WO2021253589A1 - Procédé de traitement et de fabrication d'un élément de substrat monocristallin de niobate de tantalate de potassium - Google Patents

Procédé de traitement et de fabrication d'un élément de substrat monocristallin de niobate de tantalate de potassium Download PDF

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WO2021253589A1
WO2021253589A1 PCT/CN2020/106855 CN2020106855W WO2021253589A1 WO 2021253589 A1 WO2021253589 A1 WO 2021253589A1 CN 2020106855 W CN2020106855 W CN 2020106855W WO 2021253589 A1 WO2021253589 A1 WO 2021253589A1
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crystal
polishing
processing
ktn
orientation
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PCT/CN2020/106855
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Chinese (zh)
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王旭平
吴丰年
陈芙迪
邱程程
刘冰
张飞
杨程凯
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齐鲁工业大学
山东省科学院新材料研究所
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28DWORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/11Lapping tools
    • B24B37/20Lapping pads for working plane surfaces
    • B24B37/24Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28DWORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0005Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by breaking, e.g. dicing
    • B28D5/0011Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by breaking, e.g. dicing with preliminary treatment, e.g. weakening by scoring
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28DWORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0058Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28DWORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0058Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
    • B28D5/0082Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material for supporting, holding, feeding, conveying or discharging work
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28DWORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/02Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by rotary tools, e.g. drills
    • B28D5/022Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by rotary tools, e.g. drills by cutting with discs or wheels
    • B28D5/028Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by rotary tools, e.g. drills by cutting with discs or wheels with a ring blade having an inside cutting edge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28DWORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/04Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
    • B28D5/045Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools by cutting with wires or closed-loop blades
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01SDEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/10Controlling the intensity, frequency, phase, polarisation or direction of the emitted radiation, e.g. switching, gating, modulating or demodulating

Definitions

  • the invention relates to a processing and preparation method of artificial crystal material for electro-optical modulation, and belongs to the field of laser components.
  • Electro-optic crystal material is one of the basic materials of all solid-state lasers, which can realize the modulation of laser propagation characteristics. Electro-optic modulation has the advantages of high efficiency, good stability, fast response and no inertia. Electro-optic crystals are a kind of functional crystals with important applications. The invention of the development of high-efficiency electro-optic crystals is of great significance to the development and application of all-solid-state laser technology.
  • Potassium tantalum niobate (KTa 1-x Nb x O 3 , KTN) crystal is a solid solution mixed crystal of potassium tantalate (KTaO 3 , KT) and potassium niobate (KNbO 3 , KN), with excellent electro-optical properties And photorefractive performance, KTN crystal has a wide range of application prospects in beam deflectors, Q-switches, high-speed optical shutters, holographic storage, optical intensity modulators, optical phase modulators and other fields; at the same time, KTN is also an excellent film Materials, substrate materials have a wide range of applications.
  • KTN crystal is a typical hard and brittle material.
  • the KTN crystal with high niobium content also has mechanical properties such as cleavage and anisotropy.
  • KTN crystal is a typical secondary electro-optic crystal material. It is generally believed that the higher the order of nonlinear modulation, the smaller the nonlinear coefficient. Therefore, the focus of electro-optic modulation research has been limited to linear electro-optic materials and devices for a long time. Commonly used are lithium niobate (LN), lithium tantalate (LT), rubidium titanyl phosphate (RTP) and lanthanum gallium silicate (LGS), etc. The corresponding modulation components are for these linear electro-optic crystals. In addition, due to the infinite solid solution characteristics of KTN crystals, it is very difficult to grow high-quality large-size single crystals, which has greatly restricted its research and application.
  • LN lithium niobate
  • LT lithium tantalate
  • RTP rubidium titanyl phosphate
  • LGS lanthanum gallium silicate
  • KTN crystals Even show better performance than linear electro-optic crystals in terms of laser modulation. Whether it is compared with traditional acousto-optic, mechanical modulation, etc., or existing linear electro-optic modulation, electro-optic modulation based on KTN crystal Kerr effect is significantly better than the former in many aspects such as light transmission band, modulation efficiency and response time. Therefore, electro-optic modulation based on the secondary electro-optic effect of KTN crystal has advantages in reducing driving voltage and device size, and can better meet the needs of future laser wide-band, miniaturization, and integrated development.
