CN105869807B - A kind of preparation method of zinc oxide bismuth thin film piezoresistor - Google Patents
A kind of preparation method of zinc oxide bismuth thin film piezoresistor Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
- H01C7/105—Varistor cores
- H01C7/108—Metal oxide
- H01C7/112—ZnO type
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- H—ELECTRICITY
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- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
- H01C17/075—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thin film techniques
- H01C17/12—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thin film techniques by sputtering
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Abstract
The present invention relates to a kind of preparation method of zinc oxide bismuth thin film piezoresistor, belongs to electronic information material preparation and its applied technical field.The present invention utilizes radio frequency magnetron sputtering method, using the sintering ZnO of non-stoichiometricn(n<1) it is matrix target, other metals or its oxide are doping target, and under the sputtering technology of optimization, deposition obtains the zinc-oxide film of low-resistivity on conductive substrate, then it is embedded in bismuth oxide powder and carries out hot dipping, obtains zinc oxide bismuth thin film piezo-resistance.The features such as this thin film piezoresitive device non-linear behaviour is excellent, pressure sensitive voltage is controllable, leakage current is small, have wide practical use in extensive or super large-scale integration overvoltage protection.This method thin film deposition and hot dipping condition are strictly controllable, and process repeatability is good, can be formed on large area substrates, structure and thin-film device in uniform thickness, are adapted to large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of zinc oxide-bismuth oxide thin film piezoresitive device, belong to electronic information material
Preparation and its applied technical field.
Background technology
Piezoresistor (Varistor) is that electric current by it is with applying at a certain temperature with particular voltage range
The voltage increase that adds and the semiconductor material devices that increased dramatically, it is widely used in suppressing the valve components of transmission line of electricity surge and each
Over-voltage protection element of kind electronic component etc..
At present, commercialized piezoresistor is mainly with ZnO-Bi2O3For the composite ceramic material electronic component of base.And
This ZnO varistor material is formed with zinc oxide, bismuth oxide and various other additive metal oxide mixed sinterings,
Such as (F.Jiang, et al.Journal of Advanced such as nickel oxide, manganese oxide and rare-earth oxide
Ceramics,2013,2:201-212.).The key structure of this piezo-resistance is the zinc oxide grain of semiconduction by high resistance
Bi2O3Grain boundary layer coats, and the two is mutually combined closely forms double Schottky barriers between crystal grain, turns into a piezo-resistance
Unit, then multiple piezo-resistance units are by being composed in series a piezoresistor.In other words, ZnO-Bi2O3Ceramics are pressure-sensitive
The pressure-sensitive character of resistor comes from its grain boundary effect, and its typical structure is that the oxidized bismuth thin film of zinc oxide grain is coated with shape completely
Into effective crystal boundary；Grain resistance is lower, and grain boundary structure is more complete or resistance is higher, piezo-resistance it is non-linear better.
With developing rapidly for electronic technology, the size of electronic device constantly reduces, to the small form factor requirements of element increasingly
Strongly, operating voltage constantly reduces, and the piezoresistor as protection semiconductor element must also develop towards low pressure direction.
Realize ZnO-Bi2O3Ceramic varistor device low pressureization and the main path of miniaturization are：Control ZnO crystallite dimensions and reduce and press
Quick resistance thickness.Conventional method has solid sintering technology, the tape casting etc..But solid sintering technology prepares low-voltage ZnO-Bi2O3Pressure
Sensitive resistor is difficult to further minimize due to the limitation of technology；And the tape casting prepares low-voltage ZnO-Bi2O3Piezoresistor technique
Process is complicated, and homogeneity of product is poor.On the other hand, due to the development of surface engineering technology, it is small that filming turns into piezoresistor
One effective way of type, causes extensive concern.Such as Suzuoki utilizes rf magnetron sputtering sputtering method on a glass substrate
It deposited ZnO/Bi2O3Bilayer film, thickness are respectively l μm/0.3 μm, and device pressure sensitive voltage is less than 10V, and with larger non-
Linear coefficient (Y.Suzuoki, et al.Journal of Physics D, 1987,20:511-517).In addition, with other
Thin film technique, such as Sol-Gel spray heating decompositions, pulsed laser deposition can also prepare the various pressure-sensitive electricity of ZnO polycrystal films
Hinder device.These researchs show, filming is to develop the effective means of low-voltage piezoresistor, and to be advantageous to element small-sized for filming
Change and integrated.
