CN1800799A - Wide range electron tunneling type zinc oxide nano probe vacuum gauge and preparation method thereof - Google Patents
Wide range electron tunneling type zinc oxide nano probe vacuum gauge and preparation method thereof Download PDFInfo
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- CN1800799A CN1800799A CN 200510095556 CN200510095556A CN1800799A CN 1800799 A CN1800799 A CN 1800799A CN 200510095556 CN200510095556 CN 200510095556 CN 200510095556 A CN200510095556 A CN 200510095556A CN 1800799 A CN1800799 A CN 1800799A
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Abstract
The invention special relates to wide-range nano vacuum gauge in nanometer application field, which comprises: a nano-scale tunnel built by conductive electrode, and a nano ZnO rod-shape single-crystal probe with tip curvature radius less than 5nm. Wherein, fixing probe tail end on silicon oxide film/silicon substrate or silicon nitride/silicon substrate by metal electrode location deposition as well as another carbon film electrode; arranging the probe pinpoint pointed to the carbon film but off-connection with distance more than 5nm. This invention uses normal MEMS technology, optimizes the technique control parameters, and has high reliability.
Description
Technical field
The present invention relates to the applied technical field of nanometer preparation, nanoprocessing and nano-device, particularly wide-range nano vacuum rule and preparation method thereof.
Background technology
Existing in the market vacuum gauge mainly can be divided into the resistance vacuum gauge, thermocouple vacuum gage and ionization vacuum ga(u)ge etc.The resistance vacuum gauge be utilize that the resistance of heating element is relevant with temperature, the temperature of the element relevant principle with gaseous conductance again, come the vacuum gauge of measurement of vacuum by bridge diagram, its measurement range 1 * 10
4Handkerchief～1 * 10
-1Handkerchief.Thermocouple vacuum gage be utilize the electromotive force of thermopair relevant with the temperature of heating element, relevant with the heat conduction of the gas again principle of temperature of element comes the vacuum gauge of measurement of vacuum, its measurement range 1 * 10
2Handkerchief～1 * 10
-1Handkerchief.Ionization vacuum ga(u)ge is made of tubular collector, aperture plate and the filament that is positioned at the aperture plate center, the tubular collector utilizes hot cathode emitting electrons ionized gas molecule in the aperture plate outside, and ion is collected the utmost point and collects, come measurement gas pressure, its measurement range 1 * 10 according to the ion flow size of collecting
-1Handkerchief～1 * 10
-6Handkerchief.When the vacuum tightness scope at atmosphere 1 * 10
5Handkerchief is to high vacuum 1 * 10
-5In the time of between the handkerchief, need the multiple vacuum gauge of use to carry out duplex measurement, make the volume of measuring system increase on the one hand, cost increases, and is not easy to microminiaturization, on the other hand, because every kind of vacuum gauge use is different with condition of work, makes measuring operation loaded down with trivial details.Use resistance, thermocouple or ionization gauge to realize that the wide-range vacuum measurement from the atmosphere to the high vacuum does not appear in the newspapers so far separately based on the prior art manufacturing.
Along with the continuous development of nanosecond science and technology, zinc oxide material has obtained paying close attention to widely in nanometer electronic device.Zinc paste is wide bandgap semiconductor, also is the excellent in chemical sensing material, and it has stronger chemisorption character to having polarity with the molecule that has oxidation-reduction quality, and this chemisorption can the significant electrology characteristic that changes zinc paste.Especially, have the zinc oxide nano rod of one-dimensional space configuration, its length breadth ratio is big, makes it have bigger specific surface area, thereby higher than body material and film to the susceptibility of molecular adsorption.The preparation method of a kind of tip curvature radius less than the zinc paste bar-like single crystal nano-probe of 5 nanometers disclosed among the CN 200410014149.1, this zinc paste bar-like single crystal nano-probe specific surface area is very big, the tip has polarity and extensive chemical activity, have very high sensing (sensing) performance, this feasible nanometer electronic device based on this probe is used and is become possibility.The high sensitivity detection that for example is used for some specific gas, chemistry and biomolecule, even single-molecule detection field comprise the preparation that it is used for wide-range high sensitivity vacuum gauge.
Summary of the invention
The objective of the invention is to,, provide device architectures of a kind of nanometer monocrystalline zinc oxide probe vacuum gauge and preparation method thereof according to not enough in the prior art.
Purpose of the present invention realizes in the following manner.
