CN106315503A - Ordered array of silicon-based quasi three-dimensional nanostructure and preparation method thereof - Google Patents
Ordered array of silicon-based quasi three-dimensional nanostructure and preparation method thereof Download PDFInfo
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- CN106315503A CN106315503A CN201610704386.3A CN201610704386A CN106315503A CN 106315503 A CN106315503 A CN 106315503A CN 201610704386 A CN201610704386 A CN 201610704386A CN 106315503 A CN106315503 A CN 106315503A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00206—Processes for functionalising a surface, e.g. provide the surface with specific mechanical, chemical or biological properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00341—Processes for manufacturing microsystems not provided for in groups B81C1/00023 - B81C1/00261
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00388—Etch mask forming
- B81C1/00404—Mask characterised by its size, orientation or shape
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00841—Cleaning during or after manufacture
- B81C1/00849—Cleaning during or after manufacture during manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
- B81C2201/0156—Lithographic techniques
Abstract
The invention provides an ordered array of a silicon-based quasi three-dimensional nanostructure and a preparation method thereof. The quasi three-dimensional nanostructure is a nanoscale columnar structure with two big ends and a small middle portion, and a proportion of the diameter of the two ends of the columnar structure to the diameter of the middle portion of the columnar structure is 3-20:1. Compared with the existing silicon-based nano ordered structure array, the ordered array of the silicon-based quasi three-dimensional nanostructure provided by the invention has the more complex quasi three-dimensional structure is highly ordered, high in precision, extremely small in size, and controllable in structure, has special optical and electrical properties, and has important value in fields of electronic information, solar cells and biochemical sensing. Preparation of the ordered array of the silicon-based quasi three-dimensional nanostructure with more complex structure is achieved by adjusting a reactive ion etching technology, and the size of the nanostructure can be adjusted in a controllable manner. The ordered array of the silicon-based quasi three-dimensional nanostructure provided by the invention has wide application prospects in aspects of photoelectric devices and sensing chips.
Description
Technical field
The present invention relates to micro-nano technology preparation field, more particularly, to a kind of silica-based orderly battle array of quasi-3-D nano, structure
Row and preparation method thereof.
Background technology
Silicon is the semi-conducting material that a kind of range is the widest, under the background that current information technology is fast-developing, and two poles
Pipe, audion, IGCT, field effect transistor and various integrated circuit, including the CPU etc. in computer, be all as former material with silicon
Material.Meanwhile, silicon can also be made into solaode, and radiation can be converted to electric energy, has in terms of the exploitation of clean energy resource
There is important value.Additionally, pure silicon dioxide can make the glass fibre of the high grade of transparency, can be used for fiber optics communications, have
Weight is little, contain much information, capacity of resisting disturbance is strong, confidentiality advantages of higher.
Along with the development of nanosecond science and technology, research is found that nano material has significant interface and skin effect, little
The special natures such as dimensional effect, quantum size effect and macro quanta tunnel effect.These characteristics make nano material present
It is different from the electromagnetism of traditional structural materials, optics, thermodynamics and chemical property, thus at photoelectric device, sensing chip etc.
Aspect has broad application prospects.
Nano material is as emerging material, and the most maximum problem is how to prepare batch, uniform, pure this micro-
Type material, thus study actual performance and the mechanism thereof of this kind of material further.From the point of view of current research conditions, at all Donnas
In rice material, the research temperature of the grapheme material of one-dimensional CNT and two dimension is the highest, and the report of quasi-3-D nano, structure
Road is fewer, and the most diversified quasi-3-D nano, structure and preparation method thereof still has important value.
Summary of the invention
It is desirable to provide a kind of silica-based quasi-3-D nano, structure oldered array and preparation method thereof, thus at e-mail
The fields such as breath, clean energy resource, biochemical sensitive play a role.
To achieve these goals, the present invention uses techniques below means: a kind of silica-based orderly battle array of quasi-3-D nano, structure
Row, described quasi-3-D nano, structure is the column structure that big centre, nano level two is little;Two of described column structure
Diameter and the ratio of diameter of centre of column structure be 3 ~ 20:1.