In numerous membrane deposition methods, magnetron sputtering method is a kind of ripe film preparing technology, is widely used；With it
Its method is compared, and magnetron sputtering method deposited thin film material has that tack is good, and consistency is high, and growth temperature is low, and deposition velocity is fast,
It can be considered as being very suitable for large-scale industry metaplasia in different growth atmospheres the advantages that large-area preparation of thin film material
Production.But because magnetron sputtering method prepares composite zinc oxide-bismuth oxide laminated film and multilayer zinc oxide/bismuth oxide film pressure
The process of quick resistance is relative complex or is not easy to build ZnO-Bi2O3The typical structure of piezoresistor, preparation hitherto
ZnO-Bi2O3The nonlinear factor of thin film piezoresitive is generally relatively low.
Therefore, the present invention utilizes radio frequency magnetron sputtering method, with the sintering ZnO of non-stoichiometricn(n<1) it is matrix target
Material, other metals or its oxide are doping target, and under the magnetron sputtering technique of optimization, deposition obtains low on conductive substrate
The zinc-oxide film of resistivity, then it is embedded in bismuth oxide powder and carries out hot dipping, to builds with complete crystal boundary
ZnO-Bi2O3The typical structure of piezoresistor, obtain high performance zinc oxide-bismuth oxide thin film piezoresitive.With this side
Thin film piezoresitive device prepared by method, have the controllable composition of material, simple in construction, piezoresistor device shape and film thickness can
Control, compact structure, the features such as non-linear behaviour is excellent, pressure sensitive voltage is controllable, leakage current is small, extensive or ultra-large integrated
Have wide practical use in the overvoltage protection of circuit.And zinc oxide-bismuth oxide thin film piezoresitive is prepared in this way,
Thin film deposition and hot dipping condition are strictly controllable, and process repeatability is good, can be formed on large area substrates, structure and thickness
Uniform thin-film device is spent, is adapted to large-scale production.
The content of the invention
It is an object of the invention to propose a kind of preparation method of zinc oxide-bismuth oxide thin film piezoresitive.With this side
Thin film piezoresitive device prepared by method, the zinc oxide grain in rheostat film be oxygen-starved zinc oxide or doping zinc-oxide, electric
Resistance rate is low；And zinc oxide grain is oxidized bismuth thin layer and coated completely, grain boundary structure is complete, forms effective crystal boundary, therefore obtained
The non-linear behaviour for obtaining zinc oxide-bismuth oxide piezo-resistance is excellent.This thin film piezoresitive device, the composition with material can
Control, simple in construction, piezoresistor device shape and film thickness is controllable, compact structure, non-linear behaviour are excellent, pressure sensitive voltage can
Control, the features such as leakage current is small, have wide practical use in extensive or super large-scale integration overvoltage protection.And
Zinc oxide-bismuth oxide thin film piezoresitive is prepared in this way, and thin film deposition and hot dipping condition are strictly controllable, and technique repeats
Property it is good, can be formed on large area substrates, structure and thin-film device in uniform thickness, be adapted to large-scale production.
The preparation method of zinc oxide-bismuth oxide thin film piezoresitive proposed by the present invention, it is characterised in that methods described profit
With radio frequency magnetron sputtering method, using the sintering ZnO of non-stoichiometricn(n<1) it is matrix target, other metals or its oxidation
Thing is doping target, and under the magnetron sputtering technique of optimization, deposition obtains the zinc-oxide film of low-resistivity on conductive substrate,
Then it is embedded in bismuth oxide powder and carries out hot dipping, obtains high performance zinc oxide-bismuth oxide thin film piezoresitive.
