CN106006539B - A kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire - Google Patents
A kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire Download PDFInfo
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- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
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- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
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- G01L9/06—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of piezo-resistive devices
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Abstract
The present invention relates to a kind of B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, including atomic force microscope probe (coating containing Pt/It), Si pieces and the B that is carried on Si pieces adulterate SiC nanowire.Its preparation method is:Organic precursor pre-process and obtains organic precursor powder, it is raw material to take organic precursor powder and boron oxide powder;Catalyst is formed in flexible substrate;Then raw material and flexible substrate are placed in atmosphere sintering furnace together, are grown through programmed cooling again after being pyrolyzed through temperature programming, prepare B doping SiC nanowires.Then B doping SiC nanowire is scattered in solvent and forms mixed solution, then B doping SiC nanowire is carried on Si pieces by the mixed solution, is prepared into the B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire that a kind of coefficient of strain is high, sensitivity is high.
Description
Technical field
The present invention relates to a kind of pressure sensor, more particularly to a kind of B doping SiC nanowire highly sensitive pressures of the big coefficient of strain
Force snesor, belongs to sensor technical field.
Background technology
Semiconductor pressure sensor because its size is small, the excellent properties such as low, sensitivity is high are consumed, in microelectromechanical systems
Received much concern in research.With the continuous progress of science and technology, people are to possessing the high sensibility pressure transducer of the big coefficient of strain
Demand is increasingly urgent.At present, use silicon materials, but silicon materials pressure sensor to be difficult to severe pressure sensor both domestic and external more
In the environment of use, particularly hot environment (250 DEG C of >).
Low-dimension nano material is considered as possessing bigger pressure drag performance because its unique pattern and structure, causes wide
General concern.At present, people are to C nano rod, ZnO nano-structure, Si3N4The pressure drag performance of the low-dimension nano materials such as nanobelt is done
Further investigation.Particularly 2006, the U.S. reported the coefficient of strain that Si nano wires possess about 5000 first, its pressure drag because
Son is higher than nearly 50 times of its body material.Further demonstrate using semiconductor low-dimension nano material as functional unit, be expected to be passed
The incomparable Large strain coefficient piezoresistive characteristic of system body material.
SiC is a kind of important third generation semi-conducting material, and its low-dimensional nano structure is due to energy gap high, height
The advantageous characteristic such as thermal conductivity and electronics saturation mobility, in photoelectricity, the power fax such as luminous, field-effect transistor and power electricity conversion
Sensor field has unique application prospect.At present, substantial amounts of work both at home and abroad reports the pressure drag spy of SiC low-dimensional nano structures
Property, such as Al doping SiC nanowire possess about 79 the coefficient of strain, N doping SiC nanowire possess about 46.2 strain system
Number, SiC nano thin-films possess about 30.3 coefficient of strain.
However, not being reported also for B doping SiC nanowire piezoresistive characteristic researchs, and possess the big coefficient of strain
Atom doped SiC nanostructureds are even more rarely has document report.
The content of the invention
The purpose of the present invention is directed to the above-mentioned problems in the prior art, it is proposed that a kind of coefficient of strain is high, sensitive
The degree B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire high.
The purpose of the present invention can be realized by following technical proposal:A kind of big coefficient of strain Gao Ling of B doping SiC nanowires
Quick pressure sensor, the pressure sensor includes atomic force microscope probe (coating containing Pt/It), Si pieces and is carried on Si pieces
On B doping SiC nanowire.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, the B doping SiC receives
Rice noodles are mono-crystalline structures.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, the pressure sensor
Preparation method be:The preparation method of the pressure sensor is:B doping SiC nanowire is scattered in solvent and forms mixing
, be carried on B doping SiC nanowire on Si pieces by the mixed solution then by solution, is prepared into pressure sensor.
Functional unit of the present invention using B doping SiC nanowires as pressure sensor, in AFM conduction mode
Under be prepared into SiC nanowire pressure sensor, by probe apply different pressures, realize the electrical signal detection under different pressures.
Preferably, the solvent is ethanol or deionized water.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, the B doping SiC receives
The preparation method of rice noodles is:Organic precursor pre-process and obtains organic precursor powder, take organic precursor powder and
Boron oxide powder is raw material;Catalyst is formed in flexible substrate;Then raw material and flexible substrate are placed in into atmosphere together to burn
In freezing of a furnace, grown through programmed cooling again after being pyrolyzed through temperature programming, prepare B doping SiC nanowires.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, organic precursor
It is the organic precursor containing Si and C element, further preferred polysilazane.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, the pretreatment includes
Heat cross-linking solidifies and grinds.
