WO2012077599A1 - 光変換用セラミック複合体及びその製造方法 - Google Patents
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- WO2012077599A1 WO2012077599A1 PCT/JP2011/077918 JP2011077918W WO2012077599A1 WO 2012077599 A1 WO2012077599 A1 WO 2012077599A1 JP 2011077918 W JP2011077918 W JP 2011077918W WO 2012077599 A1 WO2012077599 A1 WO 2012077599A1
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- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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- H01L33/50—Wavelength conversion elements
Definitions
- the present invention relates to a ceramic composite for light conversion used for a light emitting diode used for a display, illumination, backlight light source, and the like, and a method for producing the same.
- white light emitting devices using a blue light emitting element as a light source have been actively conducted.
- white light-emitting devices using blue light-emitting elements have a long life span and not only consume less power than incandescent and fluorescent lamps, but also do not use harmful substances such as mercury.
- the used lighting equipment is being put into practical use.
- the most common method for obtaining white light using blue light from a blue light emitting element as a light source is to obtain a pseudo white color by mixing yellow having a complementary color relationship with blue.
- a blue light emitting element is sealed with a transparent resin containing a phosphor that emits yellow light (for example, a YAG (Y 3 Al 5 O 12 ) phosphor).
- Blue light (wavelength 450 to 460 nm) is emitted from the blue light emitting element, and the YAG phosphor is excited by a part of the blue light, and yellow light is emitted from the phosphor.
- a white light emitting device which is configured by using a ceramic composite for light conversion composed of a solidified body formed continuously and three-dimensionally intertwined with each other and a blue light emitting element.
- the ceramic composite for light conversion can stably obtain homogeneous yellow fluorescence because the phosphor phase is uniformly distributed, and it is excellent in durability because it is a ceramic, and occurs when encapsulated with an epoxy resin or the like. It is possible to solve the problem and provide a highly reliable white light emitting device.
- the configuration of the white light emitting device using the ceramic composite for light conversion is, for example, a circuit board on which a blue light emitting element that is flip-chip mounted and a wiring pattern that receives and supplies power to the blue light emitting element are formed. And a ceramic composite for light conversion directly bonded to the blue light emitting element.
- a single crystal layer capable of forming a light emitting diode element, and at least two oxide crystal phases selected from a single metal oxide and a composite metal oxide There has been proposed a substrate for a light emitting diode in which a ceramic composite layer for light conversion composed of a solidified body which is continuously and three-dimensionally entangled with each other is laminated.
- a ceramic composite layer for light conversion composed of a solidified body which is continuously and three-dimensionally entangled with each other is laminated.
- a method of directly joining at a high temperature and a method of interposing a very small amount of a low melting point material as a joining layer are shown.
- the bonding surface between the single crystal layer and the ceramic composite layer for light conversion is flat, not only the above method but also the surface activated bonding method can be used to directly bond the ceramic composite layer for light conversion and the single crystal layer. Therefore, it is important that the joint surface is flat.
- a polycrystalline body composed of a plurality of oxide crystal phases is composed of a large number of crystal grains having different crystal plane orientations, and the processing speed differs depending on the plane orientation in polishing processing. There is a problem that there is a limit.
- the present invention provides a ceramic composite for light conversion having a flat surface even if it is a solidified body in which a plurality of oxide crystal phases are continuously and three-dimensionally entangled with each other, and its production It aims to provide a method.
- the present inventors have conducted extensive studies, and as a result, the surface of a solidified body having a structure in which an Al 2 O 3 phase and an oxide crystal phase are continuously and three-dimensionally entangled with each other.
- the surface of the solidified body comprising the Al 2 O 3 phase and the oxide crystal phase other than Al 2 O 3 is flattened by adjusting the pH of the polishing liquid to 11 to 12 and performing CMP (Chemical Mechanical Polishing). Specifically, it was found that the step can be formed to 0.010 ⁇ m or less.
- the present invention includes a polishing step of performing CMP on the surface of a solidified body having a structure in which an Al 2 O 3 phase and an oxide crystal phase other than Al 2 O 3 are continuously and three-dimensionally entangled with each other.
- the present invention also comprises a solidified body having a structure in which oxide crystal phases other than Al 2 O 3 phase and Al 2 O 3 are continuously and three-dimensionally entangled with each other, and Al on the surface of the solidified body A ceramic composite for light conversion in which a step between the 2 O 3 phase and the oxide crystal phase is 0.010 ⁇ m or less.
- the surface thereof has a flat surface.
- a composite and a method for producing the same can be provided.
- FIG. 1 is a perspective view showing a surface shape of a ceramic composite for light conversion according to Example 1.
