US20100081561A1 - Optical material and optical element - Google Patents

Optical material and optical element Download PDF

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US20100081561A1
US20100081561A1 US12/551,822 US55182209A US2010081561A1 US 20100081561 A1 US20100081561 A1 US 20100081561A1 US 55182209 A US55182209 A US 55182209A US 2010081561 A1 US2010081561 A1 US 2010081561A1
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optical element
particles
raw materials
sintering
optical
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Kohei Nakata
Michio Endo
Kentaro Doguchi
Shigeru Fujino
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Canon Inc
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Canon Inc
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Assigned to CANON KABUSHIKI KAISHA reassignment CANON KABUSHIKI KAISHA ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: FUJINO, SHIGERU, DOGUCHI, KENTARO, ENDO, MICHIO, NAKATA, KOHEI
Publication of US20100081561A1 publication Critical patent/US20100081561A1/en
Priority to US13/076,471 priority Critical patent/US8338003B2/en
Priority to US13/363,492 priority patent/US8202813B2/en
Abandoned legal-status Critical Current

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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/02—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of crystals, e.g. rock-salt, semi-conductors
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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    • C04B35/62605—Treating the starting powders individually or as mixtures
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
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    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/252—Glass or ceramic [i.e., fired or glazed clay, cement, etc.] [porcelain, quartz, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]

Definitions

  • the present invention relates to an optical element, in particular, a highly accurate optical element used for a lens or the like.
  • the high refractive index and low dispersibility which are absent in the conventional optical glass, can be realized by using a crystal material, and in order to use the crystal material as a material which has a good transmittance and is suitable for optical applications, there has been a method involving using a single-crystal material or a method involving sintering crystal particles and using the resultant.
  • the single-crystal material is extremely expensive, and it is difficult to obtain a material which has a large diameter and is suitable for an optical lens. That is, in the method involving sintering crystal particles, when the particle diameter is large, a large grain boundary occurs during sintering to cause decrease in a transmittance as an optical lens, and a defect occurs on a lens surface due to a grain boundary at the time of processing the material into a lens shape, and hence, it has been difficult to obtain a good optical lens.
  • the present invention has been accomplished in view of the problems of the above-mentioned related art, and it is, therefore, an object of the present invention to provide an optical element having optical properties of high refractive index and low dispersibility.
  • a first optical element for solving the above-mentioned problems is formed by vacuum-sintering a molded body of ceramic particles having an average particle diameter of 1 ⁇ m or more and 10 ⁇ m or less and comprising Ln x Al y O [x+y] ⁇ 1.5 (Ln represents a rare-earth element, x represents 1 ⁇ x ⁇ 10, and y represents 1 ⁇ y ⁇ 5).
  • a second optical element for solving the above-mentioned problems is formed by vacuum-sintering a molded body of particles having a two-layer structure, the particles being formed by coating, on surfaces of ceramic particles having an average particle diameter of 1 ⁇ m or more and 10 ⁇ m or less and comprising Ln x Al y O [x+y] ⁇ 1.5 (Ln represents a rare-earth element, x represents 1 ⁇ x ⁇ 10, and y represents 1 ⁇ y ⁇ 5), a coating layer comprising a ceramic having a lower sintering temperature than a sintering temperature of the ceramic particles.
  • the FIGURE is a cross-sectional view illustrating an optical element according to the present invention.
  • the optical element of the present invention is formed by vacuum-sintering, by using specific ceramic particles, crystal particles at a lower temperature than a temperature during an ordinary sintering process, and has optical properties of high refractive index and low dispersibility without any defects.
  • the optical element of the present invention can be applied to a lens and a prism used for various optical systems.
  • An optical element according to Example 1 of the present invention is formed by vacuum-sintering a molded body of ceramic particles having an average particle diameter of 1 ⁇ m or more and 10 ⁇ m or less and including Ln x Al y O [x+y] ⁇ 1.5 (Ln represents a rare-earth element, x represents 1 ⁇ x ⁇ 10, and y represents 1 ⁇ y ⁇ 5).
