TWI606745B - Process for preparing transparent ceramic plates of phosphorescent - Google Patents

Process for preparing transparent ceramic plates of phosphorescent Download PDF

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TWI606745B
TWI606745B TW105138216A TW105138216A TWI606745B TW I606745 B TWI606745 B TW I606745B TW 105138216 A TW105138216 A TW 105138216A TW 105138216 A TW105138216 A TW 105138216A TW I606745 B TWI606745 B TW I606745B
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phosphorescent
ceramic plate
yag phosphor
present disclosure
transparent ceramic
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TW105138216A
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Chinese (zh)
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TW201735726A (en
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李相俊
鄭蒙權
金泳植
李性勳
孫源培
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曉星股份有限公司
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48Semiconductor devices with at least one potential-jump barrier or surface barrier 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
    • H01L33/50Wavelength conversion elements
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00Electroluminescent light sources
    • H05B33/02Details
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00Electroluminescent light sources
    • H05B33/10Apparatus or processes specially adapted to the manufacture of electroluminescent light sources

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Luminescent Compositions (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Led Device Packages (AREA)

Description

用於製備透明磷光性陶瓷板的製程 Process for preparing transparent phosphorescent ceramic plates

本發明有關於一種製備透明磷光性陶瓷板的方法,特別有關於簡單且能改善產率的一種製備透明磷光性陶瓷板的方法。 The present invention relates to a method of preparing a transparent phosphorescent ceramic plate, and more particularly to a method of preparing a transparent phosphorescent ceramic plate which is simple and can improve the yield.

本說明書中所用的名詞“LED”是發光二極體的縮寫,表示使用半導體之pn接合構造以製造小數量載子(電子或電洞)以被注入,且藉由再組合上述而發光的發光二極體。 The term "LED" as used in the specification is an abbreviation of a light-emitting diode, and means a pn junction structure using a semiconductor to fabricate a small number of carriers (electrons or holes) to be implanted, and to emit light by recombining the above. Diode.

本說明書中所用的名詞”LD”是雷射二極體的縮寫,表示以一半導體而製造的雷射二極體,係使用當大量載子被注入半導體、當電子和電洞再組合且釋放能量而得到的發光效應。 The term "LD" as used in this specification is an abbreviation for laser diode, which means a laser diode fabricated by a semiconductor, which is used when a large number of carriers are injected into a semiconductor, and when electrons and holes are recombined and released. The luminescence effect obtained by energy.

光學半導體設備,例如LED設備和LD發光設備,具有光學半導體裝置,例如LED裝置或LD裝置,以及一磷光層,設置於該光學半導體裝置上。此光學半導體設備由光學半導體裝置發光,例如,藉由通過磷光層的藍光以及在磷光中的一些藍光經過波長轉換而得到的黃光之有色混光,而發出白光。 Optical semiconductor devices, such as LED devices and LD illuminators, have optical semiconductor devices, such as LED devices or LD devices, and a phosphor layer disposed on the optical semiconductor device. The optical semiconductor device emits light by an optical semiconductor device, for example, by a colored mixed light of yellow light obtained by wavelength conversion of blue light of a phosphor layer and some blue light in phosphorescence.

光學半導體設備,以LED設備占優勢,其包括一LED封裝,其中LED係以一透明封裝材料封裝;以及一磷光帶,層疊在其上表面。此磷光帶具有一磷光層,以及丙烯酸系壓感性黏著層,層疊在其另外表面,且磷光層係經由黏著層而黏附於LED封裝的表面上。然而,磷光帶很容易變性,因為其溫度很容易因LED發光而變高,這會導致LED設備的亮度漸弱。因此,在一磷光黏著片中,磷光層由磷光性陶瓷而被形成為一磷光性陶瓷板。 Optical semiconductor devices, which are dominated by LED devices, include an LED package in which the LEDs are packaged in a transparent encapsulating material; and a phosphor strip laminated on the upper surface thereof. The phosphor ribbon has a phosphor layer, and an acrylic pressure-sensitive adhesive layer laminated on the other surface thereof, and the phosphor layer is adhered to the surface of the LED package via the adhesive layer. However, the phosphorescent tape is easily denatured because its temperature is easily increased by the LED light, which causes the brightness of the LED device to become weaker. Therefore, in a phosphorescent adhesive sheet, the phosphor layer is formed of a phosphorescent ceramic plate as a phosphorescent ceramic plate.

