CN1683917A - United measuring system and its measuring technology for scanning channel microscope and scanning micro electrode - Google Patents
United measuring system and its measuring technology for scanning channel microscope and scanning micro electrode Download PDFInfo
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- CN1683917A CN1683917A CN 200510052314 CN200510052314A CN1683917A CN 1683917 A CN1683917 A CN 1683917A CN 200510052314 CN200510052314 CN 200510052314 CN 200510052314 A CN200510052314 A CN 200510052314A CN 1683917 A CN1683917 A CN 1683917A
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Abstract
The present invention relates to measurement system and measurement technology with combined scanning tunnel microscope (STM) and scanning micro electrode. The measurement system consists of STM measuring platform, scanning micro probe and control/driving unit; tunnel current signal and micro area potential signal measuring unit; and measuring signal controlling and processing unit. The present invention utilizes micro scanning probe in simultaneous detection of surface tunnel current and surface potential distribution, adopts scanning mode interchange between micro piezoelectric scanning and mechanical step motor scanning, and uses tunnel current as indication of micro scanning electrode reaching the surface of sample, to realize the quantitative control of the distance between the tip of micro scanning electrode and the sample surface and to raise the spatial resolution in the measurement. The present invention provides opened platform for various surface spatial resolution measuring technology.
Description
Technical field
The present invention relates to a kind of scanning tunnel microscope and scanning microelectrode coupling measuring technique.
Background technology
Nineteen eighty-two, International Business Machines Corp. Zurich laboratory Binnig etc. succeeds in developing first scanning tunnel microscope (Scanning Tunneling Microscope, STM), its ultimate principle is the tunnel effect of utilizing in the quantum theory, by scanning microprobe test sample surface electronic density-of-states distribution, thereby obtain the sample surfaces pattern indirectly.The appearance of STM makes people might obtain to have the surface topography and the structure of atom spatial resolution in position, in real time, STM has further excited the continuous release of other various scanning microprobes micro-(SPM) new technology again, and has greatly promoted the fast development of whole nanosecond science and technology.So far, SPM has become observation material surface appearance structure and has carried out one of surface micromachined the strongest instrument.
Yet, along with going deep into and development of science and technology of research, the some critical drawback and the deficiency of scanning microprobe (SPM) technology manifest further, single scanning microprobe technology has been difficult to satisfy complicated synthetic study, only be suitable for observation as SPM to high alignment surfaces structure, and big to the SPM image interpretation difficulty of most of polycrystalline or non-crystalline material; SPM has only the susceptibility of surface microscopic appearance, but lacks the chemical property susceptibility of surperficial microcell, and the surface microscopic appearance is difficult to the physicochemical characteristics of surperficial microcell interrelated.In view of this, the compound scanning microprobe technology of development becomes a current international important topic of studying mutually unexpectedly.Obviously, people have been not content with the atom pattern on the high orientation texture surface that scanning tunnel microscope or atomic force microscope etc. only provide, and hope obtains the chemically active information of more microcell, and make that microcell appearance structure-chemically active integrated information is interrelated, make intramundane understanding is constantly deepened.Interrelated for from the integrated information between high-space resolution level understanding component-structure-chemical activity, begun to explore development STM/SNOM (optical microscope for scanning near field in the world, Scanning Nearfield Optical Microscope) coupling technique attempts to measure simultaneously microcell appearance structure and chemical composition; Development STM/SECM (scan-type electrochemical microscope, Scanning ElectrochemicalMicroscope) coupling is soundd out and is measured microcell appearance structure and chemical activity simultaneously; Development CFM (chemical force microscope, Chemical Force Microscope) with AFM (atomic force microscope, Atomic Force Microscope) coupling, sound out the information of measuring microcell appearance structure and chemical composition simultaneously, though these researchs of compound scanning microprobe coupling technique that have novelty are also just at the early-stage, but caused international great interest and attention, become an important research focus and the trend of development.
Summary of the invention
The purpose of this invention is to provide a kind of can measure simultaneously the surface topography image with nano-resolution degree and surperficial microcell electrochemical activity distributed image, to realize scanning tunnel microscope and scanning microelectrode coupling measuring system and measuring technique to surface topography-chemically active interrelated research with micron resolution.
