TWI485383B - System and method for the detection of the number of graphene layers - Google Patents
System and method for the detection of the number of graphene layers Download PDFInfo
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本發明係關於一種石墨烯薄膜檢測系統及檢測方法,尤關於一種應用於石墨烯薄膜層數檢測的影像分析系統及方法。The invention relates to a graphene film detecting system and a detecting method, in particular to an image analyzing system and method applied to the graphene layer layer number detecting.
隨著石墨技術的發展,石墨烯薄膜的可視化,亦即如何確定石墨烯薄膜厚度及其層數,尤其是如何確定低層數石墨烯薄膜(few-layer graphene,FLG)之層數,即成極為重要之課題。既有技術判別石墨烯薄膜層數方式包括有:拉曼(Raman)光譜技術、穿透頻譜技術、使用原子力顯微鏡(AFM)之技術以及使用光學顯微鏡之技術。With the development of graphite technology, the visualization of graphene film, that is, how to determine the thickness of graphene film and its number of layers, especially how to determine the number of layers of low-layer graphene film (FLG), is extremely Important topic. Existing techniques for discriminating graphene film layers include: Raman spectroscopy, penetration spectroscopy, techniques using atomic force microscopy (AFM), and techniques using optical microscopy.
(一)拉曼頻譜技術及穿透頻譜技術(1) Raman spectrum technology and penetration spectrum technology
如參考文獻17所述,拉曼頻譜技術可以藉由判別G-band之強度改變,以及2D-band之拉曼頻率改變,對於石墨烯薄膜之層數進行檢測。As described in reference 17, the Raman spectrum technique can detect the number of layers of the graphene film by discriminating the intensity change of the G-band and the Raman frequency change of the 2D-band.
參考文獻19揭露有藉由拉曼頻譜,於二氧化矽/矽(SiO2 /Si)基板上,計算原子面數層石墨之技術。其藉由拉曼頻譜於二氧化矽/矽(SiO2 /Si)基板上計數原子面數層石墨,測量石墨峰和矽的光學聲子峰綜合強度比,而能在石墨烯薄膜層數大於4層(N>4)之範圍,發揮獲取石墨烯 薄膜層數資訊之效果。Reference 19 discloses a technique for calculating an atomic number of layers of graphite on a ceria/ytterbium (SiO 2 /Si) substrate by Raman spectrum. The Raman spectrum is used to count the atomic plane layer graphite on the cerium oxide/cerium (SiO 2 /Si) substrate, and the comprehensive intensity ratio of the optical phonon peak of the graphite peak and the ytterbium is measured, and the number of layers of the graphene film is larger than The range of 4 layers (N>4) is used to obtain the information of the number of layers of graphene film.
如參考文獻18所述,單層石墨烯薄膜的穿透率為97.7%,穿透頻譜技術可以透過量測穿透率的方式得到石墨烯薄膜層數資訊。As described in Reference 18, the transmittance of the single-layer graphene film is 97.7%, and the penetration spectrum technique can obtain the graphene layer number information by measuring the transmittance.
當採用前述拉曼頻譜技術和穿透頻譜技術時,需要拉曼頻譜與穿透頻譜驗證過程,該驗證過程極為耗時耗力。例如,使用拉曼頻譜的成像技術,需3個小時方得確定完成一件大約50 μm2 之石墨烯薄膜檢測;此外,拉曼頻譜的檢測方式,仍存有若干模糊區域,導致無法確定真實石墨烯薄膜的層數。When the aforementioned Raman spectrum technique and the penetration spectrum technique are employed, a Raman spectrum and a penetration spectrum verification process are required, which is extremely time consuming and labor intensive. For example, using the imaging technique of the Raman spectrum, it takes 3 hours to determine the completion of a graphene film detection of about 50 μm 2 ; in addition, the detection method of the Raman spectrum still has a number of blurred regions, which makes it impossible to determine the true The number of layers of graphene film.
(二)使用原子力顯微鏡之技術(2) Technology using atomic force microscopy
如參考文獻19所示,單層石墨烯薄膜之厚度約為0.34 nm,使用原子力顯微鏡之技術可藉由判別表面的粗糙度,得到石墨烯薄膜層數資訊。然而該使用原子力顯微鏡之技術,亦需極長之測量時間。As shown in reference 19, the thickness of the single-layer graphene film is about 0.34 nm, and the technique of atomic force microscopy can be used to determine the roughness of the surface to obtain the graphene layer number information. However, the technique of using atomic force microscopy also requires extremely long measurement times.
