CN112432898A - Method for distinguishing KDP crystal cone column growth area and measuring device - Google Patents
Method for distinguishing KDP crystal cone column growth area and measuring device Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
A method and a device for distinguishing a KDP crystal cone column growth area are disclosed, wherein the method comprises the following steps: measuring initial energy E of deep ultraviolet laser beam with certain wavelength1Or the optical power P1Placing KDP crystal on the deep ultraviolet laser path, and measuring the laser beam energy E after the KDP crystal is penetrated2Or the optical power P2Using the formula T ═ E2/E1100% or T ═ P2/P1The transmission T at the KDP-like crystal measurement point was calculated at 100%. Judging the growth area of the crystal cone column according to the transmittance T: the transmittance T is higher than 70%, and is a conical growth area of the KDP crystal; the transmittance T is lower than 50 percent and is a cylindrical growth area of KDP crystals;the transmittance T is (50%, 70%)]And the crystal is a cone-column boundary area of the KDP crystal. The method can simply and quickly judge the type of the conical column growth area for quickly growing the KDP crystal.
Description
Technical Field
The invention relates to a method for distinguishing a conical column growth area of a KDP crystal which grows rapidly and a measuring device, in particular to a method for distinguishing the conical column growth area of the KDP crystal by using the transmittance value of a KDP crystal element under a deep ultraviolet laser wave band.
Background
Potassium dihydrogen phosphate (KH)2PO4Abbreviated KDP) and Deuterides (KD)XH(2-X)PO4DKDP for short), ammonium dihydrogen phosphate (NH)4H2PO4ADP for short, and deuteride thereof (N (D)XH1-X)4(DYH1-Y)2PO4DADP for short) and the like are collectively referred to as KDP-based crystal materials. The tetragonal KDP crystal has the advantages of wide light transmission wave band, excellent laser damage resistance, high nonlinear conversion efficiency, capability of growing into a large-size single crystal, easiness in processing and the like, and is widely applied to the high-technology fields of laser frequency conversion, high-speed Q-switch and the like. In recent years, Inertial Confinement Fusion (ICF) engineering has attracted general attention from countries around the world, such as the "national ignition" in the united states. The KDP crystal with large size is the only nonlinear optical material which can be used for electro-optical switching and frequency conversion in ICF engineering so far, and along with the continuous improvement of laser energy transmission in ICF engineering, the improvement of crystal quality and laser damage resistance also becomes one of the research focuses.
The preparation methods of KDP crystals mainly comprise two methods, namely a traditional growth method and a point-seed crystal rapid growth method. Wherein, the growth of the traditional KDP crystal only grows slowly along the [001] direction at the speed of 0.5-1mm/d, the growth period is as long as 1-2 years, and a seed crystal recovery area with larger volume exists, the crystal quality of the area is poor and far lower than the engineering use requirement, so the growth method has long period, large risk, high cost and low crystal utilization rate. The point seed crystal rapid growth technology developed in recent years enables crystals to stably grow at the speed of 10-20mm/d along the directions of [100] and [001], the growth cycle of the crystals is greatly shortened, the cost is reduced, the recovery area of the crystals is small, and the utilization rate of the crystals is greatly improved. Therefore, the KDP crystal rapid growth method has great application prospect.
According to the BCF theory, the low-index growth surfaces of the KDP crystals obtained by the rapid growth method are respectively a (100) surface and a (101) surface, and the growth areas formed by the two are respectively a cylindrical surface growth area and a conical surface growth area. However, the exposed faces of KDP crystals (100) are always [ PO ]4]3-O in the group has electronegativity, so that the (100) surface is easy to adsorb cations and cationic groups such as Fe3+、Cr3+And the like, so that the cylindrical growth area of the crystal has obvious light absorption under the irradiation of the deep ultraviolet band laser, and the transmittance is obviously reduced; the KDP crystal (101) plane is double-layer K + and double-layer [ PO ]4]3-The group alternate arrangement structure is not easy to adsorb ions and ion groups, so that the influence on the deep ultraviolet transmittance is small. The difference of the deep ultraviolet transmittance of the conical surface growth region and the cylindrical surface growth region of the KDP crystal grown by the rapid growth method can provide a simple and rapid means for distinguishing the conical cylindrical surface growth region of the KDP crystal grown rapidly.
