TW200426203A - Orange color phosphor powder formula and production method thereof - Google Patents

Abstract

This invention discloses an orange color phosphor powder formula containing Y2O2Smaterial with Ti and Mg dopants, and a production method thereof. The invented phosphor material uses Y2O2S as a matrix and Ti and Mg dopants as activation agents and has a chemical composition of (Y2-x-yTixMgy)O2S, in which 0.001 ≤ x ≤ 0.5 and 0.001 ≤ y ≤ 0.5 are satisfied. When excited by a light source, such as ultraviolet light, at the wavelength of 300-450 nm, an orange light is emitted. When the light source for excitation is removed, the material emits orange phosphorescence. The invented material exhibits merits such as pure color light and long emitting time. Moreover, the disclosed formula by the invention can produce single phase Y2O2S powder through various synthesis methods such as solid state reaction, co-precipitation, gelation or micro emulsification. The invented production method is simple and easy for mass production and the finish product has industrial application value.

Description

200426203 V. Description of the invention (1), ^-[Technical field to which the invention belongs] The present invention discloses an orange-yellow phosphorescent powder containing titanium and magnesium mixed with 202 S material formula and a preparation method thereof. "[Previous technology], a phosphorescent material is a kind of phosphor with luminous storage, which can be excited by ultraviolet rays (or other external energy equivalent to ultraviolet rays). After stopping the excitation, it is still visible to the naked eye for a considerable time (a few minutes to several hours) ) Afterglow (af ter gj 0 w). Because it can illuminate in the dark, it is quite widely used in daily life. It is often used as clock scales, emergency exits and route guidance, night pedestrian safety clothing, toys, etc. It is a material with great potential for application. At the beginning of the 20th century, people added radioactive element radium (radium (88Ra)) to zinc sulfide edge-lighting materials to make materials with residual elasticity (aherg 1 0w). The long half-life and the radiant energy during the decay process continue to excite the characteristics of the fluorescent materials to increase the afterglow brightness of the luminescent materials. By the mid-twentieth century, Japan used artificial radiation element moments (promethium, 61Pm in consideration of cost, brightness and safety) ) Instead of radium, and in Europe, it is replaced by the hydrogen isotope tritium (3H). However, all these radioactive substances are harmful to humans. It has a negative impact on the environment and the environment, so the development of new long-lasting light-filling materials with long light holding time and harmless to the human body and the environment is an important issue. Recently, Yoshihiko Muramura and others of Bengen Special Chemical Co., Ltd. revealed that (China) Republic of China Invention Patent No. 07 6 3 19) A compound using MA12〇4 (M is based on Sr, Ba) as a parent compound, by adding at the same time 0.00% (mole percentage) or more '10% (Percent of mole) The following eu (eu) is activation

Page 5 200426203 V. Description of the invention (2) The agent and at least one element (selected from 钸, 镨, ', Peng, Ji, 镝, oblique, mirror, fierce, tin, silk) below the Molar number in the same range are activated Agent. This new phosphor emits yellow-green and blue light after being irradiated with ultraviolet and visible light at 200 ~ 450 nm at room temperature. Its light retention (lasting time) is longer than the traditional zinc sulfide ZnS, and This new compound is not radioactive, and it is not easy to interact with moisture in the air, so it can be applied to indoor and outdoor displays, and can be used outdoors. Compared to green, blue, and red phosphors, orange phosphors are scarce. However, in terms of applications, orange phosphors are no less important than the three light-color phosphors. [Summary of the Invention] The present invention discloses a formula of Y202 S material in which an orange-yellow phosphor powder system is doped with titanium and magnesium, and a preparation method thereof. The main purpose of the present invention is to provide a formula of orange-yellow phosphorescent powder, which at least contains a compound (Y2-x-yTixMgy) made of titanium (Ti) and magnesium (Mg) doped yttrium oxide (Y20 2S) material. ) 02S, where the X content is 0.001 'x $ 0.5, and the y content is 0.001, and preferably 0.05 $ χ $ 0 · 2 and 0e05Sy $ 0.2 〇 The aforementioned orange-yellow phosphor powder is at a wavelength of 3 0 0 ~ 4 50 nm Under the light source, it can emit orange-yellow phosphorescence. Another object of the present invention is to provide a method for preparing orange-yellow phosphorescent powder, which comprises at least the following steps: mixing a specific ratio of element K, sulfur, titanium-containing compound, and magnesium-containing compound; sintering at high temperature in an inert gas environment The aforementioned mixture to form (Y 2-X-y T i XM gy) 0 2 S; and

