WO2021088126A1 - Procédé de polissage double face pour substrat de niobate de lithium ultra-mince de grande taille - Google Patents

Procédé de polissage double face pour substrat de niobate de lithium ultra-mince de grande taille Download PDF

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Publication number
WO2021088126A1
WO2021088126A1 PCT/CN2019/119601 CN2019119601W WO2021088126A1 WO 2021088126 A1 WO2021088126 A1 WO 2021088126A1 CN 2019119601 W CN2019119601 W CN 2019119601W WO 2021088126 A1 WO2021088126 A1 WO 2021088126A1
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Prior art keywords
lithium niobate
thin lithium
polishing
size
double
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PCT/CN2019/119601
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English (en)
Chinese (zh)
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沈浩
王勤峰
徐秋峰
朱海瀛
丁孙杰
曹焕
汤卓伦
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天通控股股份有限公司
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Publication of WO2021088126A1 publication Critical patent/WO2021088126A1/fr

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    • 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
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/30—Niobates; Vanadates; Tantalates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08—Etching
    • C30B33/10—Etching in solutions or melts

Definitions

  • the invention relates to the field of semiconductor materials, in particular to a double-sided polishing method for a lithium niobate substrate as a semiconductor substrate material.
  • Lithium niobate (LiNbO 3 , hereinafter referred to as LN) is a multifunctional material integrating piezoelectric, ferroelectric, pyroelectric, nonlinear, optoelectronic, photoelastic, and photorefractive functions.
  • LN has received more and more attention due to its excellent physical properties, and has been widely used in aviation, aerospace, and civil optoelectronic products.
  • the LN substrate after double-sided polishing is widely used in sensors, acousto-optic devices, optical gyroscopes, etc. Unlike silicon crystals and sapphire crystals, it is characterized by extremely low fracture toughness and hardness.
  • the material removal rate is proportional to the polishing speed, polishing pressure, and polishing temperature.
  • the unevenness of the positive polishing pressure will cause uneven polishing wear, worsen the polishing quality, and deteriorate the roughness and flatness.
  • the technical problem to be solved by the present invention is to provide a double-sided polishing method for large-size ultra-thin lithium niobate substrates, which can be polished once, mass-produced, with high polishing efficiency and high flatness of the surface of the produced lithium niobate substrates.
  • the characteristics determine that the lithium niobate substrate is not easy to be broken in device applications, the material utilization rate is high, and the processing yield is high.
  • the technical solution adopted by the present invention to solve the technical problem is: a double-sided polishing method for a large-size ultra-thin lithium niobate substrate, which specifically includes the following steps:
  • the large-size ultra-thin lithium niobate double-sided reduced flakes are directly chemically corroded in a closed container containing nitric acid, hydrofluoric acid and a slow-release agent uniformly mixed, the corrosion temperature is 20 °C ⁇ 25 °C, and the corrosion time is 12 ⁇ 48 hours, make the roughness of the large-size ultra-thin lithium niobate wafer ⁇ 50nm and flatness ⁇ 2um, and then perform ultrasonic cleaning to obtain the large-size ultra-thin lithium niobate corrosion wafer with random and disordered pit structure on the surface;
  • the large-size ultra-thin lithium niobate corroded sheet is polished on both sides with a double-sided polishing machine and a polishing liquid.
  • the polishing unit surface pressure is 200g/cm 2 ⁇ 1400g/cm 2
  • the polishing temperature is 20 ⁇ 25°C to make the big
  • the roughness of ultra-thin lithium niobate wafers of size ⁇ 0.50nm, flatness ⁇ 1um, the lateral dimension of the pits and depressions are 0.10 ⁇ 0.30um, the longitudinal depth is 0.10nm ⁇ 0.50nm, and the surface area of the recesses accounts for the surface area of the large ultra-thin niobium 20%-80% of the surface area of the lithium oxide substrate is then ultrasonically cleaned to obtain the final large-size ultra-thin lithium niobate double-thinning film.
  • the thickness of the lithium niobate cutting sheet is 200-250um
  • the thickness of the double-sided polishing sheet is 170-220um
  • the thickness of the double-sided thinning sheet is 160-210um.
  • the abrasive is a mixture of one or more of boron carbide, diamond, aluminum oxide or silicon carbide.
  • the roughness of the lithium niobate abrasive sheet depends on the particle size of the silicon carbide abrasive used. Generally speaking, the larger the particle size, the greater the roughness.
  • the double-sided thinning refers to the large-size ultra-thin lithium niobate substrate double-sided polishing sheet through the two-sided small particle size grinding wheel thinning method for flatness control, warpage control, and reduction of double-sided polishing sheet Damaged layer, reducing polishing time.