  • KTN crystal electro-optic modulation devices are currently shifting from laboratory research to industrial applications.
  • the processing and preparation of their components is critical to the performance of crystal devices.
  • the existing processing and preparation technologies of laser modulation components are mostly aimed at linear electro-optic crystal materials.
  • the actual application of the electro-optic crystal material is closely related to the unique physical and chemical properties of the crystal. Therefore, the present invention develops a special KTN electro-optic modulation element processing and preparation technology according to the characteristics of the secondary electro-optic effect and the crystallographic characteristics of the KTN crystal. This technology can not only greatly advance
  • the application and promotion of KTN electro-optic modulator also has extensive reference significance for secondary electro-optic modulation technology.
  • the present invention aims to provide a method for processing and manufacturing substrate elements of KTN series crystal secondary electro-optic modulation devices with different composition ratios and different crystal phases.
  • High-efficiency KTN secondary electro-optic modulator provides component preparation solutions.
  • the technical scheme of the present invention is as follows: a method for processing and manufacturing a potassium tantalum niobate single crystal substrate element, the KTN crystal has a Nb composition of 0 ⁇ x ⁇ 1, and a crystal phase of cubic (m3m) and tetragonal (4mm) Or orthogonal (mm2), doping ions are Cu, Fe, Sn, Ti, Li, Na, Mn single-doped or mixed multi-doped KTa 1-x Nb x O 3 or M: KTa 1-x Nb x O 3 Crystal.
  • the method steps mainly include orientation, cutting, assembly, grinding, polishing and unloading of KTN crystals, which are specifically as follows:
  • Orientation According to the crystallization and growth characteristics of KTN crystals, its orientation includes single crystal crystal plane orientation and internal growth dissociation fringe orientation, through cutting and grinding trimming to achieve the crystal plane and geometric plane coincide within a certain error. Mark the direction relationship between the growth cleavage stripes and the geometric plane.
  • the diamond cutting tool Based on the orientation plane of the crystal, according to the application requirements of the diversified light direction of the KTN crystal, the diamond cutting tool is used to cut the wafer with the designed crystal orientation and size.
  • the cutting size error is less than 10 ⁇ m, and the crystal orientation error is less than 0.5°.
  • Composition Select glass or crystals similar in hardness and elastic modulus to the processed KTN crystal as the fixture material, design the fixture shape and size according to the geometric dimensions of the crystal processing surface, and make the fixture through cutting and shaping. According to the application requirements and the Curie temperature value of the wafer, choose paraffin or 502 adhesive to combine the crystal and the fixture into a processing block.
  • Polishing At a temperature of 22 ⁇ 2°C and a humidity of 30-70%, according to the mechanochemical properties of KTN crystals, use water-based polishing fluids and polishing pads with an abrasive particle size of less than 1 ⁇ m to perform fine grinding on the crystals.
  • the surface can achieve no damage after fine polishing, the surface profile is better than ⁇ /8, the root mean square roughness (RMS) is less than 1nm, and the parallelism of the upper and lower surfaces is within 5";
  • the abrasive may be: diamond or cerium oxide or silicon dioxide;
  • the polishing pad may be: a polyurethane polishing pad, a non-woven polishing pad, a flannel polishing pad, or an asphalt polishing pad.
  • Coating protective film and unloading plate After finishing polishing the processed surface in the ultra-clean workbench, use a dust-free cloth to clean it with acetone and alcohol, and then self-leveling or spin-coating a layer of shellac paint sheet alcohol solution as
  • the concentration of the shellac paint flakes is 5wt%-20wt%, placed for 30 minutes, air-dried, and then heated to 60-70°C with a baking lamp to melt the paraffin wax unloading fixture.
  • For the processing block using 502 adhesive soak it in acetone solution for 5-12 hours after cleaning, and remove the jig after the 502 adhesive is dissolved.
  • step (1) of the method of the present invention the crystal plane orientation is completed by using an X-ray directional instrument, and the error is less than or equal to 5'.
  • the orientation of the internal growth cleavage fringe is observed with a magnifying glass or microscope on the light-transmitting surface.
