WO2021253589A1 - Method for processing and manufacturing potassium tantalate niobate single crystal substrate element - Google Patents

Method for processing and manufacturing potassium tantalate niobate single crystal substrate element 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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French (fr)
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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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/11—Lapping tools
    • B24B37/20—Lapping pads for working plane surfaces
    • B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0005—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by breaking, e.g. dicing
    • B28D5/0011—Fine 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0058—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/0058—Accessories specially adapted for use with machines for fine working of gems, jewels, crystals, e.g. of semiconductor material
    • B28D5/0082—Accessories 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/02—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by rotary tools, e.g. drills
    • B28D5/022—Fine 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
    • B28D5/028—Fine 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28D—WORKING STONE OR STONE-LIKE MATERIALS
    • B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
    • B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
    • B28D5/045—Fine 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES 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
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/10—Controlling 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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  • Physics & Mathematics (AREA)
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Abstract

A processing and manufacturing method capable of customizing a high-precision potassium tantalate niobate (KTa1-xNbxO3, where 0<x<1, which is abbreviated to KTN) single crystal substrate element. The present invention belongs to the field of the processing and preparation of artificial crystals and glass materials. The method mainly comprises carrying out orientation, cutting, formulation, grinding, polishing and unloading on KTN-series crystals. The method provides a complete solution for the fabrication of a KTN single crystal substrate element, and can provide a sample foundation for the KTN crystal to be used as electro-optical modulation elements such as an optical waveguide, an optical switch and a deflector, and a substrate material.

Description

一种钽铌酸钾单晶基片元件的加工制作方法Method for processing and manufacturing potassium tantalum niobate single crystal substrate element 技术领域Technical field
本发明涉及一种电光调制用人工晶体材料的加工制备方法，属于激光元器件领域。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.
背景技术Background technique
电光晶体材料是全固态激光的基础材料之一，可实现激光传播特性的调制，电光调制具有效率高、稳定性好、响应快及无惯性等优势。电光晶体是一类具有重要应用的功能晶体，发明高效电光晶体的发展，对于全固态激光技术的发展和应用具有重要意义。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.
钽铌酸钾(KTa 1-xNb xO 3,KTN)晶体是钽酸钾(KTaO 3,KT)和铌酸钾(KNbO 3,KN)两种晶体的固溶体混晶，具有优异的电光性能和光折变性能，KTN晶体在光束偏转器、Q开关、高速光快门、全息存储、光强度调制器、光位相调制器等领域都有着广泛的应用前景；同时，KTN还作为一种优秀的薄膜材料，衬底材料有着广泛的应用。 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.
激光调制用光开关、光快门、偏转器等器件对调制核心元件的晶向偏差、晶格完整性、表面平整度等要求极高。为了获得高质量激光调制元件，要求KTN晶片无晶向偏差、表面晶格完整且表面平滑无损伤。即使极小的角度偏差或晶面缺陷，都将破坏激光的调制效率和性能，甚至导致结晶构造的变化，影响元件的调制精度和稳定性。KTN晶体属典型的硬脆材料，高铌含量的KTN晶体还有解理性和各向异性等机械力学性能。Devices such as optical switches, optical shutters, and deflectors for laser modulation have extremely high requirements on the crystal orientation deviation, crystal lattice integrity, and surface flatness of the modulation core components. In order to obtain a high-quality laser modulation element, the KTN wafer is required to have no crystal orientation deviation, a complete surface lattice, and a smooth surface without damage. Even very small angular deviations or crystal plane defects will destroy the modulation efficiency and performance of the laser, and even lead to changes in the crystal structure, affecting the modulation accuracy and stability of the component. 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晶体是一种典型的二次电光晶体材料，一般认为，阶次越高的非线性调制，其非线性系数越小，因此长久以来电光调制研究的重点一直局限于线性电光材料和器件。常用的有铌酸锂(LN)、钽酸锂(LT)、磷酸钛氧铷(RTP)和硅酸镓镧(LGS)等，相应的调制元器件都是针对这些线性电光晶体的。另外，由于KTN晶体的无限固熔体特性，生长高质量大尺寸的单晶非常困难，这使其研究和应用一直受到很大限制。近年来，随着晶体制备技术的不断进步，人们成功获得了符合实用要求的英寸级、高质量KTN单晶，这使KTN的研究和应用越来越受到重视。研究显示，KTN晶体在激光调制方面甚至表现出比线性电光 晶体更为优异的性能。不论是对比传统的声光、机械调制等，还是现有的线性电光调制，基于KTN晶体Kerr效应的电光调制在透光波段、调制效率和响应时间等诸多方面都明显优于前者。因此，基于KTN晶体二次电光效应的电光调制在降低驱动电压、减小器件尺寸方面更具优势，更能满足未来激光器宽波段、小型化、集成化发展的需要。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. In recent years, with the continuous advancement of crystal preparation technology, people have successfully obtained inch-level, high-quality KTN single crystals that meet practical requirements. This has made the research and application of KTN more and more important. Studies have shown that 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晶体电光调制器件目前从实验室研究转向产业化应用，其元件加工制备对晶体器件的性能至关重要，而现有激光调制元件的加工制备技术大都是针对线性电光晶体材料的，同时一种电光晶体材料的实际应用与该晶体特有的物理化学性能密切相关，因此本发明针对二次电光效应特点和KTN晶体结晶学特性发展了专门的KTN电光调制元件加工制备技术，该技术不仅可以大大推进KTN电光调制器的应用推广，还对二次电光调制技术具有广泛借鉴意义。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.
