CN1977159A - Method for manipulating microscopic particles and analyzing the composition thereof - Google Patents
Method for manipulating microscopic particles and analyzing the composition thereof Download PDFInfo
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- CN1977159A CN1977159A CNA2004800379489A CN200480037948A CN1977159A CN 1977159 A CN1977159 A CN 1977159A CN A2004800379489 A CNA2004800379489 A CN A2004800379489A CN 200480037948 A CN200480037948 A CN 200480037948A CN 1977159 A CN1977159 A CN 1977159A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2204—Specimen supports therefor; Sample conveying means therefore
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B21/00—Microscopes
- G02B21/32—Micromanipulators structurally combined with microscopes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/30—Electron or ion beam tubes for processing objects
- H01J2237/317—Processing objects on a microscale
- H01J2237/3174—Etching microareas
- H01J2237/31745—Etching microareas for preparing specimen to be viewed in microscopes or analyzed in microanalysers
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Abstract
We disclose a method for analyzing the composition of a microscopic particle resting on a first sample surface. The method comprises positioning a micro-manipulator probe near the particle; attaching the particle to the probe; moving the probe and the attached particle away from the first sample surface; positioning the particle on a second sample surface; and, analyzing the composition of the particle on the second sample surface by energy-dispersive X-ray analysis or detection of Auger electrons. The second surface has a reduced or non-interfering background signal during analysis relative to the background signal of the first surface. We also disclose methods for adjusting the electrostatic forces and DC potentials between the probe, the particle, and the sample surfaces to effect removal of the particle, and its transfer and relocation to the second sample surface.
Description
Technical field
The present invention relates to a kind ofly from sample surfaces, particularly the method for molecule is removed and is analyzed on the semiconductor samples surface.
Background technology
In the semi-conductor industry production run, inevitably particle contamination will make output reduce.The characteristic dimension of composition live width because the semiconductor industry is concentrating one's energy greatly to reduce always is so the particle minimum dimension that performance is reduced also reduces rapidly.It is generally acknowledged, estimate that rationally " critical defect " size on the semiconductor wafer should be greater than 1/3rd of minimum feature size.
Although the semiconductor manufacturing is to carry out in the toilet with strict particle standard, yet, still can pollute inevitably owing to there being reasons such as movement of objects, personnel's turnover, gas condensation and room are aging.Controlling and removing these particles is lasting processes.In most cases, only know about the source and could remove degranulation better.Many particles or defective are very little; can't find with common optical check microscope; therefore need take the higher method of resolution, use as charged particle microscopes such as scanning electron microscope (SAM), transmission electron microscope (TEM), scanning Auger microprobe (SAM) or focused ion beam instruments.
Only usually can't find the source of particle according to the image of particle, we also need more information.Basis has very high using value in differentiating the defective process.Use above-mentioned charged particle microscope to do this work by many methods.Yet most analytical approachs are subjected to the particle restriction of background signal on every side.
Productive capacity also is the key factor during semiconductor is made.The method of the particulate component on the existing analyzing semiconductor wafer need be taken off wafer usually from production line, use following method to carry out off-line analysis then, and this will greatly reduce output.
Because the variation of the relative size of particle and penetration deepth of electron relation, and the difference of material around characteristic in the sample, make and utilize electron beam that the particle of sample surfaces is differentiated the very complexity that becomes.Along with electron beam and bulk solid material interact, it will disperse and be full of the drop-shaped space, and off-energy.Atomic interaction in light beam and this space produces distinctive low-energy Auger electron of this element and X ray.
The X ray that produces depends on the energy and the other factors of electronics in Atom of Elements, the mechanism.When adopting traditional energy dispersion type X ray spectrophotometric method (EDS) to differentiate unknown particle, the energy of electron beam must be enough big, to produce the hypostracum X ray on all possible coherent element, for the semiconductor industry, this may comprise the element such as high atomic numbers such as tungsten., this energy may make penetration depth much larger than the particle that will differentiate, to such an extent as to produce X ray at sample surfaces.These X ray are interfered mutually with the signal that sends from particle, make and differentiate very difficulty of particulate material uniquely.Traditional solution comprises X ray of resolving different elements or the energy that reduces the excitation electron bundle.
For example, come the intensity of measured X x ray diffraction and angle of diffraction to detect by reference crystal or wavelength dispersion type x-ray spectrometry (WDS) and analysing particulates in the X ray that produces by electron beam.The selected crystal atoms spacing of people can make the X ray of different elements separate with the X ray of the given energy of deflection (with high resolving power).The method has the energy resolution higher than EDS, but its output is lower.In addition, as a rule, particle may be the same with the composition of sample surfaces, and then this method just can not be measured the composition of particle uniquely.
