CN110579474A - device for simultaneously observing crystal morphology and measuring concentration field around crystal - Google Patents

device for simultaneously observing crystal morphology and measuring concentration field around crystal Download PDF

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Publication number
CN110579474A
CN110579474A CN201910904388.0A CN201910904388A CN110579474A CN 110579474 A CN110579474 A CN 110579474A CN 201910904388 A CN201910904388 A CN 201910904388A CN 110579474 A CN110579474 A CN 110579474A
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China
Prior art keywords
lens
light source
crystal
beam splitter
splitter prism
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CN201910904388.0A
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Chinese (zh)
Inventor
戴国亮
史建平
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Institute of Mechanics of CAS
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Institute of Mechanics of CAS
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Priority to CN201910904388.0A priority Critical patent/CN110579474A/en
Publication of CN110579474A publication Critical patent/CN110579474A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N2021/0106General arrangement of respective parts
    • G01N2021/0112Apparatus in one mechanical, optical or electronic block
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • G01N2021/8477Investigating crystals, e.g. liquid crystals

Abstract

The embodiment of the invention relates to a device for simultaneously observing the appearance of a crystal and measuring a concentration field around the crystal, which comprises: the system comprises a first light source, an auxiliary condenser, a second light source, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism, an ocular lens and a CCD (charge coupled device); the system comprises a first light source, an auxiliary condenser, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism and a CCD (charge coupled device), wherein the first light source, the auxiliary condenser, the reflector, the field diaphragm, the first lens, the sample crystal, the second lens, the phase plate, the knife edge, the third lens, the beam splitter prism and the CCD are sequentially; the second light source is arranged above or below the reflector, and the ocular lens is arranged obliquely above or below the beam splitter prism; the field diaphragm, the phase plate and the beam splitter prism are fixed in the same module, and the knife edge and the third lens are fixed in the same module.

