CN101308101B - Device and method for real time observing colloid matter crystal internal defect - Google Patents
Device and method for real time observing colloid matter crystal internal defect Download PDFInfo
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- CN101308101B CN101308101B CN2008101165294A CN200810116529A CN101308101B CN 101308101 B CN101308101 B CN 101308101B CN 2008101165294 A CN2008101165294 A CN 2008101165294A CN 200810116529 A CN200810116529 A CN 200810116529A CN 101308101 B CN101308101 B CN 101308101B
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Abstract
The invention discloses an apparatus for observing colloidal crystal internal defects in real time, which comprises: a light source, an illuminating beam change-over device, a sample stage, a defect imaging device and a central processing unit, and the illuminating beam change-over device, the sample stage and the defect imaging device are arrayed sequentially in tandem. The invention also discloses a method for observing colloidal crystal internal defects in real time, which concretely comprises the steps of: 1) irradiating a sample vertically by monochromatic light; 2) determining the direction of colloidal crystal diffracted light; 3) determining the direction of oblique incidence beams in the illuminating beam change-over device according to the direction of the diffracted light; 4) recording diffraction contrast images of colloidal crystal; and 5) image processing. The apparatus adopted in the invention can acquire bright and dark field images of diffraction contrast images of colloidal crystal internal defects, the bright or dark field images can be obtained without adjusting the crystal or moving the imaging device when observing the dark field images, a microscope objective is vertical to the surface of the sample all the time in the imaging process, thereby facilitating the usage of the objective with short working distance and high enlargement factor when in image formation.
Description
Technical field
The present invention relates to a kind of method and imaging device of real time observing colloid matter crystal internal defect, belong to colloidal crystal (containing photonic crystal) structure and Study of Defects field.
Background technology
Photonic crystal is the forbidden photon band material.From material structure, photonic crystal is that a class has the periodically artificial design of dielectric structure and the crystal of manufacturing on the optical wavelength yardstick.Similar with semiconductor lattice to the modulation phase of electron wave function, photonic bandgap material can be modulated the electromagnetic wave with respective wavelength---when electromagnetic wave is propagated in photonic bandgap material, owing to existing Bragg diffraction to be modulated, electromagnetic energy forms band structure.Between being with and being with band gap appears, i.e. photon band gap.Institute's prodigiosin is in the photon in the photon band gap, can not enter this crystal.Photonic crystal and semiconductor have many similarities on basic model and research thinking, people can and make photonic crystal and device thereof by design in principle, reach the purpose of control photon motion.The appearance of photonic crystal (claiming the forbidden photon band material again) is handled people and the dream of controlling photon becomes possibility.Colloidal crystal is a kind of of photonic crystal, colloid is meant the dispersant system of mean particle dia between 1～1000nm, interaction between the colloidal solid can make colloidal solid be self-assembled into the colloidal crystal of colloidal solid queueing discipline, as the opaline of occurring in nature, wing of butterfly or the like.Various defectives in the crystal such as hole, dislocation, fault etc. all have very big influence to the character and the application of material.
Colloidal crystal is than traditional crystal, and its grating constant is wanted big several orders of magnitude, and corresponding therewith electromagnetic wavelength is in the visible region.Use electron microscope when usually people study crystal structure and defective thereof, is because of the grating constant of the wavelength of electron waves and atomic crystal quite or littler; For similar idea, when studying the structure of colloidal crystal and defective, we adopt visible light to study the structure and the defective of colloidal crystal.Existing electron microscope can be observed the feature on colloidal crystal surface, but the defective of studying crystals must be utilized the feature of diffraction, the yardstick of colloidal crystal does not have diffraction effect to electronics, therefore need utilize colloid that the strong diffraction of visible light is studied matter crystal internal defect.The diffraction contrast image principle is as follows: monochromatic light irradiation colloidal crystal, only the angle theta in each interplanar distance d and crystal face and laser beam satisfies Bragg's law: 2nd sin (2 θ)=m λ, wherein n is the sample refractive index, λ, the monochromatic light ray wavelength, just can be concerned with to strengthen and produce diffracted beam, colloidal solid in the colloid matter crystal internal defect field departs from the normal position, thereby make the d value of local and θ value not satisfy Bragg's law, this part does not produce relevant the enhancing, therefore the intensity of the picture of this part is very low, has so just formed the different picture of light and shade contrast, i.e. diffraction contrast image.Diffraction contrast image can reflect Burgers vector, fault vector of the feature of matter crystal internal defect such as dislocation defects or the like.