  • Ln includes rare-earth elements, and specific examples thereof include Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu. Of those rare-earth elements, it is particularly preferred that Ln be at least one kind or more selected from La, Gd, Yb, and Lu.
  • the average particle diameter of the ceramic particles is desirably 1 ⁇ m or more and 10 ⁇ m or less.
  • the average particle diameter is less than 0.1 ⁇ m, the particles are too fine and partial agglomeration occurs, and hence, it is difficult to sufficiently densify the particles at the time of pressurizing, and the optical element after sintering has remaining bubbles, and hence, the resultant element is unsuitable to be used as an optical element.
  • the average particle diameter exceeds 10 ⁇ m, a void is easily formed at the time of pressurizing and a grain boundary easily occurs in the crystal obtained after sintering, and hence, detachment of the particles occurs during polishing, so that an optical element having a satisfactory surface cannot be obtained.
  • the shape of the ceramic particle is preferably spherical.
  • the optical element preferably has a refractive index of 1.8 or more and has transmissivity.
  • a method of producing the optical element of the present invention is as follows. First, spherical ceramic particles having an average particle diameter of 1 ⁇ m or more and 10 ⁇ m or less are prepared by a method such as plasma melting. Next, the spherical ceramic particles are subjected to casting, dry molding, or wet molding to thereby prepare a preliminary molded body. Furthermore, the preliminary molded body is sintered under a vacuum, followed by grinding and polishing processes, and as a result, an optical element for an optical lens or the like is obtained.
  • the optical element is a preferred mode.
  • crystal particles are vacuum-sintered at a lower temperature than the temperature during an ordinary sintering process, and hence, an optical element having optical properties of high refractive index and low dispersibility without any defects can be obtained.
  • the degree of vacuum in vacuum-sintering is preferably 0.1 Pa or less.
  • La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% or more were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 1 to 8 in Table 1, and the oxide raw materials were mixed.
  • the raw materials were introduced into thermal plasma, and were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, and as a result, spherical particles having an average particle diameter of 1 ⁇ m were obtained.
  • the heating temperature was set at 1,500° C. or higher and 3,200° C. or lower. When the heating temperature was lower than 1,500° C., the melting was not performed sufficiently and the spherical particles were not obtained. When the heating temperature exceeded 3,200° C., the volatilization of the raw materials occurred, and there were obtained only the particles in spherical shape each having a small particle diameter.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 2 mm was obtained.
  • the preliminary molded body was sintered at a temperature range of 1,100° C. or higher and 1,500° C. or lower shown in the table below under a vacuum of 10 ⁇ 1 Pa or lower. Incidentally, the time taken for sintering was set to 6 hours or more and 24 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain an optical element having a thickness of 1 mm as shown in the FIGURE.
  • Table 1 shows the measurement results of the refractive index and the Abbe number of the obtained optical element.
  • the Abbe number is a value which represents the dispersibility.
  • Each optical element had optical properties of high refractive index and low dispersibility. Furthermore, when the surface thereof was observed with an optical microscope, detachment of surface particles or a flaw on the surface caused in the polishing step was absent, and hence, the satisfactory optical element was obtained.
  • the refractive index is represented by a value (nd) determined by measuring a refractive index at a wavelength of 587 nm using a Pulfrich refractometer (trade name “KPR-2000”; manufactured by Shimadzu Device Corporation).
  • La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% or more were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 1 to 9 in Table 1, and the oxide raw materials were mixed.
  • the raw materials were introduced into thermal plasma, and were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, and as a result, spherical particles having an average particle diameter of 3 ⁇ m were obtained.
  • the heating temperature was set at 1,500° C. or higher and 3,000° C. or lower. When the heating temperature was lower than 1,500° C., the melting was not performed sufficiently and the spherical particles were not obtained. When the heating temperature exceeded 3,000° C., the volatilization of the raw materials occurred, and there were obtained only the particles in spherical shape each having a small particle diameter.