Additionally provide the preparation method of a kind of silica-based quasi-3-D nano, structure oldered array, including substrate, preparation side simultaneously
Method comprises the following steps:
S1. develop a film: choose monocrystalline silicon piece and be carried out, dry up, obtain a clean smooth silicon base;
S2. whirl coating: the silicon substrate surface obtained by S1 is coated with last layer electron beam resist thin layer, the thickness of electron beam resist thin layer
Degree is 50 ~ 1000nm;
S3. exposure: design exposing patterns and correct, then the electron beam resist thin layer of silicon base being carried out electron beam exposure
Process;
S4. development: the silicon base after exposure is immersed in the tetramethylammonium hydroxide aqueous solution of 10%, removes uncrosslinked electricity
Son bundle photoresist;
S5. etching: silicon base be put on load plate, carries out reactive ion etching to silicon base with the face of electron beam resist;
S6. remove photoresist: wash away the electron beam resist of residual with the aqueous hydrogen fluoride solution of 10%, clean and dry up, obtain silica-based accurate three
Dimension nanometer construction oldered array.
As a further improvement on the present invention, described S1 includes procedure below: choose sizeable silicon chip, first with aseptic
Cloth dips dehydrated alcohol wiping silicon substrate surface;Then silicon chip is immersed in acetone, cleans 5 with the power ultrasonic of 180 W
min;Then silicon chip is immersed in ethanol, cleans 5 min with the power ultrasonic of 180 W, with pure water, Wafer Cleaning is clean;?
After silicon chip dry nitrogen air-flow is dried up, obtain the most smooth silicon base.
As a further improvement on the present invention, the step of S4 is: the silicon chip sample after exposure is first immersed in the tetramethyl of 10%
In base ammonium hydroxide aqueous solution, jiggle 1 min;Then clean water silicon chip sample is used;Finally with drying nitrogen slowly
Stream dries up silicon chip sample.
Particularly, the operation of step S5 is: silica-based being positioned on load plate is carried out reactive ion etching, by controlling load plate
Material and the relative amount of size regulation reactive ion gas, it is ensured that silicon base does not occur over etching to produce fracture, obtains one
Silica-based quasi-three-dimensional manometer column structure.
Particularly, the operation of step S5 is: silica-based being positioned on load plate is carried out reactive ion over etching, obtains a kind of cone
Shape nanostructured;The bus of this cone-shaped nano structure is arc.
The present invention mainly make use of the isotropism and anisotropy that reactive ion gas etches in silicon chip, by regulation
The concentration of reactive ion gas and the ratio of area to be etched, it is achieved the orderly battle array of silica-based quasi-3-D nano, structure of many sizes
The controlled preparation of row.
The present invention possesses following beneficial effect.
1. compared with existing silicon-based nano ordered structure array, the silica-based quasi-3-D nano, structure oldered array of the present invention
Having more complicated quasi-three dimensional structure, this structure height is orderly, high-precision, size are minimum, structure-controllable, has special light
, electrical properties, have important value in fields such as electronic information, solaode, biochemical sensitives;
2. the present invention is by adjusting reactive ion etching process, it is achieved that the more complicated silica-based quasi-3-D nano, structure of structure is orderly
The preparation of array, and can controllably regulate the size of nanostructured;
Provide a kind of silica-based quasi-three-dimensional manometer column oldered array and the silica-based quasi-orderly battle array of three-dimensional manometer taper of one the most simultaneously
Row, have broad application prospects at the aspect such as photoelectric device, sensing chip.
Accompanying drawing explanation
Fig. 1 is the preparation flow schematic diagram of difform silica-based quasi-3-D nano, structure oldered array;
Fig. 2 is the microstructure Electronic Speculum figure after the silicon chip sample of electron beam exposure develops;
After Fig. 3 is reactive ion etching, silica-based quasi-three-dimensional manometer column oldered array and the silica-based quasi-orderly battle array of three-dimensional manometer taper
The microstructure Electronic Speculum figure of row;
Fig. 4 is the silica-based quasi-three-dimensional manometer column oldered array after removing photoresist and the microcosmic of silica-based quasi-three-dimensional manometer taper oldered array
Structure Electronic Speculum figure;
Wherein, 1 is substrate, and 2 be electron beam resist thin layer, a be reactive ion gas appropriate under the conditions of synthesize silica-based accurate three
Wiener rice column oldered array, b is the silica-based quasi-three-dimensional manometer taper oldered array of preparation under the conditions of over etching.
Detailed description of the invention
The present invention is further described below in conjunction with the accompanying drawings with specific embodiment.Unless stated otherwise, the present invention uses
Reagent, equipment and method be the art conventional commercial reagent, equipment and conventional use of method.