2004, Peter Scha11 human laser diffraction micro-imaging techniques such as (coming from document Science 305 1944 (2004)) is observed dislocation defects, need adjust imaging device with complicated optional equipment when observing the darkfield image of diffraction light, the optical axis of imaging system is overlapped with diffraction light, and this method requires high to the mechanical precision of wheelwork.The situation of especially severe is to require microcobjective and sample surfaces inclination (angle of diffraction) at angle in this device.Because the microcobjective enlargement factor is big more, camera lens is more little to the distance of sample, and this has seriously limited the slewing area of imaging device, has also limited the enlargement factor and the spatial resolution of imaging device.In addition, camera lens and sample show when having angle to influence micro-imaging focuses, and causes image fog.
Summary of the invention
Problem at the prior art existence, the object of the present invention is to provide a kind of device and method of real time observing colloid matter crystal internal defect, adopt this method can obtain the diffraction contrast image of colloid matter crystal internal defect: to comprise bright field image, details in a play not acted out on stage, but told through dialogues, realize switching bright, dark field image quickly and easily, and do not need to add any optional equipment and adjust motion and the differentiation that imaging device just can Real-time and Dynamic observation dislocation.
For achieving the above object, the device of a kind of real time observing colloid matter crystal internal defect of the present invention comprises: light source, illuminating bundle switching device shifter, sample stage, defective imaging device and central processing unit, illuminating bundle switching device shifter, sample stage and defective imaging device front and back are successively arranged, described illuminating bundle switching device shifter comprises completely reflecting mirror, semi-transparent reflection mirror, long-focus condenser lens and switch, described switch can block light beam to be passed through, described illuminating bundle switching device shifter can be realized to shining the switching of the incident light on the sample, to obtain bright field image and dark field image; Described sample stage and light shaft coaxle, and can be with optical axis with perpendicular to the rotation of the axis of optical axis, sample is placed on the sample stage and can moves on perpendicular to the plane of optical axis, realizes the selected diffraction of sample and selects different diffracted beam imagings; The defective imaging device is to be made of microcobjective and CCD (charge-coupled image sensor), microcobjective place sample the back and and CCD (charge-coupled image sensor) be fixed on the same guide rail, guide rail can wind the axis rotation perpendicular to optical axis, guarantee through the light vertical irradiation behind the sample on microcobjective, it is triangular apart from imaging to regulate sample, microcobjective, CCD (charge-coupled image sensor), and the image information that CCD (charge-coupled image sensor) obtains is transferred to central processing unit and carries out data processing.
Further, described light source is the monochromatic light light source.
The method of a kind of real time observing colloid matter crystal internal defect of the present invention, concrete steps are:
1) use monochromatic light along optical axis direction vertical irradiation sample;
2) determine radiation direction behind the monochromatic light irradiation sample diffraction;
3) monochromatic light produces two bundle incident raies irradiation samples through the illuminating bundle switching device shifter, and two light beam irradiates are to the same point of sample, and wherein, the radiation direction of determining in a branch of incident ray and the step 2 is identical, and another restraints incident ray and optical axis coincidence;
4) two light beams see through sample respectively by the imaging of defective imaging device, and direct light irradiation imaging obtains bright field image, and oblique incident ray irradiation imaging obtains dark field image;
5) image information obtained of defective imaging device is transferred to central processing unit and carries out data processing.
