201002620 九、發明說明： 【發明所屬之技術領域】 本發明係有關於一種二氧化鈦（Ti〇2)的製備方法，尤 指一種利用兩乳夥技術製備光催化用奈米含氮之二氧化鈦 (Ti〇2-xNx)微粉的方法。 【先前技術】 —氧化欽（Τι〇2)由於具有光催化作用，因此可用於殺 囷、除汙以及物體表面清潔等應用。然而，目前既有的二 氧化鈦必須照射到波長小於38〇奈米的紫外線方能觸發光 催化作用，因此為了充份利用太陽光（包含紫外線與可見光） 的忐罝，以提昇二氧化鈦的光催化效率，所以，如何使二 氧化錶可以吸收可見光即成為研究的重要課題。 根據研究報導指出，摻雜碳（c)、氮（Ν)、氟（F)、磷（ρ) 有助光觸媒吸收可見光（H· j F jansen and A j Freeman,201002620 IX. Description of the invention: [Technical field of the invention] The present invention relates to a method for preparing titanium dioxide (Ti〇2), in particular to a titanium dioxide containing titanium dioxide (Ti〇 for photocatalysis). 2-xNx) method of micropowder. [Prior Art] - Oxidation (Τι〇2) can be used for applications such as killing, decontamination, and surface cleaning of objects due to its photocatalytic action. However, the existing titanium dioxide must be irradiated with ultraviolet light having a wavelength of less than 38 nanometers to trigger photocatalysis, so in order to fully utilize the enthalpy of sunlight (including ultraviolet and visible light) to enhance the photocatalytic efficiency of titanium dioxide, Therefore, how to make the dioxide table absorb visible light has become an important topic of research. According to research reports, doping carbon (c), nitrogen (Ν), fluorine (F), and phosphorus (ρ) helps photocatalysts absorb visible light (H· j F jansen and A j Freeman,
Total energy full potential linearized augmented plane wave (FLAP W)method for bulk solids: electronic and structural properties of tungsten”，Physical Review. B, 30(1 984) 561- 569.) ’而其中以氮的摻雜可使光觸媒的能隙窄化（Band_gap narrow)而效果最佳。Asahi等學者研究指出摻雜氮的二氧 化鈦（Τι〇2_χΝχ)光觸媒在可見光（波長小於5〇〇奈米）下，對 亞甲基藍和氣態乙醛（acetaldehyde)具有良好的光分解效果 (R. Asahi, T. Morikawa, T. Ohwaki, K. Aoki and Y. Taga, “Visible-Light Photocatalysis in Nitrogen-Doped Titanium Oxides”，Science，293(2001) 269-271.) 〇 5 201002620 ，冗，二：：：製備二氧化欽微粉的方法中’因為在溶液中 二乳化鈦前導物’再瑕燒成二氧化鈦粉末的方法η :造：—全：價格便宜’故為最可行的方式。但此種方法： ^卢乳化鈦粉末，由於其生長顆粒形狀不規則和粒押 為其最大缺點。由文獻得ΓΓ;; 粒的品質不穩定 由文獻侍知上述之沉澱缺失可藉由逆 Z 技術(RevulsiQn preeipitatiGn 細㈣獲得 ^ 低人ΓΙΓ ’ u的研究“制逆乳㈣術可有效降 低合成粉末顆粒的大小，尤其利用兩乳谬法（TW0_e则 —更可製得奈米級的微粉。Tai等學者 乳踢技術製備氧化鍅⑽2)微粒，其顆粒尺寸約為5_5〇Γ 未，边小於由乳膠沉澱法製備之顆粒（0.2-8微米）。 τ 此外’現有二氧化鈦粉末的製備方法常使用金屬燒氧 化合物_al aIkoxide)為起始原料，以製備化學組成均勻 性的二氧化鈦粉末’此法雖可製得品質優異之粉體，但起 始原料Ti(OR)4等金屬貌氧化物極易與溼氣作用，先行水 解（Hydrolysis)而使化學成份不均勻。 目月』雖已有干者利用二乳膠技術成功製造氧化锆微 粒’但利用二乳膠技術製備含氮之二氧化欽微粉的方法仍 待研，與實驗，而其製造材料與製程條件亦為製造分散性 佳及尚品質之二氧化鈦微粉的重要關鍵。 【發明内容】 有鑑於現有製備二氧化鈦微粒的方法並不易製得分散 201002620 奈+級二氧化鈦微粉，其常有生長顆粒形狀不規則 :扛刀佈廣等缺㉟，本發明之目的在於提供一種利用兩 :1術製備光催化用奈米含氮之二氧化鈦微粉的方法， /、可製備分散性佳的奈米含氮之二氧化鈦微粉。 為達成U上的目的，本發明利用兩乳膠技術製備光催 化用奈米含氮之二氧化鈦微粉的方法係包括： ^提供第—乳膠液：該第一乳膠液係為水相/油相（w/0) 二’ X义相係為乙醯丙酮（Acetylacetone)螫合鈦離子（Ti4 + ) 之水溶液液滴； /提彳〃第—礼膠液.该第二乳膠液係為水相/油相（W/0) 系統，該水相係為鹼性水溶液液滴； 、混合兩乳膠液：將該第-與第二乳膠液混合反應以形 成含有前導物的混合反應液； 蒸顧·蒸館該混合反應液以去除油相； 乾燥月ij ‘物.將已去除油相之混合反應液中的前導物 加以過濾乾燥；以及 炸又k别導物·將已乾燥之前導物於氨氣氣氛下煆 燒’即可獲得可見光下具光催化性質之奈米含氮二氧化鈦 (Ti02.xNx)光觸媒微粒。 較佳的S，該第一乳膠液之製備係先使有機非極性溶 劑、界面活性劑以及乙醯丙酮與鈦烷氧化物（Ti(〇R)4)之混 合水溶液混合，而後加入共界面活性劑進行乳化混合 (Emulsificati〇n Mixing)所形成。 較佳的是，該鈦烷氧化物係為異丙氧基鈦。 