(三)使用光學顯微鏡之技術(3) Technology using optical microscopy
另就使用光學顯微鏡之既有技術而言,參考文獻14所揭露者,係於諸如二氧化矽/矽基板、二氧化矽(SiO2 )、氮化矽(Si3 N4 )、三氧化二鋁(Al2 O3 )等不同介電層,更加徹底地分析多層石墨烯薄膜之顏色,以藉由薄膜光學辨識出層數的差異性。In addition to the prior art using optical microscopy, the disclosure of reference 14 is based on, for example, a cerium oxide/cerium substrate, cerium oxide (SiO 2 ), cerium nitride (Si 3 N 4 ), and trioxide. Different dielectric layers such as aluminum (Al 2 O 3 ) are used to more thoroughly analyze the color of the multilayer graphene film to optically identify the difference in the number of layers by the film.
參考文獻12揭露一種特定基板上進行顯微影像技術檢測石墨烯薄膜層數的方法,從其研究可以發現在矽基板上鍍上一層300奈米的SiO2 ,可以分辨石墨烯薄膜,若是在100奈米的二氧化矽上觀察石墨烯薄膜,有最 好的視覺效果。該文獻指出於285奈米氧化層之二氧化矽/矽基板可以大幅提高石墨烯薄膜之可視性,並利用計算色差之方法,驗證其理論之合理性。Reference 12 discloses a method for detecting the number of layers of graphene film by microscopic imaging technology on a specific substrate. From the research, it can be found that a layer of 300 nm of SiO 2 is plated on the substrate, and the graphene film can be distinguished. The graphene film is observed on the nanometer cerium oxide and has the best visual effect. This paper points out that the cerium oxide/germanium substrate in the 285 nm oxide layer can greatly improve the visibility of the graphene film, and the rationality of the theory is verified by the method of calculating the color difference.
參考文獻13揭露一個多頻譜技術之光學方法,提出識別和測量用奈米厚度和石墨當基礎材料的有效光學特性,而此材料是用薄絕緣層上矽的基板作為基礎材料。透過選擇適當的光學性能和絕緣層厚度的石墨烯薄膜為基礎材料和基板之間的高度做對比。石墨氧化物的有效折射率和光吸收係數、熱還原氧化石墨和石墨可被獲得透過比較預測和實測的差別。Reference 13 discloses an optical method of a multi-spectral technique, which proposes a nanometer thickness for identification and measurement and an effective optical characteristic of graphite as a base material, which is a substrate made of a thin insulating layer. The height between the base material and the substrate is compared by selecting a graphene film of appropriate optical properties and thickness of the insulating layer. The effective refractive index and light absorption coefficient of graphite oxide, thermally reduced graphite oxide and graphite can be obtained by comparing the predicted and measured differences.
參考文獻15揭露針對諸如碳化矽(SiC)、二氧化矽/矽、石英(quartz)、矽、玻璃等不同基板,由於不同材料有不同的晶格常數以及電子結構,石墨烯薄膜之觀測即受到基板效應影響,造成對於觀測石墨烯薄膜層數之差異。該文獻指出於石英基板及二氧化矽/矽基板觀測石墨烯薄膜層數,有著較高的色差對比。Reference 15 discloses that for different substrates such as tantalum carbide (SiC), ruthenium dioxide/ruthenium, quartz, tantalum, glass, etc., since different materials have different lattice constants and electronic structures, the observation of graphene films is affected. The influence of the substrate effect causes a difference in the number of layers of the graphene film observed. This document points out that the number of layers of graphene film is observed on a quartz substrate and a ceria/germanium substrate, which has a high contrast of color difference.