  • the KTN growth fringe is a parallel linear fringe, generally in the same direction, and its direction is affected by the direction of the crystal crystal plane, but there is no fixed angle relationship between the two. Therefore, according to the growth characteristics and application purposes of KTN single crystals of different compositions, only the crystal plane orientation and cleavage fringe orientation of the single crystal blanks can fully avoid and utilize the unique properties of growing cleavage fringes and realize the diversified applications of KTN crystals.
  • the cutting tool can be: a diamond inner circle or a scribing or wire cutting machine.
  • the linear speed of the blade or the cutting line is selected as 1000-1500cm/s, cutting feed speed is 4-8mm/min.
  • the linear speed of the blade or cutting line is preferably 1500cm/s, and the feed speed is 5mm/min, depending on the composition or doping.
  • the ions cause the hardness of the crystal to change, and the cutting parameters can be adjusted appropriately.
  • step (3) of the method of the present invention according to the Mohs hardness of the KTN crystal material, the Mohs hardness is 6-7, and when the crystal face processing surface requirement is lower than ⁇ /12, considering the processing and manufacturing cost, K9 glass is preferred as the fixture material.
  • KTN crystal material is preferred as the fixture material, and KTN crystal of the same composition as the processed sample is more preferred as the fixture material.
  • the shape of the processing surface of the processing block is similar to the shape of the processing surface of the wafer, and when it is inconsistent, a square shape is preferred.
  • the selection of the binder is based on the Curie temperature point of the processed KTN crystal and the required surface precision requirements, because the Curie temperature of the KTN crystal can vary from tens of degrees below zero to hundreds of degrees above zero with the change of the ratio of tantalum and niobium. KTN crystals will undergo vertical and four-directional transformations at the Curie temperature. Affected by various unavoidable microstructure defects inside the crystal, the phase change will inevitably affect the surface accuracy of the crystal processing surface. Therefore, in the present invention, when the demand for surface processing is lower than ⁇ /12, the convenient and time-saving yellow glue is used as the adhesive, and when the demand for surface processing is above ⁇ /12, 502 is used as the adhesive.
  • Steps (4) and (5) of the method of the present invention can be implemented manually or by machine. Since the composition and performance of the KTN series crystals can be adjusted, the diversity of their performance and uses can be realized. In view of the variety of uses, processing shapes and sizes of KTN crystals, the steps of the processing method of the present invention can select a manual operation method that is easy to design flexibly according to processing requirements, or a machine processing method that is consistent in size and efficient processing can be selected.
  • step (4) of the method of the present invention according to the grinding mechanism of the KTN crystal material and different grinding materials, it is preferable to perform rapid shaping and rough grinding with emery.
  • the alumina abrasive is finely ground and finely ground to reduce the damage and scratches left by the abrasive on the crystal processing surface, which is beneficial to the subsequent rapid and high-quality polishing.
  • step (5) of the method of the present invention according to the hardness of the KTN crystal, a polyurethane polishing pad is preferred for rough polishing, and an asphalt polishing pad is preferred for fine polishing, so that the polishing effect can be achieved quickly and with high quality.
  • a self-prepared, highly dispersed acidic water-based W0.8 cerium oxide polishing solution is preferably used for rough polishing.
  • the composition includes: 0.5wt%-5wt% W0.8 cerium oxide powder, 55wt%-70wt % Deionized water, 0.2wt%-15wt% KMnO4, 3wt%-10wt% ethylene glycol, 0.1wt%-1wt% potassium nitrate, 0-1wt% nitric acid, 0-1wt% potassium hydroxide, 0.1wt%-2wt % Polyacrylic acid (PAA).
  • PAA Polyacrylic acid
  • the above-mentioned W0.8 cerium oxide polishing liquid and colloidal silica (average particle size of 80nm, concentration of 25wt%) suspension mixture is preferred, the volume ratio of the two is preferably 1:1), the above-mentioned polishing liquid has a pH value It is 5-10, preferably 5-7.
  • the self-prepared and highly dispersed acidic water-based W0.8 cerium oxide polishing liquid is formulated for the hardness, plasticity, and chemical stability of KTN series crystals. It has good dispersibility and can quickly realize the chemistry of KTN series crystals. Mechanical polishing, and the polishing quality is better.
