200842183 九、發明說明： 【發明所屬之技術領域】 本發明係有關於一種螢光粉之製備方法，特別係有關 於一種以水熱法合成之螢光粉之製備方法。 【先前技術】 習知應用於白光LED之螢光粉（SrSi〇3:Dy3+)大都是 以固態燒結法（Solid-state Method)製作，然而，以固態燒 …法‘作螢光粉其所需之燒結溫度較高（13⑽。C以上），且 燒結時間也較長，此外，固態燒結衫僅無法有效控制螢 光粕之粒k，其所製作之螢光粉組成均勻度亦不佳，嚴重 影響螢光粉之發光特性及色純度。 【發明内容】 本备月之主要目的係在於提供一種螢光粉之製備方 法，其係以硝酸鳃（SMNO3)2)、矽酸鈉（Ν^δί〇3)、硝酸鏑 (Dy(N〇3)3)及純水混合形成—第—溶液，並將該第一溶液 與:驗性物質混合以形成―第二溶液，接著對該第二溶液 進^一水熱法合成步驟，以形成一螢光粉前驅物，最後燒 結該榮光粉前驅物，以形成—螢光粉（SrSiQ3:Dy3V本發 明係主要利用水熱法合成該螢光粉（以叫：Dy3 + )，其功效 除了可降低螢光粉之製程溫度外（較固態燒結法低了數 ^ a以水熱法合成之該螢光粉（SrSi〇3:W粒徑微細 句勻、結晶性佳且化學組成均勻，可大幅提高該螢光粉 (SrSi〇3:Dy3 + )之發光特性及色純度。 本I月之-人一目的係在於提供一種螢光粉之製備方 5 20U842183 法，其另包含對該勞光粉前 係以離心分離方式去除”光二仃—去除雜質步驟’其 丄。 寶九粉前驅物中的雜皙。 本發明之i目雜負 法，其另包含對兮發光中“ 種螢光粉之製備方 乾該螢光粉前驅物，以去 九、乾步驟，其係烘 ~彳去除该勞光粉前驅物中的水分。 依據本發明之一種螢制 第-溶液，該第一、、容、、夜… 法，其包含提供- ma s.〇 , /合液係由確酸鳃（Sr(N〇3)2)、石夕酸鈉 (n_〇3)、確酸鏑(Dy⑽3)3)及純水混合而成，且該第一 吩液係具有—第一 pH * ;提供一驗性物質，該驗性 係用以調整該第—溶液之該卜卜㈣ 與該驗性物質以形成―第二溶液，該第二溶液係具有一第 二阳值：對該第二溶液進行一水熱法合成步驟，以形成 一螢光粉前驅物；以及燒結該螢光粉前驅物，以形成一螢 光粉（SrSi〇3:Dy3 + )。 【實施方式】 請參閱第1圖，其係本發明之一較佳實施例，一種螢 光私之製備方法’其步驟係詳述如下：首先，請參閱步驟 (a) ’提供一第一溶液，該第一溶液係由硝酸|思（Sr(N03)2)、 石夕酸鈉（Na^SiOi)、石肖酸鏑（Dy(N〇3)3)及純水混合而成，且 該第一溶液係具有一第一 pH值，在本實施例中，石肖酸錄 (Sr(N03)2)、矽酸鈉（Na2Si03)、硝酸鏑（Dy(N03)3)及純水係 可以攪拌方式混合；接著，請參閱步驟（b)，提供一鹼性物 質，該鹼性物質係用以調整該第一溶液之該第一 pH值， 在本實施例中’該驗性物質係可為氫氧化納（NaOH);之 6 200842183 後-月參閱步驟⑷，混合該第一溶液與該驗性 該第二溶液係具有-第…，在本= Π亥弟-溶液之該第二PH值係大於該第一溶液之該 阳值’且该第二pH值係介於Η至Μ之間，較佳地， =ΓΡΗ值料13;接著，請參閱步驟⑷，對該第二溶 ’Γ丁—水熱法合成步驟，該水熱法合成步驟係、為依序將 成弟二溶液密封於_六π + 最後將該壓力釜置入谷的者將置入-壓力蚤， 下 釜置入—烘箱，以使該第二溶液在中溫高壓 中=欠熱反應’進而形成一螢光粉前驅物，在本實施例 地’以共箱之設定溫度係介於10吖至275t之間，較佳 俜^亥棋箱之設定溫度係為25(rc，且該烘箱之設定 你為48小時·夕1 义 4 ，睛參閱步驟（e)，必要時，可對該螢 尤私W驅物進行一丰 該螢光粉前驅物晉 /在本實施例中，其係將 水）， * W 入離心试官中並加入液體（如去離子 太杂、 刀離方式去除該螢光粉前驅物中的雜質，在 只方包例中，施 l4〇〇ft 心分離之設定轉速及時間係分別為 WOOr.p.m 及 10 分於•換 # ^ ^ 粉前驅物進行一二：’接者’請參閱步驟⑺，對該榮光 去广# M， ，、乾步驟，其係烘乾該螢光粉前驅物，以 定:：光粉前驅物中的水分，在本實施例中，烘乾之設 驟^及時間係分別為啊及24小時；最後，請參閱步 (srSi〇3.=該勞光粉前驅物，以形成一營光粉 度係不…二本實:謝，燒結該榮光粉前驅物之温 (SrSi〇3:Dy3+w“、 卜’在本貫施例中’該螢光粉 /、可以波長365nm之紫外光激發而產生波長 200842183 分別為480nm、572nm及664nm之三色光，如第2圖之榮 光光譜圖所示，此外，480nm、572nm及664nm等三色光 係可混合成白光，如第3圖之色度座標圖所示。 本發明係利用水熱法合成該螢光粉（SrSi〇3:Dy3 + )，其 功效上除了可降低螢光粉之製程溫度外（較固態燒結法低 了數百。c)，以水熱法合成之該螢光粉（SrSi〇3:Dy3+)之粒徑 微細均勻、結晶性佳且化學組成均勻，可大幅提高該螢光 粉（SrSi〇3:Dy3 + )之發光特性及色純度。 本發明之保護範圍當視後附之申請專利範圍所界定 者為準，任何熟知此項技藝者，在不脫離本發明之精神和 犯圍内所作之任何變化與修改，均屬於本發明之保護範 圍。 【圖式簡單說明】 第1圖·依據本發明之一較佳實施例，一種螢光粉之製備 方法流程圖。 第2圖·依據本發明之一較佳實施例，以紫外光激發螢光 ^ 粉（SrSi03:Dy3 + )之螢光光譜圖。 第3圖·依據本發明之一較佳實施例，以紫外光激發螢光 粉（SrSi〇3:Dy3 + )所產生之白光之色度座標圖。 【主要元件符號說明】 (a) 提供一第一溶液 (b) 提供一鹼性物質 (C)混合該第—溶液與該驗性物質以形成—第二溶液 ⑷對該第二溶液進行—水熱法合成步驟以形成一螢光粉 8 200842183 前驅物 (e) 對該螢光粉前驅物進行一去除雜質步驟 (f) 對該螢光粉前驅物進行一烘乾步驟 (g) 燒結該螢光粉前驅物以形成一螢光粉 9200842183 IX. DESCRIPTION OF THE INVENTION: TECHNICAL FIELD The present invention relates to a method for preparing a phosphor powder, and more particularly to a method for preparing a phosphor powder synthesized by a hydrothermal method. [Prior Art] Conventionally, the fluorescent powder (SrSi〇3: Dy3+) applied to white LEDs is mostly produced by a solid-state method, however, it is required to use a solid-state burning method as a fluorescent powder. The sintering temperature is higher (13 (10) C or more), and the sintering time is also longer. In addition, the solid sintered shirt can only effectively control the particles of the fluorescent enamel, and the uniformity of the phosphor powder produced is also poor. Affects the luminescent properties and color purity of the phosphor powder. SUMMARY OF THE INVENTION The main purpose of this preparation month is to provide a method for preparing a phosphor powder, which is strontium nitrate (SMNO3) 2), sodium citrate (Ν^δί〇3), and yttrium nitrate (Dy (N〇). 