The existing patent technology has no research on how to distinguish the conical column growth area of the fast growing KDP crystal and the optical uniformity thereof, and therefore, a method and a device for establishing a system are urgently needed to realize judgment of the conical column growth area of the KDP crystal and measurement and identification of the optical uniformity thereof.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for judging the growth area of the KDP crystal cone column and a device for measuring the transmittance, and can realize the measurement and identification of the integral optical uniformity of the crystal.
The technical solution of the invention is as follows:
a method for distinguishing a KDP crystal cone column growth area is characterized in that deep ultraviolet laser transmittance measurement is carried out on a KDP crystal to be detected, and the cone column growth area is judged according to the transmittance T value: the transmittance T is higher than 70%, and is a conical growth area of the KDP crystal; the transmittance T is lower than 50 percent and is a cylindrical growth area of KDP crystals; the transmittance T is [ 50%, 70% ], and the crystal is a cone-column boundary region of KDP crystals.
The KDP crystal material comprises potassium dihydrogen phosphate and isotope compound deuterated potassium dihydrogen phosphate crystal thereof, ammonium dihydrogen phosphate and deuterated ammonium dihydrogen phosphate crystal.
The KDP crystal is obtained by growing through a rapid growth method, and the surface of the crystal is free of processing defects such as obvious scratches after being processed by cutting, polishing and the like.
Measuring the deep ultraviolet laser transmittance of the KDP crystal to be measured, and specifically comprising the following steps:
measuring initial energy E of deep ultraviolet laser beam1Or initial optical power P1；
Placing the KDP crystal to be tested in the emission direction of the deep ultraviolet laser beam, and vertically injecting the deep ultraviolet laser beam to the KDP crystal to be tested;
measuring the energy E of transmitted light beam penetrating through the KDP crystal to be measured2Or transmitted light power P2And calculating the transmittance T of the KDP crystals to be detected, wherein the formula is as follows:
T＝E2/E1100% or T ═ P2/P1*100％
Fourthly, according to the transmittance T, the crystal growth area of the KDP crystal at the measuring point can be judged;
moving the KDP crystal to be measured in a plane perpendicular to the deep ultraviolet laser beam to enable the measuring points to be paved on the surface of the KDP crystal to be measured, and judging the crystal growth areas of all measuring points of the KDP crystal to be measured;
drawing the transmittance T of all the measurement points according to a moving rule to obtain a transmittance surface distribution graph of the KDP crystal, and judging the optical uniformity of the KDP crystal: if all the measurement points are conical surface growth areas (or cylindrical surface growth areas), the KDP crystal is measured to have good optical uniformity; if the cone-column boundary growth region exists, the optical uniformity is poor.
The transmittance measuring device for implementing the method for distinguishing the KDP crystal conical column growth area comprises a laser source for generating a laser beam with a specific deep ultraviolet band, a moving platform for placing a KDP crystal to be detected, a spectroscope, a first light beam detector and a second light beam detector;
laser beams generated by the laser light source are divided into reflected light and transmitted light through the spectroscope, wherein the reflected light is directly incident on the first light beam detector, and the transmitted light is incident on the second light beam detector after being transmitted by the KDP crystal to be detected; the mobile platform, the first light beam detector and the second light beam detector are respectively connected with a computer, the two-dimensional movement of the mobile platform is controlled through the computer, and the reading of the light beam detectors in a certain time is read through corresponding software on the computer.
The laser light source can emit continuous or pulse laser, the laser energy fluctuation is as small as possible (such as less than or equal to 1 percent), and the laser wavelength is a certain specific wavelength within the range of 200nm-290 nm. The laser light source, the spectroscope, the mobile platform and the light beam detector are all arranged on a shock-absorbing optical platform in a darkroom.