- FIG. 6 is a perspective view showing a surface shape of a ceramic composite for light conversion according to Example 2.
- FIG. 6 is a perspective view showing a surface shape of a ceramic composite for light conversion according to Example 3.
- FIG. 10 is a graph showing a pH state during CMP processing of the ceramic composite for light conversion according to Example 5.
- FIG. 6 is a perspective view showing a surface shape of a ceramic composite for light conversion according to Comparative Example 1.
- FIG. 6 is a perspective view showing a surface shape of a ceramic composite for light conversion according to Comparative Example 2.
- FIG. 10 is a perspective view showing a surface shape of a ceramic composite for light conversion according to Comparative Example 3.
- a ceramic composite for light conversion and a method for producing the same according to the present invention will be described.
- the polishing rate of the oxide crystal phase can be controlled, whereby the step difference between the surfaces of the Al 2 O 3 phase and the oxide crystal phase other than Al 2 O 3 can be made 0.010 ⁇ m or less.
- the step difference between the surfaces of the Al 2 O 3 phase and the oxide crystal phase other than Al 2 O 3 can be made 0.010 ⁇ m or less.
- the Al 2 O 3 phase on the surface of the solidified body constituting the ceramic composite for light conversion and the oxide crystal phase other than Al 2 O 3 The inter-phase step is parallel to the surface to be processed, two points of an arbitrary point on the surface of one crystal phase constituting the convex shape and an arbitrary point on the surface of the other crystal phase constituting the concave shape. Using an arbitrary plane as a reference plane, the height of the two points is obtained, and the absolute value of the difference between the two heights is obtained.
- an arbitrary point on the surface of the crystal phase constituting such a convex shape and an arbitrary point on the surface of the crystal phase constituting the concave shape constitute a concave shape with the crystal phase constituting the convex shape.
- the points close to each other across the interface of the crystal phase to be used are preferable.
- twelve measurement points including two points are set, and the step difference between the phases is an average value of the measurement results. . Therefore, the step difference between the Al 2 O 3 phase and the oxide crystal phase other than Al 2 O 3 is 0.010 ⁇ m or less means that the measurement result of the step difference between the individual 12 points in the above method is used. It means that the average value is 0.010 ⁇ m or less.
- the polishing liquid used is adjusted to a slurry and preferably contains silica particles, and the content thereof is 0.1 to 5% by mass. Is preferably less than 0.4, more preferably 0.4 to 4% by mass.
- the polishing rate may be lowered.
- the polishing rate is improved, but the Al 2 O 3 phase.
- the step difference between the oxide crystal phases other than Al 2 O 3 increases.
- the polishing liquid used is obtained, for example, by adjusting the pH by adding an alkaline solution such as sodium hydroxide to a commercially available CMP polishing liquid.
- an alkaline solution such as sodium hydroxide
- CMP polishing liquid for example, "COMPOL (registered trademark) Type 20", "COMPOL (registered trademark) Type 50", “COMPOL (registered trademark) Type 80" of colloidal silica polishing slurry manufactured by Fujimi Incorporated, “COMPOL (registered trademark) Type 120”, “Quortron (registered trademark) PL series” of colloidal silica polishing slurry manufactured by Fuso Chemical Industry Co., Ltd., and the like can be used.
- These slurries are diluted with pure water as necessary to adjust the content of silica particles, and the pH is adjusted by adding an alkaline solution to obtain a polishing liquid used in the present invention. be able to.
- the pH of the polishing liquid may be lowered during CMP, so that it may fall within the range of 11 to 12 by adding an alkaline solution as needed. adjust.
- the pH of the polishing liquid during CMP is adjusted to 11 to 12, and more preferably to 11.3 to 11.6.
- the pH of this polishing liquid is set based on the stability of the polishing liquid, in addition to the above-described step difference between the Al 2 O 3 phase in which CMP is performed and the oxide crystal phase other than Al 2 O 3 .
- the pH of the polishing liquid exceeds 12, problems such as agglomeration of silica particles in the polishing liquid occur, and it is difficult to stably supply the polishing liquid.
- the pH of the polishing liquid is less than 11, it becomes difficult to eliminate the inter-step difference between the Al 2 O 3 phase and the oxide crystal phase other than Al 2 O 3 .
- CMP can be performed using any polishing apparatus.
- CMP is performed by attaching a solidified body, which is a complex oxide, to a rotary polishing head, and a solidified body attached to a polishing head rotating at about 50 rpm (rotation / minute) is applied to a polishing pad rotating at about 50 rpm.
- CMP can be performed by pressing.