7 201002620 ^較佳的是，該第二乳膠液之製備係先使有機非極性溶 ^界面'舌性劑以及鹼性水溶液混合，而後加入共界面活 ! 生诏進行乳化混合Mixing)所形成。 車乂 ^土的疋，該有機非極性溶劑係為正己烷（n-Hexane)， 該共界面活性劑係為異丙醇（IpA)，該驗性水溶㈣為濃度 大於8M之氨水。 較佳的是，煆燒前導物步驟中的煆燒溫度為400〜600 0C。 較佳的是，該第一與第二乳膠液係具有相同之水相"由 相（W/0)體積比。 較佳的是，該乙醯丙酮與鈦烧氧化物之混合水溶液中 之異丙氧基鈦與乙醯丙酮的莫耳數比為丨：4。 較佳的是’該界面活性劑與正己烧之體積比為0 03:Total energy full potential linearized augmented plane wave (FLAP W)method for bulk solids: electronic and structural properties of tungsten", Physical Review. B, 30(1 984) 561-569.) 'where the doping with nitrogen can The photocatalyst has the best bandgap narrow effect. Asahi et al. have pointed out that the nitrogen-doped titanium dioxide (Τι〇2_χΝχ) photocatalyst is in the visible light (wavelength less than 5 nanometers), methylene blue and gaseous acetaldehyde. (acetaldehyde) has a good photodecomposition effect (R. Asahi, T. Morikawa, T. Ohwaki, K. Aoki and Y. Taga, "Visible-Light Photocatalysis in Nitrogen-Doped Titanium Oxides", Science, 293 (2001) 269 -271.) 〇5 201002620 , verbose, two::: Method for preparing bismuth micropowder in the method 'because the second emulsified titanium precursor in solution' is then calcined into titanium dioxide powder η: Manufacture: - all: cheap 'Therefore is the most feasible way. But this method: ^ Lu emulsified titanium powder, due to its irregular shape of the growing particles and graining is its biggest disadvantage. From the literature to obtain ΓΓ; Instability is known from the literature. The above-mentioned precipitation loss can be obtained by the inverse Z technique (RevulsiQn preeipitatiGn fine (4) obtained ^ low human ΓΙΓ 'u research" "preverse milk (four) surgery can effectively reduce the size of synthetic powder particles, especially the use of two milk thistle Method (TW0_e - more can be made of nano-grade micro-powder. Tai and other scholars to kick the technology to prepare cerium oxide (10) 2) particles, the particle size of about 5_5 〇Γ not, the side is smaller than the particles prepared by latex precipitation method (0.2- 8 μm) τ In addition, 'the existing titanium dioxide powder is prepared by using the metal alkoxide compound _al aIkoxide as a starting material to prepare a titanium dioxide powder having a uniform chemical composition'. This method can produce a powder of excellent quality. However, the metal oxides such as the starting material Ti(OR)4 are easily reacted with moisture, and the hydrolysis is first caused to make the chemical composition uneven. Although the eye has been successfully used to produce zirconia particles by using two latex technology, the method of preparing nitrogen-containing oxidized fine powder by using the two-lact technology is still to be studied and experimentally, and the manufacturing materials and process conditions are also manufactured. An important key to the dispersion of good quality titanium dioxide powder. SUMMARY OF THE INVENTION In view of the existing method for preparing titanium dioxide particles, it