然而,現存的陶瓷板如第2圖所示而製備,製備由氧化釔、氧化鋁、和氧化石榴石(garnet oxide)顆粒所組成的原料粉末,將製得的原料粉末與水溶性黏著樹脂混合,對於所得的混合物另外加入蒸餾水以溼混合,然後將混合物燒結而製備一釔-鋁-石榴石(yttrium-aluminum-garnet)(以下稱”YAG”)前驅物,以烘箱乾燥此前驅物而形成一陶瓷綠片,然後在加熱且高溫的真空爐中加熱且燒結此陶瓷綠片的層板,而製得一磷光性的透明陶瓷板。然而,製造一最終板需花費長時間,而且產率是個問題。 However, the existing ceramic plate is prepared as shown in Fig. 2, and a raw material powder composed of cerium oxide, aluminum oxide, and garnet oxide particles is prepared, and the obtained raw material powder is mixed with a water-soluble adhesive resin. To the obtained mixture, distilled water was additionally added to wet-mix, and then the mixture was sintered to prepare a yttrium-aluminum-garnet (hereinafter referred to as "YAG") precursor, which was dried in an oven to form a precursor. A ceramic green sheet is then heated and sintered in a heated and high temperature vacuum furnace to produce a phosphorescent transparent ceramic plate. However, it takes a long time to manufacture a final sheet, and the yield is a problem.

基於上述,我們發現當使用現存固相方法而製備一透明陶瓷板時,在固相合成之後,磨碎YAG磷光物,製備方法簡單且產率得以改善,本揭露據此而完成。 Based on the above, we have found that when a transparent ceramic plate is prepared by using the existing solid phase method, the YAG phosphor is ground after the solid phase synthesis, the preparation method is simple and the yield is improved, and the present disclosure is completed accordingly.

依據本揭露之一實施例,一透明磷光性陶瓷板的製備為,將一小顆粒YAG磷光物磨碎至1μm或以下,然後製造(模製)成為一板,以及將所得物燒結。 According to an embodiment of the present disclosure, a transparent phosphorescent ceramic plate is prepared by grinding a small particle YAG phosphor to 1 μm or less, then manufacturing (molding) into a plate, and sintering the resultant.

本揭露的目的和品質,由以下實施例的說明以及所附圖示而明顯,其中圖示為:第1圖顯示依據本揭露製備透明陶瓷板的流程圖;第2圖顯示製備一現存透明陶瓷板的流程圖;第3圖顯示在磨碎之前使用粒徑分析儀所得之YAG粉末粒徑分佈數據;第4圖顯示在磨碎之後使用粒徑分析儀所得之YAG粉末粒徑分佈數據;以及第5圖為在不同銫濃度下,依據本揭露之透明陶瓷板和使用現存方法所製備的透明陶瓷板(第2圖)之間光譜的比較。 The object and quality of the present disclosure are apparent from the following description of the embodiments and the accompanying drawings, wherein: FIG. 1 is a flow chart showing the preparation of a transparent ceramic plate according to the present disclosure; and FIG. 2 is a view showing the preparation of an existing transparent ceramic. Flow chart of the plate; Figure 3 shows the YAG powder particle size distribution data obtained by using the particle size analyzer before grinding; Figure 4 shows the YAG powder particle size distribution data obtained by using the particle size analyzer after grinding; Figure 5 is a comparison of the spectra between a transparent ceramic plate according to the present disclosure and a transparent ceramic plate prepared using an existing method (Fig. 2) at different cerium concentrations.

