TW201531590A - Method for producing a crednerite film - Google Patents
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本發明關於一種薄膜的製造方法，且尤其攸關一種錳銅礦薄膜的製造方法。 The present invention relates to a method for producing a film, and in particular to a method for producing a manganese-copper film.
錳銅礦為用簡式CuMnO2表示，其主要可作為用於生產氫氣的光觸媒(International Journal of Hydrogen Energy,28(2003)43-48)、或用於清除一氧化碳與一氧化二氮等氣體的三效催化劑(Applied Catalyst B：Environmental,89(2009)183-188)。 Manganese ore is represented by the simple CuMnO 2 , which can be mainly used as a photocatalyst for producing hydrogen (International Journal of Hydrogen Energy, 28 (2003) 43-48), or used to remove gases such as carbon monoxide and nitrous oxide. Three-way catalyst (Applied Catalyst B: Environmental, 89 (2009) 183-188).
迄今已有許多文獻報導製造錳銅礦粉末的方法。舉例而言，M.Trari等人提出使用固態反應法來合成錳銅礦粉末(Journal of Solid State Chemistry,178(2005)2751-2758)。又舉例而言，B.Bellal等人提出利用離子交換法來製造錳銅礦粉末(Journal of Applied Electrochemistry,41(2011)867-872)。然而，至今鮮有文獻報導製造錳銅礦薄膜的方法，僅H.Horaga及其團隊提出利用脈衝雷射沉積法(pulsed laser deposition，PLD)來沉積錳銅礦薄膜於一鋁酸鎂(MgAl2O4)基材上(Applied Physics Letters,95(2009)032109-032103、Physical Review B,84(2011)041411(R))。脈衝雷射沉積法須於昂貴的儀器內操作，於是提高了錳銅礦薄膜的製造成本並阻礙其普及性。 Many methods have been reported so far for the production of manganese copper ore powder. For example, M. Trari et al. proposed the use of a solid state reaction method to synthesize manganese copper ore powder (Journal of Solid State Chemistry, 178 (2005) 2751-2758). By way of further example, B. Bellal et al. propose the use of ion exchange to produce manganese copper ore powder (Journal of Applied Electrochemistry, 41 (2011) 867-872). However, there have been few reports on the production of manganese-copper films. Only H. Horaga and his team proposed the use of pulsed laser deposition (PLD) to deposit manganese-copper films on magnesium monosilicate (MgAl 2 ). O 4 ) on a substrate (Applied Physics Letters, 95 (2009) 032109-032103, Physical Review B, 84 (2011) 041411 (R)). Pulsed laser deposition is required to operate in expensive instruments, thus increasing the manufacturing cost of the manganese bronze film and impeding its popularity.
職是之故，開發一種製造錳銅礦薄膜的方法，其可降低得到之薄膜的製造成本並提升薄膜的普及性，乃為本發明所屬技術領域相關人士積極解決的議題之一。 For this reason, the development of a method for producing a manganese-copper film, which can reduce the manufacturing cost of the obtained film and improve the popularity of the film, is one of the topics actively addressed by those skilled in the art to which the present invention pertains.
本發明之一目的在於提出一種新穎之錳銅礦薄膜的製造方法，此法可降低製造成本，並改善製得之薄膜的普及性。 An object of the present invention is to provide a novel method for producing a manganese-copper film which can reduce the manufacturing cost and improve the popularity of the obtained film.
於是，為實現上述及/或其他目的，本發明提出一種錳銅礦薄膜的製造方法，其包含以下步驟：製備一溶膠-凝膠溶液，而溶膠-凝膠溶液含有銅鹽及錳鹽；塗佈溶膠-凝膠溶液於一基材上；於空氣中與300-600℃下，鍛燒溶膠-凝膠溶液，以形成一薄膜前驅物；以及於含氮氣及氧氣的氣體氛圍中與500-800℃下，鍛燒薄膜前驅物，以形成一CuMnO2錳銅礦薄膜。 Therefore, in order to achieve the above and/or other objects, the present invention provides a method for producing a manganese copper ore film, which comprises the steps of: preparing a sol-gel solution, wherein the sol-gel solution contains a copper salt and a manganese salt; The sol-gel solution is applied to a substrate; the sol-gel solution is calcined in air at 300-600 ° C to form a film precursor; and in a gas atmosphere containing nitrogen and oxygen and 500- The film precursor was calcined at 800 ° C to form a CuMnO 2 manganese copper ore film.