- the unit load of CMP is preferably 5 to 50 kPa, and more preferably 10 to 33 kPa. If the unit load of CMP is less than 5 kPa, the polishing rate will be low, and if it exceeds 50 kPa, the polishing liquid will not easily enter between the surface to be polished and the polishing pad, resulting in a low polishing rate or a cause of polishing scratches. So it is not practical.
- the solidified solidified body is processed to a predetermined thickness, and the surface is polished in advance, such as mirror polishing, and then subjected to CMP. It is preferable to do so.
- This mirror polishing is performed by mechanical polishing (MP) or the like.
- the solidified body used in the method for producing a ceramic composite for light conversion according to the present invention is produced by melting and solidifying a raw material oxide.
- a solidified body by a simple method of cooling and condensing a melt charged in a crucible held at a predetermined temperature while controlling the cooling temperature.
- it is produced by a unidirectional solidification method. Is. This is because the unidirectional solidification causes the contained crystal phase to continuously grow in a single crystal state, thereby reducing the attenuation of light within the member.
- Such a solidified body except that it contains an oxide crystal phase that emits fluorescence, is disclosed in Japanese Patent Application Laid-Open Nos. 7-149597, 7-187893, and JP-A-8-81257, JP-A-8-253389, JP-A-8-253390, JP-A-9-67194, and corresponding US applications (US Pat. Nos. 5,569,547 and 5). , 484, 752, and 5,902, 963) can be used, and those that can be manufactured by the manufacturing method disclosed in these applications (patents) can be used. Can be used.
- the oxide crystal phase other than the Al 2 O 3 contains a YAG: Ce phase that emits fluorescence, or Ce and Gd.
- the YAG phase (hereinafter referred to as YAG: Gd, Ce phase) is preferable.
- the YAG: Ce phase or the YAG: Gd Ce phase has higher alkali resistance than the Al 2 O 3 phase
- a polishing liquid having a pH adjusted to 11 to 12 the Al
- the polishing rate of the 2 O 3 phase and the YAG: Ce phase or the YAG: Gd Ce phase can be controlled.
- the step difference between the Al 2 O 3 phase and the YAG: Ce phase or the YAG: Gd Ce phase is 0.010 ⁇ m or less. Can be.
- the oxide crystal phase other than Al 2 O 3 is a YAG: Ce phase or a YAG: Gd, Ce phase
- the Al 2 O 3 phase Transmits part of blue light
- the oxide crystal phase other than Al 2 O 3 absorbs part of blue light and emits yellow fluorescence, whereby the blue light and yellow light are mixed to emit white light.
- the oxide crystal phase other than Al 2 O 3 is a fluorescent substance that emits fluorescence
- the ceramic composite for light conversion in which YAG: Ce phase or YAG: Gd, Ce phase is known, and the present applicant It is disclosed in WO 2008-041566 and the like filed earlier.
- YAG: Ce phase is purple to blue excitation light of 400 - 500 nm, emit fluorescence having a peak wavelength of 530 ⁇ 560nm, YAG: Gd, Ce phase, since it emits fluorescence having a peak wavelength of 540 ⁇ 580 nm, Al 2 O
- the solidified body in which the oxide crystal phase other than 3 is a YAG: Ce phase or a YAG: Gd, Ce phase is used for light conversion for a white light emitting device used in combination with a light emitting element of blue light or violet light. It is suitable as a member.
- each phase of the solidified body does not have a boundary layer such as amorphous, and the oxide crystal phases are in direct contact with each other. For this reason, there is little loss of light in the ceramic composite for light conversion, and the light transmittance is also high.
- the oxide crystal phases that emit fluorescence fluorescent phases
- the oxide crystal phases are distributed uniformly in the ceramic composite for light conversion as a whole. , Homogeneous fluorescence without partial bias can be obtained.
- fluorescence from the phosphor phase and transmitted light from the transmitted light phase can be obtained simultaneously.
- the excitation light can be efficiently incident on the ceramic composite for light conversion, and strong white light can be obtained. . Therefore, by applying a very smooth joint surface between the ceramic composite for light conversion and the blue light emitting element, for example, direct bonding between the ceramic composite for light conversion and the blue light emitting element is applied by a surface activated bonding method or the like. can do.
- the solidified body is entirely composed of an inorganic oxide ceramic, it has excellent heat resistance and durability, and is not deteriorated by light. Therefore, it is possible to provide a ceramic composite for light conversion suitable for constituting a highly reliable white light emitting device with high reliability in combination with a blue light emitting element.
- the ceramic composite for light conversion according to the present invention comprises a solidified body having a structure in which an Al 2 O 3 phase and an oxide crystal phase other than Al 2 O 3 are continuously and three-dimensionally entangled with each other.
