CN107381498A - A kind of sheet liquid phase nanometer grain preparation method - Google Patents
A kind of sheet liquid phase nanometer grain preparation method Download PDFInfo
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- CN107381498A CN107381498A CN201610333421.5A CN201610333421A CN107381498A CN 107381498 A CN107381498 A CN 107381498A CN 201610333421 A CN201610333421 A CN 201610333421A CN 107381498 A CN107381498 A CN 107381498A
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- 239000007791 liquid phase Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 76
- 238000000034 method Methods 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 238000005516 engineering process Methods 0.000 claims abstract description 13
- 238000005530 etching Methods 0.000 claims abstract description 11
- 239000010409 thin film Substances 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims description 17
- 238000000151 deposition Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- 239000003292 glue Substances 0.000 claims description 9
- 238000001259 photo etching Methods 0.000 claims description 8
- 238000004528 spin coating Methods 0.000 claims description 8
- 239000002114 nanocomposite Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 238000002207 thermal evaporation Methods 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 238000004049 embossing Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010408 film Substances 0.000 claims description 4
- 238000010884 ion-beam technique Methods 0.000 claims description 4
- 229920002120 photoresistant polymer Polymers 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 230000009514 concussion Effects 0.000 claims description 3
- 239000005357 flat glass Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- 238000001020 plasma etching Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000001039 wet etching Methods 0.000 claims description 3
- 238000005240 physical vapour deposition Methods 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 230000005518 electrochemistry Effects 0.000 claims 1
- 230000003628 erosive effect Effects 0.000 claims 1
- 238000002386 leaching Methods 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 abstract description 27
- 239000002064 nanoplatelet Substances 0.000 abstract description 4
- 238000012546 transfer Methods 0.000 abstract description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 239000010931 gold Substances 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000000059 patterning Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007687 exposure technique Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
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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
- B81C1/00349—Creating layers of material on a substrate
-
- 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
-
- 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
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/00468—Releasing structures
- B81C1/00476—Releasing structures removing a sacrificial layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Micromachines (AREA)
Abstract
A kind of sheet liquid phase nanometer grain preparation method, comprises the following steps：(1) soluble thin film sacrificial layer material is deposited on flat substrate；(2) functional material is deposited on sacrifice layer again；(3) deposited in function material layer and prepare the nano-pattern of polymeric material；(4) using the nano-pattern of polymeric material as etching mask, using lithographic technique by the function material layer of nano-pattern transfer to lower floor, then unnecessary polymeric material is removed with lithographic technique；(5) sacrifice layer is dissolved using suitable liquid, while obtains the sheet functional material nano particle of liquid phase, grain shape is consistent with nano-pattern.The inventive method can be applied to prepare the sheet liquid phase nano particle of arbitrary graphic pattern, and nano particle can be that single or multiple lift different materials combine；This method preparation technology is simple, can prepare minimum dimension at low cost as 5 nanometers, minimum thickness is the liquid phase nanoplatelet of 0.1 nanometer and size uniformity, can be good at meeting actual demand with high efficiency.
Description
Technical field
The invention belongs to nano particle preparing technical field, and in particular to prepared by a kind of sheet liquid phase nano particle
Method.
Background technology
The nano-particle material of nano-particle material, particularly liquid phase is as one important point in nano material
Branch, in new-energy automobile, light-catalyzed reaction, environmental monitoring and protection, life science, medical treatment detection and
The numerous areas such as treatment, optics, photoelectric device, nano electron device, composite are applied.
However, with the development of technology, many fields start to need some special shapes, sheet it is a variety of
The composite nanoparticle materials of combination of materials.At present, one of main technology of preparing of liquid phase nano particle is exactly
Liquid phase synthesizing method, i.e., nano particle is prepared by chemical reactive synthesis in the liquid phase；Although this method cost
Low, equipment is simple, it is certain it is special under conditions of also can synthetic kernel hull shape, two-sided shape, star is bar-shaped etc.
Aspherical nano particle, but this method hardly results in the nano particle of any special shape, it is particularly more
The different Material cladding nano particle of layer, and often homogeneity is not fine.
In the last few years, with the development of semicon industry, the micro-nano process technology using photoetching technique as representative
Also obtained developing on a large scale very much.Photoetching process can realize the homogeneous photoresist battle array of arbitrary shape on flat substrate
The accurate preparation of row pattern, and pattern is accurately transfer on lower floor's functional material by subsequent etching processes.