The device of the real time observing colloid matter crystal internal defect that the present invention adopts can obtain the diffraction contrast image of colloid matter crystal internal defect: bright field image, dark field image, and can optionally allow two bundle a branch of of incident light shine on the sample by described switch, so can not be adjusted to the picture part and just directly obtain bright field image or dark field image, the method of real time observing colloid matter crystal internal defect of the present invention, utilize the light reciprocity principle when observing dark field image, obtain earlier the exit direction of light behind the diffraction along optical axis direction irradiation sample, shine sample according to the direction of light behind the diffraction then, the diffracted ray that finally obtains is the direction along optical axis, so saved the complex steps of adjusting imaging device, keep microlens vertical with sample surfaces, this method can use high power objective to improve the enlargement factor and the resolution of imaging device.
Description of drawings
Fig. 1 is colloid matter crystal internal defect Real Time Observation of the present invention and imaging device;
Fig. 2 is a sample stage partial structurtes synoptic diagram of the present invention;
Fig. 3 is colloidal crystal monochromatic light diffraction spot figure;
Fig. 4 is the bright field image of dislocation;
Fig. 5 is the dark field image of dislocation.
Embodiment
As shown in Figure 1, the device of real time observing colloid matter crystal internal defect of the present invention comprises light source, illuminating bundle switching device shifter 1, sample 2 and sample stage 7, defective imaging device, central processing unit 10, and light source is a monochromatic source; Illuminating bundle switching device shifter 1 comprises the condenser lens 5 and the switch 6 of completely reflecting mirror 3, semi-transparent semi-reflecting lens 4, two long-focus, and switch 6 is a plate washer, is used for selecting to block incident light and passes through; The defective imaging device comprises microcobjective 8 and CCD (charge-coupled image sensor) 9; Sample 2 places on the sample stage 7, and can in perpendicular to the plane of optical axis, move, illuminating bundle switching device shifter 1 and defective imaging device are separately positioned on the front and back of sample 2, the distance that adjustment microcobjective 8 and sample are 2 makes it focus on sample 2 surfaces and images on the CCD (charge-coupled image sensor) 9, the image information that CCD (charge-coupled image sensor) 9 obtains is transferred to central processing unit 10 and carries out data processing, and this central processing unit 10 comprises a main frame and display.Monochromatic light shines semi-transparent semi-reflecting lens and produces the identical light of two beam intensities thus, wherein a branch of incident ray 12 is identical with the diffraction light direction of crystal, another bundle incident ray 11 overlaps with optical axis (being the Z axle), two-beam shines on the same point of sample 2, switch 6 shelters from light beam 11, the incident light identical with diffraction light direction irradiation sample 2 also sees through sample 2 and obtains light beam with optical axis coincidence, obtain the details in a play not acted out on stage, but told through dialogues diffraction contrast image by the defective imaging device that is provided with later at sample 2, shelter from light beam 12, incident light irradiation sample 2 with optical axis coincidence, see through sample 2 along incident direction, by obtaining the light field diffraction contrast image, realize observing the quick switching between bright field image and the dark field image at the defective imaging device that is provided with thereafter.Shown in Figure 4 and 5, be incident beam irradiation resulting bright field image of sample and dark field image, compare the dark field image of bright field image and different diffraction spot, can find the frosting phenomenon of dislocation image, can extrapolate the Burgers vector measure feature of dislocation thus.
As shown in Figure 2, sample stage 7 is coaxial with optical axis (Z axle), and can be with optical axis with perpendicular to the rotation of the axis of optical axis, and sample 2 moves in the XY face can do selected diffraction by scanning samples.Be illustrated in figure 3 as colloidal crystal laser diffraction spot, determine oblique incidence light beam direction in the illuminating bundle switching device shifter by the diffraction light direction that draws along optical axis direction vertical irradiation sample.