根據本發明，所提出之方法的步驟不像先前技術提到之脈衝雷射沉積法須於昂貴的儀器內實施便可得到CuMnO2錳銅礦薄膜。如此一來，可大幅降低製造CuMnO2錳銅礦薄膜的成本，還可促進CuMnO2錳銅礦薄膜的普及性。 According to the present invention, the steps of the proposed method do not require a pulsed laser deposition method as described in the prior art to be carried out in an expensive apparatus to obtain a CuMnO 2 manganese copper ore film. As a result, the cost of manufacturing the CuMnO 2 manganese copper ore film can be greatly reduced, and the popularity of the CuMnO 2 manganese copper ore film can also be promoted.
(S1)、(S2)、(S3)、(S4)‧‧‧步驟 (S1), (S2), (S3), (S4) ‧ ‧ steps
第一圖為一流程示意圖，以說明本發明一實施方式之錳銅礦薄膜的製造方法。 The first figure is a schematic flow chart for explaining a method for producing a manganese-copper film according to an embodiment of the present invention.
第二圖為一掃描式電子顯微鏡照片，以呈現製備例1之薄膜前驅物的外觀。 The second figure is a scanning electron microscope photograph showing the appearance of the film precursor of Preparation Example 1.
第三圖為一掃描式電子顯微鏡照片，以呈現製備例1之錳銅礦薄膜的外觀。 The third figure is a scanning electron microscope photograph showing the appearance of the manganese-copper film of Preparation Example 1.
第四圖為一掃描式電子顯微鏡照片，以呈現製備例2之錳銅礦薄膜的外觀。 The fourth figure is a scanning electron microscope photograph showing the appearance of the manganese-copper film of Preparation Example 2.
第五圖為一掃描式電子顯微鏡照片，以呈現製備例3之錳銅礦薄膜的外觀。 The fifth drawing is a scanning electron microscope photograph showing the appearance of the manganese-copper film of Preparation Example 3.
第六圖為一掃描式電子顯微鏡照片，以呈現製備例6之錳銅礦薄膜的外觀。 The sixth drawing is a scanning electron microscope photograph showing the appearance of the manganese-copper film of Preparation Example 6.
第七圖為一X射線繞射分析儀圖譜，以顯示製備例1之薄膜前驅物的化學組成。 The seventh figure is an X-ray diffraction analyzer map showing the chemical composition of the film precursor of Preparation Example 1.
第八圖為一X射線繞射分析儀圖譜，以顯示製備例1至5之錳銅礦薄膜的化學組成。 The eighth figure is an X-ray diffraction analyzer map showing the chemical compositions of the manganese-copper films of Preparation Examples 1 to 5.
第九圖為一X射線繞射分析儀圖譜，以顯示製備例6至9之錳銅礦薄膜的化學組成。 The ninth panel is an X-ray diffraction analyzer map showing the chemical compositions of the manganese-copper films of Preparation Examples 6 to 9.
第十圖為一(吸收係數x光子能量)2對光子能量的曲線圖，以推估製備例1之錳銅礦薄膜的直接能隙。 The tenth graph is a graph of (absorption coefficient x photon energy) 2 versus photon energy to estimate the direct energy gap of the manganese-copper film of Preparation Example 1.
第十一圖為一(吸收係數x光子能量)2對光子能量的曲線圖，以推估製備例2之錳銅礦薄膜的直接能隙。 The eleventh figure is a graph of (absorption coefficient x photon energy) 2 versus photon energy to estimate the direct energy gap of the manganese-copper film of Preparation 2.