Said scanning tunnel microscope of the present invention and scanning microelectrode coupling measuring system are made up of 4 unit: scanning tunnel microscope (STM) measuring table, scanning microprobe and control/driver element; The control of tunnel current signal and micro-potential signals measuring unit and measuring-signal and processing unit.The STM measuring table is based on opening commercial STM instrument.Said scanning microprobe and control/driver element comprise scanning microprobe, the three-dimensional piezoelectric micromotor scanner of X-Y-Z and step motor drive X-Y two-dimentional machinery scanner, wherein scanning microprobe is Pt-Ir alloy silk, adopt the tip of electrochemical etching method or mechanical shearing method preparation scanning microprobe, adopt polymethylstyrene that scanning microprobe tip is sealed, this scanning microprobe can detect tunnel current and electrochemical potential signal simultaneously; The piezoelectric micromotor scanner is used for the surface measurements tunnel current, sweep limit: 30-100 μ m2, stepper motor driven X-Y two-dimentional machinery scanning is used for surface measurements electrochemical potential distribution signal.As the indication that scans microelectrode arrival sample surfaces, finely tune the accurate distance of controlling microprobe tip and sample surfaces with tunnel current by the coarse adjustment and the Z axial compression electricity of stepper motor.The measuring unit of tunnel current signal and micro-potential signals comprises the advance signal conversion/amplification of tunnel current and the advance signal conversion/amplifying circuit of feedback circuit and micro-potential signals, and the advance signal conversion/amplification of tunnel current is identical with commercial STM tunnel current metering circuit with feedback circuit.The prime amplifier of the advance signal conversion/amplifying circuit of micro-potential signals amplifies secondary circuit by impedance conversion and difference and forms, signal is at first through the buffer amplifier of following of two high input impedances, its output signal subtracts through instrumentation amplifier and handles and acquisition current potential relative difference, promptly record the average potential on surface by reference probe, by scanning the local potential that microprobe records the sample surfaces zones of different, the relative current potential difference of the two is as microcell potential measurement signal.The control of measuring-signal and processing unit are 16 ADC processors, microcell potential measurement signal that obtains through tunnel current signal and micro-potential signals measuring unit and STM measuring-signal are all by an electronic switch, directly send 16 ADC to handle and be transformed to numerical signal, further signal is amplified, handles and analyzes subsequently.
Said scanning tunnel microscope and scanning microelectrode coupling measuring technique coupling measuring technique for combining and set up based on scanning tunnel microscope measuring principle and scanning microelectrode surface measurements electrochemical potential principle, detect surperficial tunnel current and electrochemical potential distribution signal simultaneously by same scanning microprobe, arrive the indication of sample surfaces with the tunnel current that measures as the scanning microelectrode, quantitatively the most advanced and sophisticated distance with sample surfaces of gated sweep microelectrode.By surface topography image and the surperficial microcell electrochemical activity distributed image that the surperficial tunnel current that measures and electrochemical potential distribution signal obtain the nano-resolution degree, realize surface topography-chemically active interrelated research.