is not easy to obtain a dispersion of 201002620 nano-grade titanium dioxide fine powder, which often has an irregular shape of growth particles: a wide range of files such as a trowel cloth, and the object of the present invention is to provide a utilization of two : 1 method for preparing photocatalytic nanometer titanium dioxide fine powder of titanium, /, can prepare nanometer titanium dioxide fine powder with good dispersibility. For the purpose of U, the method for preparing photocatalytic nanometer-containing titanium dioxide fine powder by using two latex technology includes: providing a first emulsion liquid: the first latex liquid is an aqueous phase/oil phase (w) /0) The second 'X sense phase is an aqueous solution of Acetylacetone conjugated titanium ion (Ti4 + ); / 提 彳〃 - 礼 液. The second latex is aqueous / oil In the phase (W/0) system, the aqueous phase is an alkaline aqueous solution droplet; and the two emulsion liquids are mixed: the first and second latex liquids are mixed and reacted to form a mixed reaction liquid containing a precursor; steaming and steaming The mixing reaction solution is used to remove the oil phase; drying the month ij '. The precursor in the mixed reaction liquid from which the oil phase has been removed is filtered and dried; and the mixture is fried and then the indicator is dried. Nitrogen-containing titanium dioxide (Ti02.xNx) photocatalyst particles with photocatalytic properties under visible light can be obtained under the atmosphere. Preferably, the first latex solution is prepared by mixing an organic non-polar solvent, a surfactant, and a mixed aqueous solution of acetamidine with titanium alkoxide (Ti(〇R)4), and then adding a common interfacial activity. The agent is formed by emulsification mixing (Emulsificati〇n Mixing). Preferably, the titanium alkoxide is titanium isopropoxide. 7 201002620 ^ Preferably, the preparation of the second latex liquid is firstly carried out by mixing an organic non-polar solvent interface tongue agent and an alkaline aqueous solution, and then adding a co-interface to produce emulsified mixed Mixing. In the ruthenium, the organic non-polar solvent is n-Hexane, and the co-surfactant is isopropyl alcohol (IpA). The water-soluble (IV) is an aqueous ammonia having a concentration of more than 8M. Preferably, the calcination temperature in the calcining precursor step is from 400 to 600 °C. Preferably, the first and second emulsion streams have the same aqueous phase " phase (W/0) volume ratio. Preferably, the molar ratio of titanium isopropoxide to acetamidine in the aqueous mixed solution of acetonitrile and titanium oxide oxide is 丨:4. Preferably, the volume ratio of the surfactant to the positive burn is 0 03:
