CN107238648A - The method of low temperature preparation two-dimension flexible ion sensing fet - Google Patents
The method of low temperature preparation two-dimension flexible ion sensing fet Download PDFInfo
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- CN107238648A CN107238648A CN201710440266.1A CN201710440266A CN107238648A CN 107238648 A CN107238648 A CN 107238648A CN 201710440266 A CN201710440266 A CN 201710440266A CN 107238648 A CN107238648 A CN 107238648A
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- metal layer
- patterned metal
- low temperature
- flexible substrate
- photoresistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/414—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS
- G01N27/4146—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS involving nanosized elements, e.g. nanotubes, nanowires
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- 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
Abstract
The invention belongs to electrochemical sensing device manufacturing technology field, specially a kind of method of low temperature preparation two-dimension flexible ion sensing fet.In the present invention, using flexible material as substrate, patterned metal layer is deposited thereon as back electrode, insulating oxide is grown on back electrode, two-dimensional semiconductor film is shifted on insulating medium layer, the conducting channel of device is used as；Source, drain region of the patterned metal layer as the device are formed on two-dimensional semiconductor film；In channel region disposed thereon functional layer material.The present invention utilizes microwave annealing technique low-temperature treatment, on the one hand improves the interfacial characteristics between device layers, the phenomenon such as sluggish, drift caused in elimination test due to boundary defect；On the other hand, by absorption of the functional layer material to microwave, the functional layer with forming nanostructured at two-dimensional semiconductor film interface can be applied to the sensing detection of different scenes.Microwave annealing technique has quickly, and low heat budget, the manufacturing cycle is short, the advantages of with low cost.
Description
Technical field
The present invention relates to two-dimensional material and electrochemical sensing device manufacturing technology field, more particularly to microwave annealing technique.
Background technology
In past decades, chemical signal is converted to electric signal and surveyed by the biology sensor based on field-effect transistor
Amount, with non-marked, quick response, low-power consumption is portable, and low cost, large-scale integrated etc. are realized using microelectronics manufacture
Advantage, in biology, medical science, industry is manufactured, and the field such as environment measuring has obtained extensive research and application.Field-effect transistor
Channel material generally has the body silicon of three-dimensional, and two-dimentional graphene, transient metal sulfide, black phosphorus, the carbon of one-dimensional nano structure are received
Mitron, silica-based nanowire etc..Wherein two-dimensional material compares three-dimensional material, because planar structure has excellent static characteristic, compares again
One-dimensional material is more stablized, it is easy to manufacture, particularly molybdenum disulfide nano sheet, and switching current ratio is far above graphene, and forbidden band is wide
Adjustable, bio-compatible is spent, is the preferable biology sensor channel material based on field-effect transistor.Molybdenum disulfide film can be with
Atomic layer level thickness is reached, therefore the input feature vector of channel carrier is very sensitive to gas absorption, produces the transfer of electric charge, is adapted to
For gas sensor.And can be carried out on molybdenum disulfide superficial growth sensitive media layer and functionalization sensitive membrane surface different
Sensor detection application.
With the progress of nano science, nano material is also widely used in the sensor of biological or environment measuring.Receive
Rice material has excellent structure, catalysis and electrochemical properties, by metal, metal oxide and carbon material of nano-scale etc.
, can be with the composition nanostructured such as the as noted above one-dimensional, two-dimensional material of nano material of different-shape as sensing interface
Significantly improve the performance of electrochemical sensor.For example, can be used for gas detection in molybdenum disulfide surface finish nano gold grain
Conductive current can be improved；Molybdenum disulfide/gold nano grain hybrid structure is modified on gold electrode, glucose oxidase is thereon
Glucose detection can be realized by completing self assembly；Nanogold particle can be used for the functionalization of sensor with oligonucleotides, realize
DNA sequencing etc..The mode of the above-mentioned useful applied field electrode of detection means, measurement electric current or impedance, also useful film is brilliant
The modes such as body pipe measurement electric current.For thin film transistor (TFT), due to the above-mentioned biology sensor advantage based on field-effect transistor, behaviour
Make more flexible and convenient, means of testing more enriches, more with application prospect.By thin film transistor (TFT) and nano-modified material knot
Close, the characteristics of such nanostructured has high sensitivity, high electron transport speed, low background current, and can be with functionalization
Sensing surface, realizes sensing measurement demand, while also make it that measurement process is simpler, convenient.
