CN105651792A - SEM transmission electron Kikuchi diffraction apparatus and analytical method - Google Patents
SEM transmission electron Kikuchi diffraction apparatus and analytical method Download PDFInfo
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Abstract
本发明提供了一种扫描电镜中透射电子菊池衍射装置及分析方法，该装置包括：用于对样品照射电子束的电子束照射单元；位于所述电子束照射单元下方的背散射电子衍射探测器和样品台；所述样品台配置为使载置于其上的所述样品与水平面之间形成倾斜角；所述探测器具备配置为采集并接收所述样品发出的透射电子信号的磷屏。本发明能够获得清晰的透射电子菊池衍射图谱，实现对纳米尺度晶粒的相鉴定及相比例计算、纳米尺度织构及取向差分析，晶粒尺寸及形状的分析，晶界、亚晶及孪晶性质的分析等。
The invention provides a transmission electron Kikuchi diffraction device and analysis method in a scanning electron microscope, the device comprising: an electron beam irradiation unit for irradiating an electron beam to a sample; a backscattered electron diffraction detector located below the electron beam irradiation unit and a sample stage; the sample stage is configured to form an inclined angle between the sample placed on it and the horizontal plane; the detector is provided with a phosphor screen configured to collect and receive transmitted electronic signals emitted by the sample. The invention can obtain clear transmission electron Kikuchi diffraction pattern, realize phase identification and phase ratio calculation of nanoscale grains, analysis of nanoscale texture and misorientation, analysis of grain size and shape, grain boundary, subgrain and twin Analysis of crystal properties, etc.
Description
Technical field
The present invention relates to the microstructure analysis equipment of Material Field, particularly, relate to transmission electricity in a kind of ESEMSub-Kikuchi diffraction device and analytical method.
Background technology
Field emission scanning electron microscope (FESEM) is the microstructure analysis equipment that is widely used in Material Field both at home and abroad, noOnly can Inorganic Non-metallic Materials microstructure be characterized approaching reset condition (non-plating conducting film state), can also determine simultaneouslyChemical composition and structural information in property, quantitative measurment microcosmos area are research and development, improvement in performance, the failure analysis of advanced materialDeng scientific basis is provided. In existing FESEM, the analysis means of material crystals is only had to EBSD (ElectronBackscatterDiffraction, EBSD), by the Kikuchi style of EBSD, can analyze micro-meter scaleCrystal grain texture, misorientation, crystal boundary, subgrain and twin etc. Compare with other characterization techniques, EBSD technology has following characteristics:
(1) can even within the scope of mm-scale, provide material microstructure, structure, distribution of orientations and crystalline substance at hundreds of micron simultaneouslyThe much informations such as grain size distribution.
(2) especially responsive to the variation of crystal orientation, be particularly suitable for the variation of crystal orientation in research material. EBSD technologyIn Kikuchi band be always distributed in the both sides of hkl crystal face, the width of Kikuchi band always equals the distance of transmission spot to diffraction spotFrom. So along with the variation of crystal orientation, correspondingly the position of Kikuchi band also can occur significantly to change. Therefore, EBSD canTo carry out well the sign of crystal orientation.
(3) sample sample preparation is simple, can the larger bulk sample of Direct Analysis. EBSD technology is attached as ESEMPart, sample is without attenuate, and sample making course is relatively simple. But, because EBSD is logical in tens nanometer range of specimen surfaceCross that electronic diffraction generates, require the smooth and not distortion of specimen surface to be analyzed, specimen surface or sub-surface without deformation layer,Pollutant, oxide or reaction product layer. Owing to existing larger angle of inclination (to be generally between specimen surface and electron beam70 °), therefore sample surface flatness is had relatively high expectations.
(4) poor to the certainty of measurement of cell parameter, must rely on Energy disperaive quantitative analysis (EnergyDispersiveSpectrometry, EDS) or wave spectrum quantitative analysis (WavelengthDispersiveSpectroscopy, WDS) abilityCarry out the identification of phases more accurately.
