CN109950157A - Biochemical sensor and preparation method thereof based on nanometer sheet stacked structure - Google Patents
Biochemical sensor and preparation method thereof based on nanometer sheet stacked structure Download PDFInfo
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Abstract
The invention discloses a kind of biochemical sensor and preparation method thereof based on nanometer sheet stacked structure.The hanging stacked structure of the multilayer with sensitive material that the multiple pileup layer that the biochemical sensor includes: SOI substrate, is made of selective etch sacrificial layer/sensitive material is formed, the positive electrode being formed on the hanging stacked structure of multilayer and negative electrode, the active film to be ended up with active group for being attached to the hanging stacked structure surface of multilayer；When biochemical sensor works, positive electrode, negative electrode are connected with the cathode of the anode of variable voltage source and ammeter respectively, and the cathode of variable voltage source is connected with the anode of ammeter.Its production method includes: cleaning silicon chip；Grow sacrificial layer/sensitive material multiple pileup layer；Graphical multiple pileup layer；Make electrode；Sacrificial layer part in selective etch multiple pileup layer；Active agent modification.Biochemical sensor of the invention is at low cost, sensitivity and precision are high；The present invention being capable of batch micro operations biochemical sensor efficiently at low cost.
Description
Technical field
The present invention relates to a kind of biochemical sensor and preparation method thereof based on nanometer sheet stacked structure, belongs to biochemical sensitive
Device technical field.
Background technique
Biological and chemical sensor (biochemical sensor) is in many necks such as biomedicine, chemical industry, environmental monitoring, food hygiene
Domain has extensive and important application.The application demand constantly extended proposes higher and higher performance to biochemical sensor and wants
Ask, not only will selectively good, high sensitivity, analysis speed it is fast, at low cost, also to have micromation, it is integrated, automate and
The advantages that can continuously being monitored on-line in complex system.Biochemical sensor can substantially be divided into: resistor-type, it is capacitive, two
Pole pipe type, bipolar transistor cast and field-effect cast；Wherein, resistor-type biochemical sensor because its structure is simple, precision is high,
Measurement range is wide, the service life is long and is easily achieved micromation etc., studies the most extensive.Resistor-type biochemical sensor base
Present principles are exactly the variation of measurand to be converted into the variation of resistance value, then show or record quilt through corresponding measuring circuit
The variation of measured value.
So far, in the manufacturing process of biochemical sensor, it usually needs it is tested to provide to make additional fluid channel
The carrying environment of object.The production of fluid channel needs the process flow of a series of complex such as photoetching, overmolded and bonding, largely
On improve device design and production complexity, increase cost of manufacture.In order to reduce the cost of manufacture of device while meet
Sight has been turned to three-dimensional (3D) device by sensor micromation and integrated requirement, researcher, is glued using with graphene
The internal stress that the attached good SU-8 photoresist of property is formed under non-abundant exposure, driving graphene film self assembly are with specific
Three-dimensional (3D) device of shape.Three-dimensional (3D) structure makes the haptoreaction of graphene and tested substance in unit chip area
Area greatly increases, and provides more attachment points for measured object Molecular Adsorption and doping, to improve the entirety of sensor
Performance.This micro-pipe shape 3D graphene sensor based on SU-8 stressor layers has a natural fluid channel, without additional system
The devices such as fluid channel, sealing are made, the complexity of device design and production is reduced, but the device manufacture difficulty is big, operation
Weak, the poor reliability of property, to limit it in the application in biochemical sensor field.
Summary of the invention
The purpose of the present invention is to provide a kind of biochemical sensors based on nanometer sheet stacked structure, to overcome conventional planar
The problems such as two-dimentional (2D) biochemical sensor is at high cost, sensitivity and precision are low.
Another object of the present invention is to provide a kind of production methods of biochemical sensor, being capable of efficient, low cost
Three-dimensional (3D) biochemical sensor of the miniature stack of ground batch micro operations.
To achieve the above object, the invention adopts the following technical scheme:
A kind of biochemical sensor based on nanometer sheet stacked structure, comprising: SOI substrate, by selective etch by sacrificing
Layer/sensitive material constitute multiple pileup layer and formed the hanging stacked structure of the multilayer with sensitive material, be formed in multilayer
The vacantly positive electrode on stacked structure and negative electrode, the work to be ended up with active group for being attached to the hanging stacked structure surface of multilayer
Property film；When the biochemical sensor works, positive electrode, the negative electrode cathode with the anode of variable voltage source and ammeter respectively
It is connected, the cathode of variable voltage source is connected with the anode of ammeter.
The sacrificial layer is the thin-film materials such as germanium (Ge), germanium silicon (SiGe), and selection criteria is that the etching liquid of sacrificial layer will not
Sensitive material, positive electrode and negative electrode are had an impact；The sensitive material is silicon (Si), the conductive films such as silver-colored (Ag)
Material；Multilayer refers to two layers or two layers or more.Wherein each sacrificial layer, sensitive material thickness be respectively 10nm-100 μm.