Because scanning tunnel microscope is different with the measuring principle of two kinds of technology of scanning microelectrode: the scanning tunnel microscope measuring principle is according to the tunnel effect in the quantum mechanics, by the tunnel current on scanning microprobe test sample surface, realize the measurement of surface topography image; And the measurement of scanning microelectrode is based on electrochemical principle, by scanning microelectrode detecting electrode/solution interface Electric Field Distribution, thereby obtains the surface potential distributed image.The resolution of the two measurement is also obviously different, and the former resolution is atom or nanometer scale, and latter's resolution is generally micron dimension.The present invention utilizes same scanning microprobe to detect surperficial tunnel current and surface measurements Potential distribution simultaneously, carry out the exchange of two kinds of scanning survey patterns with piezoelectric micromotor scanning and stepper motor mechanical scanning, and utilize tunnel current to arrive the indication of sample surfaces as the scanning microelectrode, thereby when having overcome traditional scanning microelectrode method surface measurements microcell electrochemical corrosion potential and having distributed, the technical barrier that is difficult to quantitative gated sweep microelectrode tip and sample surfaces distance, realized of the quantitative control of scanning microelectrode tip, can significantly improve the spatial resolution that surface measurements microcell electrochemical potential distributes with the sample surfaces distance.This system can measure the surface topography image with nano-resolution degree and the surperficial microcell electrochemical activity distributed image of the same area simultaneously, realization is to surface topography-chemically active interrelated research, can mutually combine for kinds of surface spatial discrimination measuring technique provides a kind of, the open platform of mutual supplement with each other's advantages, association study, has important scientific meaning for the research that promotes Surface Physical Chemistry, and this scanning tunnel microscope and scanning microelectrode coupling measuring system can become a kind of scientific instrument of commercialization, is with a wide range of applications.
Description of drawings
Fig. 1 is the schematic block diagram of scanning tunnel microscope and scanning microelectrode coupling measuring system.
Fig. 2 is STM prime amplifier and galvanochemistry micro-potential signals prime amplifier fundamental diagram.
Fig. 3 is scanning microprobe synoptic diagram.
The 2205 two phase stainless steels surface STM shape appearance figure that Fig. 4 obtains for using coupling measuring system of the present invention.
Fig. 5 is exposed to 5% FeCl for 18/8 austenitic stainless steel of using coupling measuring system of the present invention actual measurement
3The distributed image of surface electrochemistry corrosion potential in the solution.
Fig. 6 is exposed to 5% FeCl for 18/8 austenitic stainless steel of using coupling measuring system of the present invention actual measurement
3The STM shape appearance figure (b) of distributed image of surface electrochemistry corrosion potential (a) and corrosion activity point in the solution.
Embodiment
Below by embodiment the present invention is elaborated.
Scanning tunnel microscope and scanning microelectrode coupling measuring system are made up of 4 unit: scanning tunnel microscope (STM) measuring table, scanning microprobe and control/driver element: the control and the processing unit of tunnel current signal and micro-potential signals measuring unit and measuring-signal.The STM measuring table is open commercial STM instrument, see Fig. 1, scanning microprobe and control/driver element comprise scanning microprobe 21, the three-dimensional piezoelectric micromotor scanner 22 of X-Y-Z and step motor drive X-Y two-dimentional machinery scanner 23, wherein scanning microprobe is that diameter is the Pt-Ir alloy silk (see figure 3) of 0.3mm, adopt mechanical shearing method preparation scanning microprobe tip, tip diameter is a nanometer scale, adopt polymethylstyrene that scanning microprobe tip is sealed, this scanning microprobe can detect tunnel current and electrochemical potential signal simultaneously; The piezoelectric micromotor scanner is used for the surface measurements tunnel current, sweep limit: 30-100 μ m
2, stepper motor mechanical scanning is used for surface measurements electrochemical potential distribution signal.As the indication that scans microelectrode arrival sample surfaces, finely tune the accurate distance of controlling microprobe tip and sample surfaces with tunnel current by the coarse adjustment and the Z axial compression electricity of stepper motor.Tunnel current signal and micro-potential signals measuring unit comprise the advance signal conversion/amplification of tunnel current and the advance signal conversion/amplifying circuit 32 of feedback circuit 31 and micro-potential signals, referring to Fig. 2, the advance signal conversion/amplification of tunnel current and feedback circuit are with commercial STM tunnel current metering circuit.The prime amplifier of the advance signal conversion/amplifying circuit of micro-potential signals amplifies secondary circuit by impedance conversion and difference and forms, signal is at first through the buffer amplifier of following of two high input impedances, its output signal subtracts through instrumentation amplifier and handles and acquisition current potential relative difference, promptly record surperficial average potential by reference probe, record the sample surfaces local potential by the scanning microprobe, the relative current potential difference of the two is as microcell potential measurement signal.The control of measuring-signal and processing unit 4 are 16 ADC processors, microcell potential measurement signal that obtains through tunnel current signal and micro-potential signals measuring unit and STM measuring-signal are all by an electronic switch, directly send 16 ADC to handle and be transformed to numerical signal, further signal is amplified, handles and analyzes subsequently.