參考文獻14所揭露之既有技術採用不同波段之光源對二氧化矽/矽基板、氮化矽、三氧化二鋁做不同層數石墨烯薄膜觀測做色差模擬,結果指出於氮化矽適用於觀測低層數石墨烯薄膜、於二氧化矽/矽適用於觀測中層數石墨烯薄膜、於三氧化二鋁適用於觀測高層數石墨烯薄膜。The prior art disclosed in Reference 14 uses different wavelengths of light sources to simulate the erbium dioxide/germanium substrate, tantalum nitride, and aluminum oxide as different layers of graphene film. The results indicate that the tantalum nitride is suitable for Observing the low-layer graphene film, the ceria/矽 is suitable for observing the middle layer graphene film, and the aluminum oxide is suitable for observing the high-order graphene film.
參考文獻16則揭露分別在二氧化矽/矽與二氧化矽/空氣(SiO2 /air)不同基材做色差之分析,其述及各種絕緣層上沉積多層石墨和石墨烯薄膜氧化物的顏色,且分析對材料厚度的影響、絕緣層的類型和矽基板後部的存在進 行了分析。其雖指出二氧化矽/矽基板上的氧化石墨層顏色被發現會隨著材料厚度的增加而有週期性地改變,然而,在同一基板上的石墨層顏色呈現飽和而無類似之週期性變化。Reference 16 discloses the analysis of the color difference between different substrates of cerium oxide/cerium and cerium oxide/air (SiO 2 /air), which describes the color of various layers of graphite and graphene thin film oxide deposited on various insulating layers. And analysis of the effect on the thickness of the material, the type of insulation layer and the presence of the back of the ruthenium substrate were analyzed. Although it is pointed out that the color of the graphite oxide layer on the ceria/germanium substrate is found to change periodically as the thickness of the material increases, however, the color of the graphite layer on the same substrate is saturated without similar periodic changes. .
綜上所述,既有技術使用光學顯微鏡提供快速成像速度,特別是利用多頻譜技術,可作為一種快速和直觀的方式,以檢測多層石墨烯薄膜之層數。但是,這種使用光學顯微鏡的既有技術,需要特定厚度的基板,而在透明基板上,無法實施該使用光學顯微鏡之既有技術。In summary, the prior art uses optical microscopy to provide fast imaging speeds, particularly with multi-spectral techniques, as a quick and intuitive way to detect the number of layers of a multilayer graphene film. However, such a technique using an optical microscope requires a substrate of a specific thickness, and on a transparent substrate, the prior art using an optical microscope cannot be implemented.
此外,既有使用光學顯微鏡檢測石墨烯薄膜層數之技術,雖可於特定基板厚度結構下,透過顯微鏡以視覺辨識檢測石墨烯薄膜的層數,例如,在矽基板上鍍上300奈米的二氧化矽介電層,然後將石墨烯薄膜鍍於該結構之基板下,再檢測石墨烯薄膜的層數)。然而,該使用光學顯微鏡之既有技術的缺點,卻增加了製作石墨烯薄膜電子元件所需之步驟及流程。In addition, there is a technique of detecting the number of graphene film layers by using an optical microscope. Although the number of layers of the graphene film can be visually recognized through a microscope under a specific substrate thickness structure, for example, 300 nm is plated on the tantalum substrate. The ruthenium dioxide dielectric layer is then plated with a graphene film under the substrate of the structure, and the number of layers of the graphene film is detected. However, the disadvantages of the prior art using optical microscopy have increased the steps and processes required to fabricate graphene thin film electronic components.
又該使用光學顯微鏡之既有技術,在檢測低層數石墨烯薄膜層數的視覺對比上尚待加強。例如:對於轉印在玻璃基板上的五層石墨烯薄膜,實施該使用光學顯微鏡之既有技術,可發現其於光學顯微鏡下視覺對比不足,幾乎無法觀測石墨烯薄膜,從而無法檢測石墨烯薄膜之層數。In addition, the prior art using optical microscopy has yet to be strengthened in visual comparison of the number of layers of graphene films. For example, for a five-layer graphene film transferred onto a glass substrate, the prior art using an optical microscope can be found to have insufficient visual contrast under an optical microscope, and it is almost impossible to observe a graphene film, thereby failing to detect a graphene film. The number of layers.