发明内容Summary of the invention
本发明针对二次电光效应特点和KTN晶体结晶学特性，旨在提供一种应用于不同组分配比和不同晶相的KTN系列晶体二次电光调制器件的基片元件的加工制作方法，为发明高效KTN二次电光调制器提供元件制备方案。In view of the secondary electro-optic effect characteristics and the crystallographic characteristics of KTN crystals, 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.
本发明的技术方案如下：一种钽铌酸钾单晶基片元件的加工制作方法，所述KTN晶体为Nb组分为0<x<1，晶相为立方(m3m)、四方(4mm)或正交(mm2)，掺杂离子为Cu、Fe、Sn、Ti、Li、Na、Mn单掺或混合多掺的KTa 1-xNb xO 3或M:KTa 1-xNb xO 3晶体。 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.
所述方法步骤主要包括针对KTN晶体的定向、切割、组方、研磨、抛光及卸盘，具体如下：The method steps mainly include orientation, cutting, assembly, grinding, polishing and unloading of KTN crystals, which are specifically as follows:
(1)定向：根据KTN晶体结晶和生长学特性，其定向包括单晶结晶面定向和内部生长解离条纹定向，通过切割和研磨修整实现结晶面与几何面在一定误差内重合。标记出生长解理条纹与几何面的方向关系。(1) 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.
(2)切割：以晶体的定向面为基准，根据KTN晶体多样化的通光方向应用需求，采用金刚石切割工具切割出具有设计晶向和尺寸的晶片，切割尺寸误差小于10μm，晶向误差小于0.5°。(2) Cutting: 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 10μm, and the crystal orientation error is less than 0.5°.
(3)组方：选取与所加工KTN晶体硬度和弹性模量相近的玻璃或晶体作为夹具材料，根据晶体加工面的几何尺寸设计夹具形状与尺寸，并通过切割整形制 作夹具。根据应用需求和晶片的居里温度值，选择石蜡或502粘合剂将晶体与夹具组合成加工方块。(3) 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.
(4)研磨：在20-25℃、湿度为30-70％环境下，根据KTN晶体的硬度特性，使用磨料对方块进行整形，并进行粗磨，细磨和精磨，精磨之后样品粗糙度RMS在150μm以内，厚度均匀性≤2μm。所述的整形，粗磨，细磨和精磨磨料均可使用金刚砂、碳化硼或氧化铝；(4) Grinding: Under the environment of 20-25℃ and 30-70% humidity, according to the hardness characteristics of KTN crystals, use abrasives to shape the square, and perform rough grinding, fine grinding and fine grinding. After the fine grinding, the sample is rough The degree of RMS is within 150μm, and the thickness uniformity is ≤2μm. The said shaping, rough grinding, fine grinding and fine grinding abrasives can all use emery, boron carbide or alumina;
(5)抛光：在温度为22±2℃，湿度为30-70％环境下，根据KTN晶体的机械化学性能，使用磨料粒度小于1μm的水基抛光液和抛光垫对精磨之后的晶体进行粗抛和精抛，精抛之后表面可实现无损伤，面型优于λ/8，均方根粗糙度(RMS)小于1nm，上下表面平行度在5″以内；所述水基抛光液的磨料可为：金刚石或氧化铈或二氧化硅；所述抛光垫可以为：聚氨酯抛光垫、无纺布抛光垫、绒布抛光垫、沥青抛光垫。(5) 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 1μm to perform fine grinding on the crystals. Rough polishing and fine polishing, the surface can achieve no damage after fine polishing, the surface profile is better than λ/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.