  • the spherical particles were sintered by dry molding under a vacuum in the same manner as in Example 1, and the obtained sintered body was ground and polished, to thereby obtain a sample having a thickness of 1 mm.
  • the refractive index and the Abbe number of the obtained optical element were optically measured.
  • the results were the same as those shown in Table 1, and the optical element had optical properties of a high refractive index and a low dispersibility. Furthermore, when the surface thereof was observed with an optical microscope, detachment of surface particles or a flaw on the surface caused in the polishing step was absent, and hence, the satisfactory optical element was obtained.
  • La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% or more were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 1 to 9 in Table 1, and the oxide raw materials were mixed.
  • the raw materials were introduced into thermal plasma, and were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, and as a result, spherical particles having an average particle diameter of 10 ⁇ m were obtained.
  • the heating temperature was set at 1,500° C. or higher and 3,000° C. or lower. When the heating temperature was lower than 1,500° C., the melting was not performed sufficiently and the spherical particles were not obtained. When the heating temperature exceeded 3,000° C., the volatilization of the raw materials occurred, and there were obtained only the particles in spherical shape each having a small particle diameter.
  • the spherical particles were sintered by dry molding under a vacuum in the same manner as in Example 1, and the obtained sintered body was ground and polished, to thereby obtain a sample having a thickness of 1 mm.
  • the refractive index and the Abbe number of the obtained optical element were optically measured.
  • the results were the same as those shown in Table 1, and the optical element had optical properties of a high refractive index and a low dispersibility. Furthermore, when the surface thereof was observed with an optical microscope, detachment of surface particles or a flaw on the surface caused in the polishing step was absent, and hence, the satisfactory optical element was obtained.
  • La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% or more were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed the compounds shown in Sample Nos. 1 to 8 in Table 1, and the oxide raw materials were mixed.
  • the raw materials were introduced into thermal plasma, and were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, and as a result, spherical particles having an average particle diameter of 0.1 ⁇ m were obtained.
  • the heating temperature was set at 3,500° C. or higher.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 2 mm was obtained.
  • the preliminary molded body was sintered at a temperature range of 1,100° C. or higher and 1,500° C. or lower shown in the table below under a vacuum of 10 ⁇ 1 Pa or lower. Incidentally, the time taken for sintering was set to 6 hours or more and 24 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain a sample having a thickness of 1 mm.
  • the obtained optical element was observed with an optical microscope, there were a large number of bubbles formed in the element, and hence, the obtained optical element was unsuitable to be used as an optical element.
  • La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% or more were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed the compounds shown in Sample Nos. 1 to 7 in Table 1, and the oxide raw materials were mixed.
  • the raw materials were introduced into thermal plasma, and were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, and as a result, spherical particles having an average particle diameter of 100 ⁇ m were obtained.
  • the heating temperature was set at 1,500° C. or higher and 3,200° C. or lower.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 2 mm was obtained.
  • the preliminary molded body was sintered at a temperature range of 1,100° C. or higher and 1,500° C. or lower shown in the table below under a vacuum of 10 ⁇ 1 Pa or lower. Incidentally, the time taken for sintering was set to 6 hours or more and 24 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain a sample having a thickness of 1 mm.
  • the obtained optical element was observed with an optical microscope, there were a large number of detachments of surface particles and flaws on the surface caused in the polishing step, and hence, the obtained optical element was unsuitable to be used as an optical element.
  • An optical element according to Example 2 of the present invention is formed by vacuum-sintering a molded body of particles each having a two-layer structure, the particles being formed by coating surfaces of ceramic particles having an average particle diameter of 1 ⁇ m or more and 10 ⁇ m or less and including Ln x Al y O [x+y] ⁇ 1.5 (Ln represents a rare-earth element, x represents 1 ⁇ x ⁇ 10, and y represents 1 ⁇ y ⁇ 5) with a coating layer including a ceramic having a lower sintering temperature than a sintering temperature of the ceramic particles.