較佳的是，該異丙醇與異丙氧基鈦之莫耳比為23 本發明可達成的具體功效包括： 1 .本發明係利用乙醯丙酮與異丙氧基鈦螯合，因此 可降低異丙氧基鈦的水解速率，以形成均句性較佳之顆 粒，並可提昇膠體顆粒之顆粒大小的分佈均勻丨生，且亦可 降低二氧化鈦微粉之合成溫度，谁 及進而如咼含氮二氧化鈦微 粉之品質。 2 ·本發明利用實驗規書彳、、表才a +、，π 規去來求出最適化的製程條 件，藉由此最適化的製程條件將^ ^ 町j U付分散性佳的奈米含 氮二氧化鈦微粉，且此含氮-4各μ他丨、 3忒一虱化鈦微粉的吸收範圍明顯 8 201002620 往可見光區移動 率。 有助於提高二氧化鈦微粉的光催化效 【實施方式】 :發明方法的較佳實施例係包括以下步驟： 提供第-乳膠液：該第—乳膠液係為水相/油相（) 系、統，該水相係為乙酸丙酮（Acetylacet〇ne)整合欽離子（ :水溶液液滴，該第一乳膠液之製備係可先使有機非極性 /谷劑（如正己貌（n_Hexane))、界面活性劑七晰）以及乙 T丙酮與鈦燒氧化物（Ti(0R)4)之混合水溶液於㈣下混 合，.而後加入共界面活性劑進行乳化混合⑽ ng)所H其巾該鈦烧氧化物係可為異丙氧基欽，該 =鯭丙酮係與異丙氧基鈦螯合而使異丙氧基鈦水解速率緩 慢，該界面活性劑係可為非離子型介面活性劑，如SPAN 4〇/80 類界面活性劑或 HLB(hydr〇PhiliC-lipophilic balance) 值介於3-8之界面活性劑，該混合水溶液中之鈦離子、乙 I醯丙酮與水的莫耳數比可為^4:25，該共界面活性劑係 可為異丙醇（IPA); 提供第二乳膠液：該第二乳膠液係為水相/油相（W/0) 系統’該水相係為鹼性水溶液液滴，該第二乳膠液之製備 系"T先使有機非極性溶劑（如正己烧（n_Hexane))、界面活性 劑以及鹼性水溶液於45〇c下混合，而後加入共界面活性劑 進行乳化混合（EmulsiHcation Mixing)所形成，其中該界面 /舌丨生A彳仏可為非離子型介面活性劑，如SPAN 40/80類界 面活性劑或 HLB(hydrophilic-lipophilic balance)值介於 3-8 9 201002620 之界面活性劑，該鹼性水溶液係可為濃度大於8M(如】2m) 之氨水溶液（NH4〇H)，該共界面活性劑係可為異丙醇 (IPA)’該第一與第二乳膠液係可具有相同之水相/油相（w/0) 體積比； 扣5兩乳膠液.將該第一與第二乳膠液於45。匚下混合 反應1小時以形成含有前導物的混合反應液； 口 瘵餾：利用真空減壓濃縮機蒸餾該混合反應液以去除 油相， ’ 乾燥前導物：將已去除油相之混合反應液中的前導物 加以過濾乾燥；以及 煆燒前導物：將已乾燥之前導物於400〜600 V的氨氣 (NH3)氣氛下煆燒，即可獲得可見光下具光催化性質之奈米 含氮二氧化鈦（Ti〇2-xNx)光觸媒微粒。 ★以下列冑幾個實施例以使本發明之特徵及優點更為清 楚’但以下之實施例並非用來限制發明的範圍，而是用^ 指示實施本發明的方法及材料，本發明的範圍應以所附之 申請專利範圍為準。 實施例一、二氧化鈦前導物製備 第一乳膠液以有機非極性溶劑（如正己烧）為油相，加 入親油性界面活性劑（Span系列）攪掉均勾，水相溶液為乙 酿丙酮配位異丙氧基鈦製得之乙酿丙酮(八⑽一咖 合鈦離子（Ti，etylacetonate)水溶液；第二乳膠液以有機非 :性溶劑(如正己烷)為油相，水相溶液為氨水水溶液，兩 7相溶液採用相同計量比個別混入油相中形成兩種不同、由 201002620 中水滴型的逆微胞乳膠液系統，再將適量共界面活性劑（異 丙醇）滴入兩乳膠液系統中，第一乳膠液逐漸變為澄清亮 透明狀淡黃色溶液，黃色的第二乳膠液也慢慢變為透明狀 逆乳膠溶液；而後兩乳膠液相互混合使其微胞與溶液產生 碰撞或擴散及成核反應，再經迴轉濃縮蒸餾，於200 °C乾 燥得到二氧化鈦之前導物（Precursor)。 實施例二、含氮二氧化鈦微粉製備 ，將實施例之二氧化鈦前導物以高溫燒結法於氨氣氣氛 下進行煆燒’使氮原子取代二氧化鈦中的部分氧原子，藉 此以增加二氧化鈦在可見光區的吸收，本實施例中控制氨 氣氣體流置為8 〇 m 1 / m i η，在6 0 0。C下t亙溫3小時，勢備 出含氮二氧化鈦（Ti〇2_xNx)。製備得到後的產品分別利用 X-ray粉晶繞射（XRD)、化學分析電子光譜儀（ESCA)和紫 外光-可見光譜儀（UV-Vis)檢視其性質，並且利用不同的製 程參數變化探討對製備性質的影響，製程參數變化包括恨 ◦燒温度（300〜700。〇、水相比、油相比、氨水濃度及共界 面活性劑量等，上述實施例請參見第一圖所示之製程。 在含氮一氧化欽微粉之性質方面，在400。〇下 Γ闻始有 銳鈦礦晶相產生，當溫度提高到700 oc發現晶相轉變為金 紅石結構’粉末顆粒大小約10〜30 nm，比表面積平均約 30〜95 m2/g，改質成功的二氧化鈦微粉顏色由原本二： 為淡黃色粉末，由XRD分析，改質溫度不會產生相轉變， 經由ESCA分析，在束缚能399 eV的位置有吸收峰存在 證明利用氨氣（NH3)可改質二氧化鈦形成含氮二& a 一乳化鈦 201002620 (ΤΑ·χΝχ胸，在uv_vis >析可明顯得知，含氮二氧化 I太（Τι·〇2·χΝχ)微粉的吸收笳圍 及收靶圍由波長400nm左右偏移至波 長550nm，明顯往可見光區移動。 在製程參數變化之摈_ 航堪七、+ 之^方面’本發明利用Box-Behnken /規S!i實驗’所得之最適化製程條件為：油相中界 ==己貌之體積比為°·。3:1、氨水濃度…Μ =相體積比_、異丙氧基銳與乙醯丙酮的莫耳* f、l · 4、異丙醇與異丙氧基鈦之莫耳比為加」， 疋延微乳膠溶液，經由確實 乂心 2/ ^ 叛果传到其比表面積約91 m g而為奈米級微粉，預測姓 、 分相折“旦 貝J、，，°果為941仏與實驗結果十 大：助：Γ化條件所製備出的粉末比表面積值為最 大，有助於提升光催化的效率。 巧取 研究指出乙醯丙嗣（AcetyIacetone)能 鈦整合，並於乙酿丙嗣配位之前導物中^=氧基 之燒氧基團比乙酿丙酮基團較容易被抽= 生較低 丙氧基欽水解速率緩慢，以形成Μ 此可使異 可改善勝體顆粒之顆粒大小 之顆粒。如此， 、刀怖均勻等物理,14暂 低陶究粉末之合成溫度，所以本發明之較佳實施針且降 知丙曝鈦離子(Ti，之水溶 、用乙 水相，以提高本發明所生產含氮 =為第—乳膠液的 外士找 氣—乳化銳微粉之品晳 用I:。利用實驗規劃法來求出最適化的製程:件另 ^此寺製程條件將可獲得分散性佳的奈米含氮二^敛 【圖式簡單說明】 12 201002620 第一圖為本發明較佳實施例的流程圖。 【主要元件符號說明】 無 13Preferably, the molar ratio of the isopropyl alcohol to the titanium isopropoxide is 23. The specific achievable effects of the present invention include: 1. The present invention utilizes acetamidine acetone to chelate with titanium isopropoxide, thereby Decreasing the hydrolysis rate of titanium isopropoxide to form particles with better homogeneity, and increasing the uniform distribution of the particle size of the colloidal particles, and also reducing the synthesis temperature of the titanium dioxide micropowder, and further, such as nitrogen The quality of titanium dioxide micropowder. 