Preferably, the heat cross-linking solidification is incubated 15-50min under an inert atmosphere in being carried out at 200-300 DEG C.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, organic preceding body in raw material
The mass ratio of body powder and boron oxide powder is (3-10):1.
Preferably, the flexible substrate is carbon cloth.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, the catalyst is Co
(NO3)2、Fe(NO3)3、FeCl3In one or more.
Preferably, the catalyst forms solution in being dissolved in solvent, the concentration of catalyst is 0.01-0.1mol/L.
Preferably, the pyrolysis atmosphere argon gas in the atmosphere sintering furnace, purity is 99.99%.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, described program heats up
For:1350-1450 DEG C first is warmed up to 25-35 DEG C/min heating rates, then continues to heat up with 20-30 DEG C/min heating rates
To 1450-1600 DEG C.
In a kind of above-mentioned B doping big coefficient of strain high sensibility pressure transducers of SiC nanowire, described program cooling
For:1000-1200 DEG C first is cooled to 10-15 DEG C/min rate of temperature fall, room temperature is then cooled to the furnace.
The present invention, with carbon cloth as substrate, realizes the system of B doping SiC nanowires by organic precursor pyrolysismethod
It is standby.The B doping SiC nanowires that the preparation method is prepared are mono-crystalline structures, and with the coefficient of strain very high, sensitivity is very
It is high.Using B doping SiC nanowires as pressure sensor functional unit, pressure applied is B doping SiC nanowire footpath
To pressure, it is achieved thereby that prepared by the big highly sensitive high-temp pressure sensor of the coefficient of strain.
Compared with prior art, the present invention has following advantage:
1. the present invention is by organic precursor pyrolysismethod, with carbon cloth as substrate, realizes that the coefficient of strain is high, sensitivity
The preparation of B doping SiC nanowires high.
2. the present invention adulterates SiC nanowire as functional unit using the B that the coefficient of strain is high, sensitivity is high, realizes big
The preparation of the highly sensitive high-temp pressure sensor of the coefficient of strain.
3. the pressure sensor that the present invention is prepared has the coefficient of strain very high, and sensitivity is very high.
Brief description of the drawings
Fig. 1 is surface sweeping Electronic Speculum (SEM) figure, the transmission electron microscope of the B doping SiC nanowires obtained by the embodiment of the present invention 1
(TEM) figure, SEAD (SAED) figure and high-resolution-ration transmission electric-lens (HRTEM) figure;
Fig. 2 is X-ray diffraction (XRD) figure of the B doping SiC nanowires obtained by the embodiment of the present invention 1;
Fig. 3 is B doping SiC nanowire power spectrum (EDX) figures obtained by the embodiment of the present invention 1;
Fig. 4 is the B doping SiC nanowire pressure sensor structure schematic diagrames obtained by the embodiment of the present invention 1;
B doping SiC nanowire pressure sensors of the Fig. 5 obtained by the embodiment of the present invention 1 is under different pressures effect
Current-resistance (I-V) curve map;
B doping SiC nanowire pressure sensors of the Fig. 6 obtained by the embodiment of the present invention 1 is under different pressures effect
Resistance change curves figure;
B doping SiC nanowire pressure sensors of the Fig. 7 obtained by the embodiment of the present invention 1 is under different pressures effect
Coefficient of strain change curve.
Specific embodiment
The following is specific embodiment of the invention, and be described with reference to the drawings to technical scheme make further retouch
State, but the present invention is not limited to these embodiments.
Embodiment 1:
Initial feed chooses polysilazane, and being incubated 30min in 260 DEG C under Ar atmosphere protections carries out heat cross-linking solidification.Will
The solid that obtains of solidification is fitted into nylon resin ball grinder, and ball mill grinding is into powder.Weigh the polysilazane and 60mg of 300mg
Boron oxide powder is placed in graphite crucible bottom after uniformly mixing.5 × 5cm of carbon cloth (long × wide) is cut, is immersed in and contained
There are the Co (NO of 0.05mol/L3)2Nature is taken out in ethanol solution, after 5min to dry.Carbon cloth after treatment is placed in graphite
Crucible top, and be placed in the atmosphere sintering furnace of graphite resistance heating.Atmosphere furnace is first evacuated to 10-4Pa, being re-filled with purity is
99.99% Ar gas, until pressure is an atmospheric pressure (~0.11Mpa), hereafter pressure is constant.First with the speed of 30 DEG C/min
It is rapidly heated to 1400 DEG C from room temperature, then 1500 DEG C is continuously heating to 25 DEG C/min heating rates, then with 13 DEG C/min
Rate of temperature fall is cooled to 1100 DEG C, and last stove is cooled to room temperature, prepares B doping SiC nanowires.