Other method comprises the energy that reduces once electron beam, with space that guarantee the to activate volume less than the particle of being surveyed.The reduction of primary electron beam energy makes characteristic X-ray have lower energy (M or L shell X ray rather than K shell).The detector of the based semiconductor of tradition cooling produces and collects electron hole pair, to measure energy ionizing radiation (according to different detecting materials, each electron hole pair produces the energy of several eV).Reduce the energy of X ray, just reduced the right quantity in hole, cause the sensitivity of particulate material is reduced.In addition, the resolution of these detectors is by the decision of the statistic in the production process of electron hole, and the energy that reduces the X ray that detects can cause the discriminating of detection element indeterminate usually.Use X ray microcalorimeter method to survey these faint X ray signals in the prior art, the heat by being delivered to detector rather than the electron hole pair of generation are measured.The method can measure very low X ray energy, but microcalorimeter is very expensive, need carry out complicated cooling, and specific rate is slower mutually with other method.Simultaneously, electron beam must be less than the minimum dimension of detection particle, thereby in fact the method can't survey little, asymmetric particle.
The particle that the scanning Auger microprobe analysis also uses the electron beam irradiation to be surveyed, but it does not survey the X ray of generation, but the Auger electron that the detecting material atom sends.These Auger electron send from shell, and have relatively low energy.Can produce the composition of every kind of element in the exosyndrome material from the Auger electron energy of material, Auger conversion modalities and accurate energy provide the chemical bond information of element in the material (as phase place and composition information).These electronics flee from the degree of depth very little (a few nanometer), so auger analysis is mainly used in the surface of analytic sample.This is of value to analyzes diameter smaller particles (＜10 nanometer).As analyzing bigger particle, can use ion beam sputtering to penetrate particle and produce the go forward side by side measurement of line period of depth profile, but because the ion abrasive action among the SAM, cause inevitably the destruction of sample on every side, and it need carry out context analyzer to the sample around the particle position.For light element, auger analysis is analyzed sensitivity than the EDS of standard usually, makes it be more suitable for differentiating organic material.Yet,, need to use high electron beam current usually in order to improve statistical precision.This will amplify the influence of hot machine drift and sample charge shift.This means that electron beam is positioned on the particle with " dot pattern " operation SAM,, exist electron-beam point to float to risk on the circumgranular sample along with the prolongation of time.For electron beam is stayed on the particle, use the raster pattern of electron beam can more anti-drift, but can produce significant pollution to the result from the signal of material around.Under any circumstance, auger analysis result's background contamination all is a serious problem, need identify the signal from particle to the auger analysis of material around uniquely.Context analyzer will reduce output and damage sample.
TEM is commonly used to analyze the surface and goes up or its inner particle.There are many methods can isolate the particle that to analyze, comprise and duplicate, mention or zone that crosscut is surveyed.These methods all will be destroyed sample surfaces, and want off-line to carry out, thereby can increase cost and prolong cycle period.
Still be that auger analysis carries out element and differentiates no matter, particle is tested from the environment that first sample surfaces moves to easier control, can greatly improve successful probability and output with EDS.The key component of this process is the method for mobile particle.The invention discloses a kind of new method, the particle that will survey can be taken off from sample surfaces with it, and be sent to second sample surfaces with in check X ray or Auger background, use the whole bag of tricks mentioned above to carry out the X ray or the Auger electron analysis of electron beam-induced at there then.This will not need the analytical technology of high spatial resolution, still, have the technology of high spatial resolution, and for example the EDS that uses in SEM and SAM analysis analyzes normally preferred.Can be successfully applied to reduce or glitch-free background on the technology analyzed of particle with non-high spatial resolution for example comprise x-ray photoelectron power spectrum (XPS) and x-ray fluorescence analysis (XRF), this is highly profitable under unique and clear and definite situation.
This method that is used for particle disposal and EDS X-ray analysis can be on existing wafer fabrication equipment online carrying out.That uses existing manufacturing and checkout equipment has greatly reduced the cycling time of removing pollutant at line process.SEM is the conventional method of wafer inspection, uses the analytical approach of electron beam to improve output than off-line analysis in the SEM system.
Although the present invention is mainly set forth the use of handling and detecting the new method of the particle that becomes pollutant in semiconductor fabrication, but the reader should be noted that it is not the material of pollutant that " particle " speech here is also included within other environment, as chemical deposition thing, biomaterial or micromechanics mechanism.Under latter event, the new method of the described processing of the application can be used for handling these materials, is generally used for other purposes except that electron beam X ray or Auger electron analysis.
Description of drawings
Fig. 1 moves to the step of second surface to analyze for particle is attached on the narishige probe and with particle.
Fig. 2 is attached to method on the narishige probe for other three kinds with particle.
Fig. 3 is to change the process of electrostatic force with polarizable microparticle bombardment.
Fig. 4 is the method for observing particle simultaneously and changing the particle charge state.
Fig. 5 is for to be fixed to second surface so that the several method of analyzing with particle.
The process of Fig. 6 for when particle being fixed on the narishige probe tip, particle being analyzed.
Fig. 7 is to moving to the process that second surface is analyzed with the particulate component of analyzing.