The positive electrode and negative electrode use chrome gold (Cr/Au), titanium/gold (Ti/Au), palladium/gold (Pd/Au), titanium/platinum
(Ti/Pt) the common electrodes material production such as, wherein the adhesive layer materials such as chromium (Cr), titanium (Ti), palladium (Pd) with a thickness of 5nm-
30nm, golden (Au), platinum (Pt) etc. conductive layers with a thickness of 10nm-1 μm.
The active film includes 3- (2,3 the third oxygen of epoxy) propyl trimethoxy silicane, 3- aminopropyl triethoxysilane
And glutaraldehyde etc., being formed by active group is amino, carboxyl or aldehyde radical.
A kind of production method of the biochemical sensor based on nanometer sheet stacked structure, includes the following steps:
Step 1: cleaning silicon chip.SOI substrate is placed in the hydrogen peroxide and sulfuric acid mixture liquid that proportion is 1: 4, at 85 DEG C
Silicon wafer is boiled into 15min, removes superficial stain, then with diluted hydrofluoric acid clean 3min, removes surface natural oxidizing layer, finally
It is rinsed with deionized water, is dried with nitrogen or dryer dries.
Step 2: growth sacrificial layer/sensitive material multiple pileup layer.Utilize chemical vapor deposition (CVD) or reduced pressure chemical
The film deposition techniques such as vapor deposition apparatus (RPCVD) grow sacrificial layer/sensitive material multiple pileup layer in SOI substrate.
Step 3: graphical multiple pileup layer.Using photoetching technique, using photoresist as barrier layer, etched with RIE non-lithography
Glue covers multiple pileup layer, cleans the photoresist of multiple pileup layer surface with acetone later；
Step 4: production electrode.Using photoetching technique, sputtering or electron beam evaporation technique, removing (lift-off) technology system
Standby positive electrode and negative electrode.Photoresist aperture is formed in positive electrode and negative electrode region by photoetching first, then uses thermal evaporation
Or electron beam evaporation technique deposits metal material, finally removes the metal of photoresist and attachment on a photoresist using stripping technology
Material leaves electrode pattern, completes the preparation of positive electrode 3 and negative electrode 4；
Step 5: the sacrificial layer part in selective etch multiple pileup layer.Chip after the electrode that completes is immersed into etching
In liquid, the etching sacrificial layer that etching liquid can be selective forms the three-dimensional (3D) with the hanging stacked structure of multilayer of sensitive material
Structure；After the water cleaning 5min that the laboratory sample etched is taken out to and spent immediately ion, dried up with high pressure nitrogen；
Step 6: active agent modification.Chip after etching sacrificial layer is immersed to the mixing of 70 DEG C of the concentrated sulfuric acid and hydrogen peroxide
In solution, constant temperature 1-5h carries out hydroxylating processing；It cleans, dries immediately after, be immersed in concentrated hydrochloric acid and the nothing that volume ratio is 1: 1
Sour processing is carried out in the mixed liquor of water-ethanol, the processing time is 1-24h；It is immersed in active agent solution, soaks after cleaning drying
The bubble time is 0.5-7d；5min successively is cleaned with ethyl alcohol and deionized water later, is put into baking oven drying, active agent is completed and repairs
Decorations；
Step 7: positive electrode, negative electrode are connected with the cathode of the anode of variable voltage source and ammeter respectively, it is adjustable
The cathode of voltage source is connected with the anode of ammeter；Complete the production of the biochemical sensor based on nanometer sheet stacked structure.
Compared to the prior art the present invention, has the advantages that
(1) compared with two-dimensional surface sensor, this three-dimensional (3D) biochemical sensor based on nanometer sheet stacked structure is big
While amplitude reduces chip area footprints, holding even increases sensitive material and contacts with test substance (gas or liquid)
With the area to react, the responsiveness and susceptibility of sensor are improved.The micromation of this and biochemical sensor, integrated hair
Exhibition trend is consistent.
(2) stacked structure reduces the complexity of design and the production of biochemical sensor, improves its reliability.It is based on
The three-dimensional stacked formula structure that the biochemical sensor of nanometer sheet stacked structure is formed by selective etch, its spacing is at tens nanometers
Adjustable in tens micron ranges, to have stronger capillarity to liquid test substance, when work, can be by denier
Solution to be measured be automatically drawn into sensitive material conduction channel region complete detection.This self assembly sensor is not necessarily to additional miniflow
The accessories such as road, sealing device improve reliability to reduce the difficulty and cost of manufacture craft.
Detailed description of the invention
Fig. 1 is that the present invention is based on the structural schematic diagrams of the biochemical sensor of nanometer sheet stacked structure.