The preparation method of zinc oxide-bismuth oxide thin film piezoresitive proposed by the present invention, comprises the following steps and content：
(1) in magnetron sputtering apparatus, with the sintering ZnO of non-stoichiometricn(n<1) it is matrix target, other metals
Or its oxide is doping target, and target is fixed on target position；Cleaning substrate is fixed on sample stage；Open mechanical pumping
To low vacuum, system vacuum opens molecular pump when reaching 0.1Pa, until the vacuum of system reaches 2 × 10-4More than Pa.
(2) argon working gas is passed through, carries out pre-sputtering first, the pollutant of target material surface is removed with this；When aura is steady
After deciding, start the sputtering sedimentation of zinc-oxide film.
(3) prepared film sample is taken out from magnetron sputtering apparatus, the zinc-oxide film prepared is embedded in Bi2O3
Hot dipping is carried out in powder.After hot dipping, by sample furnace cooling to room temperature.
(4) in the upper and lower surface (film and substrate) of the sample of gained laminated film containing zinc oxide-bismuth oxide respectively by
Electrode, that is, obtain the piezoresistor.
In above-mentioned preparation method, the magnetron sputtering apparatus in the step (1) is rf magnetron sputtering device.
In above-mentioned preparation method, the sintering ZnO of the non-stoichiometric in the step (1)nMiddle n 0.6-0.99 it
Between.
In above-mentioned preparation method, the doping target in the step (1) is in metal Fe, Co, Ni, Mn and its oxide
One or more.
In above-mentioned preparation method, the substrate in the step (1) is one in highly doped conductive silicon chip, copper sheet, platinized platinum
Kind.
In above-mentioned preparation method, the method for substrate cleaning treatment is in the step (1)：First by substrate be put into acetone,
10min is cleaned with ultrasonic wave respectively in ethanol, removes the greasy dirt and other pollutants of substrate surface；Then, rushed through deionized water
Wash；Finally, with dry N2Vacuum chamber is quickly put into after air-blowing is dry.
In above-mentioned preparation method, the purity of the argon gas in the step (2) is in more than 99.99vol.%.
In above-mentioned preparation method, the argon gas pre-sputtering time is 2-10min in the step (2).
In above-mentioned preparation method, the zinc-oxide film sputtering sedimentation condition in the step (2) is：Using Ar as sputtering gas
Body, in Ar or Ar/O2In mixed gas, at ambient temperature, ZnO is sputterednTarget and doping metals or oxide target, sputtering power
For 60-220W, sputtering pressure 0.4-4.0Pa, sedimentation time 20-75min.
In above-mentioned preparation method, in the step (2) when thin film sputtering deposits, the purity of used oxygen exists
More than 99.99vol.%, O2The volume ratio of the two is 1-2 in/Ar mixed gas.
In above-mentioned preparation method, sputtering sedimentation is obtained in the step (2) zinc-oxide film undoped with when be
Oxygen-starved zinc-oxide film, it is doping zinc-oxide film in doping.
In above-mentioned preparation method, the Bi in the step (3)2O3Powder is pure for commercially available analysis.
In above-mentioned preparation method, the hot-dip process condition in the step (3) is：In Muffle furnace, temperature 200-
600 DEG C, soaking time 20-120min.
In above-mentioned preparation method, the electrode material in the step (4) is one kind in silver, aluminium, palladium, platinum, gold.