以下,將詳細說明本揭露,以下的實施例或例子僅為說明之用,本揭露的範圍並不以此為限。 In the following, the disclosure will be described in detail, and the following examples or examples are for illustrative purposes only, and the scope of the disclosure is not limited thereto.

依據本揭露的一實施例,製備透明磷光性陶瓷板的方法包括,如第1圖所示,以研磨方式將一小顆粒YAG磷光物磨碎至1μm或以下;將該磨碎的YAG磷光物在一烘箱中乾燥;對於該乾燥的磨碎的YAG磷光物施加壓力而模製成一板;以及將該模製板燒結及後處理。 According to an embodiment of the present disclosure, a method of preparing a transparent phosphorescent ceramic plate includes, as shown in FIG. 1, grinding a small particle YAG phosphor to 1 μm or less by grinding; the ground YAG phosphor Drying in an oven; applying a pressure to the dried ground YAG phosphor to form a plate; and sintering and post-treating the molded plate.

依據本揭露,磨碎一YAG磷光物,較佳是使用一球磨機進行研磨。如果磷光物不被磨碎至1μm或以下,板的厚度會不均勻,這會導致當使用於高輸出發光二極體(LED)和雷射二極體(LD)中,無法確保穩定性和可靠度。第3圖顯示在磨碎之前使用一粒徑分析儀而得到的YAG粉末粒徑分佈數 據,第4圖顯示在磨碎之後使用一粒徑分析儀而得到的YAG粉末粒徑分佈數據。 In accordance with the present disclosure, a YAG phosphor is ground, preferably using a ball mill. If the phosphor is not ground to 1 μm or less, the thickness of the plate may be uneven, which may result in stability and reliability when used in high-output light-emitting diodes (LEDs) and laser diodes (LD). degree. Figure 3 shows the particle size distribution of YAG powder obtained by using a particle size analyzer before grinding. According to Fig. 4, the YAG powder particle size distribution data obtained by using a particle size analyzer after grinding is shown.

依據本揭露,將磨碎的YAG磷光物在一烘箱中的乾燥,較佳是在100℃ to 150℃的溫度範圍下進行1至24小時。 According to the present disclosure, the dried YAG phosphor is dried in an oven, preferably at a temperature ranging from 100 ° C to 150 ° C for 1 to 24 hours.

依據本揭露,施加壓力的模製,較佳是使用冷均壓(CIP)方法在1000Mpa至3000Mpa的壓力範圍下進行。 According to the present disclosure, the molding of the applied pressure is preferably carried out using a cold equalization (CIP) method at a pressure ranging from 1000 MPa to 3000 MPa.

依據本揭露,燒結較佳係在還原化環境(reducing environment)或在空氣中使用大氣爐(atmosphere furnace),在1400℃至1800℃的溫度範圍中進行8小時至15小時。 According to the present disclosure, the sintering is preferably carried out in a reducing environment or in an air atmosphere furnace in the temperature range of 1400 ° C to 1800 ° C for 8 hours to 15 hours.

依據本揭露,經燒結的透明陶瓷板的後處理,較佳係在一表面磨光製程中使用一自動磨光機(auto polishing machine)以磨光表面而進行。 According to the present disclosure, the post-treatment of the sintered transparent ceramic plate is preferably carried out by using an auto polishing machine to polish the surface in a surface polishing process.

當製造本揭露之透明陶瓷板時,銫較佳的使用量為0.01mol至0.03mol濃度以作為活化劑。以下表1係在不同活化劑濃度下,比較依據本揭露之透明陶瓷板和使用現存方法所製備的透明陶瓷板(第2圖)之間的輻射強度(1m)。依據表1可看出,使用本揭露之方法所製備之透明陶瓷板的輻射強度是相當優異的。 When the transparent ceramic plate of the present disclosure is produced, cerium is preferably used in an amount of from 0.01 mol to 0.03 mol as an activator. Table 1 below compares the radiant intensity (1 m) between a transparent ceramic plate according to the present disclosure and a transparent ceramic plate (Fig. 2) prepared using an existing method at different activator concentrations. As can be seen from Table 1, the radiant intensity of the transparent ceramic plate prepared by the method of the present disclosure is quite excellent.