Page 6 200426203 V. Description of the invention (3) The finished product can be ground into powder to obtain orange-yellow phosphorescent powder. The aforementioned yttrium oxysulfide (Y202 S) is the precursor, and titanium and magnesium doping act as the activator. Its chemical composition is (Υ2-χ-7T i xMgy) 02S (0 · 0 0 1 SX $ 0.5. ^ 0.001 ^ 0.5, and preferably 0. 05 $ χ $ 0 · 2 and 0.05Sy $ 0.2). Excited by ultraviolet light and other light sources, it can emit orange light under a light source with a wavelength of 300 to 4500 nm. When the excitation light source is removed, the material can emit orange yellow scale light. The aforementioned yttrium element is selected from yttrium metal compounds or salts thereof, such as yttrium oxide or yttrium nitrate. The aforementioned titanium-containing compound is selected from titanium metal oxides or salts thereof, such as titanium dioxide. The aforementioned magnesium-containing compound is selected from magnesium metal oxides or salts thereof, such as magnesium oxide. The sulfur element is selected from sulfur powder or nitrogen sulfide gas. The aforementioned method can further add sodium carbonate as a fluxing agent; the aforementioned sintering procedure is pre-sintered at a temperature of 4 0 ~ 80 0 ° C (preferably 6 0 ~ 7 0 0 ° C) 0 · 1 ~ 5 Hours (preferably 0 · 5 ~ 2 · 5 hours), and then sintering at 8 1 0 ~ 1 5 0 ° C (preferably 8 5 0 ~ 1 1 5 0 ° C) 0 · 5 ~ 12 hours (preferably 1.5 hours to 4.5 hours). The aforementioned inert gas system may be argon, helium, nitrogen, or a mixture thereof. The material of the invention has the advantages of pure light color and long light holding time. The conventional Eu-doped Y202S powder has only red fluorescence, but not phosphorescence. In addition, the formula disclosed in the present invention can use a variety of synthetic methods to prepare single-phase iY202S powder, such as solid state reaction method, co-precipitation method, gel method or microemulsion method. The manufacturing method of the invention is simple and easy to mass-produce.

Page 7 200426203 V. Description of Invention (4) Value. [Embodiment] The advantages of the orange-yellow phosphorescent powder of the present invention and the preparation method thereof will be described by the following examples. Example:

3.000 grams of yttrium oxide (Υ203), 0.0007 grams of titanium dioxide (TiO 2), 0.0054 grams of magnesium oxide (MgO) and 2.5767 grams of sulfur powder (S) (that is, according to Y 1. 9 8 0 2 S: T i: M g = 1: 0 · 0 1 ·· 〇 · 〇1 ratio) and mix well, and add 1.4 2 2 7 grams of sodium carbonate (Na2C03) as a flux (ie, according to丨 丨 9s: Na 2C03 = 1: 1) Grind and mix thoroughly in a mortar, place the homogeneous mixture in an alumina crucible, then place the alumina crucible in a high temperature furnace under a nitrogen environment at 60 ° C is pre-sintered for 0.5 hours and then heated to 950 ° C for 2 · 5 hours. The heating and cooling rates of the sintering process are both 5 ° C / mi η. After sintering, grind it with a grinding spider to make it into a powder with uniform particles to obtain a finished product. (Y2-x-yTixMgy) 〇2S (X = 0 · 0 1 ′ y = 0 · 0 1) sample ′ prepared according to the embodiment of the present invention was identified by X-ray powder diffractometer for crystal phase purity

The results are shown in Figure 1 (a). Comparing the X-ray powder diffraction pattern of the sample prepared by the present invention with the standard yttrium oxysulfide compound (JCPDS no: 24-1424) in the first (b), it can be seen that the yttrium oxysulfide phosphor disclosed in the present invention is a single phase With a hexagonal structure (he X ag ο na 1), its lattice constants are a = b = 3. 78524 (8) A, c = 6. 58809 (14) A; cold = 90. , Γ = 1 2 0 〇 ο

The second figure is (Y2_x-yTixMgy) 02S prepared by an embodiment of the present invention.