有鑒於既有使用拉曼頻譜與穿透頻譜之技術需要耗時耗力的驗證過程、既有使用原子力顯微鏡之技術需 要昂貴儀器長時間測量,既有使用光學顯微鏡之技術需要特定厚度的基板導致於無法實施於透明基板上之缺點,加上以及既有使用光學顯微鏡之技術檢測低層數石墨烯薄膜的視覺對比不足之缺點,本發明之目的在於改善該等缺點,搭配顯微鏡、感光耦合元件(Charge-Coupled Device,CCD)等取像裝置使用多頻譜色彩影像再現技術,於透明基板或不透明基板對低層數之石墨烯薄膜進行快速檢測,且可資應用於相關產業進行諸如良率、品質之檢測,進而提供快速的判別、佐證石墨烯薄膜層數之技術手段。In view of the time-consuming and labor-intensive verification process required to use the Raman spectrum and the penetrating spectrum, there is a need for the use of atomic force microscopy. Long-term measurement of expensive instruments, the use of optical microscopy technology requires a certain thickness of the substrate to cause the failure to implement on the transparent substrate, plus the use of optical microscopy technology to detect low-layer graphene film visual contrast Disadvantages of the present invention are to improve the disadvantages, and to use a multi-spectral color image reproduction technology with a microscope, a photosensitive coupling device (CCD), or the like, to use a multi-spectral color image reproduction technique on a transparent substrate or an opaque substrate to lower the number of layers of graphite. The olefin film is rapidly detected and can be applied to related industries such as detection of yield and quality, thereby providing a rapid method for judging and verifying the number of layers of graphene film.
為達到前述目的,本發明所採用之技術手段係使用色彩學之多頻譜影像技術,基於在石墨烯薄膜不同層數間諸如破壞性干涉或建設性干涉等不同的頻譜表現,結合主軸成分分析,量化頻譜數據,以第一主軸與第二主軸之比重係數定義出不同層數間之群落,並藉由群落之區分檢測低層數石墨烯薄膜層數之光學顯微鏡影像,進而提供應用於石墨烯薄膜層數檢測的影像分析系統以及分析方法。In order to achieve the foregoing objectives, the technical means adopted by the present invention uses a multi-spectral image technique of chromaticity, based on different spectral expressions such as destructive interference or constructive interference between different layers of graphene films, combined with spindle component analysis, Quantifying the spectral data, defining a community between different layers by the specific gravity coefficient of the first main axis and the second main axis, and detecting the optical microscope image of the number of layers of the low-layer graphene film by the distinction of the community, thereby providing the application to the graphene film Image analysis system and analysis method for layer number detection.
具體而言,本發明可使用多頻譜技術進行主軸成分分析並判定閥值,得到不同層數間之模擬重建的影像圖形,以達到快速檢測低層數之石墨烯薄膜層數(N)之效果。Specifically, the present invention can use the multi-spectral technique to perform spindle component analysis and determine the threshold value, and obtain an image image of the simulated reconstruction between different layers to achieve the effect of rapidly detecting the number of layers (N) of the graphene film having a low number of layers.
本發明克服既有技術之問題,不僅突破基板厚度與結構之限制,且能更為及時而正確地檢測石墨烯薄膜。又本發明之多頻譜技術透過主軸成份分析法搭配色適應轉換以及線性回歸等方法,得以實現細胞之色彩再現, 無須控制顯微鏡內照明光源的顏色變化,採用明確且單純之儀器及演算法參數,即可有效實現石墨烯薄膜檢測與分析。因此本發明得以省去傳統耗時耗力的拉曼頻譜與穿透頻譜驗證過程,亦無需使用原子力顯微鏡等昂貴儀器進行長時間之測量,確實能夠提供有效率、低成本、低工時之技術,以發揮便利檢測低層數石墨烯薄膜層數之發明效果。The invention overcomes the problems of the prior art, not only breaks through the limitation of the thickness and structure of the substrate, but also can detect the graphene film more timely and correctly. The multi-spectral technology of the present invention achieves color reproduction of cells through a spindle component analysis method combined with color adaptive conversion and linear regression. It is not necessary to control the color change of the illumination source in the microscope, and the detection and analysis of the graphene film can be effectively realized by using clear and simple instruments and algorithm parameters. Therefore, the invention can save the traditional time-consuming and labor-intensive Raman spectrum and the penetration spectrum verification process, and does not need to use an expensive instrument such as an atomic force microscope for long-term measurement, and can indeed provide efficient, low-cost, low-time technology. In order to facilitate the invention of the effect of detecting the number of layers of the graphene film in the lower layer.
