波工程学院 | SiC nano-array |
| CN105926026A (en) * | 2016-04-19 | 2016-09-07 | 宁波工程学院 | Preparation method for highly-oriented SiC nano-arrays |
| CN107680705A (en) * | 2017-09-19 | 2018-02-09 | 壹号元素（广州）科技有限公司 | A kind of isotope battery of the wide forbidden region semi-conductor nano tube/linear of ordered arrangement |
| CN108251888B (en) * | 2017-11-29 | 2020-01-31 | 宁波工程学院 | Preparation method of transparent 4H-SiC nanopore arrays |
| CN109904004B (en) * | 2019-01-30 | 2020-10-09 | 宁波工程学院 | Preparation method of SiC nanowire array film and application of SiC nanowire array film in supercapacitor electrode |
| CN110739880B (en) * | 2019-10-28 | 2021-04-02 | 北京科技大学 | Preparation method of silicon carbide nanowire array-based piezoelectric nano-generator |
| CN113497361B (en) * | 2021-07-07 | 2023-10-13 | 东莞理工学院 | Patterned SiC microstructure and application thereof |
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| US7977798B2 (en) * | 2007-07-26 | 2011-07-12 | Infineon Technologies Ag | Integrated circuit having a semiconductor substrate with a barrier layer |
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