Fig. 4 and Fig. 5 are exposed to 5% FeCl for application scanning tunnel microscope and surperficial STM feature image and 18/8 austenitic stainless steel that scanning microelectrode coupling measuring system actual measurement 2205 two phase stainless steels are exposed in the varying environment
3The distributed image of surface electrochemistry corrosion potential in the solution.The essential condition of STM test is: I
t=1nA, V
Bias=0.08V.Laboratory sample is selected 2205 two phase stainless steels and 18-8 austenitic stainless steel for use.The samples with water dry sanding paper is from coarse to fine polishes to 2000#, uses the Al of 1 μ m and 0.3 μ m more respectively
2O
3Powder is polished to minute surface, and is with ethanol and washed with de-ionized water, stand-by after the air dry.2205 two-phase stainless steel samples are in advance at 1.5mol/L HNO
3Carry out electrokinetic potential scanning in the+0.1mol/L NaCl system to obtain tangible two-phase pattern difference.At first sample is carried out the measurement of STM surface topography in the air, the result shows that this coupling measuring system can know indication two phase stainless steel surface microscopic topographic structure shown in Fig. 4 (a).Drip 0.1mol/LNaCl solution at sample surfaces then, and carry out the test of original position STM surface topography in same scanning survey position.The result is shown in Fig. 4 (b).Show that this coupling measuring system can be used for measuring the material surface structure and morphology in the aqueous solution, help carrying out the STM in site measurement, the dynamic behaviour and the influence factor of research surface structure pattern.
With the Pt-Ir alloy electrode serves as that the scanning microprobe is measured 18/8 austenitic stainless steel at 5%FeCl
3Surface electrochemistry corrosion potential distributed image in the solution.The same with the STM measuring process, at first make the scanning microprobe approach sample surfaces automatically, after detecting tunnel current, stop inserting needle, to scan upwards (Z direction) mobile 5 μ m of microprobe by computer program then, when promptly realizing distributing for the surface measurements electrochemical potential, the most advanced and sophisticated quantitative automatic control of distance with sample surfaces of scanning microelectrode.And then adding 5%FeCl
3Solution carries out the scanning survey of microcell electrochemical potential, and scan area is 5mm * 5mm.Surface electrochemistry potential image measurement result is shown in Fig. 5.5 (a) are the gray scale equipotential diagram, and Fig. 5 (b) is corresponding 3 D stereo potential image.The result shows that scanning tunnel microscope of the present invention and scanning microelectrode coupling measuring system not only can measure STM surface structure pattern, but also can detect the distributed image of surperficial microcell electrochemical corrosion potential.
Fig. 6 is exposed to 5% FeCl for 18/8 austenitic stainless steel of using coupling measuring system of the present invention actual measurement
3The STM shape appearance figure (b) of distributed image of surface electrochemistry corrosion potential (a) and corrosion activity point in the solution.At first make the scanning microprobe approach sample surfaces automatically, after detecting tunnel current, stop inserting needle, will scan upwards (Z direction) mobile 5 μ m of microprobe by computer program then.And then adding 5%FeCl
3Solution carries out the scanning survey of microcell electrochemical potential, and scan area is 5mm * 5mm.Surface electrochemistry Potential distribution measurement result is shown in Fig. 6 (a) with the form of 3 dimensional drawing.From the visible stainless steel surfaces of Fig. 6 (a) a plurality of corrosion activity points are arranged, select one of them obvious corrosion active site, will scan microprobe again and move on to this position, carry out the STM scanning survey, the STM topography measurement the results are shown in Fig. 6 (b).Fig. 6 (b) as seen has the pitting corrosion pit in corrosion activity point position, and the pit periphery has the accumulation of corrosion product.Proved scanning tunnel microscope of the present invention thus and scanned microelectrode coupling measuring system and can measure the structure and morphology of same sample surfaces and the distributed image of surperficial microcell electrochemical corrosion potential simultaneously, realized surface topography-chemically active interrelated research.