(6)涂覆保护膜及卸盘：对精抛之后的加工表面在超净工作台内使用无尘布依次进行丙酮、酒精清洗之后，自流平或旋涂一层虫胶漆片酒精溶液作为保护漆，其虫胶漆片浓度为5wt％-20wt％，放置30min，晾干，再使用烤灯加热至60-70℃熔融石蜡卸夹具。对于使用502粘合剂的加工方块，则在清洗之后放在丙酮溶液中浸泡5-12h，待502粘合剂溶解后卸下夹具。(6) 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 For the protective paint, 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.
本发明所述方法步骤(1)中结晶面定向使用X射线定向仪完成，所述误差≤5′。内部生长解理条纹定向使用放大镜或显微镜在通光面逆光观察，KTN生长条纹为平行线状条纹，一般方向一致，其方向受晶体结晶面方向影响，但二者无固定角度关系。因此根据不同成分KTN单晶的生长特性和应用目的，只有对单晶胚料进行结晶面定向和解理条纹定向，才能充分规避和利用生长解理条纹的特有性能，实现KTN晶体多样化应用。In 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.
本发明所述方法步骤(2)中，所述切割工具可为：金刚石内圆或划片或线切割机，依据不同成分KTN晶体特有的硬度及脆性性能，选择刀片或切割线的线速度为1000-1500cm/s，切割进刀速度为4-8mm/min。对于Nb组分含量x＜0.5时的纯KTa 1-xNb xO 3晶体，优选刀片或切割线的线速度为1500cm/s，进刀速度为5mm/min，随着成分变化或掺杂不同离子造成晶体硬度变化，可适量调节切割参数。 In step (2) of the method of the present invention, the cutting tool can be: a diamond inner circle or a scribing or wire cutting machine. According to the unique hardness and brittleness of KTN crystals of different compositions, the linear speed of the blade or the cutting line is selected as 1000-1500cm/s, cutting feed speed is 4-8mm/min. For pure KTa 1-x Nb x O 3 crystals with Nb component content x<0.5, 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.
本发明所述方法步骤(3)中，根据KTN晶体材料莫氏硬度在6-7，当晶面加工面型需求低于λ/12时，考虑到加工制作成本，优选K9玻璃作为夹具材料。对于加工面型要求在λ/12以上时，优选KTN晶体材料作为夹具材料，进一步优选与所加工样品为同一成分的KTN晶体作为夹具材料。所述加工方块的加工面形状与晶片加工面形状相似，不一致时，优选方形。所述加工方块尺寸满足：晶片加工面面积:夹具加工面面积＝1:50-1:2，优选1:15-1:5。所述粘合剂选择依据为所加工KTN晶体的居里温度点和所需加工面型精度需求，因为KTN晶体居里温度随钽铌比例变化可出现零下几十度至零上几百度的变化范围，而KTN晶体在居里温度上下会发生立方向和四方向的转变，受晶体内部不可避免的各种微结构缺陷的影响，相变必然会影响晶体加工面的面型精度。因此，本发明中对于面型加工需求低于λ/12时，使用便捷省时的黄胶作为粘合剂，当面型加工需求在λ/12以上时，采用502作为粘合剂。In 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 λ/12, considering the processing and manufacturing cost, K9 glass is preferred as the fixture material. When the processing surface is required to be above λ/12, 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 size of the processing block satisfies: wafer processing surface area: fixture processing surface area=1:50-1:2, preferably 1:15-1:5. 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 λ/12, the convenient and time-saving yellow glue is used as the adhesive, and when the demand for surface processing is above λ/12, 502 is used as the adhesive.
本发明所述方法步骤(4)和(5)可手工实现，也可以机器实现。由于KTN系列晶体的成分与性能可调节，可以实现其性能及用途的多样性。针对KTN晶体的用途、加工形状和尺寸多样性，本发明所述加工方法步骤可根据加工需求即可选择易灵活设计的手工操作方法，也可选择尺寸一致，高效加工的机器加工方法。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.
本发明所述方法步骤(4)中，根据KTN晶体材料与不同研磨材料的磨削机理，优选金刚砂进行快速整形和粗磨。优选氧化铝磨料进行细磨和精磨，以减小磨料在晶体加工表面留下的损伤和划痕，有利于后续快速，高质量抛光。In 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. Preferably, 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.
本发明所述方法步骤(5)中，根据KTN晶体的硬度，粗抛优选聚氨酯抛光垫，精抛优选沥青抛光垫，可以快速，高质量实现抛光效果。In 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.