Summary of the invention
The invention discloses the method that a kind of analysis is fixed on the molecule composition on first sample surfaces.Usually, particle is the pollutant in the semiconductor producing system, and the method is not only limited under this environment and uses.The method comprises the narishige probe is put near the particle; Particle is attached on the probe; From first sample surfaces probe and accompanying particle are removed; Particle is placed on second sample surfaces; Analyze the composition of the particle on second sample surfaces by energy dispersion type x-ray method, auger microprobe analytic approach or other suitable analytical technology.In analytic process, the background signal of the relative first surface of second surface has the background signal (applicant's background signal that will weaken or that do not have interference is called the background signal of " controlled " in the claims) that weakens or do not have interference.The application also discloses the method for adjusting electrostatic force and DC voltage between probe, particle and the sample surfaces, uses the method can take off particle, is sent to second sample surfaces, and reorientates thereon.Comprise and adjust electrostatic force between probe and particle, to produce attractive force.Adjust electrostatic force and comprise local energy or the intensity (intensity refers to the line of electronics or ion beam) that incides the electron beam on the single component, ion beam or photon beam in the sample system of adjusting, between particle and probe tip, to produce electrostatic attraction, or between the particle and first sample surfaces, producing electrostatic repulsion forces, these assemblies comprise probe tip, particle and first sample surfaces.The process that particle is sent to second sample surfaces from probe tip in contrast.
Second sample surfaces also may be a probe tip itself.In this case, probe tip is made up of in check background material.Because these small particles are possibility transmission potential bundle also, or energy beam scattered to following surface, therefore be necessary that the probe tip that will be attached with particle is converted to the surface of being made up of in check material, or the probe tip that this controlled background material is positioned at be attached with particle below.In this article, " following " refer to a side (that is transmissive side) relative on the particle with a side that is subjected to energy beam incident.
Embodiment
Semiconductor manufacturing industry uses scanning electron microscope (SEM), focused ion beam (FIB) instrument or scanning Auger microprobe (SAM) to analyze molecule usually.The FIB instrument has single beam or two kinds of patterns of twin-beam (SEM and ion beam).FIB instrument commonly used is by Hillsboro, and FEI Co. of Oregon makes, and 200,235,820,830 and 835 several models are arranged.The probe of hereinafter mentioning 120 is assemblies that are connected to the narishige of the FIB instrument with vacuum feedthrough.This type of narishige of a kind of routine is by Dallas, the 100 type narishiges that the Omniprobe company of Texas makes.Typical SAM instrument comprises Peabody, JAMP-7810 and JAMP-7830F that the JEOL USA company of Massachusetts makes.
Fig. 1 describes the common apparatus of processing and analysing particulates.Figure 1A is the particle that will survey 100 that rests on first sample surfaces 110.Narishige probe 120 is positioned near the particle 100.Probe tip particle and first sample surfaces relatively has static charge.Perhaps, a voltage source 130 can be connected between the probe 120 and first sample surfaces 110.Can change partial electrostatic lotus on the particle with the charged particle beam irradiation particle.Figure 1B shows respectively with photon or charged particle beam 140 irradiation particles 100 and first sample surfaces 110 so that particle 100 is attached on the probe 120 to 1D, probe 120 and the particle 100 that is attached on it are removed from first sample surfaces 110, and, particle 100 is deposited to second sample surfaces 150 for analysis.These figure are not drawn to scale.
Particle is attached on the probe
Particle in the vacuum has powerful electrostatic force.Because the existence of static charge on particle 100 and the probe 120 causes producing image charge in facing surfaces.The power that these image charges produce is directly proportional with the area of exposure, and the distance between object is inversely proportional to.Reduce or increase exposed area the power that acts on the particle 100 will be reduced or increase, finally influence the adhesion of 100 of probe 120 and particles.Make in this way, can directly the particle that will survey be taken off from sample by the probe 120 that conducts electricity or insulate.The probe of conduction has more function, and it can be incorporated into probe 120 from voltage source or static charge source 130 with static or time dependent voltage or static charge, shown in Figure 1A.
The shape at probe 120 tips also can have influence on most advanced and sophisticated electric field.The influence power of pair particle that aligns with this tip of the static charge on more blunt tip is than big at sharp-pointed tip.On the contrary, under the situation that has DC voltage on the conductive tip, sharp-pointed tip can produce the most powerful electric field at this place, tip.For example, when using electron beam 140 imagings of FIB instrument, probe 120 can move to very the place near particle 100, shown in Figure 1B.Electron beam also can influence the CHARGE DISTRIBUTION in surface-particle-probe system, thereby can help particle 100 is attached on the probe 120.The application of this effect will be discussed below.Should be understood that it also can is charged particle beam or photon beam at the electron beam 140 shown in Figure 1B and other figure, also may comprise ion beam.Herein, these bundles and the photon beam that sends from laser all are called as " energy " bundle in the claim part.