(5) spatial resolution is poor. The identification of phases of EBSD technology and the spatial resolution master of orientation analysisDepend on that the backscattered electron that diffraction occurs produces scope. Sample certain angle that need to tilt during EBSD analyzes, causes electricitySon bundle is slightly variant with the resolution ratio of vertical direction in the horizontal direction. No matter be horizontal direction or the spatial discrimination of vertical directionRate is all inferior to the spatial resolution of secondary electron image in ESEM or backscattered electron image far away.
But EBSD analyzes and requires sample precise polished (surperficial no marking and residual stress), requires sample necessary simultaneouslyConduction, plating conducting film can seriously be covered style contrast, causes style None-identified. Therefore, EBSD is at present in metal material fieldApply more. And it is less that EBSD is applied to the report of non-conductive Inorganic Non-metallic Materials. The accelerating potential that traditional E BSD analyzesFor 20kV, the sphere of action of incident electron and block sample is larger, and the spatial resolution of EBSD is poor, is about 150nm, Bu NengfenAnalyse orientation and the crystallography information of nanoscale; And EBSD necessarily requires sample by precise polished, at the large angle of inclination of 70 °Under, the height relief on surface can be blocked the transmission path of diffraction electronics, nano particle that therefore can not analyzing irregular shape.
Within 2012, start to have report abroad, by repacking ESEM (SEM) sample stage and EBSD detector position, realizeOn SEM, use EBSD detector acquisition of transmission electronics Kikuchi diffraction spectrogram, improved the spatial resolution that EBSD analyzes, stillIn the world without relevant equipment, also there is no the report of pertinent instruments scrap build both at home and abroad at present.
Summary of the invention
In view of the problem of above existence, technical problem to be solved by this invention is to provide transmission in a kind of ESEMElectronics Kikuchi diffraction device and analytical method, can obtain transmitted electron Kikuchi diffraction collection of illustrative plates clearly, realizes nanoscaleThe identification of phases of crystal grain and the calculating of phase ratio, nanoscale texture and misorientation analysis, the analysis of crystallite dimension and shape, crystal boundary,The analysis of subgrain and twin character etc.
In order to solve the problems of the technologies described above, on the one hand, to the invention provides transmitted electron Kikuchi in a kind of ESEM and spread outInjection device, comprising: for the electron beam irradiation unit to sample irradiation electron beam; Be positioned at described electron beam irradiation unit belowEBSD detector and sample stage; Described sample stage be configured to make described sample thereon of mounting and horizontal plane itBetween form inclination angle; Described detector possesses the phosphorus screen that is configured to gather and receive the transmitted electron signal that described sample sends.Preferably, to be configured to make angulation between described sample thereon of mounting and horizontal plane be 20 ° to described sample stage.
Transmitted electron Kikuchi diffraction device in ESEM of the present invention, is the repacking to existing FESEM-EBSD system,Realizing the Kikuchi that utilizes EBSD detector to receive transmitted electron on existing high-resolution field emission scanning electron microscope spreads outPenetrate the method for style. Be specifically related to the Design & reform of sample stage, to obtain transmitted electron Kikuchi diffraction collection of illustrative plates clearly, realizeThe nanoscale identification of phases and the calculating of phase ratio, nanoscale texture and misorientation are analyzed to dividing of nanoscale, crystal grain and shapeAnalyse nanoscale, crystal boundary, the analysis of subgrain twin etc. Compared with the conventional method, advantage of the present invention is by scrap build, utilizesOriginal back scattering detector phosphorus screen changes collection into from gathering, receive backscattered electron (EBSD system), receives transmitted electronSignal (t-EBSD system), brings up to 20nm by the spatial resolution of EBSD by 150nm.
Again, in the present invention, can be also described detector and described electron beam irradiation unit distance in vertical directionFrom being 1～6mm. Described EBSD detector is described electron beam irradiation unit working distance in vertical directionFrom, best effort distance is 1 ~ 6mm.
According to the present invention, by adjusting the position of EBSD detector, be conducive to shorten the work of ESEM under transmission modeMake distance, solve EBSD detector and sample interval from larger problem.
