CN106645357B - A kind of preparation method of crystalline nanowire bioprobe device - Google Patents
A kind of preparation method of crystalline nanowire bioprobe device Download PDFInfo
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- CN106645357B CN106645357B CN201610899426.4A CN201610899426A CN106645357B CN 106645357 B CN106645357 B CN 106645357B CN 201610899426 A CN201610899426 A CN 201610899426A CN 106645357 B CN106645357 B CN 106645357B
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- G—PHYSICS
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- 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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- 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
- G01N27/4145—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS specially adapted for biomolecules, e.g. gate electrode with immobilised receptors
Abstract
A kind of preparation method of crystalline nanowire bioprobe device, comprising: 1) using with certain degree of hardness, surface of the supportive material of resistance to 350 DEG C of temperature as clean substrates；2) the guidance channel of depth about 90nm-350nm bioprobe shape is produced by chemical wet etching technology on substrate；3) growing method is guided by plane nano line, grows the crystalline nanowire of diameter about 50 ± 10nm diameter exactly along the guidance channel, form the nano wire of bioprobe shape；4) pass through photoetching and evaporation coating technique in the bimetallic arm of the production 80-120nm thickness of bioprobe nano wire two sides as metal electrode；5) pass through transfer nano wire bioprobe on substrate.The present invention, which can facilitate, to be carried out other electricity device connections and integrates, so that more convenient to the measurement of micro- sodium substance.The technology provides key technology basis for high performance field effect transistors, sensor and photoelectric device based on planar semiconductor nano wire.
Description
One, technical field
The present invention relates to biomaterial and devices field, more particularly to crystalline nanowire bioprobe device and preparation,
It is related on substrate using channels direct transverse direction nanowire growing technique, by micro fabrication, production forms the spy of micro-nano biology
The production method of needle device products.The present invention is the integrated planar semiconductor nano wire preparation of channels direct oriented growth, electricity
Bioprobe method.
Two, background technique
The semiconductor devices such as current social, microelectronics and opto-electronic device have been widely used for modern science and technology, national warp
Every aspect in Ji and daily life, the epitaxy technology of these Semiconductor Devices and Materials various in style are closely related.
The mechanism of liquid-liquid phase-solid phase (SLS) growth mechanism SLS growth is somewhat similarly to VLS mechanism, the area with VLS mechanism
It is not only that, in VLS mechanism growth course, required raw material are provided by gas phase；And in SLS mechanism growth course, institute
The raw material needed is provided from solution, and in general, in the method common low-melting-point metal (such as In, Sn or Bi), which is used as, helps
Solvent (fluxdroplet), the catalyst being equivalent in VLS mechanism.
The magnitude and biological cell scale of nano wire are close, and silica-base material is similar with the carbon based material attribute of structoure of the human body,
It is harmless, it is degradable, silicon-based nano science and technology and biological field are combined, huge effectiveness will be obtained.
Three, summary of the invention
In view of the above-mentioned problems, preparing high quality flat surface semiconductor bioprobe nanometer it is an object of the present invention to provide a kind of
The method of line device part.Especially planar semiconductor nano-wire devices are prepared along specific channel oriented growth, transfer and integrated approach.
The present invention takes following technical scheme: a kind of preparation method of crystalline nanowire bioprobe device, feature step
It suddenly include: 1) using with certain degree of hardness, surface of the supportive material of resistance to 350 DEG C of temperature as clean substrates；2) in substrate
The upper guidance channel that depth about 100 ± 10nm (it is deep to be no more than 350nm) bioprobe shape is produced by chemical wet etching technology；
3) it reuses lithography alignment technology and defines catalyst area on the specific position of channel, guided and grown by plane nano line
Method grows the crystalline nanowire of diameter about 50 ± 10nm diameter exactly along the guidance channel of probe location, shape
At the nano wire of bioprobe shape；Electrode evaporation metal (e.g., Al, Pt), be guide channel specific position formed tens to
Electrode section of 100 nanometers of the metal film pattern as metal probe；
Further, the bimetallic arm of 80-120nm thickness is made on bioprobe by photoetching and evaporation coating technique；4)
On substrate by transfer nano wire bioprobe, it is encapsulated to obtain the final product, micro-nano cell, solution can be detected after test.