Generally speaking, electrostatic force in the Adjustment System comprises adjusts the energy that is incident on the electron beam 140 on particle 100, probe 120 and the first surface 110, between particle 100 and probe 120, setting up relative electrostatic attraction, and between the particle 100 and first sample surfaces 110, form relative electrostatic repulsion forces.This process can be finished under the assistance that is connected in the voltage source 130 between first sample surfaces 110 and the probe 120.Obviously, colliding beam 140 can be a photon beam also, has enough energy and discharges photoelectron, CHARGE DISTRIBUTION and electrostatic force in the energy change system.
The preferred embodiment also can use bonding agent 160 to carry out on probe 120, shown in Fig. 2 A.Suitable bonding 160 can be any material with lower vapor pressure, as the glue of vacuum grease, low melt wax or other low-vapor pressure.In this case, although there is electrostatic force to exist, bounding force is only caught particle 100.
Shown in Fig. 2 B, in another embodiment, the tweezers 170 that link to each other with probe 120 are caught particle 100, and it is removed from first sample surfaces 110.Berkeley, the MEMS Precision Instruments of CA just produce the appropriate device that has tweezers 170 and similar clip.
Also have another to adjust the method for electrostatic field in particle-probe-surface system, to adhere to and mobile particle 100, it comprises conductive material is deposited on first sample surfaces 110 or second sample surfaces 150, in this case, distribute and adjust the lip-deep static charge at particle place, to produce required attractive force or the repulsive force that acts on the particle.Fig. 3 A shows the deposit of polarisable particle 250 (as water) on sample surfaces 11.Fig. 3 B shows the deposit by the conductive film 255 of the evaporation generation in source.The direct jet 240 that Fig. 3 C shows gas 245 is sprayed onto the surface 110 that is attached with particle 100.Gas 245 is decomposed by energy beam 140, and this energy beam may be electron beam, ion beam or the photon beam that sends from laser.
Fig. 4 is the method for observing particle 100 simultaneously and adjusting the particle charge state in vacuum system.In typical FIB instrument, the object that SEM bundle and ion beam will be surveyed with raster pattern 260 scannings.Send secondary electron in scanning, produce electric signal, this signal is shown to the operator of equipment with the form of image.Because scanning beam comprises charged particle inevitably, and causes sample to send charged particle, as secondary electron, therefore, itself just can be used for changing the state of charge of particle 100.The FIB instrument uses the digital scanning generator usually, and it increases the position of bundle spot by raster pattern digitizing ground, and each delegation is reverse in the ranks usually, to eliminate the characteristics of every row back flyback that the traditional analog scanner has.So the computer program of operator or gated sweep can be determined the residence time on each pixel.For example, program can be set at zero residence time, direct empty mistake during scanning with the overcover on the particle (or accurate particle outline).Arbitrary residence time can be set to the maximum time by the line frequency decision, to avoid scalloping in single scanning.Also can be in alternate sweep around the overcover, then with different parameter scanning overcover inside, this action is very fast, and human eye is not seen interruption.
Fig. 4 shows and is comprising the step of looking grating run-down electron beam 270 on the electric field of particle 100, the secondary electron 280 that generation and detection and once electron beam 270 are synchronous, change raster formatted picture 260, to specify in 260 on the grating relevant specifically the residence time and the position of pixel with making up and add to particle 100 among the master grating figure.When having parked grating 260, particle 100 stands a negative charge effect excessive or that reduce with respect to sample surfaces 150.Like this, just can adjust the electrostatic field between particle 100, probe 120 and the sample surfaces 150, with attractive force or the repulsive force that need to obtain.Grating must be produced in the same manner by ion beam or scan laser.
Transmit particle
In case with said method particle 100 is attached on the probe 120, just can be manually or with automatic probe 120 parts traveling probe 120 in vacuum environment.Also can rise or regain probe 120 lightly with another kind of method, and can the mobile example platform in check background material is taken to below the probe 120.
Also can particle 100 be sent to by having low background or not having second sample surfaces 150 that the controlled background material of interfering background signal is formed with probe 120.When analyzing with EDS, the material of low atomic number as carbon and beryllium, will produce low-energy X ray, can not interfere the analytic process of most of inorganic particles.Preferably atomic number is less than or equal to 12.Organic granular obviously needs inorganic background material.The carbon back slurry (gluey graphite suspension), polymeric films or the carbon tube needle that comprise photoresist, carbon flat board, beryllium paper tinsel, conduction as the example of the low background material of second sample surfaces 150.Any material that the X ray background can not interfere with typical material in manufacturing process can be used for doing second sample surfaces 150.In some cases, second sample surfaces 150 can be the different piece of first sample surfaces 110.In other cases, if know the part composition that maybe can guess particle 100, then the material of second sample surfaces 150 should have and the different background signal of expecting of signal that sends from particle 100.Must careful operation, prevent that second sample surfaces 150 from covering the signal that may send from the pollutant of making apparatus outside, as the gas that sucks or the impurity in the chemical substance.When the particle on the second surface was carried out auger analysis, second surface should or not have the Auger electron of interference background and form by low Auger electron background.The composition of second surface should have the consistent degree of depth, the degree of depth that this degree of depth detects greater than any depth profiles that will carry out on particle.The material of second surface should have the ability of heat-conductivity conducting, to minimize because the charged or hot machine drifting problem that causes of high electron beam current, but not necessarily.Earlier second surface being carried out pre-sputter before transmitting particle will eliminate original surface coating (mainly being carbon and oxygen) and simplify analytical work.Can carry out this pre-sputter with depth profiles ion gun in the Auger or the ion beam among the FIB.As everyone knows, the composition of second surface has been removed context analyzer from, has improved output.