  • step c) chemical etching refers to etching and leveling the polishing sheet of the lithium niobate substrate in a mixed acid to remove surface impurities, repair surface damage, and control the degree of warpage.
  • the corrosive liquid can be selected from a mixture of one, two or three of HNO3, HF, and slow-release agents.
  • the corrosion time is determined according to the flatness and warpage after polishing with lithium niobate, which can be several minutes to several tens of hours, preferably 12 to 48 hours.
  • the warpage is less than 25 ⁇ m
  • the roughness is less than 50nm
  • the flatness is less than 2um
  • the chemical corrosion can be ended.
  • the surface of the substrate after chemical etching is locally planarized, and a random and disordered pit structure is formed on the surface.
  • the formation process of the polished surface is more complicated.
  • the initial stage is mainly to remove the tiny protrusions left by the previous process.
  • the actual polishing area at this stage is extremely small, and the polishing pressure per unit area is relatively large. Therefore, the formation rate of the polished surface at this stage is high.
  • the polishing process progresses, the polished surface area of the wafer becomes larger and larger, the pressure per unit area is gradually reduced, and the formation rate of the polished surface area is gradually reduced.
  • This stage is mainly to polish the entire surface.
  • the third stage is the stage that takes the longest time in the polishing process. Most of the polished surface has been formed in the second stage.
  • the main task of this stage is to remove individual large defects on the surface of the wafer, at least twice as long as the first and second stages to remove these large defects.
  • the large-size ultra-thin lithium niobate substrate of the present invention is polished on both sides, and the polished surface roughness is less than 0.50nm, and the flatness is less than 1um, and the polished surface has a random and disordered pit structure.
  • the random and disordered pit structure on the surface of the lithium niobate substrate of the present invention the lateral dimension of the pit recess is 0.10 ⁇ 0.30um, the longitudinal depth is 0.10nm ⁇ 0.50nm, and the surface area of the recess part accounts for the surface area of the lithium niobate substrate. 20% to 80%.
  • the polishing pressure of the present invention has a great influence on the polishing rate and the polishing surface quality.
  • the polishing pressure increases, the mechanical action is enhanced, and the polishing rate also increases.
  • using too high polishing pressure will cause uneven polishing rate and increased wear of the polishing pad. Elevated and difficult to control, so that the large-size ultra-thin wafers have scratches, fragments, and chipped corners, which increase the probability of occurrence of scratches, chips, and corners, thereby reducing polishing quality and high production costs.
  • the present invention Compared with the traditional global flattened lithium niobate substrate, on the one hand, compared with the traditional double-sided rough polishing and fine polishing technology, because the lithium niobate substrate of the present invention is polished on both sides at one time and is large in size and ultra-thin, The lithium niobate substrate greatly reduces the product defect rate and processing cost.
  • the present invention adopts chemical polishing technology when polishing large-size and ultra-thin lithium niobate substrates on both sides, which can simultaneously polish a large amount of lithium niobate double-sided thinning flakes at one time, greatly increasing the polishing efficiency.
  • the surface roughness of the lithium niobate substrate of the present invention is small.
  • a lithium niobate substrate can be directly applied to optical devices; on the other hand, the internal stress caused by lattice mismatch in the subsequent process is reduced, stress concentration is reduced, the dislocation density is reduced, and the quality of the subsequent process is improved.
  • the lithium niobate substrate of the present invention has a random and disordered pit structure.
  • Such a substrate enhances the adhesion during the coating process and prevents the coating from cracking; on the other hand, it reduces the internal stress caused by the lattice mismatch between the coating and the lithium niobate substrate, relieves stress concentration, and reduces dislocation density , Improve the quality of optical devices.
  • this feature determines that the lithium niobate substrate is not easily broken in device applications, has high material utilization and high processing yield.
  • the lithium niobate substrate of the present invention is large in size and ultra-thin, this feature determines that the lithium niobate substrate has a higher single input utilization rate in device applications, and meets the requirements of miniaturization and chipization. .
  • FIG. 1 is a schematic diagram of the horizontal and vertical depth changes of pits under different processing pressures in the embodiment of the present invention.
  • Fig. 2 is a schematic diagram of roughness changes under different processing pressures in the embodiment of the present invention.
  • Fig. 3 is a schematic diagram of flatness changes under different processing pressures according to the embodiment of the present invention.