Again, in the present invention, can be also that described sample stage comprises support and is installed on the sample mounting on described supportPortion, forms described inclination angle between the upper surface of described sample mounting portion and horizontal plane. , preferably, described inclination angle is 20Degree.
According to the present invention, be conducive to make to load between sample on the upper surface of sample mounting portion and horizontal plane and form instituteNeed inclination angle.
Again, in the present invention, can be also, described sample comprises the thin slice after nano-powder and ion milling.
According to the present invention, sample type expands to nano-powder etc. by the block sample of polishing, has expanded the application of EBSDSpace, crystal structure to nano material, orientation texture, crystal boundary angle etc. provide a kind of brand-new characterization method.
Again, in the present invention, can be also that the thickness of described thin slice is tens nanometer to one hundred nanometers.
According to the present invention, can obtain the good t-EBSD style of quality.
On the other hand, the present invention also provides a kind of and adopts transmitted electron Kikuchi diffraction device in above-mentioned ESEM to carry outAnalytical method, comprising: prepare sample; Sample is loaded on sample stage; Regulate sample stage and EBSD detectorPosition and angle, described sample stage is adjusted to and makes to form inclination angle between described sample thereon of mounting and horizontal plane; AdoptWith electron beam illumination unit to described sample irradiation electron beam; Phosphorus screen by described EBSD detector gathers alsoReceive the transmitted electron signal that described sample sends.
Again, in the present invention, can be also, also comprise by described EBSD detector be adjusted to its with described inElectron beam irradiation unit distance is in vertical direction 1～6mm.
Again, in the present invention, can be also that the described step of preparing sample comprises disperses the particle of superfine powder to prepareNano sized powder sample.
Again, in the present invention, can be also, the described step of preparing sample comprises dicing sheet from bulk sample, withAfter described thin slice is ground to attenuate, the more described sample grinding after attenuate is further carried out to ion milling, with prepare fromThin slice sample after sub-attenuate.
Again, in the present invention, can be also that thickness tens nanometers to one hundred of the thin slice sample after described ion milling are receivedRice.
According to following detailed description of the invention and with reference to accompanying drawing, will understand better foregoing of the present invention and other order, feature and advantage.
Brief description of the drawings
Fig. 1 shows the generalized schematic before and after FESEM-EBSD system modification, and wherein, Fig. 1 (A) shows before repackingEBSD system, Fig. 1 (B) shows the t-EBSD system after repacking;
Fig. 2 shows Monte Carlo simulation traditional E BSD and t-EBSD pattern incident electron range of scatter, and wherein, Fig. 2 (A) illustratesThe traditional E BSD pattern incident electron range of scatter of Fig. 1 (A), Fig. 2 (B) shows the t-EBSD pattern of the present invention of Fig. 1 (B)Incident electron range of scatter;
Fig. 3 shows backscattered electron and transmitted electron Energy distribution comparison diagram under 30kV accelerating potential;
The sample that Fig. 4 shows EBSD and t-EBSD in SEM is placed schematic diagram before and after transformation, and wherein, Fig. 4 (A) shows repackingFront EBSD system photo in kind, Fig. 4 (B) shows the t-EBSD system of the present invention photo in kind after repacking, and Fig. 4 (C) showsGone out the sample mounting parts photo in kind in the system of Fig. 4 (B), the sample that Fig. 4 (D) shows in the system of Fig. 4 (B) carriesPut parts photo in kind, Fig. 4 (E) shows the sample mounting parts structural representation in the system of Fig. 4 (B);
Fig. 5 (A) and Fig. 5 (B) show in the present invention the upwards illustrative diagram of translation 6mm of EBSD detector position;
Fig. 6 shows the SiC/BN composite ceramics attenuate sample SEM characterization result that adopts apparatus of the present invention;
The schematic diagram of the impact of the thickness that Fig. 7 shows attenuate sample on t-EBSD style;
Fig. 8 shows the t-EBSD characterization result of zirconia coating, wherein Bar=1 μ m, a: crystal grain band contrast, b: zirconia is coated withThe phasor of layer, c:t-EBSD grain orientation figure;
Fig. 9 shows t-EBSD Kikuchi style and database crystal structure information matches degree;
A in Figure 10 illustrates size and distributes between the zirconia crystal grain of 30-100nm; B illustrates crystallite dimension in coatingDistribution map;
Figure 11 shows the SEM characterization result of nano titanium oxide powder, wherein Bar=200nm;
Figure 12 shows nano titanium oxide powder individual particle t-EBSD Kikuchi style, and wherein, a figure is Anatase, and b figure is golden redShi Xiang.