  • the present invention uses the W0.8 cerium oxide polishing solution and colloidal silica (average particle size of 80nm, concentration of 25wt%) suspension mixture, which can reasonably adjust the processing crystal surface and
  • the friction form before the polishing disc is beneficial to realize the synergistic polishing effect of small particles of hard silica and relatively large particles of W0.8 cerium oxide, which can improve the polishing removal rate and surface polishing quality of KTN crystals.
  • the processed KTN wafers of the present invention are (100), (110), (111) crystal orientation wafers with a crystal orientation error within ⁇ 5′, and the shape can be a cylinder, a rectangular parallelepiped, a three-sided column, a hexagonal column, and irregular shape.
  • the preparation method of the KTN single crystal substrate element of the present invention has the following advantages: According to the characteristics of the KTN series crystal crystal phase closely related to the crystal composition and the ambient temperature, according to the crystallography of the KTN crystal doped with different components and different ions at room temperature Features for precise orientation processing; using the corresponding orientation, cutting, grinding, polishing process and corresponding fixture materials, abrasives, and polishing fluids to ensure accurate crystal orientation and smooth surface of KTN substrate components to achieve laser modulation devices Production requirements, high processing efficiency, and low cost; the KTN single crystal substrate element produced by the present invention can not only meet the production needs of traditional linear electro-optic modulation devices, but also provide reference and reference for the design and production of secondary electro-optic modulation devices.
  • FIG. 1 is a schematic diagram of processing KTN single crystal substrates with different crystal orientations and different shapes according to Embodiment 1 of the present invention
  • FIG. 2 is a schematic diagram of processing KTN single crystal substrates with different crystal orientations and different shapes according to Embodiment 2 of the present invention
  • FIG. 3 is a schematic diagram of processing KTN single crystal substrates with different crystal orientations and different shapes according to the third embodiment of the present invention.
  • FIG. 4 is a schematic diagram of processing KTN single crystal substrates with different crystal orientations and different shapes according to Embodiment 4 of the present invention.
  • Embodiment 1 A high-precision cubic KTN single crystal substrate component processing, the KTN crystal composition is KTa 0.5 Nb 0.5 O 3 , the crystal phase is cubic (m3m). Carry out (100), (010), (001) three-sided directional precision polishing processing on it, the processing target size is 5mm ⁇ 5mm ⁇ 5mm cube, the processing steps are as follows:
  • Orientation use Dandong New Oriental DX-2 X-ray orientation instrument to complete the orientation of the KTN crystal embryo, use a magnifying glass and an optical microscope to determine the crystal growth cleavage fringes, and trim the two physical surfaces of the blank into (100) crystal surfaces.
  • the two oriented physical planes are respectively parallel and perpendicular to the crystal cleavage stripes, and the orientation error of the crystal plane is ⁇ 5'.
  • step (1) uses a diamond inner circle cutting machine to cut a cube crystal sample with a length, width and height of 5.5mm ⁇ 5.5mm ⁇ 5.5mm, and the cutting size error is less than 10 ⁇ m ,
  • the crystal orientation of the cutting surface is (100), (010), (001), and the crystal orientation error is less than 0.5°.
  • the grinding process in step (4) and the polishing process in step (5) in Example 1 are both manual operations, which can quickly and accurately achieve the processing goal.
  • Embodiment 2 A high-precision tetragonal Cu ion-doped KTN single crystal substrate component processing, the KTN crystal composition is Cu:KTa 0.5 Nb 0.5 O 3 , and the crystal phase is tetragonal (4 mm).
  • step (2) cuts out a length, width and height of 5.5
  • the four sides perpendicular to the (100) plane were ground into a cylindrical surface with a spheronization grinder to obtain a cylindrical crystal block with a size of 5mm in diameter ⁇ 5.5mm in height.
  • a square fixture with the same material and size as in Example 1 was used for processing operations, and finally a cylindrical Cu:KTa 0.5 Nb 0.5 O 3 wafer component as shown in FIG. 2 was obtained.
  • the upper and lower round surfaces are (100) precision polished surfaces, the surface is not damaged, the crystal orientation error is less than 5', the root mean square roughness RMS is less than 1nm, and the parallelism of the upper and lower surfaces is less than 5".