The zinc oxide-bismuth oxide thin film piezoresitive device prepared using this technology, the composition with material is controllable, structure is simple
Single, piezoresistor device shape and film thickness is controllable, compact structure, non-linear behaviour is excellent, pressure sensitive voltage is controllable, leakage current is small
The features such as, have wide practical use in extensive or super large-scale integration overvoltage protection.And because film
Thickness is controllable, and this piezoresistor can either use on high working voltage or low-work voltage electrical equipment.In addition,
Zinc oxide-bismuth oxide thin film piezoresitive is prepared in this way, and thin film deposition and hot dipping condition are strictly controllable, and technique repeats
Property it is good, can be formed on large area substrates, structure and thin-film device in uniform thickness, be adapted to large-scale production.
Brief description of the drawings
Fig. 1 is zinc oxide-bismuth oxide thin film piezoresitive device schematic diagram proposed by the invention
Fig. 2 is laminated film in oxygen-starved zinc oxide-bismuth oxide thin film piezoresitive device obtained by the embodiment of the present invention 1
SEM photograph
Fig. 3 is the E-J curves of the oxygen-starved zinc oxide-bismuth oxide thin film piezoresitive device obtained by the embodiment of the present invention 1
Fig. 4 is laminated film in doping zinc-oxide-bismuth oxide film piezoresistor obtained by the embodiment of the present invention 2
SEM photograph
Fig. 5 is the E-J curves of doping zinc-oxide-bismuth oxide film piezoresistor obtained by the embodiment of the present invention 2
Embodiment
Technical scheme is described further with reference to embodiment.
The preparation method of zinc oxide-bismuth oxide thin film piezoresitive proposed by the present invention, it is characterised in that methods described profit
With radio frequency magnetron sputtering method, using the sintering ZnO of non-stoichiometricn(n<1) it is matrix target, other metals or its oxidation
Thing is doping target, and under the magnetron sputtering technique of optimization, deposition obtains the zinc-oxide film of low-resistivity on conductive substrate,
Then it is embedded in bismuth oxide powder and carries out hot dipping, obtains high performance zinc oxide-bismuth oxide thin film piezoresitive.
The preparation method of zinc oxide-bismuth oxide thin film piezoresitive proposed by the present invention, comprises the following steps and content：
(1) in rf magnetron sputtering equipment, with the sintering ZnO of non-stoichiometricn(n=0.6-0.99) it is matrix target
One or more in material, metal Fe, Co, Ni, Mn and its oxide are doping target, and target is fixed on target position；Will be clear
Clean substrate is fixed on sample stage；Open mechanical pump and be evacuated to low vacuum, system vacuum opens molecular pump when reaching 0.1Pa, directly
Vacuum to system reaches 2 × 10-4More than Pa.
(2) argon working gas that purity is more than 99.99vol.% is passed through, pre-sputtering 2-10min is carried out first, with this
Remove the pollutant of target material surface；After aura settles out, start the sputtering sedimentation of zinc-oxide film.
(3) prepared film sample is taken out from magnetron sputtering apparatus, in Muffle furnace, the zinc oxide films prepared
Film is embedded in the commercially available pure Bi of analysis2O3Hot dipping is carried out in powder, hot dipping temperature is 200-600 DEG C, soaking time 20-120min.Heat
After leaching, by sample furnace cooling to room temperature.
(4) substrate is one kind in highly doped conductive silicon chip, copper sheet, platinized platinum, and the method for its cleaning treatment is：First will
Substrate is put into acetone, ethanol and cleans 10min with ultrasonic wave respectively, removes the greasy dirt and other pollutants of substrate surface；Then,
Through deionized water rinsing；Finally, with dry N2Vacuum chamber is quickly put into after air-blowing is dry.
(5) the sputtering sedimentation condition of the zinc-oxide film is：Using Ar as sputter gas, in Ar or Ar/O2Mixed gas
In, at ambient temperature, sputter ZnOnTarget and doping metals or oxide target, sputtering power 60-220W, sputtering pressure are
0.4-4.0Pa, sedimentation time 20-75min.And when thin film sputtering deposits, the purity of used oxygen exists
More than 99.99vol.%, O2The volume ratio of the two is 1-2 in/Ar mixed gas；The zinc-oxide film obtained undoped with when
It is doping zinc-oxide film in doping for oxygen-starved zinc-oxide film.