Detailed description of the invention
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodimentOnly for the present invention is described, and unrestricted the present invention.
In order to overcome defect of the prior art, the present invention, by the repacking to existing FESEM-EBSD system, realizesOn existing high-resolution field emission scanning electron microscope, utilize the phosphorus screen of original EBSD detector to fall apart from gathering, receive the back of the bodyRadio changes collection into, receives transmitted electron signal. By designing the position of new sample stage and adjustment EBSD detector, pieceThe ion milling of body sample to be to obtain transmitted electron Kikuchi diffraction collection of illustrative plates clearly, realize the identification of phases to nanoscale crystal grain,Texture and misorientation analysis, the analysis of crystallite dimension and shape, the analysis of crystal boundary, subgrain and twin character etc.
For this reason, the invention provides a kind of transmitted electron Kikuchi diffraction device (t-EBSD) of repacking, comprise the new sample of designThe position of product platform and adjustment EBSD detector, by utilizing original back scattering detector phosphorus screen from gathering, receive back scattering electricitySon changes collection into, receives transmitted electron signal, and the 6mm that simultaneously EBSD detector moved up makes scanning electricity under transmission modeThe operating distance of mirror is reduced to 1mm from 6mm, solves between original for example Magellan400 ESEM pole shoe and sample stageDistance is shorter, causes EBSD detector and sample interval from larger problem, and the phosphorus screen of original EBSD detector can be receivedTo clear, complete transmitted electron Kikuchi Diffraction Patterns, can realize the identification of phases, texture and orientation difference to nanoscale crystal grainAnalyse the analysis of crystallite dimension and shape, analysis of crystal boundary, subgrain and twin character etc. By the spatial resolution of traditional E BSDBring up to 20nm by 150nm, sample type expands to nano-powder etc. by the block sample of polishing, has expanded the application sky of EBSDBetween, utilize the transmitted electron Kikuchi Diffraction Patterns that sideline intensity is high simultaneously, improve the accurate of crystallographic structural analysis, orientation demarcationDegree. Crystal structure to nano material, orientation texture, crystal boundary angle etc. provide a kind of brand-new characterization method. After transformationT-EBSD system can characterize as follows:
(1) identification of phases of nanoscale and phase ratio are calculated.
(2) identification of phases: t-EBSD goes out crystal parameters by Kikuchi diffraction spectrum elucidation, to distinguish chemical composition phaseSeemingly, the different phase of crystal structure; Phase ratio is calculated: various phase transformations in research solid phase reaction process, and the measurement of conversion proportionDeng.
(3) texture of nanoscale and misorientation analysis: measure and be respectively oriented in ratio shared in sample, obtain this orientationDistribution in microscopic structure, the crystallography analysis of transcrystalline cracking, the integrality of monocrystal, along the Elements Diffusion of crystallization direction,The measurement of deformation research, thin-film material grain growth direction etc.
(4) crystal grain of nanoscale and the analysis of shape: more difficult twin, sub boundary and the little angle crystalline substance of manifesting of conventional caustic solutionBoundary, is used t-EBSD to measure the crystallite dimension of particular sample microscopic structure.
(5) crystal boundary of nanoscale, subgrain twin are analyzed: by scanning two misorientation information between adjacent area,Can study crystal boundary, subgrain, phase boundary, twin boundary etc.