Fig. 5 is sent to second sample surfaces 150 for the several method of analyzing for the particle 100 that will adhere to from probe 120.Fig. 5 A shows the particle that is suspended on the lower frame 190, and is thinner than the penetration depth of analysed beam 140.Framework 190 is the TEM grid normally, has polymeric films 195 is passed grid as FORMVAR opening part.
Fig. 5 B shows on second sample surfaces 150 usefulness bonding agents 200 particle attached to it.Fig. 5 C shows second sample surfaces 150 that the background material 210 by low elastic modulus constitutes as vacuum grease, low melt wax or low polymer.In this case, particle 100 just can be pushed in the low-modulus material 210 and be bonded at the there.
Fig. 5 D is the wrinkled surface 220 on second sample surfaces 150 of insulation.Wrinkled surface 220 can increase the contact area of the particle 100 and second sample surfaces 150, thereby can change the electrostatic force between them.
Fig. 5 E is for writing on the charging pattern 230 on second sample surfaces 150 by charged particle beam 140.The electrostatic field of this pattern helps particle is sent on second sample surfaces 150 from probe 120.
Fig. 5 F is second sample surfaces 150 with a plurality of holes or aperture.Such surface may be a millipore filter, as St.Paul, the MICROPORE series filtrator that the 3M Corporation of Minnesota makes may be a glass fiber filter also, as St.Paul, FILTRETE that the 3M Corporation of Minnesota makes or EMPORE series filtrator, perhaps " porous carbon " film as QUANTIFOIL series, is by West Chester, the Structure Probe of PA, Inc makes.These surperficial advantages are, particle 100 can be static in these surperficial holes or aperture or by electrostatic capture and keep motionless for analysis.
In some cases, may need to seek local high electrostatic field zone, be enough to particle 100 is taken off and do not come in contact (if desired) from probe 120.
Certainly, the above-described electrostatic force of adjusting in particle-probe-sample surfaces system also can be used for particle 100 is taken off and is attached on second sample surfaces 150 from probe 120 with the method that particle 100 is attached on the probe 120.Particularly, as changing rapidly from the negative charge that stores in the capacitor by probe 120, or,, make voltage or Charge Source 130 can produce fast transition or resonance phenomena as square wave or pulse by affact the time dependent voltage on the probe 120 from Charge Source 130.
Analysing particulates
X-ray analysis or auger analysis can be on probe tip 125 direct analysing particulates 100, as shown in Figure 6.Certainly, will itself produce X ray or Auger electron from probe tip 120 like this.Can use low background or not have the material of interfering background material as probe tip, as indicated above, when analyzing, will hang down background or not have the interfering background material and be placed on below the probe 120, or near all other parts platform and the probe 120 will all be lowerd, to reduce other interference signal.Analysis to particle 100 is finished, so can take off particle 100 devastatingly after this step.Many destructive methods are arranged, as probe 120 being inserted in the plasma cleans device of some type, in the such physical construction of V-type groove, rub off particle 100, in a vacuum or in atmosphere, be exposed to back optical illumination probe, or melt particle 100.
But, usually will be at second sample surfaces, 150 analysing particulates 100, as shown in Figure 7, wherein, particle 100 sends feature Auger electron or X ray 180 under the irradiation of charged particle analysed beam 140, any method that can use the application's background parts to describe is carried out constituent analysis.In the claim part, term " emission " refers to Auger electron or X ray.
At the probe tip analysing particulates
Second sample, 150 surfaces also can be that probe tip 135 is own.In this case, probe tip 135 is made up of in check background material.Wherein can carry out SAM that the surface ion bundle grinds or FIB etc. when analyzing instrument using, before particle 100 being attached to most advanced and sophisticated 135, earlier ion beam is carried out on the surface of probe tip 135 and grind, can reduce the signal that original surface coating and probe tip 135 lip-deep residues send.Because small particle also can see through energy beam 140, or energy beam 140 scattered on the following surface, therefore be necessary that the probe tip 135 that will be attached with particle 100 is transformed on the surface that is made of in check background material, or the probe tip 135 that this controlled background surface is transferred to be attached with particle 100 below.In this article, " following " refer to a side (that is transmissive side) relative on the particle 100 with a side that is subjected to energy beam 140 incidents.