- the step difference between the Al 2 O 3 phase and the oxide crystal phase other than Al 2 O 3 is 0.010 ⁇ m or less.
- the oxide crystal phases other than the Al 2 O 3 phase and Al 2 O 3 have a structure in which they are continuously and three-dimensionally entangled with each other, and the oxides other than the Al 2 O 3 phase and the Al 2 O 3 as a whole
- the crystal phase is uniformly distributed in the ceramic composite for light conversion.
- the surface of the ceramic composite for light conversion is composed of an Al 2 O 3 phase and an oxide crystal phase other than Al 2 O 3 , and is composed of an Al 2 O 3 phase and an oxide crystal phase other than Al 2 O 3 . It is preferable to form an extremely flat surface having a step difference of 0.010 ⁇ m or less. Such a step adjustment can be performed by appropriately changing the content, the pH of the CMP polishing liquid, the unit load of CMP, and the like, in which the above-described CMP polishing liquid contains silica particles.
- FIG. 1 shows a schematic cross-sectional view of a light-emitting device using a ceramic composite for light conversion produced by the method for producing a ceramic composite for light conversion according to the present invention.
- This light emitting device comprises a light emitting element 2 that emits light having a peak at a wavelength of 400 to 500 nm, and a ceramic composite 1 for light conversion including an oxide crystal phase that emits yellow fluorescence having a peak at a wavelength of 550 to 560 nm.
- the phosphor contained in the ceramic composite 1 for light conversion is irradiated with the light emitted from the light-emitting ceramic composite 1 and the light transmitted through the ceramic composite 1 for light conversion and the light emitted from the light-emitting element 2 are emitted. It is characterized by using fluorescence converted in wavelength by a phase.
- symbol 3 is a flip chip electrode terminal
- symbol 4 is an anode electrode
- symbol 5 is a cathode electrode.
- a light emitting element that emits light having a peak at a wavelength of 400 to 500 nm is an element that emits violet to blue light.
- violet to blue light emitted from a light emitting diode element or an element that generates laser light is emitted at the wavelength.
- the light is incident on the ceramic composite for light conversion whose chromaticity is adjusted so that white is obtained. Due to the structure in which the yellow fluorescence from the phosphor phase excited thereby and the violet to blue transmitted light from the non-phosphor phase are uniformly entangled with each other in a continuous and three-dimensional manner. By mixing uniformly, white light with small color unevenness can be obtained.
- a white light emitting device in which a light emitting diode element is used as the light emitting element is referred to as a white light emitting diode.
- this raw material was directly charged into a molybdenum crucible and set in a unidirectional solidification apparatus, and the raw material was melted under a pressure of 1.33 ⁇ 10 ⁇ 3 Pa (10 ⁇ 5 Torr).
- the crucible is lowered at a rate of 5 mm / hour in the same atmosphere, and the Al 2 O 3 (sapphire) phase and the fluorescent oxide crystal phase (YAG phase) are continuously and three-dimensionally mutually.
- a solidified body having an intertwined tissue was obtained.
- FIG. 2 shows the surface of a solidified body used in this mirror-polished ceramic composite for light conversion. Solidified material used in the ceramic composite for light conversion is performed a general mirror-polished, the surface shape of the Al 2 O 3 phase from the difference of material properties becomes convex, emits Al 2 O 3 phase and fluorescence A surface having a phase difference of about 0.020 ⁇ m from the oxide crystal phase (YAG phase) is formed.
- Example 1 of the ceramic composite for light conversion according to the present invention will be described.
- a disk-like sample having a diameter of 2 inches and a thickness of 0.4 mm was cut out from the solidified body produced in the reference example.
- Discoid sample, a mirror surface state in advance by mirror polishing, the surface shape and the step level difference of the disc-shaped sample was subjected to shape measurement using an AFM (atomic force microscope), Al 2 O 3 phase And the oxide crystal phase (YAG phase) emitting fluorescence was 0.020 ⁇ m.
- This disk-shaped sample was subjected to CMP under the following conditions to obtain a ceramic composite for light conversion according to Example 1.
- the polishing liquid for CMP is 1 mol / mol in “COMPOL (registered trademark) Type 120” of colloidal silica polishing slurry manufactured by Fujimi Incorporated, diluted with pure water so that the content of silica particles is 0.4% by mass.
- L aqueous NaOH solution was added to adjust the pH to 11.5.
- this CMP polishing liquid is supplied to “IC1000 (registered trademark) polishing pad” manufactured by Nitta Haas Co., Ltd. having a grid-like groove interval of 15 mm, and the polishing pad is applied to the ceramic for light conversion at a unit load of 10 kPa.