The usual process of method for synthesizing nanostructured is complicated, is difficult to control.The electricity of such as electrochemical etching or metallic particles
Deposition forms metal nanoparticle, but electrochemical method prepares nanostructured and needs professional equipment, and complex operation, cost is high
It is high；The electro-deposition of metallic particles is difficult to be formed the surface of uniform fold nano particle, limits and spreads or cause in sensing process
Diffusion layer between nano particle is overlapping, and influence is transported.Likewise, some metal oxide nanostructures such as zinc-oxide nano
Grain, generally mixes drop coating and device surface formation functionalization interface with dispersion liquid with powder solid, but the performance of device is difficult
Ensure uniformity.In addition, also there is physical technology to form film frequently with thermal evaporation, subsequent high-temperature thermal annealing causes film to reunite
Form nano particle.This physical technology is simple and easy to apply, but in view of the heat budget in integrated circuit, and bio-sensing application
The flexible material of the non-refractories such as plastics, epoxy resin is commonly used, it is necessary to find a kind of low temperature, sensor is effectively prepared and closes
Into the method for functionalization nanostructured.
The content of the invention
The present invention provides a kind of method of low temperature preparation two-dimension flexible ion sensing fet, realizes in flexible substrate
Prepare functionalized nano structure, and boost device sensing detection performance so that preparation process is simple, reduce manufacturing cost.
The method for the low temperature preparation two-dimension flexible ion sensing fet that the present invention is provided, is concretely comprised the following steps：
Non-flexible substrate is provided, the coating flexible material precursor on the non-flexible substrate forms device flexible liner after solidification
Bottom；
Patterned metal layer one is formed in the flexible substrate；
Insulating medium layer is formed in the top of patterned metal layer one；
Two-dimensional semiconductor film is shifted above the insulating medium layer as the conducting channel of device；
Patterned metal layer two is formed above the two-dimensional semiconductor film；
In the two-dimensional semiconductor film and patterned metal layer two disposed thereons modification layer material；
Process annealing processing is carried out to device using microwave annealing technique；
Device is separated from the non-flexible substrate, the device in flexible substrate with specific sensing function is obtained.
The present invention is handled using microwave annealing technique low temperature, function layer surface is reunited, in sensing interface shape
Into functionalization nanostructured, while annealing process can also improve the interfacial characteristics between each Rotating fields.
Optionally, the non-flexible substrate is monocrystalline silicon or glass etc..
Optionally, the flexible material is the organic matter for having certain ability to bear to temperature.For example, polyimides（PI）、
Polyethylene terephthalate（PET）Or epoxy resin.
Optionally, the insulating medium layer material can for once any one：
Silica（SiO2）, aluminum oxide（Al2O3）And high-k（high-k）Gate medium etc..
Optionally, the patterned metal layer one, the material of patterned metal layer two can be gold（Au）, aluminium（Al）
Deng metal.
Optionally, the forming step of the patterned metal layer one includes：
Metal level is formed in the flexible substrate；
Photoresistance is coated on the metal level, and the photoresistance is exposed and developed, graphical photoresistance is formed；
The metal level is etched using dry or wet technique, patterned metal layer one is formed.
Optionally, the forming step of the patterned metal layer one includes：
The hard mask deposition metal with figure is used in the flexible substrate, patterned metal layer one is directly formed.
Optionally, the forming step of the patterned metal layer one includes：
Metal level is formed in the flexible substrate；
Directly metal level is performed etching using focused ion beam, patterned metal layer one is formed.
Optionally, the forming step of the patterned metal layer one includes：
Photoresistance is coated in the flexible substrate；
The photoresistance is exposed and developed, patterned photoresistance is formed；
Metal level is formed on the graphical photoresistance and flexible substrate；
Using lift-off technology formation patterned metal layer one.
Optionally, the forming step of the patterned metal layer two includes：
Metal level is formed in the flexible substrate；
Photoresistance is coated on the metal level, and the photoresistance is exposed and developed, graphical photoresistance is formed；
The metal level is etched using dry or wet technique, patterned metal layer two is formed.
Optionally, the forming step of the patterned metal layer two includes：
The hard mask deposition metal with figure is used in the flexible substrate, patterned metal layer two is directly formed.
Optionally, the forming step of the patterned metal layer two includes：
Metal level is formed in the flexible substrate；
Directly metal level is performed etching using focused ion beam, patterned metal layer two is formed.