10‧‧‧觀察模組10‧‧‧Observation module
11‧‧‧載臺單元11‧‧‧stage unit
12‧‧‧照明單元12‧‧‧Lighting unit
13‧‧‧影像放大單元13‧‧‧Image magnification unit
14‧‧‧濾光單元14‧‧‧ Filter unit
20‧‧‧取像模組20‧‧‧Image capture module
21‧‧‧透鏡單元21‧‧‧ lens unit
22‧‧‧感光耦合單元22‧‧‧Photosensitive coupling unit
23‧‧‧擷取單元23‧‧‧Capture unit
30‧‧‧多頻譜色彩影像再現模組30‧‧‧Multi-spectral color image reproduction module
31‧‧‧頻譜分析步驟31‧‧‧ Spectrum analysis steps
32‧‧‧色彩增益步驟32‧‧‧Color gain step
33‧‧‧色彩影像再現步驟33‧‧‧Color image reproduction steps
40‧‧‧石墨烯薄膜樣本40‧‧‧ Graphene film samples
圖1係本發明之應用於石墨烯薄膜層數檢測的影像分析系統之示意圖。1 is a schematic diagram of an image analysis system of the present invention applied to layer number detection of graphene films.
圖2係本發明之應用於石墨烯薄膜層數檢測的影像分析系統之另一示意圖。2 is another schematic diagram of an image analysis system of the present invention applied to layer number detection of graphene films.
圖3係以拉曼頻譜分析成長有低層數石墨烯薄膜之玻璃基板之彩色圖。圖中數字符號0至5係分別標註石墨烯薄膜層數所對應之色階。Figure 3 is a color diagram of a glass substrate grown with a low number of graphene films by Raman spectrum analysis. The numerical symbols 0 to 5 in the figure respectively indicate the color gradation corresponding to the number of layers of the graphene film.
圖4係以拉曼頻譜分析成長有低層數石墨烯薄膜之玻璃基板之灰階圖。圖中數字符號0至5係分別標註石墨烯薄膜層數所對應之色階。Fig. 4 is a gray scale diagram of a glass substrate on which a low number of graphene films are grown by Raman spectrum analysis. The numerical symbols 0 to 5 in the figure respectively indicate the color gradation corresponding to the number of layers of the graphene film.
圖5係以本發明分析成長有低層數石墨烯薄膜之玻璃基板之彩色圖。圖中數字符號0至5係分別標註石墨烯薄膜層數所對應之色階。Figure 5 is a color diagram of a glass substrate having a low number of graphene films grown by the present invention. The numerical symbols 0 to 5 in the figure respectively indicate the color gradation corresponding to the number of layers of the graphene film.
圖6係以本發明分析成長有低層數石墨烯薄膜之玻璃基板之灰階圖。圖中數字符號0至5係分別標註石墨烯薄膜層數所對應之色階。Figure 6 is a gray scale diagram of a glass substrate on which a low number of graphene films are grown by the present invention. The numerical symbols 0 to 5 in the figure respectively indicate the color gradation corresponding to the number of layers of the graphene film.
圖7係於二氧化矽/矽基板成長三層石墨烯薄膜之影像。Figure 7 is an image of a three-layer graphene film grown on a ceria/ruthenium substrate.
圖8係成長有五層石墨烯薄膜之玻璃基板之外觀圖。Fig. 8 is an external view of a glass substrate on which a five-layer graphene film is grown.
圖9係成長於玻璃基板之五層石墨烯薄膜之結構示意圖。Fig. 9 is a schematic view showing the structure of a five-layer graphene film grown on a glass substrate.
圖10係對於成長有五層石墨烯薄膜之玻璃基板之劃分圖。Fig. 10 is a sectional view of a glass substrate on which a five-layer graphene film is grown.
圖11係對於成長有五層石墨烯薄膜之玻璃基板之跨不同層數區域之選取示意圖及各區域放大圖。Fig. 11 is a schematic view showing the selection of regions across different layers of a glass substrate on which five layers of graphene film are grown, and an enlarged view of each region.
圖12係以用以建立模組而量測反射頻譜之24色塊列示模擬色塊以及顯微鏡色塊之間色差之圖表。Figure 12 is a graph showing the color difference between the analog patch and the microscope patch in a 24-color block for measuring the reflected spectrum.