Wide range electron tunneling type zinc oxide nano probe vacuum gauge of the present invention, it is characterized in that, this vacuum gauge is to be made of the nanoscale tunnel junction that nano-probe and conductive electrode are constructed, described nano-probe is the zinc paste bar-like single crystal nano-probe of tip curvature radius less than 5 nanometers, its tail end is fixed on silicon oxide film/silicon chip or the silicon nitride film/silicon chip by metal electrode location deposition, also the location deposits another carbon film electrodes on this substrate, the needle point of nano-probe points to carbon film electrodes, needle point is most advanced and sophisticated to remain on not electricity connection status with carbon film electrodes, and distance is less than 5 nanometers.
Among the preparation method of wide range electron tunneling type zinc oxide nano probe vacuum gauge of the present invention, used tip curvature radius is identical with disclosed method among the CN 200410014149.1 less than the preparation method of the zinc paste bar-like single crystal nano-probe of 5 nanometers, it is characterized in that preparation process after this is
(1) the tip curvature radius is disperseed less than the zinc paste bar-like single crystal nano-probe of 5 nanometers and be assembled on silicon oxide film/silicon chip or the silicon nitride film/silicon chip: probe sample is immersed carry out ultrasonic dispersion in the ethanolic solution, suspension with this probe/ethanol drops on the silicon oxide film/silicon chip or silicon nitride film/silicon chip of cleaning again, utilize spin coating (SpinCoating) or dry gas stream (Dry Gas Flow) method to get rid of drop, nano-probe is tiled on the above-mentioned substrate, and its surface coverage (density) is controlled at is lower than in the 1/square micron, use scanning electron microscope to check screening then, keep the tip curvature radius less than 5 nanometers and undamaged nano-probe to being tiled in on-chip nano-probe;
(2) to the above-mentioned nano-probe location depositing electrode that retains by screening: the tail end (radius is greater than the part of 10 nanometers) at above-mentioned nano-probe utilizes micro electronmechanical (MEMS) technology location deposition process metal electrode;
(3) preparation nano-probe needle point-air-carbon electrode nanometer tunnel junction: locate the conduct of depositing electrically conductive carbon film to electrode in the place ahead at nano-probe tip, and the zone of control deposition is decreased in 5 nanometers carbon film and nano-probe needle tip spacing gradually, but do not contact;
(4) above-mentioned tunnel junction is screened and stabilization processes: on two electrodes, apply scanning area greater than-5～5 volts but scan repeatedly fast or apply greater than 5 volts but less than 30 deep-sited pulses towards voltage less than-20～20 volts voltage, through screening, receive more than the peace greater than 10 and volt-ampere characteristic is that specification product are become in the tunnel of curve at tunnelling current under the above-mentioned bias voltage;
(5) demarcation of vacuum gauge: under different vacuum tightness, carry out voltammertry, and add the thermocouple vacuum gauge with the ionization vacuum gauge and demarcate, determine the relation of vacuum tightness and tunnelling current, make vacuum tightness-current data conversion table.
In the above-mentioned preparation process, employed electrode metal is gold or platinum.
Vacuum gauge of the present invention, utilize conventional MEMS technology, select this contactless device architectures of special nano-probe structure and nanometer tunnel junction for use, appropriate selected processing treatment process controlled variable reaches optimal value, make vacuum gauge work in the electron tunneling pattern, sensing characteristics depends on the electron tunneling between probe tip-carbon electrode, and this has fundamentally changed resistance-type and the capacitance type sensor pattern in the tradition.By quantum mechanics and semiconductor physics principle as can be known, described nano-probe sensing sensitivity is mainly by needle point place radius-of-curvature but not the decision of probe average-size, and most advanced and sophisticated and tunnel junction characteristic plays a decisive role for tunnelling current.The present invention has used the zinc paste bar-like single crystal nano-probe of tip curvature radius less than 5 nanometers, and specific surface area, chemical activity promote greatly, thereby in the past nano wire of the remolding sensitivity that vacuum is changed (radius greater than 10 nanometers) sensor improves greatly.Simultaneously since the tunnelling current of zinc oxide nano probe-air-carbon electrode nanometer tunnel junction at atmosphere to 10
-5The handkerchief high vacuum very on a large scale in the vacuum monotone variation and change obviously, so its range can cover from the atmosphere to the high vacuum (10
5～10
-5Handkerchief) very on a large scale, all more much bigger than the range of independent use resistance, thermocouple and ionization vacuum ga(u)ge.Existing experiment shows the repeated radius-of-curvature of this probe tip about 2 nanometers, if be expected to make the nano-probe of quasiatom yardstick tip curvature radius by further optimization, this just more can further guarantee its highly sensitive vacuum sensing capabilities.Test shows, vacuum gauge of the present invention is under negative bias, and tunnelling current is at atmosphere to 10
-5The interior very on a large scale of handkerchief high vacuum normally stablized with the vacuum monotone variation, and this illustrates that its range is very wide, 10
5～10
-5In the handkerchief scope.And, because its volume very little (sub-micrometer scale), and need not toast and degas, therefore use very conveniently, can satisfy the miniaturization requirement, be expected to replace the combined type configuration that the ionization vacuum ga(u)ge that generally uses in the present high vacuum system adds the thermocouple vacuum gauge.