Optionally, the forming step of the patterned metal layer two includes：
Photoresistance is coated in the flexible substrate；
The photoresistance is exposed and developed, patterned photoresistance is formed；
Metal level is formed on the graphical photoresistance and flexible substrate；
Using lift-off technology formation patterned metal layer two.
Optionally, the metal level one, metal level two can by sputtering, thermal evaporation or electron beam evaporation etc. any one
Mode is formed.
Optionally, the functional layer for it is following any one：
Gold（Au）, silver（Ag）Deng metal or silica（SiO2）Zinc oxide（ZnO）, aluminum oxide（Al2O3）And high-k
（high-k）Gate medium etc..
Optionally, the two-dimensional semiconductor method for manufacturing thin film includes：Solid phase method, liquid phase method, vapor phase method.
The present invention utilizes microwave annealing technique low-temperature treatment, on the one hand improves the interfacial characteristics between device layers, eliminates
The phenomenons such as the sluggish, drift caused in test due to boundary defect；On the other hand, the absorption of microwave is made by functional layer material
With the functional layer with forming nanostructured at two-dimensional semiconductor film interface, the sensing detection applied to different scenes.Microwave
Annealing process has quickly, and low heat budget, the manufacturing cycle is short, the advantages of with low cost.
Brief description of the drawings
Fig. 1 is the method technological process of low temperature preparation two-dimension flexible ion sensing fet in first embodiment.
Fig. 2 ~ Fig. 8 is the method technological process of low temperature preparation two-dimension flexible ion sensing fet in second embodiment
Figure.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with each reality of the accompanying drawing to the present invention
The mode of applying is explained in detail.However, it will be understood by those skilled in the art that in each embodiment of the invention,
In order that reader more fully understands the application and proposes many ins and outs.But, even if without these ins and outs and base
Many variations and modification in following embodiment, can also realize each claim of the application technical side claimed
Case.
The first embodiment of the present invention is related to the method for low temperature preparation two-dimension flexible ion sensing fet.Below
Illustrated with reference to flow chart 1 and schematic diagram 2 ~ 8.As shown in figure 1, idiographic flow is comprised the steps of：
Step S1：Such as Fig. 2, there is provided a non-flexible substrate 101.
The non-flexible substrate can be monocrystalline silicon, glass etc..
Step S2：Such as Fig. 3, the coating flexible backing material presoma on above-mentioned non-flexible substrate 101 forms soft after solidification
Property substrate 102, the precursor material can be polyimides（PI）, epoxy resin or polyethylene terephthalate
（PET）Deng.
It is preferred that, select polyimides（PI）As flexible substrate persursor material, because the heat-resisting temperature of polyimide film
Degree can reach 350 DEG C or so.Heat budget in being prepared in view of subsequent technique is, it is necessary to using higher to temperature capacity
Material.
Step S3：Such as Fig. 4, patterned metal layer 1 is formed in above-mentioned flexible substrate.The material of metal level one can be with
For gold（Au）, aluminium（Al）.
It is preferred that, for technique and the stability of device performance, selection gold（Au）It is used as the material of patterned metal layer 1
Matter.
Forming the processing step of patterned metal layer 1 includes：
Photoresistance is coated in flexible substrate 102（It is not shown）, and photoresistance is exposed and developed, form graphical photoresistance；
In the graphical photoresistance and the top of flexible substrate 102 using any one sides such as sputtering, thermal evaporation or electron beam evaporations
The metal level of formula deposition patterned metal one 103 material of layer；
Patterned metal layer 1 is obtained using stripping technology.
In addition, patterned metal layer 1 can also carry out photoetching again using mask exposure etching or first deposited metal layer
Realized etc. mode, the conventional techniques that the technology is well known to those skilled in the art, therefore not to repeat here.
Step S4：Such as Fig. 5, insulating medium layer 104 is formed in above-mentioned flexible substrate 102 and patterned metal layer 1.
The insulating medium layer can be silica（SiO2）, aluminum oxide（Al2O3）And high-k（high-k）Grid
Any of which such as medium or several stacked combinations, are realized using techniques such as evaporation, sputtering or chemical vapor depositions.
Step S5：Such as Fig. 6, two-dimensional semiconductor film 105 is formed on above-mentioned insulating medium layer 104.The two dimension is partly led
Body material 105 can be transient metal sulfide such as molybdenum disulfide or black phosphorus, can be with by solid phase method, liquid phase method, vapor phase method
Obtain, the conventional techniques that the technology is well known to those skilled in the art, therefore not to repeat here.