Particularly, for achieving the above object, the technical solution used in the present invention is as follows:
1, the design of sample stage processing and the position of EBSD detector and the adjustment of angle
The design processing of sample stage and the adjustment of EBSD probe positions and angle must make sample stage can clamp TEM copper mesh andSample after ion milling, EBSD detector can be collected clear, complete transmitted electron Kikuchi Diffraction Patterns simultaneously; AdoptAccurately measure bleeding point position and the angle of objective pole shoe, sample stage zero coordinate points, EBSD probe. According in the probe of detectorThe crosspoint of line and objective pole shoe center line determines that the horizontal line of STEM platform zero coordinate points is criterion.
Due to sample surfaces in EBSD and phosphorus screen surfaces not parallel, when EBSD dispatches from the factory according to the probe installation position of Electronic Speculum manufacturerPut and angle parameter built-in the automatically setting of conversion of vector of coordinate system, but sample stage, the position of detector, angle after repackingDegree occurs all to change, therefore, and electron beam coordinate system CSbeam, sample coordinate system CSsample and phosphorus screen coordinate systemThe vector of CSscreen and orientation need to redefine. Use 100 known oriented single crystal silicon attenuate standard specimens of structure to carry outProofread and correct, the sample stage after design processing is repeatedly adjusted, revised, telescopic location and angle adjustment to EBSD are repaiiedJust, determine best WD value and DD value simultaneously, finally obtaining the transmitted electron Kikuchi diffraction spectrogram that style is clear and complete.
Utilize the vector under electron beam coordinate system to change formula:, sample stage under traditional E BSD patternAngle of inclination is 70 °, and its rotating vector matrix is; According to after above-mentioned design processingThe inclination angle-θ of STEM sample, obtain the rotating vector matrix under t-EBSD:, the actual orientation coordinate under t-EBSD pattern is: the orientation coordinate that manufacturer's software is measured is multiplied by conversion coefficient:.
When traditional EBSD pattern (Fig. 1 (A)), the sample rim surface zona effect of electron beam and wide-angle tilt, diffraction occursIn the interaction of backscattered electron and lattice plane, sample surfaces is verted after 60 °～70 °, backscattered electron efferent pathwayShorten, more diffraction electronics can be escaped out from surface and be received by EBSD detector, but the work of incident electron and block sampleLarger by scope, the transverse area that produces backscattered electron is the above (see figure 2) of hundreds of nanometer, and therefore spatial resolution is poor(～150nm), most backscattered electrons the evolving path in sample is longer, and after Multiple Scattering, energy attenuation is serious(in Fig. 3, [1] region is under 30kV accelerating potential, the Energy distribution of the backscattered electron producing in block sample single crystalline Si). ChangeSample stage after dress is changed into for example 20 (Fig. 1 (B)) from sample inclination 70 (Fig. 1 (A)); Simultaneously by EBSD detector position toUpper translation 6mm, obtains the t-EBSD pattern as shown in Fig. 1 (B), because thickness of sample is less, and the horizontal proliferation district of incident electronTerritory is less, and its horizontal proliferation region only has tens nanometer (see figure 2)s, and original back scattering detector phosphorus screen is from gathering, receive the back of the bodyScattered electron changes collection into, receives transmitted electron signal, and the evolving path of transmitted electron in sample is shorter, transmitted electronEnergy attenuation is few, and Energy distribution is comparatively concentrated, and ([2] region of Fig. 3 is that under 30kV accelerating potential, it is thick that incident electron penetrates 100nmThe Energy distribution of the transmitted electron producing in the single crystalline Si of degree). Therefore, the Kikuchi Diffraction Patterns of transmitted electron is more clear, spreads outThe sideline intensity of penetrating band is high, and the data precision of measuring from Kikuchi band is higher. Improved t-EBSD device can be referring to Fig. 4, Fig. 5.
2, the impact of the thickness after block sample attenuate on t-EBSD style
The sample that can carry out t-EBSD analysis is the thin slice after nano-powder and ion milling. Key prepared by powder sample be byThe particle of superfine powder disperses: step is for adopting ultrasonic stirrer, the powder that will observe or particulate samples adds water or solvent stirsMix as suspension, by the sample copper mesh that is stained with carbon supporting film again evaporation one deck carbon film to improve electric conductivity, be suspended with dropper handleDrop, on sample copper mesh, evenly spreads on supporting film powder or particulate samples, after standing and drying, observes for t-EBSD. ByPenetration capacity in electron beam is lower, and the block of analyzing for t-EBSD need carry out laminating after ion milling, conventionally palpusProcess following steps:
(1) dicing sheet from bulk sample;
(2) thin slice sample is ground to attenuate;
(3) sample that grinds attenuate is further carried out to ion milling.