3) 3) mixing with pure water to form a first solution, and mixing the first solution with: an inert substance to form a second solution, and then subjecting the second solution to a hydrothermal synthesis step to form a phosphor powder precursor, and finally the glaze powder precursor is sintered to form a phosphor powder (SrSiQ3: Dy3V. The present invention mainly utilizes hydrothermal synthesis of the phosphor powder (referred to as Dy3 + ), and its efficacy is in addition to Reducing the process temperature of the phosphor powder (slower than the solid state sintering method), the phosphor powder synthesized by hydrothermal method (SrSi〇3: W particle size is fine, uniform, crystallized and uniform in chemical composition, can be greatly Increasing the luminescent properties and color purity of the phosphor powder (SrSi〇3: Dy3 + ). The purpose of the present invention is to provide a method for preparing a phosphor powder 5 20U842183 method, which further comprises the polishing powder The former is removed by centrifugal separation to remove the "photo-diode - impurity removal step". The invention relates to the method of the invention, which further comprises: in the preparation of the phosphorescent powder, the preparation of the fluorescent powder, the drying of the phosphor powder precursor, to the nine steps, the drying step, the drying of the Moisture in the powder precursor. According to the present invention, a first solution, a solution, a method, which comprises providing a - ma s. 〇, / a liquid system from a sorghum (Sr (N〇3) 2), sodium sulphate (n_〇3), yttrium acid (Dy(10)3)3) and pure water are mixed, and the first phenoid liquid has a first pH*; An assay substance for adjusting the Bu (4) of the first solution and the test substance to form a second solution having a second positive value: performing the second solution a hydrothermal synthesis step to form a phosphor precursor; and sintering the phosphor precursor to form a phosphor (SrSi〇3: Dy3 + ). [Embodiment] Please refer to FIG. It is a preferred embodiment of the present invention, a method for preparing a fluorescent private method, the steps of which are detailed as follows: First, please refer to step (a) 'providing a first solution, the first The solution is prepared by mixing nitric acid|Sr(N03)2, sodium sulphate (Na^SiOi), bismuth sulphate (Dy(N〇3)3) and pure water, and the first solution is Having a first pH value, in the present embodiment, the succinic acid (Sr(N03)2), sodium citrate (Na2Si03), strontium nitrate (Dy(N03)3) and pure water can be mixed by stirring; Next, referring to step (b), an alkaline substance is provided for adjusting the first pH of the first solution. In the present embodiment, the test substance may be sodium hydroxide. (NaOH); 6 200842183 After the month-to-month, refer to step (4), mixing the first solution with the second solution having the -..., the second pH value of the solution is greater than the The positive value of the first solution is 'and the second pH value is between Η to ,, preferably, ΓΡΗ value 13; then, refer to step (4), the second dissolved Γ-water The thermal synthesis step, the hydrothermal synthesis step is to sequentially seal the Chengdi two solution to _six π + and finally place the autoclave into the valley, put the pressure 蚤, and place the lower kettle into