TWI248463B - Orange color phosphor powder formula and production method thereof - Google Patents

Abstract

This invention discloses an orange color phosphor powder formula containing Y2O2S material 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

1248463 V. INSTRUCTION DESCRIPTION (1) 'Technical Fields According to the Invention The present invention discloses an orange yellow phosphor powder containing titanium and magnesium doped Y2 02 S material formulation and a preparation method thereof. [Prior Art] = The light material is a light-storing phosphor that can be excited by ultraviolet rays (or other energy external to ultraviolet light), and is still visible to the naked eye for a considerable period of time (10 minutes to several hours) after stopping the excitation. Afterglow (after g1〇w). = It can be illuminated in the dark, and it is widely used in daily life. It is used as a watch scale, emergency exit and route guidance, night pedestrian safety clothing, toys, etc. It is a material with great application potential. At the beginning of the sixties century, the radioactive element radium (r a ^丨u ^, 8 8 R a ) was added to the zinc-fluorescent material to produce an afterglow (after gl〇w) material. This P utilizes a long half-life of the error and the radiant energy in the decay process constantly excites the characteristics of the fluorescing material to increase the afterglow brightness of the luminescent material. By the middle of the 20th century, Japan used artificial radiation = promethi um (6 lPm ) instead of radium in terms of cost, brightness and safety, while in Europe it used ^ = isotope gas (tritium ' 3 Η ) Instead of it. However, these all kinds of scallops have a negative impact on the human body and the environment. Therefore, the development of new long-lasting phosphorescent materials with long light-keeping time and harmless to the human body and the environment is an important issue. Murata, who is close to Japan’s Fundamental Specialty Chemicals Co., Ltd., Murayama Yoshihiko and others, reveals the Republic of China invention patent No. 637 63 1 9) with ^ 12 04 〇 as 〇 &amp; By adding 〇· 〇〇1% (% of moles) at the same time

1248463 V. INSTRUCTIONS (2) Above, 10% (% of moles) or less (Eu) is an activator and at least one element having the same range of moles or less (selected from 钸, 错, 叙, #, 纪, bismuth, steel: 镱, 猛, tin, grade) as an activator. The new stone dance light body emits yellow-green and blue light after being irradiated with ultraviolet rays and visible light of 200 to 450 nm at room temperature, and its light-holding property (afterglow time) is higher than that of the conventional sputum ZnS. Long, and this new compound is not radioactive, it is not easy to interact with moisture in the air, so it can be applied to indoor display and can be used outdoors. Compared with green, blue and red phosphors, orange phosphors are rare. However, in terms of applications, orange phosphors are as important as the above-mentioned three color phosphors. SUMMARY OF THE INVENTION The present invention discloses a Y2〇2s material formulation in which an orange phosphor powder system is doped with titanium and magnesium and a preparation method thereof. The main object of the present invention is to provide a formula of orange phosphor powder, which comprises at least a compound made of titanium (T i ) and magnesium (Mg ) doped yttria Y2 〇 2 S material (Y2-x_yTixMgy) 02S, wherein the X content is 〇·〇〇ΐ'χ^ 〇·5 'y content is 〇〇〇isy'〇.5, and preferably 〇·〇5$χ'〇·2 and 0.05Syg〇.2 . The orange phosphor powder described above can emit orange phosphorescence under the illumination of a light source having a wavelength of 300 to 45 nm. Another object of the present invention is to provide a method for preparing an orange phosphor powder, which comprises at least the following steps: cerium oxide, sulfur element, titanium-containing compound