第十二圖為一(吸收係數x光子能量)2對光子能量的曲線圖，以推估製備例3之錳銅礦薄膜的直接能隙。 Figure 12 is a graph of (absorption coefficient x photon energy) 2 versus photon energy to estimate the direct energy gap of the manganese-copper film of Preparation 3.
第十三圖為一(吸收係數x光子能量)2對光子能量的曲線圖，以推估製備例6之錳銅礦薄膜的直接能隙。 The thirteenth picture is a graph of (absorption coefficient x photon energy) 2 versus photon energy to estimate the direct energy gap of the manganese-copper film of Preparation Example 6.
為讓本發明上述及/或其他目的、功效、特徵更能明顯易懂，下文特舉較佳實施方式，作詳細說明。 The above and/or other objects, features and features of the present invention will become more apparent from the Detailed Description
請參閱第一圖，於本發明之一實施方式，揭示一種錳銅礦薄膜的製造方法，其詳細過程如下述： 首先，如步驟S1所示，製備一溶膠-凝膠溶液，而溶膠-凝膠溶液含有銅鹽及錳鹽。銅鹽的實例可以為但不限於，醋酸銅(Cu(CH3COO)2)，而錳鹽的實例可以為但不限於，醋酸錳(Mn(CH3COO)2)。操作步驟S1時，溶膠-凝膠溶液更含有三乙醇胺(triethanolamine，TEA)，含這一化合物的用意在於：於後續步驟，促進錳鹽中之錳離子(Mn2+)及銅鹽中之銅離子(Cu2+)間相互的碰撞，從而增進後續之CuMnO2錳銅礦薄膜的產生。 Referring to the first figure, in an embodiment of the present invention, a method for manufacturing a manganese copper ore film is disclosed. The detailed process is as follows: First, as shown in step S1, a sol-gel solution is prepared, and the sol-condensation is performed. The gum solution contains a copper salt and a manganese salt. Examples of the copper salt may be, but not limited to, copper acetate (Cu(CH 3 COO) 2 ), and examples of the manganese salt may be, but not limited to, manganese acetate (Mn(CH 3 COO) 2 ). In the step S1, the sol-gel solution further contains triethanolamine (TEA), and the intention of containing the compound is to promote the manganese ion (Mn 2+ ) in the manganese salt and the copper salt in the copper salt in the subsequent step. The ions (Cu 2+ ) collide with each other, thereby promoting the production of the subsequent CuMnO 2 manganese copper ore film.
其次，如步驟S2所示，塗佈溶膠-凝膠溶液於一基材上。基材的實例可以為但不限於，石英基材。 Next, as shown in step S2, the sol-gel solution is applied to a substrate. Examples of the substrate may be, but not limited to, a quartz substrate.
接著，如步驟S3所示，於空氣中與300-600℃下，鍛燒溶膠-凝膠溶液，以形成一薄膜前驅物。於本實施方式，步驟S3的溫度為500℃。此外，此步驟的時間不應受到任何限制，只要可以完成此步驟的目的即可；於本實施方式，時間約為45-75分鐘。 Next, as shown in step S3, the sol-gel solution is calcined in air at 300-600 ° C to form a film precursor. In the present embodiment, the temperature in the step S3 is 500 °C. In addition, the time of this step should not be subject to any limitation as long as the purpose of this step can be completed; in the present embodiment, the time is about 45-75 minutes.