2 · The present invention utilizes the experimental specification, the table a +, and the π rule to determine the optimum process conditions, and by means of the optimum process conditions, the ^^ machi j U pays a good dispersion of the nanometer Nitrogen-containing titanium dioxide micropowder, and the absorption range of the nitrogen-containing β-muthene, 3忒-titanium-titanium powder is obviously 8 201002620 to the visible region mobility rate. It is helpful to improve the photocatalytic effect of the titanium dioxide micropowder. [Embodiment] The preferred embodiment of the invention comprises the following steps: providing a first latex solution: the first latex solution is an aqueous phase/oil phase () system The aqueous phase is Acetylacet〇ne integrated ion (: aqueous solution droplets, the first latex solution can be first made of organic non-polar / gluten (such as n_Hexane), interface activity a mixture of ethyl acetonide and titanium oxide oxide (Ti(0R)4) is mixed under (iv), and then a co-surfactant is added for emulsification and mixing (10) ng) The system may be isopropoxy, which is chelated with titanium isopropoxide to slow the rate of hydrolysis of titanium isopropoxide, and the surfactant may be a nonionic surfactant such as SPAN 4 〇/80 surfactants or HLB (hydr〇PhiliC-lipophilic balance) surfactants with values between 3 and 8. The ratio of the molar ratio of titanium ion, acetone, acetone and water in the mixed aqueous solution can be ^ 4:25, the co-surfactant can be isopropyl alcohol (IPA); providing a second latex solution The second latex liquid is an aqueous phase/oil phase (W/0) system 'the aqueous phase is an alkaline aqueous solution droplet, and the second latex liquid is prepared by "T first to make an organic non-polar solvent (such as己 烧 (n_Hexane), a surfactant and an alkaline aqueous solution are mixed at 45 〇c, and then a co-surfactant is added for emulsification mixing (EmulsiHcation Mixing), wherein the interface/tongue A 彳仏 can be non- Ionic surfactants, such as SPAN 40/80 surfactants or surfactants with a HLB (hydrophilic-lipophilic balance) value of 3-8 9 201002620, which can be more than 8M (eg 2m) An aqueous ammonia solution (NH4〇H), the co-surfactant may be isopropanol (IPA)'. The first and second latex systems may have the same aqueous/oil phase (w/0) volume ratio ; Buckle 5 two latexes. The first and second latex solutions are at 45. Mixing reaction for 1 hour under the armpit to form a mixed reaction solution containing a precursor; Oral distillation: Distilling the mixed reaction liquid by a vacuum vacuum concentrator to remove the oil phase, 'Drying lead: Mixing reaction liquid from which the oil phase has been removed