The substrate is silicon wafer, glass or potsherd, silicon wafer p-type or n type single crystal silicon piece, p-type or N-type polycrystalline silicon
Piece, glass are simple glass, the amorphous body substrate such as quartz glass.
In step 3), lithography alignment technology catalyst area on the position of channel is reused, plane nano line is passed through
Growing method is guided, makes the crystalline nanowire of diameter about 50 ± 10nm diameter exactly along the guidance channel of probe location
Growth forms the nano wire of bioprobe shape；In is deposited, the catalyst metals such as Sn are that channel specific position is guided to be formed
Tens nanometers of metal film pattern；Plasma treatment technique is utilized in a pecvd system, is carried out in 350 DEG C, power 2-5W
Processing makes metal film contracting ball formation diameter in several hundred nanometers to the quasi- catalyzing nano-particles between several microns；Reuse PECVD
System covers the amorphous silicon of the amorphous silicon (several nanometers are arrived several hundred nanometers) of one layer of suitable thickness as presoma dielectric layer；In vacuum
It under atmosphere, anneals in 350 DEG C of environment, using IP-SLS growth pattern, so that nano wire is from catalyst area along guidance channel
Growth, forms and obtains the nano wire of bioprobe shape.
Guidance channel is made by chemical wet etching method；Wherein lithographic method wet etching: potassium hydroxide (KOH), hydrogen
The alkaline corrosions systems such as sodium oxide molybdena (NaOH) are also possible to hydrofluoric acid+nitric acid (HF+HNO3), hydrofluoric acid+nitric acid+acetic acid (HF+
The sour corrosions system such as HNO3+CH3COOH), can also be ethylene diamine pyrocatechol (Ethylene
The systems such as DiaminePyrocatechol)；Or use dry etching, i.e., it is performed etching using ICP-RIE.
Crystalline nanowire is grown, the crystalline materials such as nano wire Si, Ge, SiGe, Ga are formed.
Electrode metal uses PT (12nm)-AL (80nm) system, can be Ti-Au system, is Ni metal, and metal contact is equal
Contact performance is improved using rapid thermal annealing process.Thermal evaporation system or electron beam evaporation system can be used.
Using photoetching treatment probe window portion, window is performed etching using HF, so that probe part is hanging, side
Just it uses.Preparation method of the present invention, bioprobe are characterized in high mobility (100 ㎝ of >2/ v.s) high on-off ratio (> 106),
Subthreshold voltage is less than the high performance device of (160mV/) close to 0, SSD；
The crystalline nanowire bioprobe device obtained according to preparation method, wherein the angle of bioprobe head includes 1-
Various angles in 90 °, probe total length use length from 20nm~10um, probe nano wire in 50~100um, probe
For Si, Ge, SiGe, the preparation of the crystalline materials such as Ga, diameter is in 20-80nm.
The device of high electrology characteristic is produced with chemical wet etching.The contact of its metal uses PT (12nm)-AL (80nm) system,
Or Ti-Au system or Ni metal, metal contact improve contact performance using rapid thermal annealing process.Heat can be used to steam
Hair system or electron beam evaporation system.
Bioprobe is characterized in high mobility (100 ㎝ of >2/ v.s) high on-off ratio (> 106), subthreshold voltage is close
It is less than the high performance device of (160mV/) in 0, SSD.
The present invention, using the guiding role for guiding step in plane nano line growth course, is obtained by making specific channel
High quality is obtained voluntarily to the nano wire biological probe array of arrangement, and is shifted and is integrated with device, high-performance biology is obtained and visits
Needle device, and the method that micro-nano cell, solution can be detected.The present invention uses conventional PECVD, a variety of films such as CVD
Depositing system and micro-machining system are realized.Solve the various semiconductor nanowires using silicon as representative, in particular pilot channel
Extensive guidance growth, and it is fabricated to the key technical problem of bioprobe.The present invention emphasizes, due to such nano wire and guidance
The contact interface of channel can effectively adjust and fixation of the metal arm to nano wire, and plane nano line can be with further progress
It removes and is transferred on other flexible substrates.Due to the presence of bimetallic arm, can facilitate carry out the connection of other electricity devices and
It is integrated, so that more convenient to the measurement of micro- sodium substance.The present invention is the high-performance field-effect based on planar semiconductor nano wire
Transistor, sensor and photoelectric device provide key technology basis.