Because those skilled in the art can improve above-mentioned specific embodiment, so our claim comprises these improvement and equivalent thereof.
Claims (65)
1. the method for an analysing particulates composition, described particle stays in first sample surfaces; Said method comprising the steps of:
The narishige probe is positioned near the particle, and described probe has the tip;
Particle is attached on the described probe tip;
Probe and accompanying particle are removed from first sample surfaces;
Second sample surfaces is removed and be sent to particle from probe tip; And
Analyze the composition of the particle on second sample surfaces;
Wherein, the background signal of relative first surface, second sample surfaces has in check background signal in analytic process.
2. method according to claim 1 is characterized in that described method is implemented in atmospheric environment.
3. method according to claim 1 is characterized in that described method is implemented in vacuum environment.
4. method according to claim 1 is characterized in that, makes particle be adsorbed, move or take off in electron beam irradiation particle.
5. method according to claim 1 is characterized in that, makes particle be adsorbed, move or take off in the ion beam irradiation particle.
6. method according to claim 1 is characterized in that, makes particle be adsorbed, move or take off in photon beam irradiation particle.
7. method according to claim 1 is characterized in that, described second sample surfaces is the part of first sample surfaces.
8. method according to claim 1 is characterized in that, the step that probe and accompanying particle are removed from first sample surfaces also comprises:
The position of stationary probe;
Move first sample surfaces with respect to fixing probe, so that make first sample surfaces and probe and accompanying particle separation.
9. method according to claim 1 is characterized in that, described second sample surfaces comprises that atomic number is less than or equal to 12 material.
10. method according to claim 1 is characterized in that, described second sample surfaces comprises the different material of signal that its background signal and expection are produced by grain size analysis.
11. method according to claim 1 is characterized in that, the described step that particle is attached to probe tip comprises adjustment electrostatic force, so that produce attractive force between probe and particle.
12. method according to claim 11 is characterized in that, the step of described adjustment electrostatic force also comprises:
The energy of the energy beam on the particle is incided in adjustment, makes particle, first sample surfaces and probe tip have static charge, so that produce electrostatic attraction between particle and probe tip, and produces electrostatic repulsion forces between first sample surfaces and particle.
13. method according to claim 11 is characterized in that, described energy beam is an electron beam.
14. method according to claim 11 is characterized in that, described energy beam is an ion beam.
15. method according to claim 11 is characterized in that, described energy beam comprises photon.
16. method according to claim 11 is characterized in that, the step of described adjustment electrostatic force also comprises:
Make particle have static charge;
Depositing conductive material on first sample surfaces is with in the residing position distribution of particle and change static charge on first sample surfaces.
17. method according to claim 16 is characterized in that, the described conductive material that is deposited on first sample surfaces comprises polarizable particulate.
18. method according to claim 16 is characterized in that, is deposited on the conductive film of described conductive material for evaporating on first sample surfaces.
19. method according to claim 16 is characterized in that, described on first sample surfaces step of depositing conductive material comprise that the direct jet with gas bombards first sample surfaces, and use the energy beam decomposition gas.
20. method according to claim 19 is characterized in that, described energy beam is an electron beam.
21. method according to claim 19 is characterized in that, described energy beam is an ion beam.
22. method according to claim 19 is characterized in that, described energy beam comprises photon.
23. method according to claim 11 is characterized in that, the step of described adjustment electrostatic force also comprises:
Comprising energy beam of raster scanning on the visual field of particle;
Raster scanning is programmed to have the predetermined residence time and position so that particle has static charge, and wherein said position comprises the position of particle.
24. method according to claim 23 is characterized in that, described energy beam is an electron beam.
25. method according to claim 23 is characterized in that, described energy beam is an ion beam.
26. method according to claim 23 is characterized in that, described energy beam comprises photon.
27. method according to claim 11 is characterized in that, the step of described adjustment electrostatic force comprises: tip by making probe or limit act on controls the surface area that particle is exposed to probe on the particle, thereby obtains adhering to of particle and probe.
28. method according to claim 1 is characterized in that, the described step that particle is attached on the probe tip comprises the Dc bias of adjusting between the probe and first sample surfaces.
29. method according to claim 1 is characterized in that, describedly particle is attached to step on the probe tip comprises with tweezers and catches particle.
30. method according to claim 1 is characterized in that, the described step that particle is attached on the probe tip is included in probe tip use bonding agent.
31. method according to claim 1 is characterized in that, the described step that second sample surfaces was removed and moved to particle from probe comprises the Dc bias of adjusting between the probe and second sample surfaces.
32. method according to claim 1 is characterized in that, the described step that second sample surfaces was removed and moved to particle from probe is included in probe and applies time dependent voltage.
33. method according to claim 32 is characterized in that, described time dependent voltage is a pulse.
34. method according to claim 32 is characterized in that, described time dependent voltage is by being produced by the negative charge of the quick conversion of probe from the storage of capacitor.