  • the large-size ultra-thin lithium niobate double-sided thinning flakes are directly chemically corroded in a closed container containing nitric acid, hydrofluoric acid and a slow-release agent in a certain proportion, and the corrosion temperature is 20°C ⁇ 25°C.
  • the time is 12 to 48 hours, so that the roughness of the large-size ultra-thin lithium niobate wafer is less than 50nm, and the flatness is less than 2um, and then ultrasonic cleaning is performed to obtain a large-size ultra-thin lithium niobate corrosion wafer with a random and disordered pit structure on the surface ;
  • the large-size ultra-thin lithium niobate corroded sheet is polished on both sides with a double-sided polishing machine and polishing liquid.
  • the polishing unit surface pressure is 300g/cm 2 , and the polishing temperature is 20-25 °C, so that large-size ultra-thin niobic acid
  • the roughness of the lithium wafer is less than 0.5nm, the flatness is less than 1um, the lateral dimension of the pit and recess is 0.18um, the longitudinal depth is 0.39nm, and the surface area of the recessed part accounts for 20% ⁇ 80 of the surface area of the large-size ultra-thin lithium niobate substrate %.
  • ultrasonic cleaning is carried out to obtain the final large-size ultra-thin lithium niobate double-thin film.
  • the large-size ultra-thin lithium niobate double-sided thinning flakes are directly chemically corroded in a closed container containing nitric acid, hydrofluoric acid and a slow-release agent in a certain proportion, and the corrosion temperature is 20°C ⁇ 25°C.
  • the time is 12 to 48 hours, so that the roughness of the large-size ultra-thin lithium niobate wafer is less than 50nm, and the flatness is less than 2um, and then ultrasonic cleaning is performed to obtain a large-size ultra-thin lithium niobate corrosion wafer with a random and disordered pit structure on the surface ;
  • the large-size ultra-thin lithium niobate corrosion film is polished on both sides with a double-sided polishing machine and a polishing liquid.
  • the polishing unit surface pressure is 400g/cm 2 , and the polishing temperature is 20-25 °C, so that large-size ultra-thin niobic acid
  • the roughness of the lithium wafer is less than 0.5nm, the flatness is less than 1um, the lateral dimension of the pit and recess is 0.15um, and the longitudinal depth is 0.21nm.
  • the surface area of the recessed part accounts for 20% ⁇ 80 of the surface area of the large-size ultra-thin lithium niobate substrate %. Then ultrasonic cleaning is carried out to obtain the final large-size ultra-thin lithium niobate double-thin film.
  • the large-size ultra-thin lithium niobate double-sided thinning flakes are directly chemically corroded in a closed container containing nitric acid, hydrofluoric acid and a slow-release agent in a certain proportion, and the corrosion temperature is 20°C ⁇ 25°C.
  • the time is 12 to 48 hours, so that the roughness of the large-size ultra-thin lithium niobate wafer is less than 50nm, and the flatness is less than 2um, and then ultrasonic cleaning is performed to obtain a large-size ultra-thin lithium niobate corrosion wafer with a random and disordered pit structure on the surface ;
  • the large-size ultra-thin lithium niobate corroded sheet is polished on both sides with a double-sided polishing machine and polishing liquid.
  • the polishing unit surface pressure is 500g/cm 2 , and the polishing temperature is 20-25 °C, so that large-size ultra-thin niobic acid
  • the roughness of the lithium wafer is less than 0.5nm, the flatness is less than 1um, the lateral dimension of the pits and recesses is 0.11um, the longitudinal depth is 0.13nm, and the surface area of the recesses accounts for 20% to 80% of the surface area of the large-size ultra-thin lithium niobate substrate %.
  • ultrasonic cleaning is carried out to obtain the final large-size ultra-thin lithium niobate double-thin film.
  • the large-size ultra-thin lithium niobate double-sided thinning flakes are directly chemically corroded in a closed container containing nitric acid, hydrofluoric acid and a slow-release agent in a certain proportion, and the corrosion temperature is 20°C ⁇ 25°C.
  • the time is 12 to 48 hours, so that the roughness of the large-size ultra-thin lithium niobate wafer is less than 50nm, and the flatness is less than 2um, and then ultrasonic cleaning is performed to obtain a large-size ultra-thin lithium niobate corrosion wafer with random and disordered surface pits structure ;
  • the large-size ultra-thin lithium niobate corrosion film is polished on both sides with a double-sided polishing machine and a polishing liquid.
  • the polishing unit surface pressure is 600g/cm 2 , and the polishing temperature is 20-25 °C, which makes the large-size ultra-thin niobic acid
  • the roughness of the lithium wafer is less than 0.5nm, and the flatness is less than 1um.
  • the lateral dimension of the pit and recess is 0.20um, and the longitudinal depth is 0.32nm.
  • the surface area of the recessed part accounts for 20% to 80% of the surface area of the large ultra-thin lithium niobate substrate. %. Then ultrasonic cleaning is carried out to obtain the final large-size ultra-thin lithium niobate double-thin film.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