Fig. 2 is that the present invention is based on the production flow diagrams of the biochemical sensor of nanometer sheet stacked structure.
Specific embodiment
It elaborates with reference to the accompanying drawing to the present invention, but is not meant to limiting the scope of the invention.
As shown in Figure 1, including: SOI substrate 1 the present invention is based on the biochemical sensor of nanometer sheet stacked structure, passing through selection
Property the multiple pileup layer that is made of sacrificial layer/sensitive material of etching and the hanging stacked structure of the multilayer with sensitive material that is formed
8, the positive electrode 3 and negative electrode 4 that are formed on the hanging stacked structure of multilayer, be attached to the hanging stacked structure surface of multilayer with work
Property group ending active film 7；The biochemical sensor work when, positive electrode 3, negative electrode 4 respectively with variable voltage source 5 just
The cathode of pole and ammeter 6 is connected, and the cathode of variable voltage source 5 is connected with the anode of ammeter 6.
As shown in Fig. 2 (a)-(g), the production method of the biochemical sensor of the invention based on nanometer sheet stacked structure includes
Following steps:
Step 1: cleaning silicon chip.SOI substrate is placed in the hydrogen peroxide and sulfuric acid mixture liquid that proportion is 1: 4, at 85 DEG C
Silicon wafer is boiled into 15min, removes superficial stain, then with diluted hydrofluoric acid clean 3min, removes surface natural oxidizing layer, finally
It is rinsed with deionized water, is dried with nitrogen or dryer dries.
Step 2: growth sacrificial layer/sensitive material multiple pileup layer 2.Utilize chemical vapor deposition (CVD) or decompressionization
It learns the film deposition techniques such as vapor deposition (RPCVD) equipment and grows sacrificial layer/sensitive material multiple pileup layer in SOI substrate 1
2.Wherein sacrificial layer, sensitive material with a thickness of 10nm-10 μm.
Step 3: the multiple pileup layer 2 of graphical sacrificial layer/sensitive material.Using photoetching technique, using photoresist as resistance
Barrier etches sacrificial layer/sensitive material multiple pileup layer 2 of unglazed photoresist covering with RIE, cleans sacrifice with acetone later
The photoresist on 2 surface of multiple pileup layer of layer/sensitive material.
Step 4: production electrode.Using photoetching technique, sputtering or electron beam evaporation technique, removing (lift-off) technology system
Standby positive electrode 3 and negative electrode 4.Photoresist aperture is formed in positive electrode 3 and 4 region of negative electrode by photoetching first, then with heat
Evaporation or electron beam evaporation technique deposit metal material, finally remove photoresist using stripping technology and adhere on a photoresist
Metal material leaves electrode pattern, completes the preparation of positive electrode 3 and negative electrode 4.
Step 5: the sacrificial layer part in selective etch sacrificial layer/sensitive material multiple pileup layer 2.It will complete
Chip after electrode immerses in etching liquid, and the etching sacrificial layer that etching liquid can be selective, being formed has the multilayer of sensitive material outstanding
Three-dimensional (3D) structure of empty stacked structure；The laboratory sample etched is taken out and the water for spending ion immediately cleans 5min
Afterwards, it is dried up with high pressure nitrogen.
Step 6: active agent modification.Chip after etching sacrificial layer is immersed to the mixing of 70 DEG C of the concentrated sulfuric acid and hydrogen peroxide
In solution, constant temperature 1-5h carries out hydroxylating processing；It cleans, dries immediately after, be immersed in concentrated hydrochloric acid and the nothing that volume ratio is 1: 1
Sour processing is carried out in the mixed liquor of water-ethanol, the processing time is 1-24h；It is immersed in active agent solution, soaks after cleaning drying
The bubble time is 0.5-7d；5min successively is cleaned with ethyl alcohol and deionized water later, is put into baking oven drying, active agent is completed and repairs
Decorations.
Step 7: positive electrode 3, negative electrode 4 are connected with the cathode of the anode of variable voltage source 5 and ammeter 6 respectively,
The cathode of variable voltage source 10 is connected with the anode of ammeter 6；Complete the system of the biochemical sensor based on nanometer sheet stacked structure
Make.
Detection method using the above-mentioned biochemical sensor based on nanometer sheet stacked structure is as follows:
Sensor is placed in detection environment (liquid medium or gas medium) first；Biochemical substances particle to be measured and activity
Film 7 forms adsorption, and the surface of the hanging stacked structure 8 of multilayer with sensitive material generates the change of electric field or potential
Change, to change the resistivity of sacrificial layer/sensitive material multiple pileup layer 2；Multilayer with sensitive material vacantly stacks knot
The change of 8 resistivity of structure can be under certain anode voltage (the voltage V between positive electrode 3 and negative electrode 4), by detecting it
The variation of electric current (the electric current I between positive electrode 3 and negative electrode 4) is detected.To the hanging heap of multilayer with sensitive material
Doping level suffered by the surface of stack structure 8 (corresponding with the type of tested biochemical substances and concentration) can be detected.