May through the angle of diffraction light behind the crystal diffraction and direct light slightly difference be arranged with light in order to adjust angle between light beam 11 and 12, in experiment, can finely tune sample stage 7 is rotated to satisfy the imaging requirements of dark field image around the X-axis vertical with optical axis synchronously with the defective imaging device, wherein, the relative position of microscope camera lens and sample remains unchanged, and is same point before light beam irradiates point and the rotation.
The method of a kind of real time observing colloid matter crystal internal defect of the present invention, concrete steps are:
1) use monochromatic light along optical axis direction vertical irradiation sample;
2) determine radiation direction behind the monochromatic light irradiation sample diffraction;
3) monochromatic light produces two bundle incident raies irradiation samples through the illuminating bundle switching device shifter, and the radiation direction of determining in wherein a branch of incident ray and the step 2 is identical, another bundle incident ray and optical axis coincidence, and two light beam irradiates arrive the same point of sample;
4) the two-beam line sees through sample respectively by the imaging of defective imaging device, and direct light irradiation imaging obtains bright field image, and oblique incident ray irradiation imaging obtains dark field image;
5) image information obtained of defective imaging device is transferred to central processing unit and carries out data processing.
When if the diffraction light direction that monochromatic light vertical irradiation sample obtains and the angle of optical axis have a plurality of value, can on the direction of each angle, arrange a monochromic beam, adopt multiple beam to shine on the same point of sample, wherein a monochromic beam and optical axis coincidence, other homogeneous beam is identical with the diffraction light direction.Step 3 also can directly adopt the identical monochromatic light of two bundle wavelength irradiation sample, and wherein definite radiation direction is identical in a monochromic beam and the step 2, another monochromic beam and optical axis coincidence.Adopt this mode to save the illuminating bundle switching device shifter.
The inventive method and device can Real Time Observation and are write down bright field image, the dark field image of colloid matter crystal internal defect, and can realize switching bright, dark field image quickly and easily, and need not carry out adjusting sample and imaging device loaded down with trivial detailsly, CCD (charge-coupled image sensor) is set to image pickup mode can Real Time Observation writes down bright, dark field image variation, by analyzing motion and the dynamic process thereof that to study dislocation, fault.
Claims (4)
1. the device of a real time observing colloid matter crystal internal defect, it is characterized in that, comprise: the monochromatic light light source, the illuminating bundle switching device shifter, sample stage, defective imaging device and central processing unit, the illuminating bundle switching device shifter, sample stage and defective imaging device front and back are successively arranged, described illuminating bundle switching device shifter comprises completely reflecting mirror, the semi-transparent reflection mirror, long-focus condenser lens and switch, described switch is one can block the device that light beam passes through, described illuminating bundle switching device shifter can be realized restrainting the switching of incident light to shining two on the sample, thereby realizes bright, the quick switching of dark field image;
Described sample stage and light shaft coaxle, and can be with optical axis with perpendicular to the rotation of the axis of optical axis, sample is placed on the sample stage and can moves on perpendicular to the plane of optical axis, realizes the selected diffraction of sample and selects different diffracted beam imagings;
In the two bundle incident lights, the incident light of sample and optical axis coincidence on the vertical irradiation sample stage, the angle of another bundle incident light and optical axis satisfies Bragg diffraction law;
The defective imaging device is made of microcobjective and CCD charge-coupled image sensor, microcobjective place sample the back and and the CCD charge-coupled image sensor be fixed on the same guide rail, guide rail can wind the axis rotation perpendicular to optical axis, guarantee through the light vertical irradiation behind the sample on microcobjective, it is triangular apart from imaging to regulate sample, microcobjective, CCD charge-coupled image sensor, and the image information that the CCD charge-coupled image sensor obtains is transferred to central processing unit and carries out data processing.
