CN104776945A - Silicon nitride nanobelt high-sensitivity pressure sensor - Google Patents
Silicon nitride nanobelt high-sensitivity pressure sensor Download PDFInfo
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- CN104776945A CN104776945A CN201410501512.6A CN201410501512A CN104776945A CN 104776945 A CN104776945 A CN 104776945A CN 201410501512 A CN201410501512 A CN 201410501512A CN 104776945 A CN104776945 A CN 104776945A
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- nanobelt
- pressure transducer
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- si3n4
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Abstract
The invention discloses a method for manufacturing a Si3N4 nanobelt high-sensitivity pressure sensor. The method comprises the following specific steps: (1) putting raw materials, that is, two organic precursors polysilazane and aluminum isopropoxide into a ball-milling tank for planet ball milling in a weight ratio of 95:5; performing low-temperature cross-linking curing on the organic precursors which are uniformly mixed and reacted in the presence of N2 protecting atmosphere so as to obtain non-crystal solid; introducing 3wt% of Al metal powder as a catalyst, and performing high-energy ball-milling crushing; performing high-temperature pyrolysis on the powder obtained through high-energy ball-milling crushing by keeping the temperature of 1550 DEG C for 2 hours in the presence of the N2 protecting atmosphere, thereby preparing a Si3N4 single-crystal nanobelt; (2) performing ultrasonic dispersion on the Si3N4 single-crystal nanobelt in ethanol, and subsequently dropping and spraying onto highly oriented pyrolytic graphite. The Si3N4 nanobelt high-sensitivity pressure sensor can be constructed in an atomic force microscope conductive mode, and by exerting different pressures by using probes, electric signals can be detected under different pressures. Compared with reported operation, the Si3N4 nanobelt high-sensitivity pressure sensor manufactured by using the method can achieve feedback and detection of nN-order force, and is relatively high in sensitivity.
Description
Technical field
The present invention relates to a kind of preparation method of silicon nitride nano band high sensibility pressure transducer, belong to technical field of material.
Background technology
Sensor technology is one of gordian technique weighing modernization, being widely used of the fields such as space flight and aviation, petrochemical complex, geothermal prospecting, medical treatment and automobile.In numerous sensor, semiconductor pressure sensor receives much concern because of its excellent properties.
Along with the development of science and technology, the pressure transducer demand of people to highly sensitive high stable is day by day urgent.At present, the pressure transducer of report mainly comprises several as follows both at home and abroad: SOI (Silicon on Insulator) and the high-temp pressure sensor such as SOS (Silicon on Sapphire) monocrystalline silicon, sputtering alloy firm, polysilicon, diamond thin, optical fiber and SiC.But there is following subject matter in the sensor: 1) is difficult to the harsh operating conditions such as competent high temperature; 2) sensitivity and stability need to be improved further.
Low-dimensional Si
3n
4it is high that material has intensity, lightweight, and the excellent material resources characteristics such as good thermal shock and oxidation resistance, as structured material, are widely used at engineering field.Meanwhile, Si
3n
4belong to broadband based semiconductor (5.3 eV), be proved at present, at field of photoelectric devices such as luminescence, field effect transistors, there is unique application prospect.
2006, U.S.'s reported first piezoresistive effect of Si nanobelt.Result of study shows, its piezoresistance factor is higher than nearly 50 times of its body material, demonstrate using semiconductor low-dimension nano material as functional unit, be expected to obtain the incomparable highly sensitive piezoresistive characteristic of conventional bulk, for the research and development of high performance pressure sensor provide opportunity.In view of Si
3n
4the excellent high temperature physical characteristics of material, as adopted its monocrystal nanostructure as functional unit, will be expected to the Si realizing having excellent piezoresistive effect
3n
4the research and development of high-temp pressure sensor.But related work there is not yet bibliographical information both at home and abroad.
Summary of the invention
Technical matters to be solved by this invention realizes Si
3n
4the preparation of nanobelt high sensibility pressure transducer.
The present invention solves the problems of the technologies described above adopted technical scheme: this prepares Si
3n
4the method of nanobelt high sensibility pressure transducer, it comprises following concrete steps:
1) Si
3n
4prepared by nanobelt: by raw material polysilazane and aluminium isopropoxide two kinds of organic precursors, by weight 95:5 ratio, is placed in ball grinder planetary ball mill, makes raw material hybrid reaction even; Then by gained presoma at N
2carry out crosslinked at low temperature solidification under protective atmosphere, obtain non-crystalline solids, after high-energy ball milling abrasive dust is broken, introduces 3wt%Al metal powder while ball milling and be used as catalyzer; The powder finally obtained by high-energy ball milling, in 1550 DEG C of insulations 2 hours under N2 protective atmosphere, carries out high temperature pyrolysis, preparation Si
3n
4single crystal nano-belt.