With the development of nanofabrication technique, nanometer embossing, interfere exposure technique, phase detachment technique, from group
Dress innovation type photoetching technique occurs successively, and these technologies can realize homogeneous high-resolution function material
Expect prepared by the low-cost high-efficiency of nano-grain array pattern.On the other hand, electron-beam direct writing, laser direct-writing,
The appearance of the photoetching techniques such as focused ion beam direct write so that functional material nano particle is prepared on flat substrate
The shape of array can be arbitrary X-Y scheme, and resolution ratio is very high.However, above-mentioned photoetching technique system
Standby functional material nano-grain array is all simply on smooth solid substrate surface, and which has limited these nanometers
The application of particle.If these nano particles can be transferred in liquid phase environment, nano particle will be expanded significantly
Application.
The content of the invention
In view of the above circumstances, should it is an object of the invention to provide a kind of sheet liquid phase nanometer grain preparation method
Method obtains the nano particle on flat substrate using patterning techniques and lithographic technique, then passes through suitable liquid
Body, which dissolves sacrifice layer, is distributed to nano particle in liquid, and so as to obtain sheet liquid phase nano particle, it is special
Point is that process cycle is short, and technique is simple, efficiency high, and particle pattern is any, and embodiment is various, applicability
By force, cost is low, and the nanoplatelet size of preparation is small, and thickness of thin, homogeneity is good, reproducible, can
Prepare the nanoplatelet of the arbitrary levels combination of a variety of different materials of single or multiple lift.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of sheet liquid phase nanometer grain preparation method, comprises the following steps：
Step 1) deposits soluble thin film sacrificial layer material on flat substrate；
Step 2) deposits functional material on sacrifice layer again；
Step 3) deposits in function material layer and prepares the nano-pattern of polymeric material；
Step 4) is using the nano-pattern of polymeric material as etching mask, using lithographic technique by nano-pattern
It is transferred in the function material layer of lower floor, then unnecessary polymeric material is removed with lithographic technique；
Step 5) is dissolved sacrifice layer using suitable liquid, while obtains the sheet functional material nanometer of liquid phase
Particle, grain shape are consistent with nano-pattern.
The flat substrate of the step 1) is silicon chip, quartz plate, sheet glass, flat polymeric diaphragm.
The thin film sacrificial layer material of described step 1) is soluble polymer, oxide, metal material,
Its depositional mode is spin-coating, thermal evaporation deposition, epitaxial growth, chemical vapor deposition, and physical vapor is sunk
Product.
The functional material of the step 2) is metal, metal oxide, graphene, two-dimensional film material, half
Conductor material, polymeric material or composite；Function material layer is one or more layers combination of above-mentioned material
Form, its depositional mode is spin-coating, thermal evaporation deposition, epitaxial growth, chemical vapor deposition or physics
Vapour deposition；The thickness of function material layer is between 0.1-50000 nanometers.
The polymer nanocomposite pattern technology of preparing of the step 3) is nanometer embossing, photoetching technique, phase
Isolation technics or self-assembling technique；Polymeric material is nano impression glue, photoresist, the block that can be separated
Polymer or polymer nano-microspheres.
For the line width of the polymer nanocomposite pattern of the step 3) between 5-50000 nanometers, pattern form can be with
It is random two-dimensional plane pattern.
The lithographic technique of described step 4) is plasma etching, ion beam etching, wet etching or electrification
Learn etching.
The dissolving liquid of described step 5) is water, the aqueous solution, organic liquid, organic solution；Dissolving method
For immersion, concussion or ultrasound.
Beneficial effects of the present invention are as follows：
The invention provides a kind of sheet liquid phase nanometer grain preparation method, and skill is prepared with existing liquid phase nano particle
Art is compared and had an advantageous effect in that：The present invention is obtained on flat substrate using patterning techniques and lithographic technique
Nano particle, then sacrifice layer is dissolved by suitable liquid nano particle is distributed in liquid, so as to
Obtain sheet liquid phase nano particle.Because the material for forming nano particle is deposited by way of deposition film
On substrate, can prepare in this way a variety of different materials of single or multiple lift arbitrary levels combination piece
Shape nano particle；According to depositional mode and material difference, the most thin flake nano that can obtain 0.1 nano thickness
Particle.Because preparation process can use multiple polymers nano-pattern technology of preparing, so the preparation method has
It is that process cycle is short to have feature, and embodiment is various, and particle pattern is any, and strong applicability, cost is low, system
Standby nanoparticle size is small, and homogeneity is good, it is reproducible the advantages of.