The present invention anneals (temperature is at 280 DEG C or more) in a vacuum or in the non-oxidizing atmospheres such as hydrogen, nitrogen, utilizes
IP-SLS growth pattern obtains the nano wire of channel step guidance, as bioprobe nano wire；Existed using photoetching evaporation coating technique
Bimetallic arm is formed on bioprobe, forms device.The present invention can be with due to the contact interface of such nano wire and guidance channel
It effectively adjusts and fixation of the metal arm to nano wire, plane nano line can be removed with further progress and to be transferred to other soft
Property substrate.Due to the presence of bimetallic arm, it can facilitate and carry out other electricity device connections and integrate, so as to micro- sodium substance
Measurement it is more convenient.The present invention is high performance field effect transistors, sensor and photoelectricity based on planar semiconductor nano wire
Device provides key technology basis.
Beneficial effects of the present invention, the present invention grow receiving for channel step guidance using the methods of IP-SLS in pecvd
Rice noodles, and carry out being fabricated to bioprobe device using modern micro-processing technology.IP-SLS method can with growth plane nano wire,
The planar semiconductor monocrystal nanowire of high quality, specific shape can be grown in conjunction with step channels direct technology.Pass through light
Self-positioning, the self orientation of nanowire growth are achieved that after the catalyst area of guidance channel and positioning that lithographic technique is formed.
Since such nano wire and guidance channels cross-section can be adjusted effectively, in addition the fixation of bimetallic arm and integrated, it can be further
It is removed (such as etch removing) and is transferred on other flexible substrates.Integrated and probe due to bimetallic arm is opened
Mouthful, it may be convenient to it carries out the integrated of device and uses.The present invention prepares the method for bioprobe nano-wire devices in plane half
High performance field effect transistors, sensor, photoelectric device and the application aspect in biological detection field of nanowires have extensively
Wealthy prospect.
Four, Detailed description of the invention
Fig. 1: plane bioprobe nano-wire devices preparation process flow chart；
Fig. 2: plane bioprobe nano-wire devices schematic illustration；
Fig. 3: plane bioprobe nano-wire devices SEM shape appearance figure；
Fig. 4: plane bioprobe nano-wire devices electric property figure.
Five, specific embodiment
To make the purpose of the present invention, technical solution, effect and being a little more clearly understood that, below in conjunction with specific example, to this hair
It is bright to carry out further explanation in detail.Flow chart is as shown in Fig. 1.A kind of growth of plane bioprobe nano-wire devices turns
The technology of shifting and integrated planar semiconductor nano wire.It is that oriented growth, transfer and integrated planar semiconductor under specific channel is received
The method of rice noodles, its step are as follows: 1) passing through acetone, alcohol, deionized water ultrasonic treatment by soda acid hot solution or respectively
The crystalline substrates of covering oxide layer are handled, the impurity of removal surface attachment exposes crystal clean surface.2) light is utilized
It carves lithographic technique and defines bioprobe guidance growth channel, reuse lithography alignment technology and defined on the specific position of channel
Catalyst area.3) In is deposited, Sn metal is allowed to exist only in guidance channel specific position formation tens by lift off
The metal film pattern of nanometer；4) in a pecvd system utilize plasma treatment technique, in 350 DEG C, power 2-5W at
Reason makes metal film contracting ball formation diameter in several hundred nanometers to the quasi- catalyzing nano-particles between several microns；5) PECVD is reused
System covers the amorphous silicon of the amorphous silicon (several nanometers are arrived several hundred nanometers) of one layer of suitable thickness as presoma dielectric layer.6) true
It under empty atmosphere, anneals in 350 DEG C of environment, using IP-SLS growth pattern, so that nano wire draws from catalyst area along specific
The growth of guide channel road, forms and obtains the nano wire of bioprobe shape.7) lithography alignment technology and metal evaporation skill are utilized again
Art costs metal electrode in bioprobe nano wire two sides, serves as metal arm.8) lithographic definition probe window portion is utilized,
Window is performed etching using HF, so that probe part is hanging, is easy to use.