Claims (6)
1. scanning tunnel microscope and scanning microelectrode coupling measuring system, it is characterized in that said scanning tunnel microscope and scan microelectrode coupling measuring system forming: scanning tunnel microscope (STM) measuring table, scanning microprobe and control/driver element by 4 unit; The control of tunnel current signal and micro-potential signals measuring unit and measuring-signal and processing unit, STM measuring table are commercial apparatus; Said scanning microprobe and control/driver element comprise scanning microprobe, the three-dimensional piezoelectric micromotor scanner of X-Y-Z and step motor drive X-Y two-dimentional machinery scanner, the scanning microprobe is used to detect tunnel current and electrochemical potential signal, the piezoelectric micromotor scanner is used for the surface measurements tunnel current, and stepper motor mechanical scanning is used for surface measurements electrochemical potential distribution signal; Tunnel current signal and micro-potential signals measuring unit comprise the advance signal conversion/amplification of tunnel current and the advance signal conversion/amplifying circuit of feedback circuit and micro-potential signals, advance signal conversion/the amplification of tunnel current and feedback circuit are with commercial STM tunnel current metering circuit, the prime amplifier of the advance signal conversion/amplifying circuit of micro-potential signals amplifies secondary circuit by impedance conversion and difference and forms, signal is at first through the buffer amplifier of following of two high input impedances, its output signal subtracts through instrumentation amplifier and handles and acquisition current potential relative difference, promptly record surperficial average potential by reference probe, record the sample surfaces local potential by the scanning microprobe, the relative current potential difference of the two is as microcell potential measurement signal; The control of measuring-signal and processing unit are 16 ADC processors, microcell potential measurement signal that obtains through tunnel current signal and micro-potential signals measuring unit and STM measuring-signal are all by an electronic switch, directly send 16 ADC to handle and be transformed to numerical signal, further signal is amplified, handles and analyzes subsequently.
2. scanning tunnel microscope as claimed in claim 1 and scanning microelectrode coupling measuring system, it is characterized in that scanning microprobe is Pt-Ir alloy silk, adopt electrochemical etching method or mechanical shearing method preparation scanning microprobe tip, adopt polymethylstyrene that scanning microprobe tip is sealed.
3. scanning tunnel microscope as claimed in claim 2 and scanning microelectrode coupling measuring system is characterized in that the Pt-Ir diameter of alloy wire is 0.3mm.
4. scanning tunnel microscope as claimed in claim 1 and scanning microelectrode coupling measuring system, the sweep limit that it is characterized in that the piezoelectric micromotor scanner is 30-100 μ m
2
5. scanning tunnel microscope as claimed in claim 1 and scanning microelectrode coupling measuring system, it is characterized in that stepper motor mechanical scanning arrives the indication of sample surfaces with tunnel current as the scanning microelectrode, the most advanced and sophisticated distance with sample surfaces of coarse adjustment by stepper motor and Z axial compression electricity fine setting control microprobe.