本发明所述方法步骤(5)中粗抛优选自配的高效分散的酸性水基W0.8氧化铈抛光液，成分包括：0.5wt％-5wt％W0.8氧化铈微粉、55wt％-70wt％去离子水、0.2wt％-15wt％KMnO4、3wt％-10wt％乙二醇、0.1wt％-1wt％硝酸钾、0-1wt％硝酸、0-1wt％氢氧化钾、0.1wt％-2wt％聚丙烯酸(PAA)。精抛优选上述W0.8氧化铈抛光液和胶体二氧化硅(平均粒径为80nm，浓度为25wt％)悬浮液混合液，二者体积比例优选1:1)，以上所述抛光液PH值为5-10，优选5-7。所述自配的高效分散的酸性水基W0.8氧化铈抛光液是针对KTN系列晶体的硬度、塑 性，及化学稳定性而配制的，其具有分散性好、可以快速实现KTN系列晶体的化学机械抛光，且抛光质量较好。精抛中，结合沥青抛光盘的特点，本发明使用W0.8氧化铈抛光液和胶体二氧化硅(平均粒径为80nm，浓度为25wt％)悬浮液混合液，可以合理调节加工晶面与抛光盘之前的摩擦形式，有利于实现小颗粒硬质二氧化硅和颗粒相对较大的W0.8氧化铈的协同抛光作用，可以提高KTN晶体的抛光去除率和表面抛光质量。In step (5) of the method of the present invention, in step (5) of the method of the present invention, 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). For fine polishing, 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. In the fine polishing, combined with the characteristics of the asphalt polishing disc, 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.
本发明所述加工后的KTN晶片为晶向误差为±5′以内的(100)、(110)、(111)晶向晶片，所述形状可为圆柱体、长方体、三方柱、六方柱以及不规则形状。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.
本发明所述KTN单晶基片元件制备方法具有以下优势：针对KTN系列晶体结晶相与晶体组分、环境温度密切相关的特性，根据室温下不同组分、不同离子掺杂KTN晶体的结晶学特征进行精确定向加工；采用相应的定向、切割、研磨、抛光工艺过程及对应的夹具材料、研磨剂、抛光液的配合使用，可保障KTN基片元件晶向准确、表面光洁，达到激光调制器件制作要求，且加工效率高，成本低；本发明所制作的KTN单晶基片元件不仅可满足传统线性电光调制器件制作需要，还可为二次电光调制器件设计制作提供参考和借鉴。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.
附图说明Description of the drawings
图1为本发明实施例1所述不同晶向，不同形状KTN单晶基片加工示意图；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;
图2为本发明实施例2所述不同晶向，不同形状KTN单晶基片加工示意图；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;
图3为本发明实施例3所述不同晶向，不同形状KTN单晶基片加工示意图；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;
图4为本发明实施例4所述不同晶向，不同形状KTN单晶基片加工示意图。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.
具体实施方式detailed description
以下结合附图和实施例对本实用发明做进一步说明：The following will further explain the present invention with reference to the drawings and embodiments:
实施例1：一种高精度立方KTN单晶基片元件的加工，所述KTN晶体组分为KTa 0.5Nb 0.5O 3，晶相为立方(m3m)。对其进行(100)、(010)、(001)三面定向精抛加工，加工目标尺寸为5mm×5mm×5mm正方体，加工步骤如下： 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:
(1)定向：使用丹东新东方DX-2型X射线定向仪完成KTN晶胚定向，通过放大镜和光学显微镜确定晶体生长解理条纹，修整出胚料两个物理面为(100)结晶面，此两个定向物理面分别平行和垂直于晶体解理条纹，结晶面定向误差≤ 5′。(1) 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'.
(2)切割：以步骤(1)中的两个定向面为基准，采用金刚石内圆切割机切割出长宽高为5.5mm×5.5mm×5.5mm的正方体晶体样块，切割尺寸误差小于10μm，切割面晶向分别为(100)、(010)、(001)，晶向误差小于0.5°。(2) Cutting: Using the two orientation planes in step (1) as the reference, use 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 10μm , The crystal orientation of the cutting surface is (100), (010), (001), and the crystal orientation error is less than 0.5°.
(3)组方：选用K9玻璃作为夹具材料，使用内圆切割机切割制作4块6mm×11mm×5.1mm夹具块，并对夹具块各面垂直度进行整形。选用石蜡将晶体样块与夹具组合成加工方块，方块外形尺寸约为17mm×17mm×5.1mm。(3) Assembly: K9 glass is selected as the fixture material, and 4 pieces of 6mm×11mm×5.1mm fixture blocks are cut using an internal cutting machine, and the verticality of each surface of the fixture blocks is reshaped. Use paraffin to combine the crystal sample block and the fixture into a processing block, the size of the block is about 17mm×17mm×5.1mm.