第5圖為在不同銫濃度下,依據本揭露之透明陶瓷板和使用現存方法所製備的透明陶瓷板(第2圖)之間光譜的比較。 Figure 5 is a comparison of the spectra between a transparent ceramic plate according to the present disclosure and a transparent ceramic plate prepared using an existing method (Fig. 2) at different cerium concentrations.

本揭露製備透明磷光性陶瓷板的方法,可減少複雜的製程,由於精確的邊緣製備而有優異的均勻板厚度,達到低顏色分佈而仍能達到高顏色對比100:1或更高,減少熱顏色座標移動,具有優異的發光角度均勻性,在板裝設之前,經由磷光性質篩選而解決分級(binning)問題,而且當使用於高輸出發光二極體(LED)和雷射二極體(LD)時可有效確保穩定性和可靠度。 The method for preparing a transparent phosphorescent ceramic plate can reduce complicated processes, has excellent uniform plate thickness due to precise edge preparation, achieves low color distribution, and can achieve high color contrast of 100:1 or higher, and reduces heat. The color coordinates move, with excellent uniformity of illumination angle, solve the binning problem through phosphorescence screening before the board is installed, and when used in high output light-emitting diodes (LEDs) and laser diodes ( LD) ensures stability and reliability.

如上述,本揭露已參考實施例而做說明,然而,可理解的是,熟悉此技術人士可在不偏離本揭露所附之申請專利範圍的技術精神下調整及改變本揭露。 As described above, the present disclosure has been described with reference to the embodiments. However, it is understood that those skilled in the art can adjust and change the present disclosure without departing from the spirit of the appended claims.

Claims (4)

一種用於製備透明磷光性陶瓷板的方法,包括:以研磨方式將一小顆粒YAG磷光物磨碎至1μm或以下;將該磨碎的YAG磷光物在一烘箱中乾燥;對於該乾燥的磨碎的YAG磷光物施加壓力而模製成一板;以及將該模製板燒結及後處理。 A method for preparing a transparent phosphorescent ceramic plate, comprising: grinding a small particle YAG phosphor to 1 μm or less by grinding; drying the ground YAG phosphor in an oven; for the dried mill The broken YAG phosphor is pressed to form a plate; and the molded plate is sintered and post-treated. 如申請專利範圍第1項所述之方法,其中將該磨碎的YAG磷光物在一烘箱中的該乾燥係在100℃ to 150℃的範圍下進行1至24小時。 The method of claim 1, wherein the dried YAG phosphor is dried in an oven at a temperature ranging from 100 ° C to 150 ° C for 1 to 24 hours. 如申請專利範圍第1項所述之方法,其中該施加壓力的模製係使用冷均壓(CIP)方法在1000Mpa至3000Mpa的壓力範圍下進行。 The method of claim 1, wherein the molding of the applied pressure is performed using a cold equalization (CIP) method at a pressure ranging from 1000 MPa to 3000 MPa. 如申請專利範圍第1項所述之方法,其中該燒結係在還原化環境或在空氣中使用大氣爐(atmosphere furnace),在1400℃至1800℃的溫度範圍中進行8小時至15小時。 The method of claim 1, wherein the sintering is carried out in a reducing environment or in an atmosphere using an atmosphere furnace in a temperature range of 1400 ° C to 1800 ° C for 8 hours to 15 hours.
TW105138216A 2015-12-31 2016-11-22 Process for preparing transparent ceramic plates of phosphorescent TWI606745B (en)

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KR102121249B1 (en) * 2018-07-04 2020-06-10 한국광기술원 Phosphor Plate and Method for Manufacturing Thereof
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CN112661512A (en) * 2020-12-23 2021-04-16 新沂市锡沂高新材料产业技术研究院有限公司 Method for densification of fluorescent powder and yttrium oxide ceramic at room temperature

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