2) pressure transducer builds: by Si
3n
4nanobelt ultrasonic disperse in ethanol, then drips and is sprinkled upon on high starch breeding sheet.Si is built under atomic force microscope conduction mode
3n
4nanobelt pressure transducer, applies different pressures by probe, realizes the electrical signal detection under different pressures.
In described step (1), the raw material of use is polysilazane and aluminium isopropoxide.Institute's use sintering furnace is graphite resistance atmosphere sintering furnace.The catalyzer introduced is Al metal powder, also can adopt other metallic elements, the protective atmosphere adopted to be purity be 99% N
2.
In described step (2), the functional unit adopted is single crystalline Si
3n
4nanobelt, to apply pressure be nanobelt radial pressure.
compared with prior art, the invention has the advantages that:
1) compared with the pressure transducer had been reported, Late Cambrian of the present invention adopts single crystalline Si
3n
4nano material is functional unit, achieves the preparation with more highly sensitive nanobelt pressure transducer.
2) compared with existing nano wire pressure transducer of reporting for work, adopt nanobelt shape structure as functional unit, when building pressure transducer, there is significant advantage, such as there is the device architecture stability of larger contact area and Geng Gao.
3) in view of Si
3n
4the physical characteristics such as high temperature resistant of material system excellence, with Si
3n
4nanobelt is functional unit, is expected to the research and development of the high-temp pressure sensor realizing highly sensitive high stable.
Accompanying drawing explanation
fig. 1for the Si obtained by the embodiment of the present invention one
3n
4scanning electron microscope (SEM) figure of nanobelt.
fig. 2for the Si obtained by the embodiment of the present invention one
3n
4transmission electron microscope (TEM) figure, power spectrum (EDX) figure of nanobelt, high-resolution-ration transmission electric-lens (HRTEM) figure and SEAD (SAED) figure thereof.
fig. 3for the real Si of the present invention
3n
4nanobelt pressure sensor structure schematic diagram.
fig. 4for the Si prepared by the embodiment of the present invention one
3n
4the current-voltage of nanobelt pressure transducer under different pressures effect (
i-V) curve map.
fig. 5for the Si prepared by the embodiment of the present invention one
3n
4nanobelt pressure transducer is resistance change curves figure under different pressures effect.
fig. 6for the Si prepared by the embodiment of the present invention one
3n
4nanobelt pressure transducer when constant pressure is 43.9nN, repeated test
i-Vcurve map.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
embodiment one
By weight taking initial feed polysilazane and aluminium isopropoxide 5g altogether for 95:5, in loading nylon resin ball grinder, planetary ball mill 12 hours, mixes and is placed in 99 aluminium oxide ceramics crucibles, at the N of 0.1MPa
2under gas shielded atmosphere in pipe type sintering furnace with 10 DEG C/min from room temperature to 260 DEG C, be incubated and carry out crosslinking curing in 0.5 hour, obtain amorphous Si AlCN solid.SiAlCN solid is loaded in nylon resin ball grinder, the Al powder adding 3wt% carries out dry ball milling as catalyzer and pulverizes 12 hours in high energy ball mill, then the SiAlCN powder obtained after being pulverized by high-energy ball milling is placed in 99 aluminium oxide ceramics crucibles, at flowing (200ml/min) N of 0.1MPa
2in tubular furnace, carry out high temperature pyrolysis from room temperature to 1550 DEG C with 20 DEG C/min under gas atmosphere protection, and at 1550 DEG C, be incubated 2 hours, then with stove cool to room temperature.Fig. 1 is prepared Si
3n
4single crystal nano-belt typical scan Electronic Speculum (SEM) photo, shows prepared Si
3n
4nanobelt any surface finish, thickness is 50nm, and width is 800nm, and length can reach several millimeters, in axial direction size uniform, has better flexibility.Fig. 2 (a)-2 (b) is prepared Si
3n
4transmission electron microscope (TEM) figure of nanobelt, Fig. 2 (c) is its power spectrum (EDX) analysis result, show that the chemical analysis of nanobelt is Si and N, and its atomic ratio is about 4:3, Fig. 2 (d) is its high-resolution-ration transmission electric-lens (HRTEM) figure, show that prepared nanobelt is mono-crystalline structures, it is its SEAD (SAED) collection of illustrative plates that the upper left corner embeds figure, shows that prepared nanobelt is α-Si3N4.Fig. 3 is constructed Si
3n
4nanobelt pressure transducer schematic diagram, under atomic force microscope conduction mode, applies different stress by probe, under different stress, detects it
i-Vcharacteristic, to analyze its piezoresistive effect.Fig. 4 is under the different pressures of applying 25.6 ~ 135.3 nN, tests
i-Vcurve, shows Si
3n
4nanobelt has obvious piezoresistive effect.Fig. 5 is the resistance change curves of nanobelt under the different pressures of 25.59 ~ 153.56nN, and when applying the change of 1nN power, ~ 3 M changes will occur the resistance of nanobelt, show Si
3n
4nanobelt pressure transducer has high sensitivity, and can realize feedback and the detection of nN level power, its piezoresistance factor is 0.75 ~ 7.7 × 10
-11pa
-1.Fig. 6 for applying pressure be 43.9 nN, duplicate detection
i-Vcurve, its testing result remains unchanged substantially, shows prepared Si
3n
4nanobelt pressure transducer has good stability.