(4)研磨：在20-25℃、湿度为30-70％环境下，使用金刚砂对方块进行整形和倒角处理，得到各面平整，相邻面相互垂直，且倒角处理过的规则加工方块，并分别采用W40、W14、W7的金刚砂对方块的加工面(KTN晶体裸露的面)进行粗磨，细磨和精磨，每一加工面的粗磨去除厚度为100μm，细磨去除80μm，精磨去除50μm，精磨之后表面粗糙度RMS在150μm以内，厚度均匀性≤2μm。(4) Grinding: In an environment of 20-25℃ and 30-70% humidity, use emery to shape and chamfer the square to obtain a regular processing with flat surfaces, adjacent surfaces perpendicular to each other, and chamfering treatment. Use W40, W14, W7 emery to rough, fine and fine grind the processed surface of the cube (the exposed surface of the KTN crystal). The thickness of each processed surface is 100μm for rough grinding and 80μm for fine grinding. , Fine grinding removes 50μm, after fine grinding, the surface roughness RMS is within 150μm, and the thickness uniformity is less than 2μm.
(5)抛光：在温度为22±2℃，湿度为30-70％环境下，使用W0.8氧化铈微粉配置的酸性(PH＝5)抛光液和聚氨酯抛光垫对精磨之后的样品进行粗抛，每面去除厚度约为10μm，基本去除加工面的砂眼和深划痕，上下表面平行度为20″。然后，以W0.8氧化铈抛光液与胶体二氧化硅悬浮液混合液作为抛光液，沥青作为抛光盘材料对方块进行精抛光，每面去除厚度在10μm以内，精抛之后表面无损伤，面型为λ/8，均方根粗糙度RMS＝0.89nm，上下表面平行度＜5″。(5) Polishing: at a temperature of 22±2°C and a humidity of 30-70%, use the acidic (PH=5) polishing solution and polyurethane polishing pad configured with W0.8 cerium oxide powder to perform the fine grinding of the sample Rough polishing, the thickness of each surface is about 10μm, and the sand holes and deep scratches on the processed surface are basically removed. The parallelism of the upper and lower surfaces is 20". Then, a mixture of W0.8 cerium oxide polishing liquid and colloidal silica suspension is used as Polishing liquid, asphalt is used as the material of the polishing disc to finely polish the square. The thickness of each surface is less than 10μm. After the fine polishing, there is no damage on the surface. The surface type is λ/8, the root mean square roughness RMS=0.89nm, and the parallelism of the upper and lower surfaces ＜5″.
(6)卸盘及其它四个面的加工：对(5)中精抛之后的加工表面在超净工作台内依次进行丙酮、酒精清洗之后，均匀旋涂一层虫胶漆片保护漆，放置30min，晾干，使用烤灯加热卸夹具。再对剩余四个未抛光面进行两轮步骤(3)-(6)，得到六面抛光KTN晶块，其各面晶向分别为(100)、(010)、(001)，晶向误差小于5′，表面无损伤，均方根粗糙度RMS＜1nm，上下表面平行度＜5″。所加工KTN样块形状及晶向示意图如图1所示。(6) Unloading and processing of the other four surfaces: the processed surface after the fine polishing in (5) is cleaned with acetone and alcohol in the ultra-clean workbench, and then a layer of shellac paint sheet protective paint is evenly spin-coated. Leave it for 30 minutes, dry it, and use a baking lamp to heat and unload the fixture. Then perform two rounds of steps (3)-(6) on the remaining four unpolished surfaces to obtain six-sided polished KTN ingots. The crystal orientation of each surface is (100), (010), (001), and the crystal orientation error Less than 5', no damage on the surface, root mean square roughness RMS<1nm, parallelism of the upper and lower surfaces<5". The shape and crystal orientation of the processed KTN sample are shown in Figure 1.
实施例1中步骤(4)研磨与步骤(5)抛光过程均为手工操作，快速精确地实现加工目标。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.
实施例2：一种高精度四方Cu离子掺杂KTN单晶基片元件的加工，所述KTN晶体组分为Cu:KTa 0.5Nb 0.5O 3，晶相为四方(4mm)。对其进行(100)晶面定 向精抛加工，目标形状为直径5mm×高5mm的圆柱状样品，加工步骤与实施例1所述不同之处在于：步骤(2)切割出长宽高为5.5mm×5.5mm×5.5mm的晶体样块之后，采用滚圆磨削机将垂直于(100)面的四个侧面磨削成圆柱面，得到尺寸为直径5mm×高5.5mm的圆柱状晶体块。并采用材料和尺寸与实施例1一致的方形夹具进行加工操作，最后得到如图2所示圆柱状Cu:KTa 0.5Nb 0.5O 3晶片元件。其上下圆面为(100)精抛面，表面无损伤，晶向误差小于5′，均方根粗糙度RMS＜1nm，上下表面平行度＜5″。 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). Carry out (100) crystal plane oriented fine polishing processing, the target shape is a cylindrical sample with a diameter of 5mm x a height of 5mm. The processing steps are different from those described in Example 1 in that: step (2) cuts out a length, width and height of 5.5 After the crystal block of mm×5.5mm×5.5mm, 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".