Though employed nano-probe is very sharp-pointed at the tip among the present invention, but mean diameter reaches 100 nanometers on the whole, length-diameter ratio can reach 10～100 times, this yardstick is convenient to conventional MEMS processes processing very much, so preparation method of the present invention, whole procedure parameter control is convenient, processing technology maturation, reliability height.Because its production cycle is shorter, production cost is low, also is beneficial to very much prepared in batches processing.
Be described further below by embodiment and accompanying drawing thereof.
Description of drawings
Fig. 1 is the example structure synoptic diagram of wide range electron tunneling type zinc oxide nano probe vacuum gauge of the present invention.
Fig. 2 is the representative volt-ampere characteristic of vacuum gauge under three kinds of different vacuum tightnesss of utilizing the present invention to prepare, and illustration wherein is the representative scanning electron microscopy picture of nano-probe in the device.
Referring to Fig. 1,1 is silicon chip, the 2nd, monox or silicon nitride layer, zinc oxide nano probe 5 deposits on the monox or silicon nitride layer that is fixed on the silicon chip by the location of metal electrode 4, the needle point of nano-probe points to carbon film electrodes 3, the distance of its needle point and carbon film electrodes 3 is less than 5 nanometers, but do not contact, and forms tunnel junction 6.
Among Fig. 2, its horizontal ordinate is a voltage, and unit is a volt; Ordinate is an electric current, and unit receives peace.
Embodiment
Embodiment 1:
1. be ready to a slice smooth be 5 * 5 * 0.3 cubic millimeter the silicon single crystal polishing epitaxial substrate in (111) crystal orientation of covering of the thermal oxidation silicon film of 100 nanometers by nominal thickness, with acetone ultrasonic cleaning 3 times, each 5 minutes, make this substrate surface cleaning;
2. the nano-probe array sample that CN 200410014149.1 embodiment made immerse divide in the ethanol 3 times to sample ultrasonic concussion disperses to obtain the suspension of nano-probe/ethanol, each ultrasonic 1 minute, ultrasonic power and frequency were respectively 180 watts, 40 KHz;
3. drop on silicon oxide film/silicon chip with the transfer pipet homodisperse suspension that takes a morsel, its surface is covered by drop fully, utilize spin coating (Spin Coating) method, 2000 rev/mins of rotating speeds, regularly 2 minutes (so that getting rid of on-chip drop rapidly) makes the substrate drying;
4. the pattern of the nano-probe that the scanning electron microscope of using the focused-ion-beam lithography system to attach is disperseed tiling screens, the probe that to choose a satisfactory tip curvature radius be 2 nanometers, utilize micro electronmechanical (MEMS) processing technology to position and electro-deposition, process the platinum electrode and the pin thereof of 100 nanometer thickness at the tail end (radius is greater than the part of 10nm) of nano-probe;
5. in needle tip the place ahead, the conductive carbon film conduct of location deposition 50 nanometer thickness is to electrode, and carry out pin, the positive bias (rated current just is by carbon electrode through the direction that needle point flows to platinum electrode) that applies one 5 volts on two electrodes is monitored the electric current between carbon electrode and the platinum electrode in real time, continue simultaneously to the direction location depositing carbon film that approaches needle point, monitor that its electric current changes, receive ampere-hour and stop deposition at once when electric current reaches 100, then with microscopic carbon electrode and needle tip spacing whether in 5 nanometers with interior and be not connected as yet.Actual observation is about 1 nanometer to the carbon electrode and the needle tip spacing of present embodiment this moment;
6. between two electrodes, apply-10～10 volts of voltages fast and come flyback retrace 20 times, detect needle point and whether constitute the tunnel junction of needle point-air-carbon electrode formation and obtained electrical properties stability.If (during the scanning voltage fully not conducting or volt-ampere characteristic be straight line, get back to step 4 and continue)
7. the simple demarcation of vacuum gauge: under three kinds of different vacuum tightnesss, carry out voltammertry, and add the thermocouple vacuum gauge with the ionization vacuum gauge and demarcate, determine the relation of vacuum tightness and tunnelling current and make curve map, as Fig. 2.