35. method according to claim 32 is characterized in that, described time dependent voltage is sinusoidal voltage.
36. method according to claim 1 is characterized in that, the described step that second sample surfaces was removed and moved to particle from probe comprises that adjustment electrostatic force is to produce repulsive force between probe and particle.
37. method according to claim 36 is characterized in that, the step of described adjustment electrostatic force also comprises:
Adjustment is incident on the energy of the energy beam on the particle, makes particle, second sample surfaces and probe tip static electrification lotus, so that produce electrostatic repulsion forces between particle and probe tip, and produces electrostatic attraction between second sample surfaces and particle.
38., it is characterized in that described energy beam is an electron beam according to the described method of claim 37.
39., it is characterized in that described energy beam is an ion beam according to the described method of claim 37.
40., it is characterized in that described energy beam comprises photon according to the described method of claim 37.
41. method according to claim 36 is characterized in that, the step of described adjustment electrostatic force comprises that also particle has static charge; And depositing conductive material on second sample surfaces is to distribute on the particle position and to change electric charge on second sample surfaces.
42., it is characterized in that the described conductive material that is deposited on second sample surfaces comprises polarizable particulate according to the described method of claim 41.
43. according to the described method of claim 41, it is characterized in that, be deposited on the conductive film of described conductive material on second sample surfaces for evaporating.
44. according to the described method of claim 41, it is characterized in that, described on second sample surfaces step of depositing conductive material comprise that the direct jet with gas bombards second sample surfaces, and decompose this gas with energy beam.
45., it is characterized in that described energy beam is an electron beam according to the described method of claim 44.
46., it is characterized in that described energy beam is an ion beam according to the described method of claim 44.
47., it is characterized in that described energy beam comprises photon according to the described method of claim 44.
48. method according to claim 36 is characterized in that, the step of described adjustment electrostatic force also comprises:
Comprising energy beam of raster scanning on the visual field of particle;
Raster scanning is programmed to have the predetermined residence time and position so that particle has static charge, and wherein said position comprises the position of particle.
49., it is characterized in that described energy beam is an electron beam according to the described method of claim 48.
50., it is characterized in that described energy beam is an ion beam according to the described method of claim 48.
51., it is characterized in that described energy beam comprises photon according to the described method of claim 48.
52. method according to claim 1 is characterized in that, described second sample surfaces comprises bonding agent, to cooperate with particle.
53. method according to claim 1 is characterized in that, the elastic modulus of the elastic modulus of described second sample surfaces and the biddability of probe and particle is Comparatively speaking less.
54. method according to claim 1 is characterized in that, described second sample surfaces insulate; The charged pattern of writing is thereon arranged on second sample surfaces; Electric charge on this charged pattern and the opposite charge on the particle.
55. method according to claim 1 is characterized in that, described second sample surfaces is a fold.
56. method according to claim 1 is characterized in that, the step of described analysing particulates composition also comprises:
Shine particle with analysed beam, and
Detect the emission situation of particle.
57., it is characterized in that described analysed beam is an electron beam according to the described method of claim 56.
58., it is characterized in that described analysed beam is an ion beam according to the described method of claim 56.
59., it is characterized in that described analysed beam comprises photon according to the described method of claim 56.
60. method according to claim 1 is characterized in that, described second sample surfaces is a self-supporting, but thinner than the penetration depth of analysed beam.
61. method according to claim 1 is characterized in that, described second sample surfaces is a porous surface.
62. method according to claim 1 is characterized in that, described second sample surfaces is thinner than the penetration depth of analysed beam, and second sample surfaces is by the framework support of bottom.
63., it is characterized in that the framework of described bottom is a grid according to the described method of claim 62.
64. method according to claim 1 is characterized in that, described second sample surfaces is a probe tip; And the step that wherein said analysing particulates is formed comprises the composition of the particle on the analysis probe tip.