(6) in the upper and lower surface (film and substrate) of the sample of gained laminated film containing zinc oxide-bismuth oxide respectively by
Electrode, that is, obtain the piezoresistor (see Fig. 1).
(7) electrode material is one kind in silver, aluminium, palladium, platinum, gold.
Resulting piezo-resistance film is bluish violet film in appearance.
Under a scanning electron microscope, it may be observed that the surface compact pore-free of gained zinc oxide-bismuth oxide laminated film,
Crystal grain is uniform and circularity is high.Current-voltage performance test shows that the film of this structure has good pressure-sensitive character.
In a word, high performance zinc oxide-bismuth oxide thin film piezoresitive device can be obtained with this technology.
Embodiment 1：By ZnO0.78Target and the highly doped conductive silicon chip of cleaning are fixed on the phase of rf magnetron sputtering equipment
Answer on position, close chamber, first open mechanical pump and be evacuated to low vacuum 0.1Pa, be then turned on molecular pump and be evacuated to high vacuum 2 × 10-4Pa。
It is passed through high-purity argon gas, pre-sputtering 10min.Deposit at ambient temperature, then pass to Ar/O2Than for 1:1 mixed gas, sputtering
Power is 220W, sputtering pressure 1.0Pa, sedimentation time 20min.Obtain oxygen-starved zinc-oxide film.Then, preparing
Zinc-oxide film be embedded in analytically pure Bi2O3Carry out hot dipping in powder, temperature is 400 DEG C, soaking time 40min, after by sample with
Stove is cooled to room temperature.Silver paste is applied as electrode in sample upper and lower surface, lead of burn-oning, that is, is obtained piezoresistor, is tested its pressure
Quick performance.
The oxygen-starved zinc oxide-bismuth oxide laminated film surface compact pore-free obtained, crystal grain uniformly and circularity
High (see Fig. 2), nonlinear characteristic is excellent (see Fig. 3), nonlinear factor 15.1, the minimum 0.0223mA/cm of leakage current2, pressure
Quick voltage is 0.0176V/nm.
Embodiment 2：By ZnO0.99Target, pure Fe targets and the highly doped conductive silicon chip of cleaning are fixed on magnetron sputtering apparatus
On relevant position, chamber is closed, mechanical pump is first opened and is evacuated to low vacuum 0.1Pa, be then turned on molecular pump and be evacuated to high vacuum 2 × 10- 4Pa.It is passed through high-purity argon gas, pre-sputtering 2min.Deposit at ambient temperature, only logical argon gas, while open ZnO0.99Target and pure Fe
Target, sputtering power 60W, sputtering pressure 2.0Pa, sedimentation time 60min.Obtain Fe2O3 doping zinc-oxide film.Then,
The zinc-oxide film prepared is embedded in analytically pure Bi2O3Carry out hot dipping in powder, temperature is 500 DEG C, soaking time 60min, after will
Sample furnace cooling is to room temperature.Silver paste is applied as electrode in sample upper and lower surface, lead of burn-oning, that is, is obtained piezoresistor, is surveyed
Try its voltage-dependent characteristic.
The oxygen-starved zinc oxide-bismuth oxide laminated film surface compact pore-free (see Fig. 4) obtained, nonlinear characteristic is excellent
Different (see Fig. 5), nonlinear factor 11.8, the minimum 0.0306mA/cm of leakage current2, pressure sensitive voltage 0.0137V/nm.