Fig. 2 is the volt-ampere characteristic of nano vacuum rule under three kinds of different vacuum tightnesss of utilizing method for preparing.Can know from figure and find out that when two interelectrode voltage constants were-5 volts, when environment was atmosphere, its strength of current was received peace less than 0.1; When vacuum tightness was 1 handkerchief, its strength of current was 45 ± 0.5 to receive peace; And work as vacuum tightness is 1 * 10
-1During handkerchief, its strength of current is 90 ± 0.5 to receive peace.This is explanation just, and along with the raising of vacuum tightness, strength of current is increasing.Therefore, under fixed negative bias, just can be by measuring current value by being converted to the vacuum tightness of environment of living in.
Embodiment 2:
1. be ready to a slice smooth be 10 * 5 * 0.3 cubic millimeter the silicon single crystal polishing epitaxial substrate in (100) crystal orientation of covering of the silicon nitride film of 50 nanometers by nominal thickness, with acetone ultrasonic cleaning 3 times, each 5 minutes, make this substrate surface cleaning;
2. the nano-probe array sample that CN 200410014149.1 embodiment made immerse divide in the ethanol 3 times to sample ultrasonic concussion disperses to obtain the suspension of nano-probe/ethanol, each ultrasonic 2 minutes, ultrasonic power and frequency were respectively 180 watts, 40 KHz;
3. drop on silicon nitride film/silicon chip with the transfer pipet homodisperse suspension that takes a morsel, its surface is covered by drop fully, utilize dry nitrogen air-flow (Dry Gas Flow) method, nitrogen flow rate is 20 standard liters per minute, make the air current spray nozzle glancing incidence blow over substrate, blow on-chip drop rapidly off, and make the substrate drying;
4. the pattern of the nano-probe that the scanning electron microscope of using the focused-ion-beam lithography system to attach is disperseed tiling screens, the probe that to choose a satisfactory tip curvature radius be 1.5 nanometers, utilize micro electronmechanical (MEMS) processing technology to position and electro-deposition, process the gold electrode and the pin of 200 nanometer thickness at the tail end (radius is greater than the part of 10nm) of nano-probe;
5. deposit the conductive carbon film conduct of 100 nanometer thickness in location, needle tip the place ahead to electrode, and carry out pin, the positive bias (rated current just is by carbon electrode through the direction that needle point flows to platinum electrode) that applies one 5 volts on two electrodes is monitored the electric current between carbon electrode and the platinum electrode in real time, continue simultaneously to the direction location depositing carbon film that approaches needle point, monitor that its electric current changes, receive ampere-hour and stop deposition at once when electric current reaches 10.Then with microscopic carbon electrode and needle tip spacing whether in 5 nanometers with interior and be not connected as yet.Actual observation is about 2.5 nanometers to the carbon electrode and the needle tip spacing of present embodiment this moment;
6. between two electrodes, apply-10 volts of potential pulses 10 times, detect needle point and whether constitute the tunnel junction of needle point-air-carbon electrode formation and obtained electrical properties stability.If (during the scanning voltage fully not conducting or volt-ampere characteristic be straight line, get back to step 4 and continue)
7. the simple demarcation of vacuum gauge: under three kinds of different vacuum tightnesss, carry out voltammertry, and add the thermocouple vacuum gauge with the ionization vacuum gauge and demarcate, determine the relation of vacuum tightness and tunnelling current.Measurement result shows, when two interelectrode voltage constants were-5 volts, when environment was atmosphere, its strength of current was received peace less than 0.1, and when vacuum tightness was 1 handkerchief, its strength of current was 10 ± 0.5 to receive peace, and when vacuum tightness be 1 * 10
-4During handkerchief, its strength of current is 20 ± 0.5 to receive peace.