  • Example 3 Processing of a high-precision cubic KTN single crystal substrate component, the KTN crystal composition is KTa 0.5 Nb 0.5 O 3 , and the crystal phase is cubic (m3m).
  • the processing steps are as follows:
  • Orientation use Dandong New Oriental DX-2 X-ray orientation instrument to complete the orientation of the KTN crystal embryo, use a magnifying glass and an optical microscope to determine the crystal growth cleavage fringes, and trim the two physical surfaces of the blank into (100) crystal surfaces.
  • the two oriented physical planes are parallel and perpendicular to the crystal cleavage fringes, respectively, and the orientation error of the crystal plane is less than or equal to 5'.
  • step (2) Using the two orientation planes in step (1) as a reference, use a diamond inner circle cutting machine to cut a crystal sample with a length, width and height of 5.5mm ⁇ 5.5mm ⁇ 5.5mm, and the cutting size error is less than 10 ⁇ m.
  • the crystal orientation of the cutting surface is (100), (010), (001), and the crystal orientation error is less than 0.5°.
  • the (110) surface is cut along the diagonal direction of the (100) surface, and the error of the (110) surface is ground and trimmed to within 10' to obtain two directional trimmed three-sided prism specimens.
  • the thickness of each surface is about 10 ⁇ m, which basically removes blisters and deep scratches on the machined surface.
  • the parallelism of the upper and lower surfaces is 20" (there is no such indicator for the (110) surface, only the thickness uniformity of the sample is monitored).
  • the mixture of W0.8 cerium oxide polishing liquid and colloidal silica suspension was used as the polishing liquid, and pitch was used as the material of the polishing disc to finish polishing the squares.
  • the thickness of each surface was less than 10 ⁇ m.
  • the UNIPOL-802 double-station automatic grinding and polishing machine of Kejing is used for machine grinding and polishing, and the special mold components are used to efficiently achieve the processing goal.
  • Example 4 Processing of a high-precision cubic KTN single crystal substrate element, the KTN crystal composition is KTa 0.5 Nb 0.5 O 3 , and the crystal phase is cubic (m3m). It is processed by (100) crystal plane orientation precision polishing, and the target shape is a hexagonal prism sample with a width of 5mm ⁇ a height of 5mm.
  • the processing steps are different from those described in Example 1 in that step (2) first uses an inner circle cutting machine Cut out a crystal sample with a length, width and height of 4.85mm ⁇ 5.5mm ⁇ 5.5mm, of which the (100) orientation surface is a 4.85mm ⁇ 5.5mm surface, and then use a dicing cutter to cut the square perpendicular to the (100) orientation surface.
  • the hexagonal prism crystal block has a (100) orientation surface.
  • a square fixture with the same material and size as in Example 1 was used for processing operations, and finally a hexagonal columnar KTa 0.5 Nb 0.5 O 3 wafer element as shown in FIG. 4 was obtained.
  • the six aspects are (100) fine polishing surface, the surface is not damaged, the crystal orientation error is less than 5', the root mean square roughness RMS is less than 1nm, and the parallelism of the upper and lower surfaces is less than 5".

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Plasma & Fusion (AREA)
  • Optics & Photonics (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L'invention concerne un procédé de traitement et de fabrication permettant de personnaliser un élément de substrat monocristallin de niobate de tantalate de potassium de haute précision (KTa1-xNbxO3, où 0<x<1, dont l'abréviation est KTN). La présente invention concerne le domaine du traitement et de la préparation de cristaux artificiels et de matériaux de verre. Le procédé comprend principalement la réalisation d'une orientation, d'une coupe, d'une formulation, d'un meulage, d'un polissage et d'un déchargement sur des cristaux de série KTN. Le procédé fournit une solution complète pour la fabrication d'un élément de substrat monocristallin de KTN, et peut fournir une fondation d'échantillon pour le cristal KTN à utiliser en tant qu'éléments de modulation électro-optiques tels qu'un guide d'ondes optique, un commutateur optique et un déflecteur, ainsi qu'un matériau de substrat.
PCT/CN2020/106855 2020-06-19 2020-08-04 Procédé de traitement et de fabrication d'un élément de substrat monocristallin de niobate de tantalate de potassium WO2021253589A1 (fr)

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