Embodiment one: silica-based quasi-three-dimensional manometer column oldered array
1. develop a film: cut the monocrystalline silicon piece of 2cm × 2cm, with acetone, ethanol, clear water, silicon chip is carried out sonic oscillation cleaning successively,
Finally dry up with dry nitrogen air-flow, it is provided that a most smooth silicon base;
2. whirl coating: utilize spin coating instrument, at the electron beam resist of one layer of 700nm thickness of silicon substrate surface spin coating, by sample silicon chip
It is placed on front baking in 90 DEG C of thermal station and processes 5 min;
3. exposure: design exposing patterns is nanometer filled circles array, and circular diameter is 360 nm, and array period is 610 nm, with soft
After part carries out proximity correction, the photoresist thin layer of silicon chip sample is carried out electron beam exposure process;
4. development: the silicon chip sample after exposure is immersed in the tetramethylammonium hydroxide aqueous solution of 10%, jiggles 1 min,
Remove uncrosslinked photoresist, cleaner by clean water, dry nitrogen air-flow dries up;
5. etching: cut-off footpath is about the silica discs of 10 cm as load plate, and sample silicon chip is placed on load plate surface, right
Face, silicon base electron beam resist thin layer place carries out reactive ion etching, etching gas composition for for 15 sccm CHF3,5
Sccm SF6, pressure is 5 mTorr, and temperature is 20 DEG C, and etch period is 10.5 min;
6. remove photoresist: wash away the photoresist of residual with the aqueous hydrogen fluoride solution of 10%, cleaner by clean water, dry nitrogen air-flow blows
Dry, finally obtain silica-based quasi-3-D nano, structure oldered array.
Preparation process as shown in a in accompanying drawing 1, electron beam exposure the localized micro scanning electron microscope of acquired results after developing
Photo as shown in Fig. 2, reactive ion etching and a portion in the localized micro stereoscan photograph such as Fig. 3 of acquired results after removing photoresist
Point, in Fig. 4 shown in a part.Diameter in the middle of the diameter at gained column structure two and column structure ratio is for 8:1.
Embodiment two: silica-based quasi-three-dimensional manometer taper oldered array
1. develop a film: cut the monocrystalline silicon piece of 1cm × 1 cm, successively with acetone, ethanol, that clear water carries out sonic oscillation to silicon chip is clear
Wash, finally dry up with dry nitrogen air-flow, it is provided that a most smooth silicon base;
2. whirl coating: operate consistent with embodiment 1;
3. exposure: operate consistent with embodiment 1;
4. development: operate consistent with embodiment 1;
5. etching: operate consistent with embodiment 1;
6. remove photoresist: operate consistent with embodiment 1.
In preparation process such as accompanying drawing 1 shown in b part, the localized micro scanning electricity of acquired results after electron beam exposure development
Mirror photo as shown in Fig. 2, reactive ion etching b portion in the localized micro stereoscan photograph such as Fig. 3 of acquired results after removing photoresist
Point, in Fig. 4 shown in b part.
Claims (7)
1. a silica-based quasi-3-D nano, structure oldered array, it is characterised in that described quasi-3-D nano, structure is nanoscale
The little column structure in big centre, two.
Silica-based quasi-3-D nano, structure oldered array the most according to claim 1, it is characterised in that described column structure
The diameter at two and the ratio of diameter of centre of column structure be 3 ~ 20:1.
3. a preparation method for silica-based quasi-3-D nano, structure oldered array, including substrate, it is characterised in that include following step
Rapid:
S1. develop a film: choose cleaning monocrystalline silicon, dry up, obtain silicon base;
S2. whirl coating: the silicon substrate surface that S1 obtains is coated electron beam resist thin layer;
S3. exposure: design exposing patterns and correct, then the electron beam resist thin layer of silicon base being carried out electron beam exposure
Process;
S4. development: the silicon base after exposure is removed uncrosslinked electron beam resist;
S5. etching: the face, place with electron beam resist of S4 gained silicon base is carried out reactive ion etching;
S6. remove photoresist: wash away the electron beam resist of residual, clean and dry up, obtain silica-based quasi-3-D nano, structure oldered array.
The preparation method of silica-based quasi-3-D nano, structure oldered array the most according to claim 3, it is characterised in that pass through
Control load plate material and the relative amount of size regulation reactive ion gas, it is ensured that silicon base does not occur over etching to produce fracture.
The preparation method of silica-based quasi-3-D nano, structure oldered array the most according to claim 3, it is characterised in that control
The amount of reactive ion and etch period so that reactive ion etching generation over etching.
6. the silica-based quasi-3-D nano, structure oldered array that a preparation method according to claim 5 obtains, it is characterised in that
Described quasi-3-D nano, structure is that nano level taper is protruding.
Silica-based quasi-3-D nano, structure oldered array the most according to claim 6, it is characterised in that the mother of described taper
Line is camber line.
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