200426203 V. Description of the invention (5) (X = 0 · 0 1, y = 0 · 0 1) Spectra of (a) light excitation and (b) light emission of the sample. From the results, it is known that the phosphor emits orange-yellow fluorescent light when it is excited by a light source with a wavelength ranging from 300 nm to 450 nm. The emission spectrum data is converted into the chromaticity coordinates represented by this phosphor by the formula of the chromaticity coordinate chart (Chiromaticity diagram) established by the Commission for International Illumination (CIE) in 1931. The third picture, which is equivalent to the orange light of x = 0.4914 and y = 0.479. The (Y2-x —yTixMgy) 〇2S (χ = 〇. 〇1, y = 〇. 〇1) sample prepared in the embodiment of the present invention was excited by ultraviolet light with a wavelength of 3 2 2 nm for ten minutes, and then the light source was removed, The intensity of the scale light emitted by the sample was measured and plotted against time, and the results are not as shown in the fourth figure. It can be known from the results that the x-yTixMgy) 02S sample of the present invention does have scale characteristics. The embodiments disclosed in this application are only specific embodiments of the present invention, and the gist of the present invention is not limited thereto. Any γ yellow phosphorescent powder material doped with titanium and magnesium and its preparation method, and any changes or modifications made to the finished product are covered by the scope of the patent application.

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Claims (1)

200426203 6. Scope of patent application 1. A formula of orange-yellow phosphorescent powder, including at least a compound (Y2- made of titanium (T i) and magnesium (Mg) -doped yttrium oxide (Y2 02 S)) X-yTixMgy) 02S, where the content of x is 0.001 $ 0.5 and the content of y is 0.001 $ 0.5. 2. The formula as described in item 1 of the scope of the patent application, which can emit orange-yellow phosphorescence when illuminated by a light source with a wavelength of 300 to 450 n m. 3. The formulation as described in item 1 of the scope of patent applications, wherein the aforementioned X content is 0.05SxS0.2, and the y content is 0.05 $ y $ (K2.) 4. A method for preparing an orange-yellow phosphorescent powder, which includes at least the following Steps: Mixing elementary element, sulfur element, titanium-containing compound, and town-containing compound in a specific ratio; sintering the aforementioned mixture at high temperature under an inert gas environment to form (Y2-xy T x xMgy) 02S; and sintering the aforementioned finished product Grind into powder. 5. As the method shown in item 4 of the patent application, it can be further added with sodium carbonate as a flux. 6. The method as described in item 4 of the patent application, wherein the aforementioned sintering procedure is Including (a) pre-sintering at a temperature of 4 0 ~ 80 0 ° C for 0 · 1 ~ 5 hours; and (b) further sintering at 8 1 0 ~ 1 50 0 ° C for 0 · 5 ~ 1 2 hours 7. The method described in item 6 of the scope of patent application, wherein the sintering temperature of step (a) above is 600 ~ 700 ° C. 8. The method described in item 6 of the scope of patent application, The sintering time of the aforementioned step (a) is from 0.5 to 2.5 hours. Page 11 200426203 6. Scope of patent application 9. The method as described in item 6 of the scope of patent application, wherein the sintering temperature in step (b) above is 8 50 ~ 1 150 ° C. 10. The method according to item 6 of the scope of patent application, wherein the sintering time of the step (b) is 1.5 to 4.5 hours. 1 1. The method according to item 4 of the scope of the patent application, wherein the aforementioned inert gas may be argon, helium, nitrogen, or a mixture thereof. 12. The method according to item 4 of the scope of patent application, wherein the aforementioned X content is 0.001 ^ x ^ 0.5 and the y content is 0.001 SyS0.5. 1 3. The method according to item 12 of the patent application scope, wherein the foregoing x content is 0.05 ^ x ^ 0.2, and the y content is 0.05 〇14. The method according to item 4 of the patent application scope, wherein the foregoing contains titanium The compound is selected from titanium metal oxides or salts thereof. 15. The method according to item 14 of the scope of patent application, wherein the aforementioned titanium metal oxide is titanium dioxide. 16. The method according to item 4 of the scope of patent application, wherein the aforementioned yttrium element system is selected from the group consisting of yttrium metal oxides or salts thereof. 1 7. The method according to item 16 of the scope of patent application, wherein the aforementioned yttrium metal oxide is yttrium oxide. 18. The method according to item 16 of the scope of patent application, wherein the salt of the aforementioned yttrium metal oxide is yttrium nitrate. 19. The method according to item 4 of the scope of patent application, wherein the aforementioned magnesium-containing compound is selected from magnesium metal oxides or salts thereof. 20. The method according to item 19 of the scope of patent application, wherein the magnesium metal oxide is magnesium oxide. Page 12 200426203 Page 13