1248463

&gt; Sintering the above mixture to form (Y2_&quot;TixMg ~ gas atmosphere, the finished product is ground into a powder, which can be made; 4 dragons 2 s, and the aforementioned sintering of the above-mentioned sulfur oxysulfide (Y2 〇2 s ) is the mother body, and the color of the two-dimensional color disc. The chemical composition of the agent is (Y2_x, yTixMg, and scales are activated) · 5,0 · 0 〇1 $ y S 0 · 5, and Preferably, 〇$ S ( 0 · 0 0 1 s X ' $ y S 0 · 2 ) is irradiated by a light source of other wavelengths such as ultraviolet light, two = $ 0 · 2 and 〇 · 〇 5 4 50 nm, Radiation Orange Pu Chuanchuan ~ After the light source, the material can emit orange phosphorescence ',.' *Remove excitation 5. Description of invention (3) Mutant magnesiumation 0 The foregoing element is selected from a base metal compound or a salt thereof. The foregoing titanium-containing compound is selected from the group consisting of titanium metal oxides or salts thereof, such as titanium dioxide. The magnesium-containing compounds are selected from magnesium metal oxides or salts thereof, such as magnesium oxide. The element is selected from the group consisting of sulfur powder or hydrogen sulfide. The foregoing method may further add sodium sulphate as a fluxing agent. The sintering process is pre-sintered at a temperature of 40 0 to 80 ° C (preferably 6 〇〇 to 70 0 ° C) for 0 · 1 to 5 hours (preferably 〇 5 to 2 · 5 hours). Then, after 8 1 y~1 5 0 0. 较佳 (preferably 850~1 15 〇 it), the temperature is sintered for 5 to 12 hours (preferably 1 · 5 to 4 · 5 hours). It can be argon gas, nitrogen gas or a mixed gas thereof. The material of the invention has the advantages of pure color and long light holding time, etc. The Eu-doped Y2〇2S powder has only red fluorescence: no phosphorescence. The formulations disclosed in the present invention can be used to prepare single-phase ethyl hydrazine 2 S powder by various synthetic methods, such as solid state reaction, coprecipitation, gelation or microemulsion.

1248463 V. INSTRUCTION DESCRIPTION (4) The manufacturing method is simple, easy to mass produce, and the obtained finished product has industrial application value. [Embodiment] Advantages of the orange phosphor powder of the present invention and a method for producing the same will be described by way of the following examples. EXAMPLES: 3 · 0 0 g of yttrium oxide (Y2 03 ), 〇 · 0 1 〇 7 g of titanium dioxide (T i 02), 〇·0054 g of magnesium oxide (MgO) and 2.5 767 g of sulfur powder ( S) (ie according to the ratio of Yi.98〇2S : T i : Mg = 1 : 〇· 〇1 : 〇· 〇1), mix well and add 1 · 4 2 2 7 grams of sodium sulphate (Na2C03) The flux (ie 98 〇 2S : Na2C03 = 1 : 1 ) is ground and thoroughly mixed with a spider, and the homogeneous mixture is placed in an oxidized shackle, and then the alumina crucible is placed in a high temperature furnace under a nitrogen atmosphere to 6 0 0 t: Pre-sintering 0 · 5 hours, and then heating to 950 ° C for 2. 5 hours, the heating and cooling rates of the sintering process are 5 t: / mi η. After the sintering is completed, it is ground by a mortar to make it into a powder of uniform particles, that is, a finished product. A sample of (Y2tyTixMgy) 〇 2S (X = 0 · 〇1, y = 0 · 0 1 ) prepared according to an embodiment of the present invention, and its crystal phase purity is identified by an X-ray powder diffractometer. The result is as shown in the first (a) The figure shows. Comparing the sample prepared by the present invention with the standard bismuth oxysulfide compound (JcpDS: 24-1 4 24 ) X-ray powder diffraction pattern of the first (b) diagram, it can be seen that the sulphur oxysulfide phosphor disclosed in the present invention is a single The structure of the phase 'he X ag ο na 1 ' has a lattice constant of a = b = 3 · 785 24 ( 8 ) A, c = 6. 58 80 9 ( 1 4 ) A ; α = /3=90. ,