  • the optical element according to Example 2 of the present invention has a feature in that there are used the particles each having a two-layer structure formed by coating the surfaces of ceramic particles with a layer formed of a ceramic having a lower sintering temperature than a sintering temperature of the ceramic particles.
  • the ceramic particles used here are the same as the ceramic particles used for the first optical element.
  • the ceramic having a lower sintering temperature than a sintering temperature of the ceramic particles be crystal or glass.
  • the particles having the two-layer structure have spherical shapes. Furthermore, it is preferred that the coating layer which coats the layer formed of a ceramic having a lower sintering temperature than the sintering temperature of the ceramic particles have a thickness of 0.1 ⁇ m or more and 1 ⁇ m or less. Furthermore, as a method of forming the coating layer on the surface of the ceramic particles, a plasma melting method is employed.
  • a method of producing the optical element of the present invention is as follows. First, spherical ceramic particles having an average particle diameter of 1 ⁇ m or more and 10 ⁇ m or less are prepared by a method such as plasma melting. Next, the spherical ceramic particles are subjected to casting, dry molding, or wet molding to thereby prepare a preliminary molded body.
  • particles each having a two-layer structure and a spherical shape in which the surfaces of the spherical ceramic particles having an average particle diameter of 1 ⁇ m or more and 10 ⁇ m or less is coated with a coating layer, are prepared by a method such as plasma melting. Still further, the particles each having a two-layer structure are subjected to casting, dry molding, or wet molding to thereby prepare a preliminary molded body.
  • the preliminary molded body is sintered under a vacuum, followed by grinding and polishing steps, and as a result, an optical element such as an optical lens is obtained.
  • the vacuum-sintering method used here is the same as the vacuum-sintering method used for the first optical element.
  • Y 2 O 3 , La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 11 to 19 in Table 2, and the oxide raw materials were mixed.
  • the raw materials were introduced into a central part of thermal plasma, and a 1:1 mixture of Gd 2 O 3 and Al 2 O 3 was introduced into a peripheral part thereof, and simultaneously, they were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, to thereby obtain spherical particles having an average particle diameter of 1 ⁇ m and an average thickness of GdAlO 3 as a coating layer of 0.1 ⁇ m.
  • the heating temperature was set to 1,500° C. or higher and 3,200° C. or lower. When the heating temperature was lower than 1,500° C., the melting was not performed sufficiently and the spherical particles were not obtained. When the heating temperature exceeded 3,200° C., the volatilization of the raw materials occurred, and there were obtained only the particles in spherical shape each having a small particle diameter.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 2 mm was obtained.
  • the preliminary molded body was sintered at 1,100° C. under a vacuum of 10 ⁇ 1 Pa or lower.
  • the sintering temperature was 1,100° C. and the time taken for sintering was set to 6 hours or more and 24 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain an optical element having a thickness of 1 mm.
  • Table 2 shows the measurement results of the refractive index and the Abbe number of the obtained optical element.
  • Each optical element had optical properties of a high refractive index and a low dispersibility. Furthermore, when the surface thereof was observed with an optical microscope, detachment of surface particles or a flaw on the surface caused in the polishing step was absent, and hence, the satisfactory optical element was obtained.
  • the sintering temperatures of the samples shown in the above table are all 1,100° C.
  • Y 2 O 3 , La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 11 to 19 in Table 2, and the oxide raw materials were mixed.
  • the raw materials were introduced into a central part of thermal plasma, and a 1:1 mixture of Gd 2 O 3 and Al 2 O 3 was introduced into a peripheral part thereof, and simultaneously, they were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, to thereby obtain spherical particles having an average particle diameter of 3 ⁇ m and an average thickness of GdAlO 3 as a coating layer of 0.3 ⁇ m.