When thin slice is ground to 50 μ m left and right, then take out some diameter 3mm wafer samples from thin slice and carry out final ionAttenuate, uses ion beam to peel off sample skin-material, finally makes sample be thinned to the thickness that electron beam can pass through.
Thickness after block sample ions attenuate has larger impact to t-EBSD style, sample need be thinned to one suitableThickness. When ion milling, sample is positioned in high vacuum sample room, ar-ion beam adds from both sides at 3kV-5kV accelerating potentialThe lower bombardment specimen surface of speed, sample surfaces becomes the angle at 0o-30o angle with respect to ion beam. Ion milling method can extensively be suitable forIn mineral, pottery, semiconductor etc. Thickness after sample ion attenuate has larger impact to t-EBSD style, and sample is too thin, subtractsWhen thin, very easily produce amorphous layer, amorphous layer covers on sample, has a strong impact on diffraction pattern; For blocked up region, transmitted electronTail off, Kikuchi lines is also unintelligible. Therefore attenuate sample, only at suitable thickness range, just can obtain the good t-EBSD of qualityStyle.
Then, the thickness being described more specifically after sample attenuate has larger impact to t-EBSD style, multiple with SiC/BNClosing ceramic attenuate sample is example (referring to Fig. 6): after attenuate, A point is near the hole of attenuate, and F point is away from the hole of attenuate, from A to F, thickDegree increases gradually. A to F point is characterized with t-EBSD, its corresponding Kikuchi style is presented in Fig. 7. Can find out B pointStyle quality obviously better, be obviously better than A point, this interpret sample is too thin, very easily produces amorphous layer when attenuate, amorphous layer coverOn sample, for crossing thin region, have a strong impact on diffraction pattern. Also variation gradually of the diffraction pattern that C point is ordered to F, thisBe the increase along with thickness of sample, transmitted electron tails off, and Kikuchi lines is also unintelligible. Therefore attenuate sample is only at suitable thicknessScope, just can obtain the good t-EBSD style of quality.
Further describe the present invention by specific embodiment below.
Embodiment 1: the t-EBSD of zirconia nano coating is characterized
Thermal boundary zirconia coating is widely used in the hot-end components such as the blade of aero-engine, utilizes its lower thermal conductivity to reduceThe thermal force that matrix bears, the effect that play protection matrix, increases the service life. Understand the crystal grain group mutually of thermal boundary zirconia coatingOne-tenth and size distribution play vital effect to improving its military service performance. Zirconia coating after ion milling is carried out to t-EBSD characterizes, EBSD voltage 30kV, and electric current 6.4nA, operating distance 1mm, obtains the sign knot shown in Fig. 8Really. The variable thickness of sample causes the band contrast difference in the each region that causes sample, and obtains minimum diameter only for 30nm's((ZrO2)0.88(Y2O3)0.12) crystal grain. And according to Fig. 9, the average MAD of t-EBSD is 0.38 °, the Kikuchi diffraction flower of interpret sampleIt is very good that sample mates with the Kikuchi style in crystal storehouse. Figure 10 has also shown the distribution shape of the medium and small crystal grain of zirconia nano coating simultaneouslyCondition, by this example explanation, t-EBSD makes the face distribution space resolution ratio of EBSD be about 30nm.
Embodiment 2: the t-EBSD of nano titanium oxide powder is characterized
TiO2Be a kind of material that obtains extensive use in photocatalysis field, its common crystal formation is that photocatalysis performance is sharp preferablyTitanium ore and rutile two-phase. Crystallite dimension is to affect TiO2The key factor of photocatalytic activity, crystal grain is less, crystal activated centreCan more fully come out, be conducive to the raising of catalytic activity; Meanwhile, the photo-generated carrier of little crystal grain is more logical than large crystal grainCross diffusion from crystal grain internal migration to surface, be conducive to promote the generation of reaction, improve photocatalysis efficiency. Therefore, to nanometer chiDegree TiO2The grain size of particle and crystal formation characterize studying its photocatalysis performance significant.