最後，如步驟S4所示，於含氮氣及氧氣的氣體氛圍中與500-800℃下，鍛燒薄膜前驅物，以形成CuMnO2錳銅礦薄膜。一般而言，氣體氛圍的氮氣分壓及氧氣分壓不應受到任何侷限，只要能形成薄膜即可；於本實施方式，氮氣分壓為0.999-0.99995atm，氧氣分壓為5x10-5-10-3atm。此外，步驟S4的時間不應受到任何限制，只要能達成此步驟的目的即可；而於本實施方式，時間約為90-150分鐘。 Finally, as shown in step S4, the film precursor is calcined in a gas atmosphere containing nitrogen and oxygen at 500-800 ° C to form a CuMnO 2 manganese copper ore film. In general, the partial pressure of nitrogen and the partial pressure of oxygen in the gas atmosphere should not be subject to any limitation as long as a film can be formed. In the present embodiment, the partial pressure of nitrogen is 0.999-0.99995 atm, and the partial pressure of oxygen is 5×10 -5 -10. -3 atm. Further, the time of step S4 should not be subject to any limitation as long as the purpose of this step can be achieved; and in the present embodiment, the time is about 90-150 minutes.
本發明人不可思議地觀察到當步驟S4的溫度、氮氣分壓、與氧氣分壓滿足以下條件時，形成之CuMnO2錳銅礦薄膜的晶相僅含CuMnO2，而不含任何雜質：(1)溫度為600-700℃，而氮氣分壓為 0.99995atm，氧氣分壓為5x10-5atm；或(2)溫度為700℃，而氮氣分壓為0.999atm，氧氣分壓為10-3atm。 The inventors have inconceivably observed that when the temperature of step S4, the partial pressure of nitrogen, and the partial pressure of oxygen satisfy the following conditions, the crystal phase of the formed CuMnO 2 manganese copper ore thin film contains only CuMnO 2 and does not contain any impurities: (1) The temperature is 600-700 ° C, and the partial pressure of nitrogen is 0.99995 atm, the partial pressure of oxygen is 5x10 -5 atm; or (2) the temperature is 700 ° C, and the partial pressure of nitrogen is 0.999 atm, and the partial pressure of oxygen is 10 -3 atm. .
茲以下述實施例進一步例示說明本發明的實施方式： Embodiments of the invention are further illustrated by the following examples:
《製備例1》 Preparation Example 1
首先，將2.1962克醋酸銅．一水合物(Cu(CH3COO)2．H2O)及2.2058克醋酸錳．四水合物(Mn(CH3COO)2．4H2O)加入至30毫升95%乙醇中，並持續攪拌約1小時。接著，加入5克三乙醇胺至得到的乙醇溶液中，並持續攪拌約24小時。之後，以旋轉塗佈方式(轉速：2000rpm，時間：15秒)均勻塗佈乙醇溶液於一石英基材上。然後，將塗佈於石英基材的乙醇溶液置於一於空氣中之500℃高溫爐內，並靜置於空氣與前述溫度下約1小時，以鍛燒乙醇溶液成一薄膜前驅物。最後，通入氮氣分壓為0.99995atm，氧氣分壓為5x10-5atm的氣體氛圍至薄膜前驅物，再以升溫速度5℃/分鐘加熱薄膜前驅物至700℃，並靜放於此氣體氛圍與溫度下2小時，以鍛燒薄膜前驅物成一錳銅礦薄膜。 First, it will be 2.1962 grams of copper acetate. Monohydrate (Cu(CH 3 COO) 2 .H 2 O) and 2.2058 g of manganese acetate. The tetrahydrate (Mn(CH 3 COO) 2 .4H 2 O) was added to 30 ml of 95% ethanol and stirring was continued for about 1 hour. Next, 5 g of triethanolamine was added to the obtained ethanol solution, and stirring was continued for about 24 hours. Thereafter, the ethanol solution was uniformly applied onto a quartz substrate by a spin coating method (rotation speed: 2000 rpm, time: 15 seconds). Then, the ethanol solution coated on the quartz substrate was placed in a high-temperature furnace at 500 ° C in air, and left to stand in air at the above temperature for about 1 hour to calcine the ethanol solution to form a film precursor. Finally, a nitrogen gas partial pressure of 0.99995 atm, a partial pressure of oxygen of 5 x 10 -5 atm was applied to the film precursor, and the film precursor was heated to 700 ° C at a heating rate of 5 ° C / min, and allowed to stand at this gas atmosphere. The manganese film was formed into a manganese-copper film by calcining the film precursor at a temperature of 2 hours.