Claims (4)
1. wide range electron tunneling type zinc oxide nano probe vacuum gauge, it is characterized in that, this vacuum gauge is to be made of the nanoscale tunnel junction that nano-probe and conductive electrode are constructed, described nano-probe is the zinc paste bar-like single crystal nano-probe of tip curvature radius less than 5 nanometers, its tail end is fixed on silicon oxide film/silicon chip or the silicon nitride film/silicon chip by metal electrode location deposition, also the location deposits another carbon film electrodes on this substrate, the needle point of nano-probe points to carbon film electrodes, needle point is most advanced and sophisticated to remain on not electricity connection status with carbon film electrodes, and distance is less than 5 nanometers.
2. vacuum gauge as claimed in claim 1 is characterized in that, the tail end of described zinc paste bar-like single crystal nano-probe is fixed on silicon nitride film/silicon chip by metal electrode location deposition.
3. the method for preparing wide range electron tunneling type zinc oxide nano probe vacuum gauge as claimed in claim 1, used tip curvature radius is identical with disclosed method among the CN 200410014149.1 less than the preparation method of the zinc paste bar-like single crystal nano-probe of 5 nanometers, it is characterized in that preparation process after this is
(1) the tip curvature radius is disperseed less than the zinc paste bar-like single crystal nano-probe of 5 nanometers and be assembled on silicon oxide film/silicon chip: probe sample is immersed carry out ultrasonic dispersion in the ethanolic solution, suspension with this probe/ethanol drops on the silicon oxide film/silicon chip of cleaning again, utilize spin coating or dry gas stream method to get rid of drop, nano-probe is tiled on the above-mentioned substrate, and its surface coverage is controlled at is lower than in the 1/square micron, use scanning electron microscope to check screening then, keep the tip curvature radius less than 5 nanometers and undamaged nano-probe to being tiled in on-chip nano-probe;
(2) to the above-mentioned nano-probe location depositing electrode that retains by screening: the tail end at above-mentioned nano-probe utilizes micro electronmechanical technology location deposition process metal electrode;
(3) preparation nano-probe needle point-air-carbon electrode nanometer tunnel junction: locate the conduct of depositing electrically conductive carbon film to electrode in the place ahead at nano-probe tip, and the zone of control deposition is decreased in 5 nanometers carbon film and nano-probe needle tip spacing gradually, but do not contact;
(4) above-mentioned tunnel junction is screened and stabilization processes: on two electrodes, apply scanning area greater than-5～5 volts but carry out fast scanning repeatedly or apply greater than 5 volts but less than 30 volts pulse voltage less than-20～20 volts voltage, through screening, receive more than the peace greater than 10 and volt-ampere characteristic is that specification product are become in the tunnel of curve at tunnelling current under the above-mentioned bias voltage;
(5) demarcation of vacuum gauge: under different vacuum tightness, carry out voltammertry, and add the thermocouple vacuum gauge with the ionization vacuum gauge and demarcate, determine the relation of vacuum tightness and tunnelling current, make vacuum tightness-current data conversion table.
4. preparation method as claimed in claim 3, it is characterized in that, described preparation process (1) is the tip curvature radius is disperseed less than the zinc paste bar-like single crystal nano-probe of 5 nanometers and to be assembled on silicon nitride film/silicon chip, be about to carry out ultrasonic dispersion in the probe sample immersion ethanolic solution, the suspension with this probe/ethanol drops on the silicon nitride film/silicon chip of cleaning again.
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| CN 200510095556 CN1800799B (en) | 2005-11-18 | 2005-11-18 | Wide range electron tunneling type zinc oxide nano probe vacuum gauge and preparation method thereof |
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| CN 200510095556 CN1800799B (en) | 2005-11-18 | 2005-11-18 | Wide range electron tunneling type zinc oxide nano probe vacuum gauge and preparation method thereof |
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| CN1800799A true CN1800799A (en) | 2006-07-12 |
| CN1800799B CN1800799B (en) | 2010-11-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067159A (en) * | 2015-07-22 | 2015-11-18 | 上海交通大学 | Capacitive pressure sensor and preparing method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067159A (en) * | 2015-07-22 | 2015-11-18 | 上海交通大学 | Capacitive pressure sensor and preparing method thereof |
| CN105067159B (en) * | 2015-07-22 | 2018-01-12 | 上海交通大学 | A kind of capacitance pressure transducer, and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1800799B (en) | 2010-11-24 |
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Granted publication date: 20101124 Termination date: 20151118 |