Brief description of the drawings
The sheet liquid phase nano particle that Fig. 1 is the present invention prepares schematic diagram.
Wherein, 1 flat substrate, 2 sacrifice layers, 3 function material layers, 4 polymer nanocomposite patterns, 5 dissolving sacrifice layers
Liquid, 6 liquid phase nanoplatelets.
Fig. 2 is the annular nano-pattern scanning electron microscope diagram of nano impression glue in the technology of the present invention.
Fig. 3 is the annular liquid phase sheet gold nano grain scanning electron microscope diagram of the preparation of the present invention.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples：
Such as Fig. 1 to Fig. 3, a kind of sheet liquid phase nanometer grain preparation method, comprise the following steps：
Step 1) deposits soluble thin film sacrificial layer material on flat substrate；
Step 2) deposits functional material on sacrifice layer again；
Step 3) deposits in function material layer and prepares the nano-pattern of polymeric material；
Step 4) is using the nano-pattern of polymeric material as etching mask, using lithographic technique by nano-pattern
It is transferred in the function material layer of lower floor, then unnecessary polymeric material is removed with lithographic technique；
Step 5) is dissolved sacrifice layer using suitable liquid, while obtains the sheet functional material nanometer of liquid phase
Particle, grain shape are consistent with nano-pattern.
The flat substrate of the step 1) is silicon chip, quartz plate, sheet glass, flat polymeric diaphragm.
The thin film sacrificial layer material of described step 1) is soluble polymer, oxide, metal material,
Its depositional mode is spin-coating, thermal evaporation deposition, epitaxial growth, chemical vapor deposition, and physical vapor is sunk
Product.
The functional material of the step 2) is metal, metal oxide, graphene, two-dimensional film material, half
Conductor material, polymeric material or composite；Function material layer is one or more layers combination of above-mentioned material
Form, its depositional mode is spin-coating, thermal evaporation deposition, epitaxial growth, chemical vapor deposition or physics
Vapour deposition；The thickness of function material layer is between 0.1-50000 nanometers.
The polymer nanocomposite pattern technology of preparing of the step 3) is nanometer embossing, photoetching technique, phase
Isolation technics or self-assembling technique；Polymeric material is nano impression glue, photoresist, the block that can be separated
Polymer or polymer nano-microspheres.
For the line width of the polymer nanocomposite pattern of the step 3) between 5-50000 nanometers, pattern form can be with
It is random two-dimensional plane pattern.
The lithographic technique of described step 4) is plasma etching, ion beam etching, wet etching or electrification
Learn etching.
The dissolving liquid of described step 5) is water, the aqueous solution, organic liquid, organic solution；Dissolving method
For immersion, concussion or ultrasound.
Example is prepared as with specific annular liquid phase sheet gold nano grain and introduces preparation method.Its preparation process is as follows：
(1) layer of polyethylene base pyrrolidone polymer sacrifice layer is deposited with spin-coating method on silicon chip.
(2) deposited by electron beam evaporation deposits the functional material layer gold of one layer of nanometer grade thickness on sacrifice layer again.
(3) deposit one layer of nano impression glue with spin-coating in functional material layer gold and prepared with nanometer embossing
The annular nano-pattern (such as Fig. 2) of nano impression glue.
(4) using the annular nano-pattern of nano impression glue as etching mask, using lithographic technique by nano-pattern
It is transferred in the layer gold of lower floor, then nano impression glue is removed with lithographic technique.
(5) utilize pure water by sacrifice layer PVP by ultrasonic dissolution, while obtain the sheet of aqueous phase
Annular gold nano grain, grain shape are consistent with the nano-pattern of nano impression glue (such as Fig. 3).