Claims (3)
1. a Si
3n
4the preparation method of nanobelt high sensibility pressure transducer, it comprises following concrete steps:
1) material preparation: by raw material polysilazane and aluminium isopropoxide two kinds of organic precursors, by weight 95:5 ratio, is placed in ball grinder planetary ball mill, makes raw material hybrid reaction even; Then by gained presoma at N
2in carrying out crosslinked at low temperature solidification under protective atmosphere, obtaining non-crystalline solids, after high-energy ball milling abrasive dust is broken, introduces 3wt%Al metal powder while ball milling and being used as catalyzer; The powder finally obtained by high-energy ball milling, at N
2in 1550 DEG C of insulations 2 hours under protective atmosphere, carry out high temperature pyrolysis, preparation Si
3n
4single crystal nano-belt;
2) pressure transducer builds: by Si
3n
4nanobelt ultrasonic disperse in ethanol, then drips and is sprinkled upon on high starch breeding sheet, under atomic force microscope conduction mode, build Si
3n
4nanobelt pressure transducer, applies different pressures by probe, realizes the electrical signal detection under different pressures.
2. the highly sensitive Si of preparation according to claim 1
3n
4the preparation method of pressure transducer, is characterized in that: the pressure transducer functionality unit adopted in described step (1) and (2) is single crystalline Si
3n
4nanobelt.
3. preparation Si according to claim 2
3n
4the preparation method of high sensibility pressure transducer, is characterized in that: Si prepared in described step (2)
3n
4pressure transducer, can realize feedback and the detection of nN magnitude power, have high sensitivity.
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|---|---|---|---|
| CN201410501512.6A CN104776945B (en) | 2014-09-27 | 2014-09-27 | Silicon nitride nano band high sensibility pressure transducer |
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| CN201410501512.6A CN104776945B (en) | 2014-09-27 | 2014-09-27 | Silicon nitride nano band high sensibility pressure transducer |
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| CN104776945B CN104776945B (en) | 2018-08-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107271082A (en) * | 2017-05-26 | 2017-10-20 | 宁波工程学院 | A kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanobelts and preparation method thereof |
| CN108328586A (en) * | 2018-03-01 | 2018-07-27 | 西安交通大学 | A kind of nitridation silica aerogel of compressible reply and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1769547A (en) * | 2005-07-15 | 2006-05-10 | 清华大学 | Monocrystalline Si3N4 nanometer belt and micro belt preparation method |
| CN101054730A (en) * | 2007-01-30 | 2007-10-17 | 宁波工程学院 | Controllable doping method for Si3N4 single-crystal low-dimension nano material |
| CN103234670A (en) * | 2013-04-16 | 2013-08-07 | 宁波工程学院 | High-sensitivity SiC pressure sensor |
-
2014
- 2014-09-27 CN CN201410501512.6A patent/CN104776945B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1769547A (en) * | 2005-07-15 | 2006-05-10 | 清华大学 | Monocrystalline Si3N4 nanometer belt and micro belt preparation method |
| CN101054730A (en) * | 2007-01-30 | 2007-10-17 | 宁波工程学院 | Controllable doping method for Si3N4 single-crystal low-dimension nano material |
| CN103234670A (en) * | 2013-04-16 | 2013-08-07 | 宁波工程学院 | High-sensitivity SiC pressure sensor |
Non-Patent Citations (2)
| Title |
|---|
| FENGMEI GAO ETC.: "Mass production of very thin single-crystal silicon nitride nanobelts", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
| 高凤梅 等: "单晶Si3N4纳米带可控Al掺杂研究", 《人工晶体学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107271082A (en) * | 2017-05-26 | 2017-10-20 | 宁波工程学院 | A kind of B doping big coefficient of strain high sensibility pressure transducer of SiC nanobelts and preparation method thereof |
| CN108328586A (en) * | 2018-03-01 | 2018-07-27 | 西安交通大学 | A kind of nitridation silica aerogel of compressible reply and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN104776945B (en) | 2018-08-24 |
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