实施例3：一种高精度立方KTN单晶基片元件的加工，所述KTN晶体组分为KTa 0.5Nb 0.5O 3，晶相为立方(m3m)。对其进行(100)、(010)、(001)、(110)晶面定向精抛加工，目标形状为5mm×5mm×5mm的等腰直角三方柱状样品，加工步骤如下： 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). Carry out (100), (010), (001), (110) crystal plane orientation fine polishing processing, the target shape is 5mm×5mm×5mm isosceles right-angled trigonal prism sample, the processing steps are as follows:
(1)定向：使用丹东新东方DX-2型X射线定向仪完成KTN晶胚定向，通过放大镜和光学显微镜确定晶体生长解理条纹，修整出胚料两个物理面为(100)结晶面，此两个定向物理面分别平行和垂直与晶体解理条纹，结晶面定向误差≤5′。(1) 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'.
(2)切割：以步骤(1)中的两个定向面为基准，采用金刚石内圆切割机切割出长宽高为5.5mm×5.5mm×5.5mm的晶体样块，切割尺寸误差小于10μm，切割面晶向分别为(100)、(010)、(001)，晶向误差小于0.5°。随之，沿着(100)面的对角线方向切割出(110)面，并研磨修整(110)面误差在10′以内，获得两块定向修整的三方柱样块。(2) Cutting: 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 10μm. The crystal orientation of the cutting surface is (100), (010), (001), and the crystal orientation error is less than 0.5°. Subsequently, 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.
(3)组方：选用K9玻璃作为夹具材料，使用内圆切割机切割制作4块6mm×11mm×5.1mm夹具块，并对夹具块各面垂直度进行整形。选用石蜡将两块晶体样块与夹具组合成加工方块，方块外形尺寸约为17mm×17mm×5.1mm。当加工(110)晶面时，采用单面加工形式，夹具采用两块7mm×17mm×5.1mm和两块7mm×14mm×5.1mm的K9玻璃块，所组成加工方块尺寸为21mm×24mm×5.1mm。(3) Assembly: K9 glass is selected as the fixture material, and 4 pieces of 6mm×11mm×5.1mm fixture blocks are cut using an internal cutting machine, and the verticality of each surface of the fixture blocks is reshaped. Use paraffin to combine two crystal specimens and fixtures into a processing block, the size of the block is approximately 17mm×17mm×5.1mm. When processing (110) crystal planes, single-sided processing is used. The fixture uses two 7mm×17mm×5.1mm and two 7mm×14mm×5.1mm K9 glass blocks, and the processing block size is 21mm×24mm×5.1 mm.
(4)研磨：在20-25℃、湿度为30-70％环境下，使用金刚砂对方块进行整形和倒角处理，得到各面平整，相邻面相互垂直，且倒角处理过得规则加工方块，并分别采用W40、W14、W7的金刚砂对方块的加工面(KTN晶体裸露的面) 进行粗磨，细磨和精磨，每一加工面的粗磨去除厚度为100μm，细磨去除80μm，精磨去除50μm，精磨之后表面粗糙度RMS在150μm以内，厚度均匀性≤2μm。(4) Grinding: In an environment of 20-25℃ and 30-70% humidity, use emery to shape and chamfer the square to obtain flat surfaces, adjacent surfaces are perpendicular to each other, and the chamfering is processed regularly Use W40, W14, W7 emery to rough, fine and fine grind the processed surface of the cube (the exposed surface of the KTN crystal). The thickness of each processed surface is 100μm for rough grinding and 80μm for fine grinding. , Fine grinding removes 50μm, after fine grinding, the surface roughness RMS is within 150μm, and the thickness uniformity is less than 2μm.
(5)抛光：在温度为22±2℃，湿度为30-70％环境下，使用W0.8氧化铈微粉配置的酸性(PH＝5)抛光液和聚氨酯抛光垫对精磨之后的样品进行粗抛，每面去除厚度约为10μm，基本去除加工面的砂眼和深划痕，上下表面平行度为20″(对于(110)面无此项指标，仅用样块厚度均匀性监控)。之后，以W0.8氧化铈抛光液与胶体二氧化硅悬浮液混合液作为抛光液，沥青作为抛光盘材料对方块进行精抛光，每面去除厚度在10μm以内，精抛之后表面无损伤，面型为λ/8，均方根粗糙度RMS＝0.89nm，上下表面平行度＜5″。(5) Polishing: at a temperature of 22±2°C and a humidity of 30-70%, use the acidic (PH=5) polishing solution and polyurethane polishing pad configured with W0.8 cerium oxide powder to perform the fine grinding of the sample For rough polishing, the thickness of each surface is about 10μm, 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). Afterwards, 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 10μm. The type is λ/8, the root mean square roughness RMS=0.89nm, and the parallelism of the upper and lower surfaces is <5".