- CMP was performed by pressing against the plate-like sample of the composite and setting the processing time to 150 minutes. During processing, a 1 mol / L NaOH aqueous solution was added as needed to adjust the pH of the CMP polishing liquid to be in the range of 11-12.
- Example 2 of the ceramic composite for light conversion according to the present invention will be described.
- a ceramic composite for light conversion according to Example 2 was produced in the same manner as in Example 1 except that the content of silica particles in the polishing liquid for CMP was 4% by mass and the processing time for CMP was 60 minutes.
- Example 3 of the ceramic composite for light conversion according to the present invention will be described.
- the same disk-shaped sample as Example 1 was cut out from the solidified body manufactured in the reference example.
- Discoid sample, a mirror surface state in advance by mirror polishing, the surface shape and the step level difference of the disc-shaped sample was subjected to shape measurement using an AFM (atomic force microscope), Al 2 O 3 phase And the oxide crystal phase (YAG phase) emitting fluorescence was 0.015 ⁇ m.
- a square plate sample having a square of 15 mm ⁇ 15 mm was cut out from the disk sample, and CMP was performed under the following conditions to obtain a ceramic composite for light conversion according to Example 3.
- the polishing liquid for CMP is 1 mol / mol in “Quartron (registered trademark) PL-2L” of colloidal silica polishing slurry manufactured by Fuso Chemical Industry Co., Ltd. diluted with pure water so that the content of silica particles is 2% by mass. L aqueous NaOH solution was added to adjust the pH to 11.5. Then, this CMP polishing liquid is supplied to “IC1000 (registered trademark) polishing pad” manufactured by Nitta Haas Co., Ltd. having a grid-like groove interval of 15 mm, and the polishing pad is applied to the ceramic for light conversion at a unit load of 10 kPa.
- CMP was performed by pressing against the plate-like sample of the composite and setting the processing time to 270 minutes. During processing, a 1 mol / L NaOH aqueous solution was added as needed to adjust the pH of the CMP polishing liquid to be in the range of 11-12.
- Example 4 of the ceramic composite for light conversion according to the present invention will be described.
- the same disk-shaped sample as Example 1 was cut out from the solidified body manufactured in the reference example.
- Discoid sample, a mirror surface state in advance by mirror polishing, the surface shape and the step level difference of the disc-shaped sample was subjected to shape measurement using an AFM (atomic force microscope), Al 2 O 3 phase And the oxide crystal phase (YAG phase) emitting fluorescence was 0.015 ⁇ m.
- This disc-shaped sample was subjected to CMP under the following conditions to obtain a ceramic composite for light conversion according to Example 4.
- the polishing liquid for CMP is 1 mol / mol in “Quartron (registered trademark) PL-2L” of colloidal silica polishing slurry manufactured by Fuso Chemical Industry Co., Ltd. diluted with pure water so that the silica particle content is 2% by mass. L aqueous NaOH solution was added to adjust the pH to 11.5. Then, this CMP polishing liquid is supplied to “IC1000 (registered trademark) polishing pad” manufactured by Nitta Haas Co., Ltd. having a grid-like groove interval of 15 mm, and the polishing pad is applied to the above-mentioned ceramic for light conversion at a unit load of 13 kPa.
- CMP was performed by pressing against the plate-like sample of the composite and setting the processing time to 270 minutes. During processing, a 1 mol / L NaOH aqueous solution was added as needed to adjust the pH of the CMP polishing liquid to be in the range of 11-12.
- Example 5 of the ceramic composite for light conversion according to the present invention will be described.
- a ceramic composite for light conversion according to Example 5 was produced in the same manner as in Example 4 except that the unit load of the polishing pad was 33 kPa and the CMP processing time was 180 minutes. Moreover, about Example 5, the state of pH during processing is shown in FIG.
- Example 6 of the ceramic composite for light conversion according to the present invention will be described.
- a ceramic composite for light conversion according to Example 6 was produced in the same manner as in Example 4 except that the unit load of the polishing pad was 50 kPa and the processing time of CMP was 120 minutes.
- Example 7 of the ceramic composite for light conversion according to the present invention will be described.
- a ceramic composite for light conversion according to Example 7 was produced in the same manner as in Example 4 except that the grid-like groove interval of the polishing pad was 7 mm, the unit load of the polishing pad was 33 kPa, and the CMP processing time was 90 minutes. .