That is the type (Type) and concentration (Concentration) of test substance are the functions of I, can be acquired by analytical Calculation.
Claims (9)
1. a kind of biochemical sensor based on nanometer sheet stacked structure characterized by comprising SOI substrate is carved by selectivity
Lose the multiple pileup layer that is made of sacrificial layer/sensitive material and formed the hanging stacked structure of the multilayer with sensitive material, shape
At on the hanging stacked structure of multilayer positive electrode and negative electrode, be attached to the hanging stacked structure surface of multilayer with active group
The active film of ending；The biochemical sensor work when, positive electrode, negative electrode respectively with the anode of variable voltage source and electric current
The cathode of table is connected, and the cathode of variable voltage source is connected with the anode of ammeter.
2. biochemical sensor according to claim 1, which is characterized in that the sacrificial layer is germanium or germanium-silicon thin membrane material；
The sensitive material is silicon or silver-colored conductive film material；The multilayer is two layers or two layers or more.
3. biochemical sensor according to claim 1, which is characterized in that the thickness difference of each sacrificial layer, sensitive material
It is 10nm-100 μm.
4. biochemical sensor according to claim 1, which is characterized in that the positive electrode and negative electrode using chrome gold,
The production of titanium/gold, palladium/gold or titanium/platinum electrode material, wherein chromium, titanium, palladium adhesive layer material with a thickness of 5nm-30nm, gold, platinum
Conductive layer with a thickness of 10nm-1 μm.
5. biochemical sensor according to claim 1, which is characterized in that the active film is 3- (2,3 the third oxygen of epoxy)
Propyl trimethoxy silicane or 3- aminopropyl triethoxysilane and glutaraldehyde, be formed by active group be amino, carboxyl or
Aldehyde radical.
6. a kind of production method of the biochemical sensor described in claim 1 based on nanometer sheet stacked structure, which is characterized in that
Include the following steps:
Step 1: cleaning SOI substrate；
Step 2: growing sacrificial layer/sensitive material multiple pileup layer in SOI substrate using film deposition technique；
Step 3: using photoetching technique, using photoresist as barrier layer, etch unglazed photoresist with RIE and cover multiple pileup layer, later
The photoresist of multiple pileup layer surface is cleaned with acetone；
Step 4: positive electrode and yin are prepared using photoetching technique, sputtering or electron beam evaporation technique, removing (lift-off) technology
Electrode；
Step 5: the chip after the electrode that completes being immersed in etching liquid, the sacrificial layer portion in selective etch multiple pileup layer
Point, form three-dimensional (3D) structure with the hanging stacked structure of multilayer of sensitive material；
Step 6: being immersed in active agent solution after the chip after etching sacrificial layer is cleaned drying, carry out active agent and repair
Decorations；
Step 7: positive electrode, negative electrode are connected with the cathode of the anode of variable voltage source and ammeter respectively, adjustable voltage
The cathode in source is connected with the anode of ammeter；Complete the production of the biochemical sensor based on nanometer sheet stacked structure.
7. production method according to claim 6, which is characterized in that the film deposition technique is heavy for reduced pressure chemical vapor
Product technology.
8. production method according to claim 6, which is characterized in that the cleaning process of the SOI substrate are as follows: serve as a contrast SOI
Bottom is placed in proportion as silicon wafer is boiled 15min at 85 DEG C in 1: 4 hydrogen peroxide and sulfuric acid mixture liquid, removes superficial stain, then
With diluted hydrofluoric acid clean 3min, surface natural oxidizing layer is removed, is finally rinsed with deionized water, is dried with nitrogen or dries
Machine drying.
9. production method according to claim 6, which is characterized in that by the dense of 70 DEG C of chip immersion after etching sacrificial layer
In the mixed solution of sulfuric acid and hydrogen peroxide, constant temperature 1-5h carries out hydroxylating processing；It cleans immediately after, dries, be immersed in volume
Than carrying out sour processing in the mixed liquor of concentrated hydrochloric acid and dehydrated alcohol for 1: 1, the processing time is 1-24h；It is submerged after cleaning drying
In active agent solution, soaking time 0.5-7d；5min successively is cleaned with ethyl alcohol and deionized water later, is put into baking oven baking
It is dry, complete active agent modification.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113340950A (en) * | 2021-05-28 | 2021-09-03 | 苏州锐光科技有限公司 | Capacitive humidity sensor and manufacturing method thereof |
| CN116482051A (en) * | 2023-06-14 | 2023-07-25 | 有研工程技术研究院有限公司 | Infrared frequency band biochemical sensor and preparation method and application thereof |
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