《製備例2》 Preparation Example 2
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的，除了薄膜前驅物的鍛燒溫度為650℃。 The manganese copper ore thin film of this preparation example was formed by the method described in Reference Production Example 1, except that the calcination temperature of the film precursor was 650 °C.
《製備例3》 Preparation Example 3
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的，除了薄膜前驅物的鍛燒溫度為600℃。 The manganese bronze film of this preparation example was formed by the method described in Reference Production Example 1, except that the calcination temperature of the film precursor was 600 °C.
《製備例4》 Preparation 4
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的， 除了薄膜前驅物的鍛燒溫度為550℃。 The manganese copper ore thin film of the preparation example is formed by the method described in Reference Preparation Example 1, The calcination temperature of the film precursor was 550 ° C.
《製備例5》 Preparation Example 5
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的，除了薄膜前驅物的鍛燒溫度為500℃。 The manganese bronze film of this preparation example was formed by the method described in Reference Production Example 1, except that the calcination temperature of the film precursor was 500 °C.
《製備例6》 Preparation Example 6
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的，除了氣體氛圍的氮氣分壓為0.999atm，氧氣分壓為10-3atm，而薄膜前驅物的鍛燒溫度為700℃。 The manganese-copper film of the present preparation was formed by the method described in Reference Preparation Example 1, except that the partial pressure of nitrogen in the gas atmosphere was 0.999 atm, the partial pressure of oxygen was 10 -3 atm, and the calcination temperature of the film precursor was 700. °C.
《製備例7》 Preparation Example 7
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的，除了氣體氛圍的氮氣分壓為0.999atm，氧氣分壓為10-3atm，而薄膜前驅物的鍛燒溫度為600℃。 The manganese-copper film of the present preparation was formed by the method described in Reference Preparation Example 1, except that the partial pressure of nitrogen in the gas atmosphere was 0.999 atm, the partial pressure of oxygen was 10 -3 atm, and the calcination temperature of the film precursor was 600. °C.
《製備例8》 Preparation Example 8
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的，除了氣體氛圍的氮氣分壓為0.999atm，氧氣分壓為10-3atm，而薄膜前驅物的鍛燒溫度為550℃。 The manganese-copper film of the present preparation was formed by the method described in Reference Preparation Example 1, except that the partial pressure of nitrogen in the gas atmosphere was 0.999 atm, the partial pressure of oxygen was 10 -3 atm, and the calcination temperature of the film precursor was 550. °C.
《製備例9》 Preparation Example 9
本製備例的錳銅礦薄膜為參考製備例1所述的方法形成的，除了氣體氛圍的氮氣分壓為0.999atm，氧氣分壓為10-3atm，而薄膜前驅物的鍛燒溫度為500℃。 The manganese-copper film of the present preparation was formed by the method described in Reference Preparation Example 1, except that the partial pressure of nitrogen in the gas atmosphere was 0.999 atm, the partial pressure of oxygen was 10 -3 atm, and the calcination temperature of the film precursor was 500. °C.
《分析例1》 Analysis Example 1
本分析為透過掃描式電子顯微鏡來觀察製備例1之薄膜前驅 物、及製備例1、2、3與6之錳銅礦薄膜的外觀。如第二圖，製備例1的薄膜前驅物具有奈米晶粒(nano-granular)的外貌；然而，如第三至六圖，製備例1、2、3與6之錳銅礦薄膜具有晶粒表面的外貌。這些外貌的差異可能為製備例1、2、3與6之錳銅礦薄膜的晶相主要含CuMnO2，而製備例1之薄膜前驅物的晶相不含CuMnO2所導致的。 The analysis was carried out by observing the appearance of the film precursor of Preparation Example 1 and the manganese-copper film of Preparation Examples 1, 2, 3 and 6 by a scanning electron microscope. As shown in the second figure, the film precursor of Preparation Example 1 has a nano-granular appearance; however, as in the third to sixth figures, the manganese-copper films of Preparation Examples 1, 2, 3 and 6 have crystals. The appearance of the grain surface. The difference in these appearances may be that the crystal phase of the manganese-copper film of Preparation Examples 1, 2 , 3 and 6 mainly contains CuMnO 2 , and the crystal phase of the film precursor of Preparation Example 1 does not contain CuMnO 2 .