Figure 11 is TiO2The secondary electron image of nano-powder, the little crystallite dimension that in figure, A indicates is 19nm, to itCarry out t-EBSD analysis, its Kikuchi style is presented in a figure of Figure 12, visible, the Kikuchi style of this crystal grain and AnataseStandard Kikuchi style is identical, and this is the TiO of anatase mutually2. The size that B in Figure 11 is indicated is about the little crystal grain of 40nmCarry out t-EBSD analysis, its Kikuchi style is shown in the b figure of Figure 12, the standard Kikuchi style of the Kikuchi style of this crystal grain and Rutile TypeBe identical, determine that this crystal grain is rutile TiO2. By t-EBSD to TiO2The sign of nano-powder, proves improvedT-EBSD system can be brought up to 20nm by spatial resolution.
Do not departing under the aim of essential characteristic of the present invention, the present invention can be presented as various ways, therefore in the present inventionExample be to be illustrative rather than definitive thereof, be defined by the claims due to scope of the present invention but not limited by description,And drop on the scope that claim defines, or all changes in the full scope of equivalents of its scope defining are all understood to includeIn claims.
Claims (10)
1. a transmitted electron Kikuchi diffraction device in ESEM, is characterized in that, comprising:
For the electron beam irradiation unit to sample irradiation electron beam;
Be positioned at EBSD detector and the sample stage of below, described electron beam irradiation unit;
Described sample stage is configured to make form inclination angle between described sample thereon of mounting and horizontal plane;
Described detector possesses the phosphorus screen that is configured to gather and receive the transmitted electron signal that described sample sends.
2. transmitted electron Kikuchi diffraction device in ESEM according to claim 1, is characterized in that described detectorWith described electron beam irradiation unit distance be in vertical direction 1～6mm.
3. transmitted electron Kikuchi diffraction device in ESEM according to claim 1 and 2, is characterized in that described sampleProduct platform comprises support and is installed on the sample mounting portion on described support, between the upper surface and horizontal plane of described sample mounting portionForm described inclination angle, preferably, described inclination angle is 20 degree.
4. according to transmitted electron Kikuchi diffraction device in the ESEM described in any one in claims 1 to 3, its feature existsIn, described sample comprises the thin slice after nano-powder and ion milling.
5. transmitted electron Kikuchi diffraction device in ESEM according to claim 4, is characterized in that, described thin sliceThickness is tens nanometer to one hundred nanometers.
6. one kind adopts in claim 1 to 5 in the ESEM described in any one that transmitted electron Kikuchi diffraction device is carried outAnalytical method, is characterized in that, comprising:
Prepare sample;
Sample is loaded on sample stage;
Regulate position and the angle of sample stage and EBSD detector, described sample stage is adjusted to and makes mounting thereonDescribed sample and horizontal plane between form inclination angle;
Adopt electron beam irradiation unit to described sample irradiation electron beam;
Phosphorus screen by described EBSD detector gathers and receives the transmitted electron signal that described sample sends.
7. analytical method according to claim 6, is characterized in that, also comprises described EBSD detectorBe adjusted to it and described electron beam irradiation unit distance is in vertical direction 1～6mm.
8. analytical method according to claim 6, is characterized in that, the described step of preparing sample comprises superfine powderParticle disperses to prepare nano sized powder sample.
9. analytical method according to claim 6, is characterized in that, the described step of preparing sample comprises from bulk sampleUpper dicing sheet, grinds attenuate by described thin slice subsequently, the more described sample grinding after attenuate is further carried out to ionAttenuate, to prepare the thin slice sample after ion milling.
10. analytical method according to claim 9, is characterized in that, the thickness of the thin slice sample after described ion millingBe tens nanometer to one hundred nanometers.