Description

device for simultaneously observing crystal morphology and measuring concentration field around crystal
Technical Field
The embodiment of the invention relates to the technical field of crystal growth, in particular to a device for simultaneously observing the crystal morphology and measuring the concentration field around the crystal.
Background
The growth process of the crystal is a continuous material transportation and solute and impurity molecule combination process on the crystal surface. On a submicroscopic level, the crystal growth process is a layer-by-layer growth process of steps on a crystal face in the horizontal direction. To clarify the mechanism of crystal growth and obtain high quality crystals, the growth process of the steps on the crystal plane must be clearly known. In order to realize the aim, in-situ online observation needs to be realized, the micro-morphology of the crystal including the step morphology is obtained, and the change of the micro-morphology along with the growth time of the crystal is obtained. In addition, the change of the microscopic appearance of the crystal (such as the step growth mode and the growth rate) is related to the concentration distribution of the solution around the crystal. Therefore, if the shape and the micro-morphology of the crystal can be observed, the observation and the diagnosis of the crystal morphology and the material transportation process in the crystal growth process can be realized by taking the measurement of the boundary layer concentration distribution and the change data of the crystal as an auxiliary measure, an important basis is laid for the basic research work of the growth dynamics, the impurity influence, the crystal quality and the like of the crystal, and the important guiding significance is provided for the optimization of the crystal growth process.
In the morphological observation of crystals, the most commonly used technique is optical microscopy. In the observation of the microscopic morphology of the crystal, the step height on the crystal face is only a few nanometers, and the step morphology on the crystal face can be observed only by a laser confocal-differential interference microscopic imaging method, a phase contrast microscopic imaging method and the like in an optical microscopic imaging method.
The concentration field distribution measurement around the crystal is mostly carried out by optical methods, such as the commonly used interferometry. Compared with the interference method, the brightness of the schlieren image obtained by the schlieren method is proportional to the gradient of the concentration field, so that the gradient of the concentration field around the crystal can be directly given, and the result is quantitative and accurate.
The kinetics of crystal growth in solution involves factors such as morphology and surrounding concentration distribution. It is therefore desirable to measure the concentration profile around the crystal in a very short time (negligible changes in crystal morphology and concentration profile around the crystal over a few seconds) while observing the crystal morphology.
Disclosure of Invention
In view of this, to solve the problems in the prior art, embodiments of the present invention provide an apparatus for simultaneously observing the crystal morphology and measuring the concentration field around the crystal.
The embodiment of the invention provides a device for simultaneously observing the appearance of a crystal and measuring a concentration field around the crystal, which comprises:
The system comprises a first light source, an auxiliary condenser, a second light source, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism, an ocular lens and a CCD (charge coupled device);
The system comprises a first light source, an auxiliary condenser, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism and a CCD (charge coupled device), wherein the first light source, the auxiliary condenser, the reflector, the field diaphragm, the first lens, the sample crystal, the second lens, the phase plate, the knife edge, the third lens, the beam splitter prism and the CCD are sequentially;
The second light source is arranged above or below the reflector, and the ocular lens is arranged obliquely above or below the beam splitter prism;
the field diaphragm, the phase plate and the beam splitter prism are fixed in the same module, and the knife edge and the third lens are fixed in the same module.
In one possible embodiment, the first light source comprises a laser light source.
in one possible embodiment, the second light source comprises an LED light source.
In one possible embodiment, the mirror comprises a double layer aluminum film planar mirror.
In one possible embodiment, the double-layer aluminum film plane mirror is designed to be flip-type.
In a possible embodiment, will double-deck aluminium membrane plane mirror upset to water flat line, just under the device switches over to the condition of field of view diaphragm, looks board, beam splitter prism place module, the laser warp that laser source sent supplementary condensing lens formation of image in first lens on the field of view diaphragm, pierce through the laser warp of field of view diaphragm first lens forms the parallel laser of slope to shine the sample crystal, pierce through the laser of sample crystal assembles through the second lens to the looks board, pierces through the laser warp of looks board beam splitter prism forms two way laser, wherein a way laser directly passes through beam splitter prism formation of image in CCD, another way laser is by pass through after beam splitter prism beam splitting face and the bottom surface reflection eyepiece for the user observes.
In a possible implementation manner, under the condition that the double-layer aluminum film plane reflector is turned over to form a certain included angle with a horizontal line, and the device is switched to a module where the knife edge and the third lens are located, light emitted by the LED light source is imaged on the first lens through the double-layer aluminum film plane reflector, parallel light is formed through the first lens and irradiates the sample crystal, the light penetrating through the sample crystal is focused on the knife edge through the second lens, the light penetrating through the knife edge is imaged on the third lens, and the light penetrating through the third lens is imaged on the CCD.