Compared with the prior art, the invention has the beneficial effects that:
the method for measuring the transmittance of the crystal element in any deep ultraviolet laser band is adopted, so that the transmittance can be quickly and effectively utilized to judge the conical column growth area and the optical uniformity of the KDP crystal.
Drawings
Fig. 1 is a schematic structural diagram of a simple transmittance measuring device: 1-deep ultraviolet laser light source, 2-spectroscope, 3-mobile platform, 4-second beam detector, 5-first beam detector, 6-computer.
Fig. 2 is a KDP-based crystal transmittance plane distribution and cone growth area discrimination result measured by the measurement method according to the present invention.
Detailed Description
The present invention is further described in detail below with reference to examples and the accompanying drawings so that those skilled in the art can accurately implement the method of the present invention.
The transmittance measuring device adopted by the invention is shown in figure 1 and comprises a laser light source capable of generating laser light with a specific deep ultraviolet waveband, a spectroscope, a moving platform arranged on a laser beam passage, a first light beam detector, a second light beam detector and a computer, wherein the detection range of the first light beam detector and the second light beam detector covers the laser light with the deep ultraviolet waveband;
the laser light source, the spectroscope, the mobile platform, the first light beam detector and the second light beam detector are all arranged on the shock absorption optical platform in the darkroom, and stray light interference does not exist around the shock absorption optical platform; the spectroscope divides a laser beam emitted by the laser light source into reflected light and transmitted light, wherein the reflected light is directly incident on the first light beam detector, and the transmitted light is incident on the second light beam detector after being transmitted by the KDP crystal to be detected; the mobile platform and the light beam detector are both connected with a computer, the two-dimensional movement of the platform is controlled through the computer, and the reading of the light beam detector within a certain time is read through corresponding software on the computer.
The laser light source selected in the embodiment emits pulse laser with the wavelength of 248nm, the laser energy fluctuation is less than or equal to 1%, the detection energy precision of the light beam detector is 1 muJ, the beam splitter is a wedge-shaped piece with a wedge-shaped surface apex angle of 5 degrees, the moving precision of the two-dimensional moving platform X, Y to the direction is 100μm, the crystal is a rapidly-growing class II cutting DKDP crystal, the size of the crystal is 50mm multiplied by 10mm, and the crystal is processed by cutting, polishing and the like without obvious processing defects on the surface;
a method for distinguishing a conical column growth area of a fast-growing KDP crystal comprises the following steps:
firstly, 248nm pulse light emitted by a laser passes through a spectroscope, then transmitted light is vertically incident to a second light beam detector, and the average initial energy of the laser beam within 1min is read to be E by corresponding software in the computer1；
Secondly, a moving platform for clamping the DKDP crystal to be measured is arranged on a measuring light path, the transmitted light passing through the spectroscope vertically penetrates through the DKDP crystal arranged on the moving platform and then enters a second light beam detector, and the average energy of the laser beam is read to be E within 1min through corresponding software in the computer2；
Step three, according to the formula T ═ E2/E1100% ofCalculating the transmittance T of the DKDP crystal at the measuring point;
step four, respectively moving the crystal to be measured according to the X direction of 7mm or the Y direction of 5mm of the plane of the vertical incident light, repeating the steps from one step to three to measure the transmittance of the corresponding position of the crystal to obtain the transmittance data of 72 DKDP crystals, and drawing a DKDP crystal transmittance surface distribution diagram according to X, Y coordinates of corresponding moving measurement points, which is shown in figure 2;
and fifthly, judging the conical column growth area and the optical uniformity of the DKDP crystal according to the figure 2: the transmittance T is more than 70 percent and belongs to a conical surface growth area of the DKDP crystal; the transmittance T is less than 50% and belongs to a cylindrical growth area of the crystal; the intermediate transmittance in the interval of [ 50%, 70% ] of the crystal belongs to the cone-column boundary growth region of the crystal. The difference of numerical values of transmittance of the left area and the right area of the DKDP crystal is large, and a conical surface growth area, a conical column junction growth area and a cylindrical surface growth area exist respectively, so that the overall optical uniformity of the DKDP crystal is poor.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (8)
1. A method for distinguishing a KDP crystal cone column growth area is characterized in that deep ultraviolet laser transmittance measurement is carried out on a KDP crystal to be detected, and the cone column growth area is judged according to the transmittance T value: the transmittance T is higher than 70%, and is a conical growth area of the KDP crystal; the transmittance T is lower than 50 percent and is a cylindrical growth area of KDP crystals; the transmittance T is [ 50%, 70% ], and the crystal is a cone-column boundary region of KDP crystals.