1248463 V. Description of invention (5) r II 1 2 0 ° . The second graph is a spectrum of (a) photoexcitation and (b) light emission of a sample (Y2_x_yTixMgy)02S (X = Ο · Ο 1, y = Ο · 01) prepared according to an embodiment of the present invention. As a result, it is known that the light source emits orange fluorescent light through a light source having a wavelength range of 3 Ο 0 nm to 450 nm. The data of the emission spectrum is converted into the chromaticity coordinate represented by the phosphor by the formula of the Chromamatic diagram prepared by the Commission Internationale de l'Eclairage (CIE) in 1931. In the third figure, it corresponds to the orange light of χ = 〇 · 4914 and 乂 = 0.4799. The (Y2_&quot;TixMgy)〇2S &amp;==pre-source, prepared by the embodiment of the present invention, the phosphorescence intensity emitted by the sample in the sub-test is as shown in the fourth figure. From the results, it is understood that the present invention (? 乍囷; σ product has a phosphorescent property. Hi hMgy ) 02S The embodiment disclosed in the application is only the gist of the present invention and is not limited thereto. Any two-two-legged steam application, only the yellow phosphor powder material formula and its preparation; go, the second doped Y2〇2s orange change or modification is covered in the patented finished product of this case

1248463 Brief description of the drawings [Simplified description of the drawings] The first figure compares the samples of (1^1^社7)028 (also = 0 · 0 1 , y = 0 · 0 1) prepared in the examples of the present invention. X-ray powder diffraction pattern (a) and standard X-ray powder diffraction pattern (b) of commercially available Y2 02 S. The second graph shows the spectra of (a) photoexcitation and (b) light emission of (Y2_x_yTixMgy)02S (X = 0 · 0 1, y = 0 · 01 ) samples prepared in an embodiment of the present invention.

The third figure marks the light emission spectrum of the second (b) diagram on the C I E chromaticity coordinate map. The fourth graph shows the holding curve of the powder of (Y2_x_yTixMgy) 02S (X =0 · 0 1, y = 0 · 0 1 ) prepared in the examples of the present invention.

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Claims (1)

1248463 VI. Patent Application Range 1. An orange phosphor powder powder containing at least a compound made of titanium (T i ) and magnesium (M g ) doped sulfur oxide Y2 02 S material (Y2_x_ yTixMgy) 02S, wherein the X content is 0·001^χ$0·5, and the y content is 0.001 $ y $ 0 · 5 〇2. The formulation described in claim 1 is at a wavelength of 300 to 45 Onm. Under the illumination of the light source, orange phosphorescence can be emitted. 3. The formulation of claim 1, wherein the X content is 0. 0 5 Sx$ (K2, y content is 0.05$y$〇.2. 4. A method for preparing orange phosphor powder, At least the following steps are included: mixing a specific ratio of cerium oxide, sulfur element, titanium-containing compound, and magnesium-containing compound; sintering the mixture at a high temperature in an inert gas atmosphere to form (Y2_x_yTixMgy)02S; and grinding the sintered product Powdered; wherein the sintering procedure comprises (a) pre-sintering at a temperature of 40 0 to 80 ° C for 0 · 1 to 5 hours; and (b ) sintering at 8 1 0 to 1 500 ° C 0 · 5〜1 2小时。 5. The method of claim 4, further comprising the addition of sodium carbonate as a fluxing agent. 6. The method of claim 4, wherein the aforementioned The sintering time of the step (a) is 0. 5~2. The sintering time of the step (a) is 0. 5~2. 5 hours. 1248463 VI. Scope of Application Patent 8. The method of claim 4, wherein the sintering temperature of the foregoing step (b) is 850 to 1150 °C. The sinter time is 1. 5~4 · 5 hours, as described in the above-mentioned (b). The method of claim 4, wherein the inert gas is argon, nitrogen or a mixture thereof. 11. The method of claim 4, wherein the X content is 0.001 ^x^O. 5, and the y content is 0.001 Sy$0.5. The method of claim 11, wherein the X content is 〇. 05 ^0. 2, and the y content is 0.05 SyS0.2. 13. The method of claim 4, wherein the titanium-containing compound is selected from the group consisting of titanium metal oxides or salts thereof. The method of claim 13, wherein the titanium metal oxide is titanium dioxide. The method of claim 4, wherein the bismuth element is selected from the group consisting of ruthenium metal oxides or salts thereof. The method of claim 15, wherein the base metal oxide is cerium oxide. The method of claim 15, wherein the salt of the base metal oxide is cerium nitrate. The method of claim 4, wherein the magnesium-containing compound is selected from the group consisting of magnesium metal oxides or salts thereof. The method of claim 18, wherein the magnesium metal oxide is cerium oxide. </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; Page 13