In one possible embodiment, the LED light source power is 10W.
In one possible embodiment, the first lens has a diameter of 100mm and a focal length of 500 mm.
In one possible embodiment, the second lens has a diameter of 50.8mm and a focal length of 500 mm.
The device for simultaneously observing the crystal morphology and measuring the concentration field around the crystal integrates the schlieren method and the phase contrast microscopy method, and can realize simultaneous observation of the crystal morphology and measurement of the concentration field around the crystal.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the embodiments of the present invention, and it is also possible for a person skilled in the art to obtain other drawings based on the drawings.
Fig. 1 is a schematic structural diagram of an apparatus for simultaneously observing a crystal morphology and measuring a concentration field around a crystal according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
For the convenience of understanding of the embodiments of the present invention, the following description will be further explained with reference to specific embodiments, which are not to be construed as limiting the embodiments of the present invention.
The embodiment of the invention is based on a schlieren method and a phase contrast microscopy method, integrates the schlieren method and the phase contrast microscopy method, provides a set of devices capable of simultaneously observing the appearance of the crystal and measuring the concentration field around the crystal, and simultaneously optimizes the schlieren method.
Based on the above, as shown in fig. 1, a schematic structural diagram of an apparatus for simultaneously observing a crystal morphology and measuring a concentration field around a crystal provided in an embodiment of the present invention is shown, and the apparatus specifically includes:
The system comprises a first light source, an auxiliary condenser, a second light source, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism, an ocular lens and a CCD (charge coupled device);
the system comprises a first light source, an auxiliary condenser, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism and a CCD (charge coupled device), wherein the first light source, the auxiliary condenser, the reflector, the field diaphragm, the first lens, the sample crystal, the second lens, the phase plate, the knife edge, the third lens, the beam splitter prism and the CCD are sequentially;
the second light source is arranged above or below the reflector, and the ocular lens is arranged obliquely above or below the beam splitter prism;
The field diaphragm, the phase plate and the beam splitter prism are fixed in the same module, and the knife edge and the third lens are fixed in the same module.
In a specific embodiment, the first light source in the embodiments of the present invention includes a laser light source.
in a specific embodiment, the second light source in the embodiment of the present invention includes an LED light source.
In one embodiment, the mirror in the embodiments of the present invention comprises a double-layered aluminum film plane mirror. The double-layer aluminum film plane reflector is designed to be turnover, and switching of two light sources of a phase contrast microscopy method and a schlieren method is achieved through turnover.
Wherein in phasein the observation process of the lining microscopic method, the double-layer aluminum film plane reflector M is turned to a horizontal line, the device is switched to a module where a view field diaphragm, a phase plate and a light splitting prism are positioned, and a laser light source SphAs a light source for phase contrast microscopy, laser light emitted from the light source is passed through an auxiliary condenser lens LphField stop D for imaging on first lens L11Upper, the field diaphragm D1A ring-shaped hole, the laser penetrating the ring-shaped hole passes through a first lens L1Forming a tilted parallel laser, irradiating the sample crystal I, and passing the laser through the sample crystal I via a second lens L2Phase plate D converging on focal plane thereof2Upper, phase plate D2The annular part is coated with a film with a certain thickness, the light transmitted through the annular part is direct light, namely zero-order frequency spectrum, the amplitude is attenuated and pi/2 phase shift is generated, and the diffracted light passing through the other directions of the sample crystal I, namely other high-order frequency spectrum, is transmitted from a phase plate D2The non-coated part on the film is penetrated, which means that the film penetrates the phase plate D2The laser of (2) has two parts, and these two parts laser form two way laser through beam splitter prism P, wherein one way laser directly passes beam splitter prism P image form in CCD, another way laser is by beam splitter prism beam splitting face and bottom surface reflect back pass through the eyepiece, supply the user to observe.
in addition, in the process of observation by the schlieren method, the double-layer aluminum film plane reflector M is turned over to form a certain included angle with the horizontal line, as shown in figure 1, the device is switched to a module where the knife edge and the third lens are located, and the LED light source SslAs a light source for schlieren observation, light emitted by the light source is imaged on the first lens L through the double-layer aluminum film plane reflector M1The light passes through the first lens L1Forming parallel light, irradiating the sample crystal I, and passing through the sample crystal I via the second lens L2Focusing on the knife edge, and imaging the light penetrating the knife edge on the third lens L3And the light penetrating through the third lens is imaged on the CCD. Wherein here the third lens L3The function of (a) is to converge schlieren images for CCD acquisition.