- Comparative Example 1 As a comparison, a disk-like sample similar to Example 1 and Example 2 was cut out from the solidified body produced in the reference example, preliminarily made into a mirror surface state by mirror polishing, and light conversion according to Comparative Example 1 was performed as follows. A ceramic composite was obtained.
- a stock solution of COMPOL-120 (manufactured by Fujimi Incorporated) in which the content of silica particles in the polishing liquid for CMP is 40% by mass without being diluted with pure water is used as a polishing pad (IC-1000, lattice groove interval) 15 mm: supplied to Nitta Hass Co.), where the polishing pad, is pressed against the plate-like sample of the light converting ceramic composite for a unit load 10 kPa, CMP is performed for 60 minute processing time, Al 2
- the surface shape of the O 3 phase was convex, and the step difference between the Al 2 O 3 phase and the oxide crystal phase (YAG phase) emitting fluorescence was about 0.05 ⁇ m.
- Table 1 the surface shape of the ceramic composite for light conversion which concerns on the comparative example 1 is shown in FIG.
- Comparative Example 2 Next, as a comparison, a square plate-like sample similar to that in Example 3 was cut out from the solidified body manufactured in the reference example, and was previously made into a mirror state by mirror polishing, and the light conversion according to Comparative Example 2 was performed as follows. A ceramic composite was obtained.
- Comparative Example 3 For comparison, a rectangular plate-like sample similar to that of Example 3 was cut out from the solidified body manufactured in the reference example, and was preliminarily mirror-finished by mirror polishing.
- the light conversion ceramic according to Comparative Example 3 was as follows. A complex was obtained.
- PL-2L manufactured by Fuso Chemical Industry Co., Ltd.
- This CMP polishing liquid is supplied to a polishing pad (IC-1000, lattice groove interval 15 mm: manufactured by Nita Hass), and the polishing pad is pressed against the plate-shaped sample of the ceramic composite for light conversion at a unit load of 10 kPa.
- the CMP was performed by setting the processing time to 60 minutes, and the ceramic composite for light conversion according to Comparative Example 3 was obtained.
- Comparative Example 4 Next, as a comparison, Comparative Example 3 except that a disk-like sample similar to Example 4 was cut out from the solidified body produced in the reference example, the unit load of the polishing pad was 13 kPa, and the CMP processing time was 270 minutes. In the same manner, a ceramic composite for light conversion according to Comparative Example 4 was produced.
- the pH of the polishing slurry for CMP during processing is adjusted to 11 to 12, and the smaller the content of silica particles in the polishing slurry for CMP, the more the Al 2 O 3 phase and the oxide crystal phase that emits fluorescence (YAG The phase difference with the phase is small.