(6)卸盘及其它三个面的加工：对(5)中精抛之后的加工表面在超净工作台内依次进行丙酮、酒精清洗之后，均匀旋涂一层虫胶漆片保护漆，放置30min，晾干，使用烤灯加热卸夹具。再对剩余三个未抛光面进行两轮步骤(3)-(6)，得到五面全抛光KTN晶块，其各面晶向分别为(100)、(010)、(001)、(110)，晶向误差小于5′，表面无损伤，均方根粗糙度RMS＜1nm，上下表面平行度＜5″。所加工KTN样块形状及晶向示意图如图3所示。(6) Unloading and processing of the other three surfaces: the processed surface after the fine polishing in (5) is cleaned with acetone and alcohol in the ultra-clean workbench, and then a layer of shellac paint flake protective paint is evenly spin-coated. Leave it for 30 minutes, dry it, and use a baking lamp to heat and unload the fixture. Then perform two rounds of steps (3)-(6) on the remaining three unpolished surfaces to obtain five-sided fully polished KTN ingots. The crystal orientations of each surface are (100), (010), (001), (110). ), the crystal orientation error is less than 5', the surface is not damaged, the root mean square roughness RMS is less than 1nm, and the parallelism of the upper and lower surfaces is less than 5". The shape and crystal orientation of the processed KTN sample are shown in Figure 3.
实施例3中步骤(4)研磨与步骤(5)抛光过程均采用科晶UNIPOL-802双工位自动研磨抛光机进行机器研磨和抛光，采用特制的模具组件高效地实现了加工目标。In the step (4) grinding and step (5) polishing process of Example 3, 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.
实施例4：一种高精度立方KTN单晶基片元件的加工，所述KTN晶体组分为KTa 0.5Nb 0.5O 3，晶相为立方(m3m)。对其进行(100)晶面定向精抛加工，目标形状为宽5mm×高5mm的正六方柱状样品，加工步骤与实施例1所述不同之处在于：步骤(2)首先使用内圆切割机切出长宽高为4.85mm×5.5mm×5.5mm的晶体样块，其中(100)定向面为一个4.85mm×5.5mm面，再使用划片切割机垂直于(100)定向面切割出正六方柱晶体样块，其六边形面为(100)定向面。并采用材料和尺寸与实施例1一致的方形夹具进行加工操作，最后得到如图4所示六方柱状KTa 0.5Nb 0.5O 3晶片元件。其六方面为(100)精抛面，表面无损伤，晶向误差小于5′，均方根粗糙度RMS＜1nm，上下表面平行度＜5″。 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".

Claims (5)

  1. 一种钽铌酸钾单晶基片元件的加工制作方法，所述KTN晶体为Nb组分为0<x<1，晶相为立方、四方或正交，掺杂离子为Cu、Fe、Sn、Ti、Li、Na、Mn单掺或混合多掺的KTa 1-xNb xO 3或M:KTa 1-xNb xO 3晶体，其特征在于：所述方法步骤主要包括： A method for processing and manufacturing a potassium tantalum niobate single crystal substrate element, wherein the KTN crystal has a Nb composition of 0<x<1, a crystal phase of cubic, tetragonal or orthogonal, and doping ions of 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 crystals, characterized in that: the method steps mainly include:
    (1)定向：根据KTN晶体结晶和生长学特性，其定向包括单晶结晶面定向和内部生长解离条纹定向；(1) Orientation: According to the crystallization and growth characteristics of KTN crystal, its orientation includes single crystal crystal plane orientation and internal growth dissociation fringe orientation;
    (2)切割：以晶体的定向面为基准，采用金刚石切割工具切割出具有设计晶向和尺寸的晶片，切割尺寸误差小于10μm，晶向误差小于0.5；(2) Cutting: Use a diamond cutting tool to cut the wafer with the designed crystal orientation and size based on the orientation plane of the crystal. The cutting size error is less than 10μm, and the crystal orientation error is less than 0.5;
    (3)组方：选取与所加工KTN晶体硬度和弹性模量相近的玻璃或晶体作为夹具材料，根据晶体加工面的几何尺寸设计夹具形状与尺寸，并通过切割整形制作夹具；根据应用需求和晶片的居里温度值，选择石蜡或502粘合剂将晶体与夹具组合成加工方块；(3) Organization: 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 application requirements and For the Curie temperature value of the wafer, select paraffin or 502 adhesive to combine the crystal and the fixture into a processing block;