In the embodiment of the invention, the schlieren method is optimized, and the parameters after the schlieren method is optimized are as follows: the power of the LED light source is 10W; the diameter of the first lens is 100mm, and the focal length of the first lens is 500 mm; the diameter of the second lens is 50.8mm, and the focal length is 500 mm.
In the device provided by the embodiment of the invention, the double-layer aluminum film plane reflector is designed to be turnover, and the switching between the phase contrast microscopy method and the schlieren method can be realized through turnover.
In addition, in the device provided by the embodiment of the invention, the field diaphragm D1Photo plate D2And a beam splitter prism P fixed on a module, a knife edge and a third lens L3Is fixed on the other module. The switching between the phase contrast microscopy and the schlieren method is realized by switching the double-layer aluminum film plane reflecting mirror M and the two modules, so that the multifunction is realized in the integrated device.
Those of skill would further appreciate that the various illustrative components and algorithm steps described in connection with the embodiments disclosed herein may be implemented as electronic hardware, computer software, or combinations of both, and that the various illustrative components and steps have been described above generally in terms of their functionality in order to clearly illustrate this interchangeability of hardware and software. Whether such functionality is implemented as hardware or software depends upon the particular application and design constraints imposed on the implementation. Skilled artisans may implement the described functionality in varying ways for each particular application, but such implementation decisions should not be interpreted as causing a departure from the scope of the present invention.
The steps of a method or algorithm described in connection with the embodiments disclosed herein may be embodied in hardware, a software module executed by a processor, or a combination of the two. A software module may reside in Random Access Memory (RAM), memory, Read Only Memory (ROM), electrically programmable ROM, electrically erasable programmable ROM, registers, hard disk, a removable disk, a CD-ROM, or any other form of storage medium known in the art.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. An apparatus for simultaneously observing the morphology of a crystal and measuring the concentration field around the crystal, the apparatus comprising:
The system comprises a first light source, an auxiliary condenser, a second light source, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism, an ocular lens and a CCD (charge coupled device);
The system comprises a first light source, an auxiliary condenser, a reflector, a field diaphragm, a first lens, a sample crystal, a second lens, a phase plate, a knife edge, a third lens, a beam splitter prism and a CCD (charge coupled device), wherein the first light source, the auxiliary condenser, the reflector, the field diaphragm, the first lens, the sample crystal, the second lens, the phase plate, the knife edge, the third lens, the beam splitter prism and the CCD are sequentially;
The second light source is arranged above or below the reflector, and the ocular lens is arranged obliquely above or below the beam splitter prism;
The field diaphragm, the phase plate and the beam splitter prism are fixed in the same module, and the knife edge and the third lens are fixed in the same module.
2. The apparatus of claim 1, wherein the first light source comprises a laser light source.
3. The apparatus of claim 1, wherein the second light source comprises an LED light source.
4. The apparatus of claim 1, wherein the mirror comprises a double layer aluminum film planar mirror.
5. The apparatus of claim 4, wherein the double-layer aluminum film plane mirror is designed to be flip-chip.
6. the device of claim 5, wherein when the double-layered aluminum film plane mirror is turned to a horizontal line and the device is switched to a module with a field stop, a phase plate and a beam splitter prism, laser emitted from the laser source is imaged on the field stop of the first lens through the auxiliary condenser, the laser penetrating through the field stop forms oblique parallel laser through the first lens and irradiates the sample crystal, the laser penetrating through the sample crystal is converged on the phase plate through the second lens, and the laser penetrating through the phase plate forms two paths of laser through the beam splitter prism, wherein one path of laser directly passes through the beam splitter prism to be imaged on the CCD, and the other path of laser is reflected by the beam splitting surface and the bottom surface of the beam splitter prism and then passes through the eyepiece for observation by a user.
7. the device of claim 5, wherein when the double-layer aluminum film plane mirror is turned over to form an included angle with a horizontal line and the device is switched to a module with a knife edge and a third lens, light emitted by an LED light source is imaged on the first lens through the double-layer aluminum film plane mirror, parallel light is formed through the first lens and irradiates a sample crystal, light penetrating through the sample crystal is focused on the knife edge through the second lens, light penetrating through the knife edge is imaged on the third lens, and light penetrating through the third lens is imaged on the CCD.
8. The apparatus of claim 7, wherein the LED light source power is 10W.
9. the apparatus of claim 7, wherein the first lens has a diameter of 100mm and a focal length of 500 mm.
10. The apparatus of claim 9, wherein the second lens is 50.8mm in diameter and 500mm in focal length.
CN201910904388.0A 2019-09-24 2019-09-24 device for simultaneously observing crystal morphology and measuring concentration field around crystal Pending CN110579474A (en)

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CN111208089A (en) * 2020-01-13 2020-05-29 中国科学院上海光学精密机械研究所 Device and method for measuring defects in long-distance rough end face crystal body

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