- a surface having a very small step difference between the Al 2 O 3 phase and the fluorescent oxide crystal phase (YAG phase) is obtained. Can be formed.
- the step difference between the Al 2 O 3 phase and the fluorescent oxide crystal phase (YAG phase) is caused by the fact that the alkaline CMP polishing liquid contains silica particles, the content thereof, and the pH of the CMP polishing liquid. Further, it can be eliminated by CMP controlled by the unit load of CMP and the interval between polishing pad grooves processed on the surface of the polishing pad.
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Abstract
Description
YAG:Ce相は、400~500nmの紫~青色励起光で、ピーク波長530~560nmの蛍光を発し、YAG:Gd,Ce相は、ピーク波長540~580nmの蛍光を発することから、Al2O3以外の前記酸化物結晶相が、YAG:Ce相またはYAG:Gd,Ce相である前記凝固体は、青色光または紫色光の発光素子と組み合わせて使用される白色発光装置用の光変換用部材として好適である。
先ず、実施例に用いられる凝固体を製造した。α-Al2O3粉末(純度99.99%)をAlO3/2換算で0.82モル、Y2O3粉末(純度99.9%)をYO3/2換算で0.175モル、CeO2粉末(純度99.9%)を0.005モルとなるよう秤量した。これらの粉末をエタノール中、ボールミルによって16時間湿式混合した後、エバポレーターを用いてエタノールを脱媒して原料粉末を得た。原料粉末は、真空炉中で予備溶解し一方向凝固の原料とした。次に、この原料をそのままモリブデンルツボに仕込み、一方向凝固装置にセットし、1.33×10-3Pa(10-5Torr)の圧力下で原料を融解した。次に同一の雰囲気においてルツボを5mm/時間の速度で下降させ、Al2O3(サファイア)相と、蛍光を発する酸化物結晶相(YAG相)とが連続的にかつ三次元的に相互に絡み合った組織を有する凝固体を得た。
次に、本発明に係る光変換用セラミック複合体の実施例1について説明する。先ず、参考例において製造された凝固体から直径2インチ、厚さ0.4mmの円板状試料を切り出した。円板状試料は、あらかじめ鏡面研磨加工により鏡面状態とし、前記円板状試料の表面形状及び相間段差を、AFM(原子間力顕微鏡)を用いて形状測定を行ったところ、Al2O3相と蛍光を発する酸化物結晶相(YAG相)との相間段差が0.020μmであった。この円板状試料について、下記の条件にてCMPを行い、実施例1に係る光変換用セラミック複合体を得た。CMP用研磨液は、シリカ粒子の含有量が、0.4質量%になるように純水で希釈した(株)フジミインコーポレーテッド製コロイダルシリカ研磨スラリーの「COMPOL(登録商標)Type120」に1mol/LのNaOH水溶液を添加し、pHが11.5になるように調整した。そして、このCMP用研磨液を、格子状溝間隔が15mmのニッタ・ハース(株)製「IC1000(登録商標)研磨パッド」に供給し、その研磨パッドを、単位荷重10kPaで前記光変換用セラミック複合体の板状試料に押し当てて、加工時間を150分間とすることでCMPを行った。加工中、1mol/LのNaOH水溶液を随時添加し、CMP用研磨液のpHが11~12の範囲内になるように調整した。
次に、本発明に係る光変換用セラミック複合体の実施例2について説明する。CMP用研磨液中のシリカ粒子の含有量を4質量%、CMPの加工時間を60分間とした以外は実施例1と同様にして実施例2に係る光変換用セラミック複合体を作製した。
次に、本発明に係る光変換用セラミック複合体の実施例3について説明する。先ず、参考例において製造された凝固体から実施例1と同様の円板状試料を切り出した。円板状試料は、あらかじめ鏡面研磨加工により鏡面状態とし、前記円板状試料の表面形状及び相間段差を、AFM(原子間力顕微鏡)を用いて形状測定を行ったところ、Al2O3相と蛍光を発する酸化物結晶相(YAG相)との相間段差が0.015μmであった。この円板状試料から正方形:15mm×15mmの四角板状試料を切り出し、下記の条件にてCMPを行い、実施例3に係る光変換用セラミック複合体を得た。CMP用研磨液は、シリカ粒子の含有量が、2質量%になるように純水で希釈した扶桑化学工業(株)製コロイダルシリカ研磨スラリーの「クォートロン(登録商標)PL-2L」に1mol/LのNaOH水溶液を添加し、pHを11.5になるように調整した。そして、このCMP用研磨液を、格子状溝間隔が15mmのニッタ・ハース(株)製「IC1000(登録商標)研磨パッド」に供給し、その研磨パッドを、単位荷重10kPaで前記光変換用セラミック複合体の板状試料に押し当てて、加工時間を270分間とすることでCMPを行った。加工中、1mol/LのNaOH水溶液を随時添加し、CMP用研磨液のpHが11~12の範囲内になるように調整した。
次に、本発明に係る光変換用セラミック複合体の実施例4について説明する。先ず、参考例において製造された凝固体から実施例1と同様の円板状試料を切り出した。円板状試料は、あらかじめ鏡面研磨加工により鏡面状態とし、前記円板状試料の表面形状及び相間段差を、AFM(原子間力顕微鏡)を用いて形状測定を行ったところ、Al2O3相と蛍光を発する酸化物結晶相(YAG相)との相間段差が0.015μmであった。この円板状試料について、下記の条件にてCMPを行い、実施例4に係る光変換用セラミック複合体を得た。CMP用研磨液は、シリカ粒子の含有量が、2質量%になるように純水で希釈した扶桑化学工業(株)製コロイダルシリカ研磨スラリーの「クォートロン(登録商標)PL-2L」に1mol/LのNaOH水溶液を添加し、pHを11.5になるように調整した。そして、このCMP用研磨液を、格子状溝間隔が15mmのニッタ・ハース(株)製「IC1000(登録商標)研磨パッド」に供給し、その研磨パッドを、単位荷重13kPaで前記光変換用セラミック複合体の板状試料に押し当てて、加工時間を270分間とすることでCMPを行った。加工中、1mol/LのNaOH水溶液を随時添加し、CMP用研磨液のpHが11~12の範囲内になるように調整した。