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| CN106501292A (en) * | 2016-10-21 | 2017-03-15 | 重庆理工大学 | A kind of high-resolution crystal orientation preparation method based on scanning electron microscope |
| CN106842346A (en) * | 2016-12-23 | 2017-06-13 | 中国石油天然气股份有限公司 | Three-dimensional imaging device and method for geological reservoir |
| CN108333203A (en) * | 2018-02-09 | 2018-07-27 | 中国科学院地球化学研究所 | A kind of method of in situ detection mineral microcell EBSD images |
| JP2019027938A (en) * | 2017-07-31 | 2019-02-21 | 株式会社日立製作所 | Image processing device that realizes material informatics |
| CN109709121A (en) * | 2019-03-06 | 2019-05-03 | 内蒙古科技大学 | Sample stage and transmission mode electron backscatter diffraction (T-EBSD) system and method |
| CN110514679A (en) * | 2019-09-16 | 2019-11-29 | 南京大学 | A transmission electron microscope in-situ reaction chamber chip with a movable Raman tip probe and its application method |
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| CN111699380A (en) * | 2017-12-11 | 2020-09-22 | 法国电力公司 | Method, apparatus and program for processing diffraction image of crystalline material |
| CN113390908A (en) * | 2020-03-12 | 2021-09-14 | 中国科学院上海硅酸盐研究所 | Method for measuring interplanar spacing based on electron back scattering diffraction pattern |
| CN113804521A (en) * | 2020-06-16 | 2021-12-17 | 中国科学院上海硅酸盐研究所 | A sample stage for ultra-thin sample preparation |
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| CN106501292A (en) * | 2016-10-21 | 2017-03-15 | 重庆理工大学 | A kind of high-resolution crystal orientation preparation method based on scanning electron microscope |
| CN106842346A (en) * | 2016-12-23 | 2017-06-13 | 中国石油天然气股份有限公司 | Three-dimensional imaging device and method for geological reservoir |
| CN106842346B (en) * | 2016-12-23 | 2019-03-12 | 中国石油天然气股份有限公司 | Three-dimensional imaging device and method for geological reservoir |
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| CN108333203A (en) * | 2018-02-09 | 2018-07-27 | 中国科学院地球化学研究所 | A kind of method of in situ detection mineral microcell EBSD images |
| CN109709121A (en) * | 2019-03-06 | 2019-05-03 | 内蒙古科技大学 | Sample stage and transmission mode electron backscatter diffraction (T-EBSD) system and method |
| CN110514679A (en) * | 2019-09-16 | 2019-11-29 | 南京大学 | A transmission electron microscope in-situ reaction chamber chip with a movable Raman tip probe and its application method |
| CN110514679B (en) * | 2019-09-16 | 2021-04-30 | 南京大学 | A transmission electron microscope in-situ reaction chamber chip with a movable Raman tip probe and a method of using the same |
| CN110986790A (en) * | 2019-12-14 | 2020-04-10 | 燕山大学 | Method for measuring twin crystal face width in face-centered cubic crystal sample in transmission electron microscope |
| CN113390908A (en) * | 2020-03-12 | 2021-09-14 | 中国科学院上海硅酸盐研究所 | Method for measuring interplanar spacing based on electron back scattering diffraction pattern |
| CN113390908B (en) * | 2020-03-12 | 2023-03-10 | 中国科学院上海硅酸盐研究所 | A Measuring Method of Interplanar Spacing Based on Electron Backscattered Diffraction Pattern |
| CN111474196A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for controlling deformation generated by preparation of transmission electron microscope sample |
| CN111474196B (en) * | 2020-04-16 | 2024-01-30 | 宸鸿科技(厦门)有限公司 | Method for controlling deformation generated by sample preparation of transmission electron microscope |
| CN113804521A (en) * | 2020-06-16 | 2021-12-17 | 中国科学院上海硅酸盐研究所 | A sample stage for ultra-thin sample preparation |
| CN114609167A (en) * | 2022-03-02 | 2022-06-10 | 中国科学院上海硅酸盐研究所 | Imaging method of crystal face diffraction contrast based on electron back scattering diffraction pattern |
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