The lead in the filter is dried by filtration; and the lead is calcined: the lead is dried in an ammonia (NH3) atmosphere of 400 to 600 V, and the nanometer nitrogen having photocatalytic properties under visible light is obtained. Titanium dioxide (Ti〇2-xNx) photocatalyst particles. The following examples are presented to make the features and advantages of the present invention clearer, but the following examples are not intended to limit the scope of the invention, but rather to indicate the method and materials of the invention, the scope of the invention The scope of the attached patent application shall prevail. Example 1 Preparation of Titanium Dioxide Precursor The first latex solution is an organic non-polar solvent (such as hexanone) as an oil phase, and a lipophilic surfactant (Span series) is added to agitate the homogenate, and the aqueous phase solution is a blend of ethylene and acetone. An aqueous solution of titanium (octa-etylacetonate) prepared from titanium isopropoxide; the second emulsion liquid is an organic non-solvent solvent (such as n-hexane), and the aqueous phase solution is ammonia water. The aqueous solution, the two 7-phase solutions are separately mixed into the oil phase using the same metering ratio to form two different types of reverse microcellular latex system from the water droplet type of 201002620, and then the appropriate amount of co-surfactant (isopropyl alcohol) is dropped into the two emulsion liquids. In the system, the first latex gradually turns into a clear, transparent, pale yellow solution, and the yellow second emulsion slowly becomes a transparent inverse latex solution; the latter two latexes are mixed with each other to cause the micelles to collide with the solution or Diffusion and nucleation reaction, followed by rotary concentrated distillation, drying at 200 ° C to obtain a titanium dioxide precursor (Precursor). Example 2, nitrogen-containing titanium dioxide fine powder preparation, the titanium dioxide of the example The conductive material is calcined under a high-temperature sintering method under an ammonia gas atmosphere to replace a part of oxygen atoms in the titanium oxide with nitrogen atoms, thereby increasing the absorption of titanium dioxide in the visible light region. In this embodiment, the flow of the ammonia gas is controlled to be 8 〇. m 1 / mi η, at a temperature of 600 ° C for 3 hours, the potential of nitrogen-containing titanium dioxide (Ti〇2_xNx). The prepared products are respectively X-ray powder crystal diffraction (XRD), chemistry Analytical electronic spectrometer (ESCA) and ultraviolet-visible spectrometer (UV-Vis) were used to examine the properties, and the effects of different process parameters were used to investigate the properties of the preparation. The process parameters included the temperature of hate burning (300~700. Compared with water, oil, ammonia concentration and co-interface active dose, etc., please