Substrate can be p-type, and perhaps n type single crystal silicon substrate can be p-type or N-type polycrystalline silicon piece, be also possible to common
Glass, the amorphous body substrate such as quartz glass.
Produce the guidance channel of depth about 200nm by chemical wet etching, the guidance channel (see figure one) of probe shape,
The angle of middle bioprobe head includes various angles in 1-90 °, and probe total length uses length in 50~100um, probe
From 20nm~10um.Lithographic method can use wet etching: the alkaline systems such as potassium hydroxide (KOH), sodium hydroxide (NaOH), can also
To be the acid systems such as hydrofluoric acid+nitric acid (HF+HNO3), hydrofluoric acid+nitric acid+acetic acid (HF+HNO3+CH3COOH), can also be
The systems such as ethylene diamine pyrocatechol (Ethylene DiaminePyrocatechol)；It is also possible to dry etching system, utilizes
ICP-RIE is performed etching.
The nano wire of planar growth can be Si, SiGe, Ge, Ga plaine single crystal nano-wire array, and diameter is distributed in 40~
Between 100nm.
Metal electrode is made using photoetching evaporation coating technique, thermal evaporation system, electron beam evaporation system etc., metal electricity can be used
Pole contact uses PT (12nm)-AL (80nm) system, can be Ti-Au system, can be Ni metal, and metal electrode contact makes
Contact performance is improved with rapid thermal annealing process.
It is more specific: 300nmSiO2On oxide layer substrate plane bioprobe nano-wire devices preparation the following steps are included:
1) 300nmSiO is used2Oxide layer substrate (silicon wafer through surface oxidation) uses acetone, alcohol, deionization respectively
Water ultrasonic treatment, the impurity of removal substrate surface attachment.Pure monocrystalline or polysilicon silicon wafer can be used in silicon wafer.
2) it by there is mask lithography technology to define bioprobe pattern in substrate surface, is etched using ICP-RIE on surface
Channel is formed, forms the array of bioprobe channel after cleaning photoresist.
3) it in a pecvd system, is allowed to form diameter using plasma treatment technique under 1-50W power and be received several hundred
Rice arrives the catalyzing nano-particles between several microns；Catalyzing nano-particles of the diameter at several hundred nanometers are formed at a temperature of 350 DEG C.
4) continue to cover the amorphous silicon layer of one layer of suitable thickness in a pecvd system as presoma dielectric layer；300℃-
The amorphous silicon layer of one layer of suitable thickness is covered at 400 DEG C.Annealing exists in vacuum or in the non-oxidizing atmospheres such as hydrogen, nitrogen
At 400 DEG C, the amorphous silicon of surrounding is can be absorbed in catalysis drop after being activated, and goes out plane silicon nanowires so as to induced growth,
Nano wire can form required channel along guidance trench sidewalls oriented growth simultaneously.
5) in atmosphere of hydrogen using the amorphous silicon 15 minutes of plasma treated surface remnants until surface color recovery
Normal color.
6) lithographic definition metal arm electrode pattern is reused, using electron beam evaporation technique, 10nm platinum and 60nm is deposited
Aluminium, the photoresist washed later and remaining metal.