  • the heating temperature was set to 1,500° C. or higher and 3,000° C. or lower. When the heating temperature was lower than 1,500° C., the melting was not performed sufficiently and the spherical particles were not obtained. When the heating temperature exceeded 3,000° C., the volatilization of the raw materials occurred, and there were obtained only the particles in spherical shapes each having a small particle diameter.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 2 mm was obtained.
  • the preliminary molded body was sintered at 1,100° C. under a vacuum of 10 ⁇ 1 Pa or lower. Incidentally, the time taken for sintering was set to 6 hours or more and 24 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain an optical element having a thickness of 1 mm.
  • the refractive index and the Abbe number of the obtained optical element were optically measured, and, in the same manner as the results shown in Table 2, the optical element had optical properties of a high refractive index and a low dispersibility. Furthermore, when the surface thereof was observed with an optical microscope, detachment of surface particles or a flaw on the surface caused in the polishing step was absent, and hence, the satisfactory optical element was obtained.
  • Y 2 O 3 , La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 11 to 19 in Table 2, and the oxide raw materials were mixed.
  • the raw materials were introduced into a central part of thermal plasma, and a 1:1 mixture of Gd 2 O 3 and Al 2 O 3 was introduced into a peripheral part thereof, and simultaneously, they were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, to thereby obtain spherical particles having an average particle diameter of 10 ⁇ m and an average thickness of GdAlO 3 as a coating layer of 1 ⁇ m.
  • the heating temperature was set to 1,500° C. or higher and 3,000° C. or lower. When the heating temperature was lower than 1,500° C., the melting was not performed sufficiently and the spherical particles were not obtained. When the heating temperature exceeded 3,000° C., the volatilization of the raw materials occurred, and there were obtained only the particles in spherical shapes each having a small particle diameter.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 2 mm was obtained.
  • the preliminary molded body was sintered at 1,100° C. under a vacuum of 10 ⁇ 1 Pa or lower. Incidentally, the time taken for sintering was set to 6 hours or more and 24 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain an optical element having a thickness of 1 mm.
  • the refractive index and the Abbe number of the obtained optical element were optically measured, and, in the same manner as the results shown in Table 2, the optical element had optical properties of a high refractive index and a low dispersibility. Furthermore, when the surface thereof was observed with an optical microscope, detachment of surface particles or a flaw on the surface caused in the polishing process was absent, and hence, the satisfactory optical element was obtained.
  • Y 2 O 3 , La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 11 to 19 in Table 2, and the oxide raw materials were mixed.
  • a glass having a composition as shown in Table 3 and properties as shown in Table 4 was prepared as a coating layer.
  • the raw materials were introduced into a central part of thermal plasma, and the glass having the composition as shown in Table 3 and the properties as shown in Table 4 was introduced into a peripheral part, and simultaneously, they were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, to thereby obtain spherical particles having an average particle diameter of 10 ⁇ m and an average thickness of the glass as a coating layer of 1 ⁇ m.
  • the heating temperature was set to 1,500° C. or higher and 3,000° C. or lower. When the heating temperature was lower than 1,500° C., the melting was not performed sufficiently and the spherical particles were not obtained.
  • the heating temperature exceeded 3,000° C., the volatilization of the raw materials occurred, and there were obtained only the particles in spherical shape each having a small particle diameter.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 5 mm was obtained.
  • the preliminary molded body was sintered at a temperature of 750° C. or higher under a vacuum of 10 ⁇ 1 Pa or lower.
  • the time taken for sintering was set to 1 hour or more and 4 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain a sample having a thickness of 3 mm.
  • the refractive index and the Abbe number of the obtained optical element were optically measured, and, in the same manner as the results shown in Table 2, the optical element had optical properties of a high refractive index and a low dispersibility. Furthermore, when the surface thereof was observed with an optical microscope, detachment of surface particles or a flaw on the surface caused in the polishing step was absent, and hence, the satisfactory optical element was obtained.
  • the sintering temperature of each of the two-layered particles could be lowered to 750° C.
  • Y 2 O 3 , La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% or more were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 11 to 19 in Table 2, and the oxide raw materials were mixed.