《分析例2》 Analysis Example 2
本分析為採用X射線繞射分析儀來確認製備例1之薄膜前驅物、及製備例1至9之錳銅礦薄膜的化學組成。如第七圖，製備例1之薄膜前驅物的晶相主要為CuMn2O4；相對地，如第八、九圖，製備例1至9之錳銅礦薄膜的晶相主要含CuMnO2，且特別是製備例1、2、3及6之錳銅礦薄膜的晶相僅含CuMnO2，而不含任何雜質。 This analysis was to confirm the chemical composition of the film precursor of Preparation Example 1 and the manganese-copper film of Preparation Examples 1 to 9 by using an X-ray diffraction analyzer. As shown in the seventh figure, the crystal phase of the film precursor of Preparation Example 1 is mainly CuMn 2 O 4 ; in contrast, as in the eighth and ninth views, the crystal phase of the manganese-copper film of Preparation Examples 1 to 9 mainly contains CuMnO 2 , And in particular, the crystal phases of the manganese-copper films of Preparation Examples 1, 2, 3 and 6 contain only CuMnO 2 and do not contain any impurities.
《分析例3》 Analysis Example 3
本分析為利用可見光-紫外光光譜儀並搭配Davis-Mott模型理論，來計算製備例1、2、3與6之錳銅礦薄膜的直接能隙。如第十至十三圖，上述錳銅礦薄膜的直接能隙均落於3.43-4.22eV的範圍內。 In this analysis, the direct energy gaps of the manganese-copper films of Preparation Examples 1, 2, 3 and 6 were calculated using a visible light-ultraviolet spectrometer combined with the Davis-Mott model theory. As shown in the tenth to thirteenth graphs, the direct energy gaps of the above manganese-copper films are all in the range of 3.43-4.22 eV.
綜合上述實施例，證實了本發明之實施方式得到的CuMnO2錳銅礦薄膜不須於昂貴的儀器內便可形成；這麼一來，本發明之實施方式的方法可降低製造CuMnO2錳銅礦薄膜的成本，還可一併促進CuMnO2錳銅礦薄膜的普及性。而且，製備例1、2、3及6得到之薄膜的晶相僅含CuMnO2而不含任何雜質，更為本發明所屬技術領域中相當難得的結果。 In combination with the above examples, it was confirmed that the CuMnO 2 manganese copper ore thin film obtained by the embodiment of the present invention can be formed without using an expensive instrument; thus, the method of the embodiment of the present invention can reduce the manufacture of CuMnO 2 manganese copper ore. The cost of the film can also promote the popularity of the CuMnO 2 manganese copper ore film. Further, the crystal phases of the films obtained in Preparation Examples 1, 2, 3 and 6 contained only CuMnO 2 without any impurities, and were quite rare results in the technical field to which the present invention pertains.
惟以上所述者，僅為本發明之較佳實施例，但不能以此限定本發明實施之範圍；故，凡依本發明申請專利範圍及發明說明書內容所作 之簡單的等效改變與修飾，皆仍屬本發明專利涵蓋之範圍內。 However, the above is only the preferred embodiment of the present invention, but it is not intended to limit the scope of the present invention; therefore, the scope of the patent application and the contents of the invention are Simple equivalent changes and modifications are still within the scope of the invention.
(S1)、(S2)、(S3)、(S4)‧‧‧步驟 (S1), (S2), (S3), (S4) ‧ ‧ steps
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