the oven. To make the second solution The liquid is in the middle temperature and high pressure = underheat reaction 'to form a phosphor powder precursor, and in the embodiment, the set temperature of the common box is between 10 吖 and 275 ton, preferably 棋 ^ Set the temperature to 25 (rc, and set the oven to 48 hours, eve 1 and 4, and see step (e). If necessary, you can use the fluorescent powder precursor for the firefly. In this embodiment, it is water,) * W into the centrifuge and added liquid (such as deionized too impurity, knife removal to remove impurities in the phosphor powder precursor, only in the package In the example, the set speed and time of the l4〇〇ft heart separation are WOOr.pm and 10 points respectively. • Change # ^ ^ powder precursor for one or two: 'receiver', please refer to step (7), go to the glory广# M, ,, dry step, which is to dry the phosphor powder precursor to determine: the moisture in the powder precursor, in this embodiment, the drying process and the time are respectively And 24 hours; finally, please refer to the step (srSi〇3.= the light powder powder precursor to form a camp light powder system is not... two real: thank, sinter The temperature of the glare powder precursor (SrSi〇3: Dy3+w", Bu' in the present example, 'the phosphor powder/, can be excited by ultraviolet light with a wavelength of 365 nm to produce a wavelength of 200842183 of 480 nm, 572 nm and 664 nm, respectively. The three-color light is shown in the luminosity spectrum of Fig. 2, and the three-color light systems of 480 nm, 572 nm, and 664 nm can be mixed into white light, as shown in the chromaticity coordinate diagram of Fig. 3. The invention utilizes hydrothermal method to synthesize the phosphor powder (SrSi〇3: Dy3 + ), and its efficacy is not only lowering the process temperature of the phosphor powder (less than the solid state sintering method is several hundred. c), with water heat The phosphor powder (SrSi〇3: Dy3+) synthesized by the method has fine particle size, good crystallinity, and uniform chemical composition, and can greatly improve the light-emitting characteristics and color purity of the phosphor powder (SrSi〇3: Dy3 + ). The scope of the present invention is defined by the scope of the appended claims, and any changes and modifications made by those skilled in the art without departing from the spirit and scope of the invention are protected by the present invention. range. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing a method of preparing a phosphor powder according to a preferred embodiment of the present invention. Fig. 2 is a view showing a fluorescence spectrum of a fluorescent powder (SrSi03: Dy3 + ) excited by ultraviolet light according to a preferred embodiment of the present invention. Fig. 3 is a chromaticity coordinate diagram of white light generated by excitation of phosphor powder (SrSi〇3: Dy3 + ) by ultraviolet light according to a preferred embodiment of the present invention. [Description of main component symbols] (a) providing a first solution (b) providing an alkaline substance (C) mixing the first solution with the test substance to form a second solution (4) performing the second solution - water Thermal synthesis step to form a phosphor powder 8 200842183 precursor (e) a step of removing impurities from the phosphor powder precursor (f) a drying step (g) of the phosphor powder precursor Light powder precursor to form a phosphor 9