2. the method for a real time observing colloid matter crystal internal defect is characterized in that, concrete steps are:
1) use monochromatic light along optical axis direction vertical irradiation sample;
2) determine radiation direction behind the monochromatic light irradiation sample diffraction;
3) monochromatic light produces two bundle incident raies irradiation samples through the illuminating bundle switching device shifter, and two light beam irradiates are on the same point of sample, and wherein, the radiation direction of determining in a branch of incident ray and the step 2 is identical, and another restraints incident ray and optical axis coincidence;
4) two light beams see through sample respectively by the imaging of defective imaging device, and direct light irradiation imaging obtains bright field image, and oblique incident ray irradiation imaging obtains dark field image;
5) image information obtained of defective imaging device is transferred to central processing unit and carries out data processing.
3. the method for a kind of real time observing colloid matter crystal internal defect as claimed in claim 2, it is characterized in that, when the diffraction light direction that monochromatic light vertical irradiation sample obtains and the angle of optical axis have a plurality of value, on the direction of each angle, arrange a branch of incident monochromatic light, adopt multiple beam to shine on the same point of sample, wherein a monochromic beam and optical axis coincidence, other homogeneous beam is identical with the diffraction light direction.
4. the method for a kind of real time observing colloid matter crystal internal defect as claimed in claim 2, it is characterized in that, step 3 directly adopts two bundles to come from Different Light but the identical monochromatic light irradiation sample of wavelength, wherein the radiation direction of determining in a monochromic beam and the step 2 is identical, another monochromic beam and optical axis coincidence.
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| CN2008101165294A CN101308101B (en) | 2008-07-11 | 2008-07-11 | Device and method for real time observing colloid matter crystal internal defect |
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| CN102534782B (en) * | 2012-01-31 | 2015-06-24 | 常州亿晶光电科技有限公司 | Device for observing and sorting sapphire crystal bubbles |
| CN102914622A (en) * | 2012-10-19 | 2013-02-06 | 中国科学院物理研究所 | Colloidal crystal testing device |
| CN103645748A (en) * | 2013-12-18 | 2014-03-19 | 中国科学院空间科学与应用研究中心 | Transposition control device |
| CN107543830B (en) * | 2016-06-23 | 2022-02-22 | 中国科学院长春光学精密机械与物理研究所 | Detection device and detection method for surface defects of spherical optical element |
| CN106770329A (en) * | 2017-01-09 | 2017-05-31 | 中国工程物理研究院机械制造工艺研究所 | A kind of details in a play not acted out on stage, but told through dialogues microscopic imaging device for detecting transparent material surface and internal flaw |
| CN108489986B (en) * | 2018-03-19 | 2021-03-26 | 长沙理工大学 | Additive manufacturing online detection and repair method |
| CN108490598B (en) * | 2018-03-29 | 2024-03-19 | 中国工程物理研究院激光聚变研究中心 | Optical element body scattering defect detection device and detection method |
| CN110118782A (en) * | 2019-05-08 | 2019-08-13 | 中国科学院福建物质结构研究所 | A kind of Laser Tomographic scanner for seeing defect scattering for measuring crystals Jie |
| CN110579474A (en) * | 2019-09-24 | 2019-12-17 | 中国科学院力学研究所 | device for simultaneously observing crystal morphology and measuring concentration field around crystal |
| CN113506366B (en) * | 2021-08-06 | 2024-03-26 | 重庆大学 | Three-dimensional visualization method for dislocation characteristics |
| CN113834803B (en) * | 2021-09-22 | 2023-03-17 | 福州大学 | Multifunctional microscopic imaging optical system |
| CN114966086B (en) * | 2022-05-11 | 2023-04-07 | 上海交通大学 | Pulse laser driven particle flight speed measuring device and method |
| CN115060740B (en) * | 2022-07-08 | 2024-04-26 | 凌云光技术股份有限公司 | Surface defect detection device and method based on off-axis illumination structure |
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