Claims (4)
1. a kind of preparation method of zinc oxide-bismuth oxide thin film piezoresitive device, it is characterised in that methods described utilizes radio-frequency magnetic
Sputtering method is controlled, using the n of non-stoichiometric<1 sintering ZnOnFor matrix target, other metals or its oxide are doping
Target, under the magnetron sputtering technique of optimization, on conductive substrate deposition obtain low-resistivity oxygen-starved zinc-oxide film or
Person's doping zinc-oxide film, is then embedded in bismuth oxide powder and carries out hot dipping, and it is thin to obtain high performance zinc oxide-bismuth oxide
Film pressure-sensitive resistance, comprises the following steps：
(1) in rf magnetron sputtering equipment, with the sintering ZnO of non-stoichiometricnFor matrix target, metal Fe, Co, Ni, Mn
And its one or more in oxide are doping target, and target is fixed on target position；Cleaning substrate is fixed on sample stage
On；Open mechanical pump and be evacuated to low vacuum, system vacuum opens molecular pump when reaching 0.1Pa, until the vacuum of system reaches 2
×10-4More than Pa；
(2) argon working gas is passed through, carries out pre-sputtering 2-10min first, the pollutant of target material surface is removed with this；Work as aura
After settling out, at ambient temperature, in argon gas or in argon gas and oxygen mix atmosphere, the sputtering for starting zinc-oxide film is sunk
Product；
(3) prepared film sample is taken out from magnetron sputtering apparatus, in Muffle furnace, the zinc-oxide film prepared is buried
In the commercially available pure Bi of analysis2O3Hot dipping is carried out in powder；After hot dipping, by sample furnace cooling to room temperature；
(4) gained laminated film containing zinc oxide-bismuth oxide sample film and substrate surface respectively by electrode, that is, obtain institute
State piezoresistor.
2. according to the preparation method described in claim 1, it is characterised in that the ZnO in the step (1)nN in matrix target
Value is between 0.6-0.99；The doping target is the one or more in metal Fe, Co, Ni, Mn and its oxide；The base
Piece is one kind in highly doped conductive silicon chip, copper sheet, platinized platinum；Argon gas and oxygen in the step (2) are high-purity gas, pure
Degree is in more than 99.99vol.%；Bi in the step (3)2O3Powder is ommercially available AR；Electricity in the step (4)
Pole material is one kind in silver, aluminium, palladium, platinum, gold.
3. according to the preparation method described in claim 1, it is characterised in that the sputtering of zinc-oxide film is sunk in the step (2)
Product condition be：Using Ar as sputter gas, in Ar or Ar/O2It is at ambient temperature, independent to sputter ZnO in mixed gasnTarget, simultaneously
Sputter ZnOnTarget and doping metals target or ZnO is sputtered simultaneouslynThe oxide target of target and doping metals, sputtering power 60-
220W, sputtering pressure 0.4-4.0Pa, sedimentation time 20-75min；And thin film sputtering is deposited on pure argon or volume ratio
For 1-2 O2Carried out in/Ar mixed gas；The zinc-oxide film obtained undoped with when be oxygen-starved zinc-oxide film,
It is doping zinc-oxide film during doping.
4. according to the preparation method described in claim 1, it is characterised in that the hot dipping work of zinc-oxide film in the step (3)
Skill condition is：Hot dipping temperature is 200-600 DEG C, soaking time 20-120min.
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| CN107293384B (en) * | 2017-06-28 | 2019-10-01 | 中国地质大学（北京） | A kind of preparation method of tin oxide base thin film piezoresistor |
| CN114235904B (en) * | 2021-12-17 | 2022-11-01 | 电子科技大学 | Ppb-level hydrogen sensor and preparation method thereof |
| CN115612995A (en) * | 2022-09-15 | 2023-01-17 | 广东省科学院测试分析研究所(中国广州分析测试中心) | Preparation method of bismuth oxide film and reconfigurable photoelectric logic gate |
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| CN100481280C (en) * | 2004-04-05 | 2009-04-22 | 广州新日电子有限公司 | Low temp sintered ZnO multilyer pressure sensitive resister and manufacturing method thereof |
| CN101246770B (en) * | 2008-03-25 | 2011-03-30 | 华东师范大学 | Preparation of high-potential gradient ZnO thick film piezoresistor |
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