圖13係求出頻譜儀與取像裝置間轉換矩陣之流程圖。Fig. 13 is a flow chart for finding a conversion matrix between the spectrum analyzer and the image capturing device.
圖14係求出模擬頻譜之流程圖。Fig. 14 is a flow chart for obtaining an analog spectrum.
圖15係成長於二氧化矽/矽基板之三層石墨烯薄膜頻譜主軸成分分析圖表。Fig. 15 is a graph showing the principal component analysis of the spectrum of the three-layer graphene film grown on the ceria/germanium substrate.
圖16係成長於玻璃基板之五層石墨烯薄膜頻譜主軸成分分析圖表。Fig. 16 is a graph showing the principal component analysis of the spectrum of the five-layer graphene film grown on a glass substrate.
圖17係成長於二氧化矽/矽基板之三層石墨烯薄膜之拉曼頻譜分析之圖表。Figure 17 is a graph of Raman spectrum analysis of a three-layer graphene film grown on a ceria/ruthenium substrate.
圖18係成長於玻璃基板之五層石墨烯薄膜之拉曼頻譜分析之圖表。Figure 18 is a graph of Raman spectrum analysis of a five-layer graphene film grown on a glass substrate.
圖19係成長於玻璃基板之五層石墨烯薄膜之拉曼頻譜之2D-band與G-band比例分析圖表。Fig. 19 is a 2D-band and G-band ratio analysis chart of the Raman spectrum of a five-layer graphene film grown on a glass substrate.
圖20係成長於玻璃基板之五層石墨烯薄膜不同部分拉曼頻譜之2D-band與G-band比例分析圖表。Figure 20 is a 2D-band and G-band ratio analysis chart of different parts of the Raman spectrum of a five-layer graphene film grown on a glass substrate.
圖21係成長於二氧化矽/矽基板之三層石墨烯薄膜之穿透頻譜分析之圖表。Figure 21 is a graph showing the breakthrough spectrum analysis of a three-layer graphene film grown on a ceria/germanium substrate.
圖22係成長於二氧化矽/矽基板三層石墨烯薄膜穿透頻譜分析之較小比例範圍之圖表。Figure 22 is a graph of a smaller scale range of penetration spectrum analysis of a three-layer graphene film grown on a ceria/ruthenium substrate.
圖23係成長於二氧化矽/矽基板之三層石墨烯薄膜之反射頻譜分析之圖表。Figure 23 is a graph showing the reflection spectrum analysis of a three-layer graphene film grown on a ceria/ruthenium substrate.
圖24係成長於玻璃基板之五層石墨烯薄膜之穿透頻譜分析之圖表。Figure 24 is a graph showing the penetration spectrum analysis of a five-layer graphene film grown on a glass substrate.
圖25係成長於玻璃基板之五層石墨烯薄膜之反射頻譜分析之圖表。Figure 25 is a graph showing the reflection spectrum analysis of a five-layer graphene film grown on a glass substrate.
為了使本發明的技術特徵及實用功效能夠被詳細瞭解,並可據說明書的內容予以實施,以下配合圖式,詳就本發明實施例進行說明。In order to make the technical features and the practical functions of the present invention can be understood in detail, and can be implemented according to the contents of the specification, the embodiments of the present invention will be described in detail below with reference to the drawings.
(一)應用於石墨烯薄膜層數檢測的影像分析系統(1) Image analysis system applied to the detection of graphene film layers
本發明之應用於石墨烯薄膜層數檢測的影像分析系統,請參照圖1所示實施例,其係包括一觀察模組10、一取像模組20以及一多頻譜色彩影像再現模組30。The image analysis system of the present invention is applied to the image analysis system for the detection of the number of layers of the graphene film. Referring to the embodiment shown in FIG. 1 , the invention comprises an observation module 10 , an image capturing module 20 and a multi-spectral color image reproduction module 30 . .