The B doping SiC nanowires that embodiment 1 is prepared are taken out from atmosphere furnace, are tested, and test result is as schemed
Show.
Fig. 1 (a) is the B doping SiC nanowire SEM figures for preparing, and shows that the B for preparing doping SiC nanowire is about tens micro-
Rice, surface is smooth.Fig. 1 (b) schemes for its TEM, shows the B doping SiC nanowire diameters about 540nm for preparing.Fig. 1 (c) is
Its SEAD (SAED), shows that B doping SiC nanowires grow along [111] direction, possessesUpper surface, and be list
Crystal structure.Fig. 1 (d) is its high-resolution-ration transmission electric-lens (HRTEM) figure, shows that prepared B doping SiC nanowire is along [111]
Direction grows and crystallinity is good.
Fig. 2 is the XRD spectrum of the B doping SiC nanowires for preparing, and the phase composition for showing to prepare material is 3C-SiC, is had
Crystallinity higher.
Fig. 3 is B doping SiC nanowire power spectrum (EDX) figures for preparing, and as a result shows that B element is successfully doped into SiC nanometers
In line, and atomic ratio is about 7.18at.%.
Then B doping SiC nanowire ultrasonic disperses are formed into mixed solution in alcohol solvent, then by the mixed solution
Drop is sprinkled upon on Si pieces, B doping SiC nanowire pressure sensors is prepared under AFM conduction mode, by probe
Apply different pressures, realize the electrical signal detection under different pressures.
Fig. 4 is constructed B doping SiC nanowire pressure sensor schematic diagrames, as can be seen from Figure 4, pressure sensing of the present invention
Device includes atomic force microscope probe (coating containing Pt/It), Si pieces and the B doping SiC nanowires being carried on Si pieces.In atom
Under force microscope conduction mode, different pressures are applied in radial direction by probe, its I-V characteristic is measured under different stress, to divide
Analyse its piezoresistive effect.
Under Fig. 5 is the different stress of 51.7~181.0nN of applying, the I-V curve tested shows that B adulterates SiC nanowireSurface is radially with obvious negative pressure inhibition effect.
Fig. 6 is the resistance change curves of the B doping SiC nanowire under the different stress of 51.7~181.0nN, shows to prepare
B doping SiC nanowire resistance as the increase of pressure is constantly increasing, show as negative pressure resistance phenomenon.
Fig. 7 be 51.7~181.0nN different stress under B adulterate SiC nanowire the coefficient of strain (GF) change curve, its
The coefficient of strain is -53.0~-620.5, shows that B doping SiC nanowire possesses sensitivity very high.
In above-described embodiment and its alternative, heat cross-linking solidification temperature also include but is not limited to 200 DEG C, 205 DEG C,
210℃、215℃、220℃、225℃、230℃、235℃、240℃、245℃、250℃、255℃、265℃、270℃、275
℃、280℃、285℃、290℃、295℃、300℃;Soaking time also include but is not limited to 15min, 20min, 25min,
35min、40min、45min、50min。
In above-described embodiment and its alternative, the mass ratio of polysilazane powder and boron oxide powder is also included but not
It is limited to 3:1、4:1、6:1、7:1、8:1、9:1、10:1.
In above-described embodiment and its alternative, the concentration also including but not limited to 0.01mol/L of catalyst,
0.02mol/L、0.03mol/L、0.04mol/L、0.06mol/L、0.07mol/L、0.08mol/L、0.09mol/L、0.1mol/
L。
In above-described embodiment and its alternative, catalyst can also be Fe (NO3)3、FeCl3、Co(NO3)2With Fe
(NO3)3Mixing, Co (NO3)2With FeCl3Mixing, Fe (NO3)3With FeCl3Mixing, Co (NO3)2With Fe (NO3)3With
FeCl3Three kinds of mixing.