The above-described embodiments are merely illustrative of preferred embodiments of the present invention, not to the present invention
Spirit and scope be defined, under the premise of design concept of the present invention is not departed from, ordinary skill in this area
The all variations and modifications that technical staff makes to technical scheme, the protection of the present invention all should be fallen into
Scope, the claimed technology contents of the present invention have all been recorded in detail in the claims.
Claims (8)
- A kind of 1. sheet liquid phase nanometer grain preparation method, it is characterized in that comprising the following steps：Step 1) deposits soluble thin film sacrificial layer material on flat substrate；Step 2) deposits functional material on sacrifice layer again；Step 3) deposits in function material layer and prepares the nano-pattern of polymeric material；Step 4) is using the nano-pattern of polymeric material as etching mask, using lithographic technique by nano-pattern It is transferred in the function material layer of lower floor, then unnecessary polymeric material is removed with lithographic technique；Step 5) is dissolved sacrifice layer using suitable liquid, while obtains the sheet functional material nanometer of liquid phase Particle, grain shape are consistent with nano-pattern.
- A kind of 2. sheet liquid phase nanometer grain preparation method according to claim 1, it is characterised in that：It is described The flat substrate of step 1) is silicon chip, quartz plate, sheet glass, flat polymeric diaphragm.
- A kind of 3. sheet liquid phase nanometer grain preparation method according to claim 1, it is characterised in that：It is described The thin film sacrificial layer material of step 1) be soluble polymer, oxide, metal material, it is heavy Product mode is spin-coating, thermal evaporation deposition, epitaxial growth, chemical vapor deposition, physical vapour deposition (PVD).
- A kind of 4. sheet liquid phase nanometer grain preparation method according to claim 1, it is characterised in that：It is described The functional material of step 2) is metal, metal oxide, graphene, two-dimensional film material, semiconductor Material, polymeric material or composite；Function material layer be above-mentioned material one or more layers combination and Into its depositional mode is spin-coating, thermal evaporation deposition, epitaxial growth, chemical vapor deposition or physics Vapour deposition；The thickness of function material layer is between 0.1-50000 nanometers.
- A kind of 5. sheet liquid phase nanometer grain preparation method according to claim 1, it is characterised in that：It is described The polymer nanocomposite pattern technology of preparing of step 3) is nanometer embossing, photoetching technique, is separated Technology or self-assembling technique；Polymeric material is nano impression glue, photoresist, and the block that can be separated gathers Compound or polymer nano-microspheres.
- A kind of 6. sheet liquid phase nanometer grain preparation method according to claim 1, it is characterised in that：It is described For the line width of the polymer nanocomposite pattern of step 3) between 5-50000 nanometers, pattern form can be appointed Meaning two dimensional surface pattern.
- A kind of 7. sheet liquid phase nanometer grain preparation method according to claim 1, it is characterised in that：It is described The lithographic technique of step 4) be plasma etching, ion beam etching, wet etching or electrochemistry are carved Erosion.
- A kind of 8. sheet liquid phase nanometer grain preparation method according to claim 1, it is characterised in that：It is described The dissolving liquid of step 5) be water, the aqueous solution, organic liquid, organic solution；Dissolving method is leaching Bubble, concussion or ultrasound.
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| CN201610333421.5A CN107381498A (en) | 2016-05-17 | 2016-05-17 | A kind of sheet liquid phase nanometer grain preparation method |
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Cited By (3)
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| CN110656311A (en) * | 2019-09-20 | 2020-01-07 | 南京大学 | Method for preparing nano particles from top to bottom |
| CN110875108A (en) * | 2019-11-29 | 2020-03-10 | 南昌航空大学 | Preparation method of metal grid type transparent electrode |
| CN111424235A (en) * | 2020-04-14 | 2020-07-17 | 武汉理工大学 | Magnetic nanocrystalline sheet-shaped absorbent and preparation method thereof |
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| CN110875108A (en) * | 2019-11-29 | 2020-03-10 | 南昌航空大学 | Preparation method of metal grid type transparent electrode |
| CN111424235A (en) * | 2020-04-14 | 2020-07-17 | 武汉理工大学 | Magnetic nanocrystalline sheet-shaped absorbent and preparation method thereof |
| CN111424235B (en) * | 2020-04-14 | 2021-01-01 | 武汉理工大学 | Magnetic nanocrystalline sheet-shaped absorbent and preparation method thereof |
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