該觀察模組10具有用以固定一石墨烯薄膜樣本40並對於該石墨烯薄膜樣本40投射光源以令該石墨烯薄膜樣本40得以受到光學觀測之結構,具體而言,其包括一載臺單元11及一照明單元12。較佳的是,該觀察模組10進一步包括有一影像放大單元13以放大來自該載臺單元11之石墨烯薄膜樣本40之影像,亦即該影像放大單元13具有就該載臺單元11所固定石墨烯薄膜樣本40提供一放大影像之結構。The observation module 10 has a structure for fixing a graphene film sample 40 and projecting a light source for the graphene film sample 40 to optically observe the graphene film sample 40. Specifically, the observation module includes a stage unit. 11 and a lighting unit 12. Preferably, the viewing module 10 further includes an image magnifying unit 13 for enlarging the image of the graphene film sample 40 from the stage unit 11, that is, the image magnifying unit 13 has a fixing for the stage unit 11. The graphene film sample 40 provides a structure for magnifying the image.
該載臺單元11係用以承載欲檢測的石墨烯薄 膜樣本40。該照明單元12係提供照明光源投射於該載臺單元11上的石墨烯薄膜樣本40。該影像放大單元13係設置於該載臺單元11,進而放大該載臺單元11上的石墨烯薄膜樣本40之影像以資辨識。The stage unit 11 is used to carry the thin graphene to be detected Film sample 40. The illumination unit 12 provides a graphene film sample 40 on which the illumination source is projected onto the stage unit 11. The image magnifying unit 13 is disposed on the stage unit 11 to further enlarge the image of the graphene film sample 40 on the stage unit 11 for identification.
又該觀察模組10係可進一步包括一濾光單元14。該濾光單元14係位於該照明單元12的一光源投射路徑上,使該照明單元12所提供的照明光源予以過濾而產生所需波段的過濾光源,以提供於該載臺單元11上的石墨烯薄膜樣本40,該濾光單元14係包括紅、綠、藍、青綠、洋紅、黃的濾光片而可組合使用;另外,在不採用濾光單元14之狀況,該照明單元12亦可形成為可切換不同色系之照明元件以提供不同波段之光源。The viewing module 10 can further include a filter unit 14. The filter unit 14 is located on a light source projection path of the illumination unit 12, and the illumination source provided by the illumination unit 12 is filtered to generate a filter light source of a desired wavelength band to provide graphite on the stage unit 11. The olefin film sample 40 is a filter including red, green, blue, cyan, magenta, and yellow, and can be used in combination; and the lighting unit 12 can also be used without the filter unit 14 Light elements that can be switched in different color systems to provide different wavelengths of light.
如圖2所示,該觀察模組10之照明單元12不僅可如前述圖1所示以反射之方式針對成長於諸如二氧化矽/矽基板等不透明基板之石墨烯薄膜樣本40,對於該載臺單元11以反射方式投射照明光源,亦可在對於成長於諸如玻璃基板等透明基板之石墨烯薄膜樣本40進行觀測時,配合採用具有透光結構之載臺單元11,令該照明單元12以穿透載臺單元11所載置石墨烯薄膜樣本40之方式,朝向取像模組20投射照明光源。較佳的是,該照明單元12能夠在圖1所示以反射方式投射照明光源之狀態與圖2所示以穿透方式投射照明光源之狀態間進行切換。換言之,該照明單元12具有對於載臺單元11以反射方式投射照明光源之結構、對於載臺單元11以穿透方式投射照明光源之結構、或者可在前述二種結構之間進行切換之結構。As shown in FIG. 2, the illumination unit 12 of the observation module 10 can not only reflect the graphene film sample 40 grown on an opaque substrate such as a ceria/iridium substrate in a reflective manner as shown in FIG. 1 above. The stage unit 11 projects the illumination source in a reflective manner, and can also cooperate with the stage unit 11 having a light transmitting structure when observing the graphene film sample 40 grown on a transparent substrate such as a glass substrate, so that the illumination unit 12 The illumination source is projected toward the image capturing module 20 by penetrating the graphene film sample 40 placed on the stage unit 11. Preferably, the illumination unit 12 is switchable between a state in which the illumination source is projected in a reflective manner as shown in FIG. 1 and a state in which the illumination source is projected in a penetrating manner as shown in FIG. 2. In other words, the illumination unit 12 has a structure in which the illumination unit is projected in a reflective manner with respect to the stage unit 11, a structure in which the illumination unit is projected in a penetrating manner to the stage unit 11, or a configuration in which the above two configurations can be switched.