65. according to the described method of claim 64, it is characterized in that the step that probe and accompanying particle are removed from first sample surfaces is to remove from probe and accompanying particle by the position of the probe that is maintained fixed and with first sample surfaces to finish.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/US2004/018206 WO2005123227A2 (en) | 2004-06-08 | 2004-06-08 | Method for manipulating microscopic particles and analyzing the composition thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1977159A true CN1977159A (en) | 2007-06-06 |
Family
ID=35510284
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2004800379489A Pending CN1977159A (en) | 2004-06-08 | 2004-06-08 | Method for manipulating microscopic particles and analyzing the composition thereof |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP1754049A2 (en) |
| CN (1) | CN1977159A (en) |
| CA (1) | CA2543396A1 (en) |
| WO (1) | WO2005123227A2 (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102016525B (en) * | 2008-05-08 | 2014-07-02 | 恪纳腾公司 | In-situ differential spectroscopy |
| CN104236978A (en) * | 2014-09-30 | 2014-12-24 | 中国原子能科学研究院 | Method for measuring isotope ratio of uranium in single particle |
| CN105797867A (en) * | 2016-05-09 | 2016-07-27 | 长安大学 | Electrostatic mineral particle selector |
| CN110595848A (en) * | 2018-06-12 | 2019-12-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of micron-sized particle transmission electron microscope sample |
| CN111521623A (en) * | 2020-04-28 | 2020-08-11 | 广西大学 | Method for improving sample preparation success rate of powder sample transmission electron microscope in-situ heating chip |
| CN111693555A (en) * | 2020-06-18 | 2020-09-22 | 中国科学院地球化学研究所 | Method for in-situ preparation of TEM (transmission electron microscope) sample of nano-scale particles in complex-structure sample |
| CN113804607A (en) * | 2020-06-17 | 2021-12-17 | 阅美测量系统（上海）有限公司 | Method for fixing particles in detection of scanning electron microscope and energy spectrometer (SEM-EDX) |
| WO2022178903A1 (en) * | 2021-02-28 | 2022-09-01 | 浙江大学 | Method and device for manufacturing microdevice |
| CN116477566A (en) * | 2023-03-23 | 2023-07-25 | 清华大学 | Single-particle microelectrode preparation method based on microcapillary injection |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006045620B4 (en) | 2006-09-25 | 2009-10-29 | Roland Dr. Kilper | Device and method for receiving, transporting and storing microscopic samples |
| EP1953789A1 (en) | 2007-02-05 | 2008-08-06 | FEI Company | Method for thinning a sample and sample carrier for performing said method |
| JP5849331B2 (en) * | 2011-08-31 | 2016-01-27 | 国立大学法人静岡大学 | Micro-adhesion peeling system and micro-adhesion peeling method |
| CN112180124A (en) * | 2020-08-31 | 2021-01-05 | 上海交通大学 | Preparation method of submicron probe for atomic force microscope |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4590792A (en) * | 1984-11-05 | 1986-05-27 | Chiang William W | Microanalysis particle sampler |
| US6188068B1 (en) * | 1997-06-16 | 2001-02-13 | Frederick F. Shaapur | Methods of examining a specimen and of preparing a specimen for transmission microscopic examination |
| US6777674B2 (en) * | 2002-09-23 | 2004-08-17 | Omniprobe, Inc. | Method for manipulating microscopic particles and analyzing |
-
2004
- 2004-06-08 WO PCT/US2004/018206 patent/WO2005123227A2/en not_active Application Discontinuation
- 2004-06-08 CN CNA2004800379489A patent/CN1977159A/en active Pending
- 2004-06-08 CA CA002543396A patent/CA2543396A1/en not_active Abandoned
- 2004-06-08 EP EP04754729A patent/EP1754049A2/en not_active Withdrawn
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102016525B (en) * | 2008-05-08 | 2014-07-02 | 恪纳腾公司 | In-situ differential spectroscopy |
| CN104236978A (en) * | 2014-09-30 | 2014-12-24 | 中国原子能科学研究院 | Method for measuring isotope ratio of uranium in single particle |
| CN105797867A (en) * | 2016-05-09 | 2016-07-27 | 长安大学 | Electrostatic mineral particle selector |
| CN105797867B (en) * | 2016-05-09 | 2018-05-04 | 长安大学 | A kind of electrostatic mineral microparticle Chooser |
| CN110595848A (en) * | 2018-06-12 | 2019-12-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of micron-sized particle transmission electron microscope sample |
| CN111521623A (en) * | 2020-04-28 | 2020-08-11 | 广西大学 | Method for improving sample preparation success rate of powder sample transmission electron microscope in-situ heating chip |
| CN113804607A (en) * | 2020-06-17 | 2021-12-17 | 阅美测量系统（上海）有限公司 | Method for fixing particles in detection of scanning electron microscope and energy spectrometer (SEM-EDX) |
| CN111693555A (en) * | 2020-06-18 | 2020-09-22 | 中国科学院地球化学研究所 | Method for in-situ preparation of TEM (transmission electron microscope) sample of nano-scale particles in complex-structure sample |
| CN111693555B (en) * | 2020-06-18 | 2021-08-10 | 中国科学院地球化学研究所 | Method for in-situ preparation of TEM (transmission electron microscope) sample of nano-scale particles in complex-structure sample |
| WO2022178903A1 (en) * | 2021-02-28 | 2022-09-01 | 浙江大学 | Method and device for manufacturing microdevice |
| CN116477566A (en) * | 2023-03-23 | 2023-07-25 | 清华大学 | Single-particle microelectrode preparation method based on microcapillary injection |
| CN116477566B (en) * | 2023-03-23 | 2024-04-09 | 清华大学 | Single-particle microelectrode preparation method based on microcapillary injection |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2005123227A2 (en) | 2005-12-29 |
| WO2005123227A3 (en) | 2006-12-14 |
| CA2543396A1 (en) | 2005-12-29 |
| EP1754049A2 (en) | 2007-02-21 |
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