refer to the process shown in the first figure for the above examples. In the nature of nitrogen-containing oxidized micro-powder, at 400. The anatase phase is produced. When the temperature is increased to 700 oc, the crystal phase is transformed into a rutile structure. The powder particle size is about 10~30 nm, and the specific surface area is about 30~95 m2/g. The color of the successfully modified titanium dioxide powder is determined by original : It is a light yellow powder. It is analyzed by XRD. The reforming temperature does not produce a phase transition. According to the ESCA analysis, there is an absorption peak at the position of 399 eV at the binding energy. It is proved that the ammonia (NH3) can be used to reform the titanium dioxide to form a nitrogen-containing two & a emulsified titanium 201002620 (ΤΑ·χΝχ chest, in uv_vis > analysis, it is obvious that the absorption range of the nitrogen-containing Dioxide I too (Τι·〇2·χΝχ) fine powder and the target circumference are about 400nm Move to the wavelength of 550nm, obviously moving to the visible region. In the process parameter change _ 航 Kan7, + ^ ^ 'The invention using Box-Behnken / S! i experiment' to obtain the optimum process conditions: oil phase The volume ratio of the middle boundary == appearance is °·. 3:1, ammonia concentration... Μ = phase volume ratio _, isopropoxy sharp and acetamidine acetone * f, l · 4, isopropyl alcohol and isopropoxy titanium molar ratio is added,疋 微 micro-latex solution, through the true heart 2 / ^ defect fruit to its specific surface area of about 91 mg for the nano-scale micro-powder, predicting the surname, the phase fold "Danbei J,,, ° fruit is 941 仏 and experiment Results Top Ten: Help: The specific surface area of the powder prepared by the deuteration condition is the largest, which helps to improve the efficiency of photocatalysis. The research indicates that Acety Iacetone can integrate titanium and brew in B. Before the coordination, the alkoxy group of the ^=oxy group is easier to be pumped than the ethyl acetate group. The rate of hydrolysis of the lower propoxy group is slow to form Μ, which can improve the granules. Granules of particle size. Thus, the physics of the knife and the like, 14 temporarily lower the synthesis temperature of the powder, so the preferred embodiment of the present invention reduces the exposure of titanium ions (Ti, water soluble, with aqueous phase E, In order to improve the production of nitrogen containing the first latex solution of the present invention, the scent of the emulsified sharp micropowder is improved by I: The experimental planning method is used to find the optimum process: the process conditions of the temple will be able to obtain the nanometer nitrogen with good dispersibility. [Illustration of the drawing] 12 201002620 The first figure is a preferred embodiment of the present invention. Flowchart. [Main component symbol description] No 13