次に、本発明に係る光変換用セラミック複合体の実施例5について説明する。研磨パッドの単位荷重を33kPa、CMPの加工時間を180分間とした以外は実施例4と同様にして実施例5に係る光変換用セラミック複合体を作製した。また、実施例5について、加工中のpHの状態を図6に示す。
次に、本発明に係る光変換用セラミック複合体の実施例6について説明する。研磨パッドの単位荷重を50kPa、CMPの加工時間を120分間とした以外は実施例4と同様にして実施例6に係る光変換用セラミック複合体を作製した。
次に、本発明に係る光変換用セラミック複合体の実施例7について説明する。研磨パッドの格子状溝間隔を7mm、研磨パッドの単位荷重を33kPa、CMPの加工時間を90分間とした以外は実施例4と同様にして実施例7に係る光変換用セラミック複合体を作製した。
比較として、参考例において製造された凝固体から実施例1及び実施例2と同様の円板状試料を切り出し、あらかじめ鏡面研磨加工により鏡面状態とし、次のようにして比較例1に係る光変換用セラミック複合体を得た。
次に、比較として、参考例において製造された凝固体から実施例3と同様の四角板状試料を切り出し、あらかじめ鏡面研磨加工により鏡面状態とし、次のようにして比較例2に係る光変換用セラミック複合体を得た。
また、比較として、参考例において製造された凝固体から実施例3と同様の四角板状試料を切り出し、あらかじめ鏡面研磨加工により鏡面状態とし、次のようにして比較例3に係る光変換用セラミック複合体を得た。
次に、比較として、参考例において製造された凝固体から実施例4と同様の円板状試料を切り出し、研磨パッドの単位荷重を13kPa、CMPの加工時間を270分間とした以外は比較例3と同様にして比較例4に係る光変換用セラミック複合体を作製した。
次に、比較として、CMP用研磨液として、シリカ粒子の含有量が、0.4質量%になるように純水で希釈した(株)フジミインコーポレーテッド製コロイダルシリカ研磨スラリーの「COMPOL(登録商標)Type120」に1mol/LのNaOH水溶液を添加し、pHが12を超えるように調整した。その結果、研磨液中のシリカ粒子の凝集等の問題が発生した。
2 発光素子(発光ダイオード素子)
3 フリップチップ電極端子
4 アノード電極
5 カソード電極
Claims (6)
- Al2O3相及びAl2O3以外の酸化物結晶相が連続的にかつ三次元的に相互に絡み合った組織を有する凝固体の表面にCMPを行なう研磨工程を備え、
CMPを行なう際の研磨液のpHを11~12に調整していることを特徴とする光変換用セラミック複合体の製造方法。 - 前記酸化物結晶相が、蛍光を発する蛍光体であり、Ceを含有するYAG((Y、Ce)3Al5O12)相であることを特徴とする請求項1記載の光変換用セラミック複合体の製造方法。
- 前記研磨液のpHを11.3~11.6に調整していることを特徴とする請求項1又は2記載の光変換用セラミック複合体の製造方法。
- 前記研磨液がシリカ粒子を含有し、その含有量が0.1~5質量%未満であることを特徴とする請求項1乃至3いずれか記載の光変換用セラミック複合体の製造方法。
- 前記CMPの単位荷重が10~50kPaであることを特徴とする請求項1乃至4いずれか記載の光変換用セラミック複合体の製造方法。
- Al2O3相及びAl2O3以外の酸化物結晶相が連続的にかつ三次元的に相互に絡み合った組織を有する凝固体からなり、該凝固体の表面におけるAl2O3相及び前記酸化物結晶相の相間段差が0.010μm以下である光変換用セラミック複合体。
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JP2012547826A JP5370595B2 (ja) | 2010-12-10 | 2011-12-02 | 光変換用セラミック複合体及びその製造方法 |
US13/992,805 US9543480B2 (en) | 2010-12-10 | 2011-12-02 | Ceramic composite for light conversion and method for manufacture thereof |
EP11846090.6A EP2650082B1 (en) | 2010-12-10 | 2011-12-02 | Ceramic composite for photoconversion, and method for manufacture thereof |
CN201180058469.5A CN103260825B (zh) | 2010-12-10 | 2011-12-02 | 光转换用陶瓷复合体及其制造方法 |
KR1020137017758A KR20130103784A (ko) | 2010-12-10 | 2011-12-02 | 광변환용 세라믹 복합체 및 그 제조방법 |
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JP5370595B2 (ja) | 2013-12-18 |
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CN103260825B (zh) | 2016-05-04 |
EP2650082A1 (en) | 2013-10-16 |
JPWO2012077599A1 (ja) | 2014-05-19 |
EP2650082A4 (en) | 2018-01-03 |
CN103260825A (zh) | 2013-08-21 |
US9543480B2 (en) | 2017-01-10 |
TWI473872B (zh) | 2015-02-21 |
US20130327985A1 (en) | 2013-12-12 |
KR20130103784A (ko) | 2013-09-24 |
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