In above-described embodiment and its alternative, in Temperature Programmed Processes, heating rate first also includes but does not limit
In 25 DEG C/min, 26 DEG C/min, 27 DEG C/min, 28 DEG C/min, 29 DEG C/min, 31 DEG C/min, 32 DEG C/min, 33 DEG C/min, 34
DEG C/min, 35 DEG C/min, the temperature being warmed up to also include but is not limited to 1350 DEG C, 1360 DEG C, 1370 DEG C, 1380 DEG C, 1390 DEG C,
1410℃、1420℃、1430℃、1440℃、1450℃;The heating rate of next also include but is not limited to 20 DEG C/min, 21 DEG C/
Min, 22 DEG C/min, 23 DEG C/min, 24 DEG C/min, 26 DEG C/min, 27 DEG C/min, 28 DEG C/min, 29 DEG C/min, 30 DEG C/min,
The temperature being warmed up to also include but is not limited to 1450 DEG C, 1460 DEG C, 1470 DEG C, 1480 DEG C, 1490 DEG C, 1510 DEG C, 1520 DEG C,
1530℃、1540℃、1550℃、1560℃、1570℃、1580℃、1590℃、1600℃。
In above-described embodiment and its alternative, the speed of programmed cooling also include but is not limited to 10 DEG C/min, 11 DEG C/
min、12℃/min、14℃/min、15℃/min;The temperature that reaches of cooling also include but is not limited to 1010 DEG C, 1020 DEG C, 1030
℃、1040℃、1050℃、1060℃、1070℃、1080℃、1090℃、1110℃、1120℃、1130℃、1140℃、1150
℃、1160℃、1170℃、1180℃、1190℃、1200℃。
In view of the present invention program embodiment is numerous, each embodiment experimental data is huge numerous, is not suitable for arranging one by one herein
Explanation is lifted, but the content of checking required for each embodiment and the final conclusion for obtaining are approached, so herein not to each reality
The checking content for applying example illustrated one by one, only using embodiment 1 as representing the explanation excellent part of the present patent application.
This place embodiment, equally all will in the present invention to the claimed non-limit part of technical scope midrange
Ask in the range of protection.
Specific embodiment described herein is only to the spiritual explanation for example of the present invention.Technology neck belonging to of the invention
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be substituted using similar mode, but simultaneously
Do not deviate by spirit of the invention or surmount scope defined in appended claims.
It is skilled to this area although having made a detailed description and being cited some specific embodiments to the present invention
For technical staff, as long as it is obvious that can be made various changes without departing from the spirit and scope of the present invention or corrected.
Claims (10)
1. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire, it is characterised in that the pressure sensor
Including the atomic force microscope probe containing Pt/It coating, Si pieces and the B being carried on Si pieces doping SiC nanowires.
2. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 1, its feature
It is that the B doping SiC nanowire is mono-crystalline structures.
3. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 1 and 2, it is special
Levy and be, the preparation method of the pressure sensor is:B doping SiC nanowire is scattered in solvent and forms mixed solution, so
B doping SiC nanowire is carried on Si pieces by the mixed solution afterwards, pressure sensor is prepared into.
4. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 3, its feature
It is that the preparation method of the B doping SiC nanowire is:Organic precursor pre-process and obtains organic precursor powder,
It is raw material to take organic precursor powder and boron oxide powder;Catalyst is formed in flexible substrate;Then by raw material and flexibility
Substrate is placed in atmosphere sintering furnace together, is grown through programmed cooling again after being pyrolyzed through temperature programming, prepares B doping
SiC nanowire.
5. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 4, its feature
It is that organic precursor is the organic precursor containing Si and C element.
6. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 4, its feature
It is that the pretreatment includes heat cross-linking solidification and crushes.
7. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 4, its feature
It is that the mass ratio of organic precursor powder and boron oxide powder is (3-10) in the raw material:1.
8. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 4, its feature
It is that the catalyst is Co (NO3)2、Fe(NO3)3、FeCl3In one or more.
9. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 4, its feature
It is that described program heats up and is:First be warmed up to 1350-1450 DEG C with 25-35 DEG C/min heating rates, then with 20-30 DEG C/
Min heating rates are continuously heating to 1450-1600 DEG C.
10. a kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanowire according to claim 4, its feature
It is that described program cooling is:1000-1200 DEG C first is cooled to 10-15 DEG C/min rate of temperature fall, room is then cooled to the furnace
Temperature.
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