6. scanning tunnel microscope and scanning microelectrode coupling measuring technique, it is characterized in that said scanning tunnel microscope and scanning microelectrode coupling measuring technique coupling measuring technique for combining and set up based on scanning tunnel microscope measuring principle and scanning microelectrode surface measurements electrochemical potential principle, detect surperficial tunnel current and electrochemical potential distribution signal simultaneously by same scanning microprobe, arrive the indication of sample surfaces as the scanning microelectrode with the tunnel current that measures, the distance of quantitative gated sweep microelectrode tip and sample surfaces, by surface topography image and the surperficial microcell electrochemical activity distributed image that the surperficial tunnel current that measures and electrochemical potential distribution signal obtain the nano-resolution degree, realize surface topography-chemically active interrelated research.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329247B (en) * | 2008-02-19 | 2010-12-22 | 中国科学院物理研究所 | Combined microscope for scanning atomic force and tunnel current under atmosphere |
| CN102301245A (en) * | 2009-01-30 | 2011-12-28 | 国际商业机器公司 | High-speed scanning probe microscope |
| CN102662085A (en) * | 2010-11-23 | 2012-09-12 | F·J·吉斯布尔 | Sensor for noncontact profiling of a surface |
| CN103439532A (en) * | 2013-09-02 | 2013-12-11 | 厦门乐钢材料科技有限公司 | Microelectrode technology for metal surface microcell current distribution in-situ detection |
| CN104034765A (en) * | 2014-07-07 | 2014-09-10 | 中国船舶重工集团公司第七二五研究所 | Electrochemical detection method through partial morphology scanning |
| CN105158519A (en) * | 2015-08-24 | 2015-12-16 | 扬州大学 | Device having quantum tunnelling-based nano-scale follow-up function |
| CN106226560A (en) * | 2016-08-02 | 2016-12-14 | 河南师范大学 | The PSTM of solid-state potential barrier needle point contact mode |
| CN107192665A (en) * | 2017-06-05 | 2017-09-22 | 中国石油大学(华东) | The test system and method for the heterogeneous texture local corrosion of multi-electrode coupling |
| CN116300031A (en) * | 2023-04-07 | 2023-06-23 | 苏州矽行半导体技术有限公司 | High NA large view field multi-interface microscope objective and wafer defect detection system |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06105262B2 (en) * | 1987-11-27 | 1994-12-21 | セイコー電子工業株式会社 | Method and apparatus for electrochemical measurement and simultaneous measurement of tunnel current |
| DE69216364T2 (en) * | 1991-09-27 | 1997-04-24 | Matsushita Electric Ind Co Ltd | Probe of a scanning electrochemical microscope and process for its production |
| CN2336357Y (en) * | 1996-08-30 | 1999-09-01 | 中国科学院长春应用化学研究所 | Electrolyzer for in-situ electrochemically scanning tunnel microscope |
-
2005
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101329247B (en) * | 2008-02-19 | 2010-12-22 | 中国科学院物理研究所 | Combined microscope for scanning atomic force and tunnel current under atmosphere |
| CN102301245A (en) * | 2009-01-30 | 2011-12-28 | 国际商业机器公司 | High-speed scanning probe microscope |
| CN102662085A (en) * | 2010-11-23 | 2012-09-12 | F·J·吉斯布尔 | Sensor for noncontact profiling of a surface |
| CN102662085B (en) * | 2010-11-23 | 2015-10-28 | F·J·吉斯布尔 | For the sensor of the noncontact profile analysis on surface |
| CN103439532B (en) * | 2013-09-02 | 2016-04-13 | 厦门乐钢材料科技有限公司 | A kind of Technology of Microelectrodes in situ detection metal surface microcell distribution of current |
| CN103439532A (en) * | 2013-09-02 | 2013-12-11 | 厦门乐钢材料科技有限公司 | Microelectrode technology for metal surface microcell current distribution in-situ detection |
| CN104034765A (en) * | 2014-07-07 | 2014-09-10 | 中国船舶重工集团公司第七二五研究所 | Electrochemical detection method through partial morphology scanning |
| CN105158519A (en) * | 2015-08-24 | 2015-12-16 | 扬州大学 | Device having quantum tunnelling-based nano-scale follow-up function |
| CN105158519B (en) * | 2015-08-24 | 2018-05-25 | 扬州大学 | A kind of device that nanoscale follow-up is realized using quantum tunneling effect |
| CN106226560A (en) * | 2016-08-02 | 2016-12-14 | 河南师范大学 | The PSTM of solid-state potential barrier needle point contact mode |
| CN106226560B (en) * | 2016-08-02 | 2023-03-14 | 河南师范大学 | Scanning tunneling microscope with solid barrier needle point contact mode |
| CN107192665A (en) * | 2017-06-05 | 2017-09-22 | 中国石油大学(华东) | The test system and method for the heterogeneous texture local corrosion of multi-electrode coupling |
| CN116300031A (en) * | 2023-04-07 | 2023-06-23 | 苏州矽行半导体技术有限公司 | High NA large view field multi-interface microscope objective and wafer defect detection system |
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