La présente invention concerne un procédé de polissage double face pour un substrat de niobate de lithium ultra-mince de grande taille comprenant les étapes suivantes : a) le meulage de la tranche de niobate de lithium ultra-mince de grande taille coupée pour obtenir une feuille de meulage double face de niobate de lithium ultra-mince de grande taille présentant une structure rugueuse sur la surface ; b) puis la réalisation d'un amincissement double face et d'un nettoyage par ultrasons pour obtenir une feuille d'amincissement double face de niobate de lithium ultra-mince de grande taille présentant une structure rugueuse sur la surface ; c) la réalisation directe d'une corrosion chimique dans un récipient fermé contenant de l'acide nitrique, de l'acide fluorhydrique et un agent à libération prolongée qui sont mélangés uniformément pour obtenir une feuille corrodée de niobate de lithium ultra-mince de grande taille présentant une structure de creux aléatoire désordonnée sur la surface ; et d) la réalisation d'un polissage double face au moyen d'une machine de polissage double face et d'une solution de polissage, puis la réalisation d'un nettoyage par ultrasons pour obtenir la feuille double polie de niobate de lithium ultra-mince de grande taille finale. Selon la présente invention, un polissage en une seule fois et une production de masse sont obtenus, l'efficacité de polissage est élevée et le substrat de niobate de lithium produit présente une planéité de surface élevée. Cette caractéristique détermine que le substrat de niobate de lithium n'est pas facile à rompre dans l'application de dispositif, le taux d'utilisation de matériau est élevé et le rendement de traitement est élevé.
PCT/CN2019/119601 2019-11-06 2019-12-20 Procédé de polissage double face pour substrat de niobate de lithium ultra-mince de grande taille WO2021088126A1 (fr)

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CN112621392B (zh) * 2020-12-08 2021-10-29 天通控股股份有限公司 大尺寸超薄高精度铌酸锂晶片加工方法
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