    (4)研磨：在20-25℃、湿度为30-70％环境下，根据KTN晶体的硬度特性，使用磨料对方块进行整形，并进行粗磨，细磨和精磨，精磨之后样品粗糙度RMS在150μm以内，厚度均匀性≤2μm；所述的整形，粗磨，细磨和精磨磨料均可使用金刚砂、碳化硼或氧化铝；(4) Grinding: Under the environment of 20-25℃ and 30-70% humidity, according to the hardness characteristics of KTN crystals, use abrasives to shape the square, and perform rough grinding, fine grinding and fine grinding. After the fine grinding, the sample is rough The degree of RMS is within 150μm, and the thickness uniformity is ≤2μm; the aforementioned shaping, rough grinding, fine grinding and fine grinding abrasives can all use emery, boron carbide or alumina;
    (5)抛光：在温度为22±2℃，湿度为30-70％环境下，根据KTN晶体的机械化学性能，使用磨料粒度小于1μm的水基抛光液和抛光垫对精磨之后的晶体进行粗抛和精抛，精抛之后表面可实现无损伤，面型优于λ/8，均方根粗糙度(RMS)小于1nm，上下表面平行度在5″以内；所述水基抛光液的磨料可为：金刚石或氧化铈或二氧化硅；所述抛光垫可以为：聚氨酯抛光垫、无纺布抛光垫、绒布抛光垫、沥青抛光垫；(5) 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 1μm to perform fine grinding on the crystals. Rough polishing and fine polishing, the surface can achieve no damage after fine polishing, the surface profile is better than λ/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 can be: diamond or cerium oxide or silicon dioxide; the polishing pad can be: a polyurethane polishing pad, a non-woven polishing pad, a flannel polishing pad, an asphalt polishing pad;
    (6)涂覆保护膜及卸盘：对精抛之后的加工表面在超净工作台内使用无尘布依次进行丙酮、酒精清洗之后，自流平或旋涂一层虫胶漆片酒精溶液作为保护漆，其虫胶漆片浓度为5wt％-20wt％，放置30min，晾干，再使用烤灯加热至60-70℃熔融石蜡卸盘。(6) 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 For the protective paint, the concentration of the shellac paint flakes is 5wt%-20wt%, placed for 30 minutes, dried, and then heated to 60-70°C with a baking lamp to remove the molten paraffin from the tray.
  2. 根据权利要求1所述的单晶基片的加工制作方法，其特征在于：步骤2中所述切割工具为金刚石内圆或划片或线切割机，所述的切割线的线速度为1000-1500cm/s，切割进刀速度为4-8mm/min。The method for processing a single crystal substrate according to claim 1, wherein the cutting tool in step 2 is a diamond inner circle or scribing or wire cutting machine, and the linear speed of the cutting line is 1000- 1500cm/s, cutting feed speed is 4-8mm/min.
  3. 根据权利要求2所述的单晶基片的加工制作方法，其特征在于：所述步骤(3)夹具材料为KTN晶体材料；所述晶片加工面积:夹具加工面面积＝1:50-1:2；所述步骤(5)中，粗抛采用聚氨酯抛光垫，精抛采用沥青抛光垫。The method for processing and manufacturing a single crystal substrate according to claim 2, wherein the fixture material in step (3) is KTN crystal material; the wafer processing area: fixture processing surface area = 1:50-1: 2; In the step (5), a polyurethane polishing pad is used for rough polishing, and an asphalt polishing pad is used for fine polishing.
  4. 根据权利要求3述的单晶基片的加工制作方法，其特征在于：所述的晶片加工面积:夹具加工面积＝1:15-1:5。The method for processing and manufacturing a single crystal substrate according to claim 3, wherein the processing area of the wafer: the processing area of the fixture=1:15-1:5.
  5. 根据权利要求4的单晶基片的加工制作方法，其特征在于：所述步骤(5)中粗抛优选自配的高效分散的酸性水基W0.8氧化铈抛光液，成分包括：0.5wt％-5wt％W0.8氧化铈微粉、55wt％-70wt％去离子水、0.2wt％-15wt％KMnO4、3wt％-10wt％乙二醇、0.1wt％-1wt％硝酸钾、0-1wt％硝酸、0-1wt％氢氧化钾、0.1wt％-2wt％聚丙烯酸(PAA)。The method for processing and manufacturing a single crystal substrate according to claim 4, characterized in that: in the step (5), rough polishing is preferably a self-prepared, highly dispersed acidic water-based W0.8 cerium oxide polishing solution, the composition includes: 0.5 wt %-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).
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