S6：Such as Fig. 7, patterned metal layer is formed on the insulating medium layer 104 and the two-dimensional semiconductor film 105
106.Patterned metal 2 106 material of layer and preparation technology are identical with above-mentioned patterned metal layer 1, no longer go to live in the household of one's in-laws on getting married herein
State.
S7：Such as Fig. 8, functional layer is formed on the two-dimensional semiconductor film 105 and patterned metal layer 2 106
107。
The functional layer material can any one or a few combination once：
Gold（Au）, silver（Ag）Deng metal or silica（SiO2）Zinc oxide（ZnO）, aluminum oxide（Al2O3）And high-k
（high-k）Gate medium etc..
The functional layer 107 can be formed by the mode such as evaporation, sputtering or chemical vapor deposition, atomic layer deposition, should
The conventional techniques that technology is well known to those skilled in the art, therefore not to repeat here.
S8：Such as Fig. 1, after above-mentioned patterned structures are formed, using microwave annealing low-temperature treatment.
S9：Device in flexible substrate is separated from non-flexible substrate, the quick field of ion in flexible substrate is obtained
Effect transistor.
Wherein, microwave annealing technique can have different set according to differences such as the shapes, size, material of reaction cavity
Meter；The difference of the electromagnetic wave distribution in used microwave frequency and reaction cavity is for example combined, microwave annealing technique also may be used
To be adjusted accordingly, it is not limited thereto.In addition it is also possible to which there is specific space point according to the electromagnetic wave in cavity
Cloth, and the influence of the distribution inserted to microwave etc. of sample are adjusted accordingly.The input energy of microwave annealing technique, can
With the difference of the real material situation according to use, scope can be varied widely, the excursion of such as effective power can
To be 280W ~ 4200W, it might even be possible to bigger.The time of microwave annealing technique is generally extremely short, for example can be even 1 second in the several seconds
Within complete intended effect, the specific time can determine according to technique needs, equally be not construed as limiting herein.
Second embodiment of the present invention also relates to a kind of low temperature preparation two-dimension flexible ion sensing fet
Method.Second embodiment is improved on the basis of first embodiment, is in place of the main distinction：In the first embodiment party
In formula, microwave annealing low temperature process is used again after all patterned structures techniques are completed, main purpose is to form sensing
The nanostructured at interface, by absorption of the material to microwave, surface free energy changes, the pattern and characteristic of material
It can change, cause to agglomerate into island or nano particle, form functionalized sensing interface, realize different Application in Sensing；
And in this second embodiment, after the patterned metal layer 2 106 is formed, carry out a step microwave annealing technique, purpose
It is to improve the boundary between the insulating medium layer 104 and patterned metal layer 1 and the two-dimensional semiconductor film 105
Face characteristic, and improve the interfacial characteristics of the molybdenum disulfide 105 and the patterned metal layer by layer between 2 106, reduction can
Can the noise as caused by boundary defect and trapped charge, the elimination sluggishness from technique, raising switching current ratio, optimised devices
Energy.
A wherein described step microwave annealing technique after patterned metal layer 2 106 is formed due to it is first real
The microwave annealing purpose applied in mode is different, and from also there is different designs according to specific needs, two step microwave annealings are carried out altogether
Technique.Present embodiment has carried out corresponding improvement on the basis of first embodiment, to obtain functionalized sensing interface and excellent
The device performance of change.The ins and outs mentioned in first embodiment again in present embodiment still effectively, in order to reduce repetition,
Here repeat no more.
It will be understood by those skilled in the art that the respective embodiments described above are to realize the specific embodiment of the present invention,
And in actual applications, can to it, various changes can be made in the form and details, without departing from the spirit and scope of the present invention.
Claims (16)
1. a kind of method of low temperature preparation two-dimension flexible ion sensing fet, it is characterised in that comprise the steps of：
Non-flexible substrate is provided, the coating flexible material precursor on the non-flexible substrate forms device flexible liner after solidification
Bottom；
Patterned metal layer one is formed in the flexible substrate；
Insulating medium layer is formed in the top of patterned metal layer one；
Two-dimensional semiconductor film is shifted above the insulating medium layer as the conducting channel of device；
Patterned metal layer two is formed above the two-dimensional semiconductor film；
In the two-dimensional semiconductor film and patterned metal layer two disposed thereons modification layer material；
Process annealing processing is carried out to device using microwave annealing technique；
Device is separated from the non-flexible substrate, the device in flexible substrate with specific sensing function is obtained.
2. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
Non-flexible substrate is stated for monocrystalline silicon or glass.
3. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
Flexible material is stated for polyimides, polyethylene terephthalate or epoxy resin.
4. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
The material for stating patterned metal layer one and patterned metal layer two is gold or aluminium.
5. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
Stating the forming step of patterned metal layer one includes：
Metal level is formed in the flexible substrate；
Photoresistance is coated on the metal level, and the photoresistance is exposed and developed, graphical photoresistance is formed；
The metal level is etched using dry or wet technique, patterned metal layer one is formed.
6. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
Stating the forming step of patterned metal layer one includes：
The hard mask deposition metal with figure is used in the flexible substrate, patterned metal layer one is directly formed.
7. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
Stating the forming step of patterned metal layer one includes：
Metal level is formed in the flexible substrate；
Directly metal level is performed etching using focused ion beam, patterned metal layer one is formed.
8. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
Stating the forming step of patterned metal layer one includes：
Photoresistance is coated in the flexible substrate；
The photoresistance is exposed and developed, patterned photoresistance is formed；
Metal level is formed on the graphical photoresistance and flexible substrate；
Using lift-off technology formation patterned metal layer one.
9. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that institute
Two-dimensional semiconductor thin-film material is stated for transient metal sulfide or black phosphorus.
10. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that
The forming step of patterned metal layer two includes：
Metal level is formed in the flexible substrate；
Photoresistance is coated on the metal level, and the photoresistance is exposed and developed, graphical photoresistance is formed；
The metal level is etched using dry or wet technique, patterned metal layer two is formed.
11. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that
The forming step of the patterned metal layer two includes：
The hard mask deposition metal with figure is used in the flexible substrate, patterned metal layer two is directly formed.
12. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that
The forming step of the patterned metal layer two includes：
Metal level is formed in the flexible substrate；
Directly metal level is performed etching using focused ion beam, patterned metal layer two is formed.
13. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that
The forming step of the patterned metal layer two includes：
Photoresistance is coated in the flexible substrate；
The photoresistance is exposed and developed, patterned photoresistance is formed；
Metal level is formed on the graphical photoresistance and flexible substrate；
Using lift-off technology formation patterned metal layer two.
14. according to the method for one of claim 5-8,10-13 low temperature preparation two-dimension flexible ion sensing fet,
Characterized in that, the metal level one or metal level two are formed by sputtering, thermal evaporation or electron beam evaporation any one mode.
15. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that
The functional layer is any one or a few following combination：
Gold, silver or silica, zinc oxide, aluminum oxide and high-dielectric-coefficient grid medium.
16. the method for low temperature preparation two-dimension flexible ion sensing fet according to claim 1, it is characterised in that
The insulating medium layer is any one or a few following stacked combination：
Silica, aluminum oxide and high-dielectric-coefficient grid medium.
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| CN108376738A (en) * | 2018-02-27 | 2018-08-07 | 上海电力学院 | A method of realizing semiconductor alloy phase transformation using nano-metal particle assisted microwave synthesis |
| CN108845017A (en) * | 2018-05-31 | 2018-11-20 | 清华大学 | A kind of flexible ion transducer based on two tungsten selenides |
| CN110455875A (en) * | 2019-09-17 | 2019-11-15 | 重庆大学 | A kind of gas sensitive and gas sensor and preparation method thereof |
| CN111333045A (en) * | 2020-03-22 | 2020-06-26 | 昆明理工大学 | Method for electrochemically assisting preparation of doped nano black phosphorus |
| CN111681964A (en) * | 2020-05-25 | 2020-09-18 | 复旦大学 | Preparation method of device based on two-dimensional material |
| CN113571862A (en) * | 2020-07-06 | 2021-10-29 | 南通大学 | Rapid manufacturing method of flexible filter |
| US11908690B2 (en) | 2019-06-20 | 2024-02-20 | The Board Of Trustees Of The Leland Stanford Junior University | Multi-layered semiconductive device and methodology with polymer and transition metal dichalcogenide material |
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| US11908690B2 (en) | 2019-06-20 | 2024-02-20 | The Board Of Trustees Of The Leland Stanford Junior University | Multi-layered semiconductive device and methodology with polymer and transition metal dichalcogenide material |
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| CN113571862A (en) * | 2020-07-06 | 2021-10-29 | 南通大学 | Rapid manufacturing method of flexible filter |
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