7) carrying out window processing to probe head region using photoetching makes biology using the HF etching window region of 4% concentration
Probe head region is hanging.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
It describes in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (8)
1. a kind of preparation method of crystalline nanowire bioprobe device, characterization step includes: 1) to use to have certain degree of hardness,
Surface of the supportive material of resistance to 350 DEG C of temperature as clean substrates, the substrate are silicon wafer, glass or potsherd, silicon wafer p-type
Either n type single crystal silicon piece, p-type or N-type polycrystalline silicon piece, glass are simple glass, quartz glass；2) pass through photoetching on substrate
Lithographic technique produces the guidance channel of depth about 90nm -350 nm bioprobe shape；3) it is guided by plane nano line
Growing method grows the crystalline nanowire of diameter about 50 ± 10nm diameter exactly along the guidance channel, forms biology
The nano wire of probe shape；4) the production 80-120nm thickness by photoetching and evaporation coating technique in bioprobe nano wire two sides
Bimetallic arm is as metal electrode；5) pass through transfer nano wire bioprobe on substrate；In step 3), photoetching pair is reused
Quasi- technology catalyst area on the position of channel guides growing method by plane nano line, keeps diameter about 50 ± 10nm straight
The crystalline nanowire of diameter is grown exactly along the guidance channel of probe location, forms the nano wire of bioprobe shape；
In is deposited, Sn metal is the metal film pattern for guiding channel specific position to form tens nanometers；It utilizes in a pecvd system
Plasma treatment technique is handled in 350 DEG C, power 2-5W, so that metal film contracting ball is formed diameter and is arrived in several hundred nanometers
Quasi- catalyzing nano-particles between several microns；It reuses PECVD system and covers one layer several nanometers to the non-of several hundred nano thickness
The amorphous silicon of crystal silicon is as presoma dielectric layer；Under vacuum, anneal in 350 DEG C of environment, using IP-SLS growth pattern,
So that nano wire is grown from catalyst area along guidance channel, the nano wire of bioprobe shape is formed and obtained.
2. the preparation method of crystalline nanowire bioprobe device according to claim 1, it is characterized in that being carved by photoetching
Etching method production guidance channel；Wherein lithographic method wet etching: potassium hydroxide KOH, sodium hydroxide NaOH alkaline corrosion body
System or hydrofluoric acid+nitric acid HF+HNO3, hydrofluoric acid+nitric acid+acetic acid HF+HNO3+CH3COOH sour corrosion system or ethylenediamine
Catechol Ethylene DiaminePyrocatechol system；Or use dry etching, i.e., it is carved using ICP-RIE
Erosion.
3. the preparation method of crystalline nanowire bioprobe device according to claim 1, it is characterized in that growing crystal
Nano wire, nano wire Si, Ge, SiGe or Ga crystalline material.
4. the preparation method of crystalline nanowire bioprobe device according to claim 1, it is characterized in that metal electrode makes
With PT12nm-AL80nm system, Ti-Au system or Ni metal, metal contact improves contact using rapid thermal annealing process
Performance；Metal electrode is prepared using thermal evaporation system or electron beam evaporation system.
5. the preparation method of crystalline nanowire bioprobe device according to claim 1, it is characterized in that at using photoetching
Probe window portion is managed, window is performed etching using HF, so that probe part is hanging.
6. the preparation method of crystalline nanowire bioprobe device according to claim 1, it is characterized in that bioprobe is special
Sign is with 100 ㎝ 2/v.s of mobility >, on-off ratio > 105, height of the subthreshold voltage close to 0, SSD less than 160mV/dec
Performance device.
7. the crystalline nanowire bioprobe device that preparation method described in one of -6 obtains according to claim 1, it is characterized in that
Wherein the angle of bioprobe head includes various angles in 1-90 °, and probe total length uses length in 50 ~ 100um, probe
From 20nm ~ 10um, probe nano wire is the preparation of Si, Ge, SiGe or Ga crystalline material, and diameter is in 20-80nm.
8. the crystalline nanowire bioprobe device that preparation method described in one of -6 obtains according to claim 1, it is characterized in that
The guidance channel of depth 100 ± 10nm bioprobe shape is produced by chemical wet etching technology on substrate.
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| CN107202829A (en) * | 2017-05-02 | 2017-09-26 | 南京大学 | A kind of preparation method of crystalline nanowire bioprobe device |
| CN107460542A (en) * | 2017-06-15 | 2017-12-12 | 南京大学 | A kind of preparation method of the stretchable crystalline semiconductor nano wire based on plane nano line Alignment Design and guiding |
| CN109908464A (en) * | 2019-04-16 | 2019-06-21 | 北京师范大学 | A kind of biodegradable silicon nanometer needle injection and its application |
| CN110544656B (en) * | 2019-09-19 | 2021-10-26 | 南京大学 | Method for realizing huge transfer of Micro-LED (Micro-light-emitting diode) by using super-stretchable crystalline nanowire |
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