2. The method for discriminating a conical column growth region of a KDP crystal according to claim 1, wherein the KDP crystal material includes potassium dihydrogen phosphate and an isotopic compound thereof, deuterated potassium dihydrogen phosphate crystals, ammonium dihydrogen phosphate crystals, and deuterated ammonium dihydrogen phosphate crystals.
3. The method for discriminating the conical column growth region of a KDP crystal according to claim 1, wherein the KDP crystal is grown by a rapid growth method, and the crystal is cut, polished and the like without processing defects such as obvious scratches on the surface.
4. The method for distinguishing the conical column growth area of the KDP crystal as claimed in claim 1, wherein the deep ultraviolet laser transmittance measurement is performed on the KDP crystal to be measured, and the specific steps are as follows:
measuring initial energy E of deep ultraviolet laser beam1Or initial optical power P1；
Placing the KDP crystal to be tested in the emission direction of the deep ultraviolet laser beam, and vertically injecting the deep ultraviolet laser beam to the KDP crystal to be tested;
measuring the energy E of transmitted light beam penetrating through the KDP crystal to be measured2Or transmitted light power P2And calculating the transmittance T of the KDP crystals to be detected, wherein the formula is as follows:
T＝E2/E1100% or T ═ P2/P1*100％
Fourthly, according to the transmittance T, the crystal growth area of the KDP crystal at the measuring point can be judged.
5. The method for distinguishing the conical column growth area of the KDP-based crystal according to claim 4, wherein the KDP-based crystal to be measured is moved in a plane perpendicular to the deep ultraviolet laser beam so that the measurement points are spread over the surface of the KDP-based crystal to be measured, and the crystal growth area at all the measurement points of the KDP-based crystal to be measured can be judged.
6. The transmittance measuring device for implementing the method for distinguishing the conical column growth area of the KDP crystal according to any one of claims 1 to 5, wherein the device comprises a laser source for generating a laser beam in a specific deep ultraviolet band, a moving platform for placing the KDP crystal to be detected, a spectroscope, a first light beam detector and a second light beam detector;
laser beams generated by the laser light source are divided into reflected light and transmitted light through the spectroscope, wherein the reflected light is directly incident on the first light beam detector, and the transmitted light is incident on the second light beam detector after being transmitted by the KDP crystal to be detected;
the mobile platform, the first light beam detector and the second light beam detector are respectively connected with a computer, the two-dimensional movement of the mobile platform is controlled through the computer, and the reading of the light beam detectors in a certain time is read through corresponding software on the computer.
7. The transmittance measuring apparatus according to claim 5, wherein the laser light source emits continuous or pulsed laser light, the laser light energy fluctuation is as small as possible (e.g., ≦ 1%), and the laser wavelength is a specific wavelength in the range of 200nm to 290 nm.
8. The transmittance measurement device according to claim 5, wherein the laser light source, the beam splitter, the movable stage and the beam detector are disposed on a shock-absorbing optical stage in a dark room.
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Cited By (1)
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| CN114635189A (en) * | 2022-03-23 | 2022-06-17 | 中国科学院福建物质结构研究所 | KDP crystal and preparation method thereof |
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