  • the raw materials were introduced into a central part of thermal plasma, and a 1:1 mixture of Gd 2 O 3 and Al 2 O 3 was introduced into a peripheral part, and simultaneously, they were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, to thereby obtain spherical particles having an average particle diameter of 0.1 ⁇ m and an average thickness of GdAlO 3 as a coating layer of 0.01 ⁇ m.
  • the heating temperature was set to 3,500° C. or higher.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 2 mm was obtained.
  • the preliminary molded body was sintered at a temperature ranging from 1,100° C. or higher to 1,500° C. or lower shown in the table below under a vacuum of 10 ⁇ 1 Pa or lower. Incidentally, the time taken for sintering was set to 6 hours or more and 24 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain a sample having a thickness of 1 mm.
  • the obtained optical element was observed with an optical microscope, there were a large number of bubbles formed in the element, and hence, the obtained optical element was unsuitable to be used as an optical element.
  • Y 2 O 3 , La 2 O 3 , Gd 2 O 3 , Yb 2 O 3 , Lu 2 O 3 , and Al 2 O 3 which were oxide raw materials each having a purity of 99.9% or more were prepared.
  • the raw materials were each adjusted to have a proportion in such a manner that there can be formed ceramic particles having the compounds shown in Sample Nos. 11 to 19 in Table 2, and the oxide raw materials were mixed.
  • the raw materials were introduced into a central part of thermal plasma, and the glass having the composition as shown in Table 3 and the properties as shown in Table 4 was introduced into a peripheral part, and simultaneously, they were heated and melted, followed by cooling, by a thermal plasma method for obtaining fine particles, to thereby obtain spherical particles having an average particle diameter of 100 ⁇ m and an average thickness of the glass as a coating layer of 10 ⁇ m.
  • the spherical particles were subjected to dry molding under a pressure of 9,800,000 Pa (100 kgf) to 196,000,000 Pa (2,000 kgf), and as a result, a preliminary molded body having a diameter of 20 mm and a thickness of 5 mm was obtained.
  • the preliminary molded body was sintered at a temperature of 750° C. or higher under a vacuum of 10 ⁇ 1 Pa or lower.
  • the time taken for sintering was set to 1 hour or more and 4 hours or less.
  • the obtained sintered body was ground and polished, to thereby obtain a sample having a thickness of 3 mm.
  • the surface of the obtained optical element was observed with an optical microscope, there were a large number of detachments of surface particles and flaws on the surface caused in the polishing step, and hence, the obtained optical element was unsuitable to be used as an optical element.
  • the thickness of the coating layer was one tenth of the diameter of the particle and the cross-sectional area ratio was 1:100, and hence, the optical physical properties of the obtained optical element were approximately equal to those of the central ceramic.
  • the present invention is not limited to the above examples.
  • a composite oxide such as La 3 Al 5 O 12
  • oxides there may be also used carbonates and nitrates.
  • the production of the preliminary molded body can be also performed by casting or wet molding. In the production, a small amount of an organic binder may be added thereto.
  • rare-earth elements in addition to Y, La, Gd, Yb, and Lu, there can also be used Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, and Tm.
  • hot isostatic pressing can be performed to thereby shorten the time taken for heating to 3 to 24 hours.
  • a preliminary molded body and a sintered body each having a diameter of 20 mm or more and a thickness of mm or more can be also produced. Furthermore, there could be produced a preliminary molded body and a sintered body each having a size of a diameter of 20 mm or more and a thickness of 5 mm or more.
  • a coating layer there can be also used glass having a composition other than that of the examples of the present invention.

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US9040439B2 (en) 2013-03-08 2015-05-26 Canon Kabushiki Kaisha Optical glass, optical element, and method for manufacturing optical glass

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KR102840132B1 (ko) * 2022-03-11 2025-07-30 나노아이텍(주) 플라즈마 가열 방식의 유리 렌즈 가공 방법

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