該取像模組20具有用以對於對於前述石墨烯薄膜樣本40進行光學觀測之結構,具體而言,該取像模組20係位於該觀察模組10的輸出路徑(即該石墨烯薄膜樣本40可被光學觀測之路徑),且包括一感光耦合(CCD)單元22、一透鏡單元21以及一擷取單元23。The image capturing module 20 has a structure for optically observing the graphene film sample 40. Specifically, the image capturing module 20 is located at an output path of the viewing module 10 (ie, the graphene film sample) 40 is optically observable) and includes a photosensitive coupling (CCD) unit 22, a lens unit 21, and a capture unit 23.
該感光耦合單元22係由複數矩形的感光元件以橫列和縱列方式構成陣列,藉由橫維度以及縱維度的感光元件紀錄為電子影像的像素。該感光耦合單元22係感測經該影像放大單元13所放大之來自該載臺單元11之石墨烯薄膜樣本40的影像。The photosensitive coupling unit 22 is formed by an array of a plurality of rectangular photosensitive elements in a row and a column, and is recorded as a pixel of an electronic image by a photosensitive element of a horizontal dimension and a vertical dimension. The photosensitive coupling unit 22 senses an image of the graphene film sample 40 from the stage unit 11 amplified by the image magnifying unit 13.
該透鏡單元21係設置於該感光耦合單元22,並將來自該影像放大單元13所放大的石墨烯薄膜樣本40的影像予以聚焦,且提供給該感光耦合單元22,以獲得清晰的石墨烯薄膜樣本40的放大影像。更佳地,該透鏡單元21係可聚焦來自該照明單元12的透射光源;該擷取單元23係連接於該感光耦合單元22以擷取經過聚焦的石墨烯薄膜樣本40的放大影像。又,該擷取單元23係可為一照相機或一頻譜儀;更佳地,該頻譜儀係可為Konica Minolta公司所生產之型號CS1000A或Ocean Optics公司所生產之型號QE65000的頻譜儀(spectrometer,又稱「分光光度計」或「光譜儀」)。The lens unit 21 is disposed on the photosensitive coupling unit 22, and focuses an image of the graphene film sample 40 amplified by the image amplifying unit 13 and supplies the image to the photosensitive coupling unit 22 to obtain a clear graphene film. A magnified image of sample 40. More preferably, the lens unit 21 can focus the transmitted light source from the illumination unit 12; the capture unit 23 is coupled to the photosensitive coupling unit 22 to capture an enlarged image of the focused graphene film sample 40. Moreover, the capturing unit 23 can be a camera or a spectrum analyzer; more preferably, the spectrum analyzer can be a spectrometer of the model QE65000 produced by Konica Minolta Co., Ltd. model CS1000A or Ocean Optics. Also known as "spectrophotometer" or "spectrometer").
該多頻譜色彩影像再現模組30係可操作地連接於前述取像模組以提供石墨烯薄膜層數檢測資料。具體而言,該多頻譜色彩影像再現模組30,係擷取來自該擷取單元23之經過聚焦的石墨烯薄膜樣本40的放大影像,經 過頻譜分析步驟31,配合影像之判別分類進行色彩增益步驟32以及色彩影像再現步驟33,以重新處理並呈現前述石墨烯薄膜樣本40的放大影像,並據此提供予使用者以進行直觀而快速之石墨烯薄膜層數檢測。The multi-spectral color image reproduction module 30 is operatively coupled to the image capture module to provide graphene film layer detection data. Specifically, the multi-spectral color image reproduction module 30 captures an enlarged image of the focused graphene film sample 40 from the capture unit 23, After the spectrum analysis step 31, the color gain step 32 and the color image reproduction step 33 are performed in conjunction with the discriminant classification of the image to reprocess and present the enlarged image of the graphene film sample 40, and provide the user with an intuitive and fast image accordingly. Graphene film layer number detection.
(二)石墨烯薄膜層數檢測方法(2) Graphene film layer number detection method
以下說明本發明石墨烯薄膜層數檢測方法。The method for detecting the number of layers of the graphene film of the present invention will be described below.
前述檢測方法包括有一石墨烯薄膜層數頻譜資料庫建立流程,其首先建置一低層數石墨烯薄膜頻譜資料庫,並根據該低層數石墨烯薄膜頻譜資料庫,藉由多頻譜色彩再現影像對於石墨烯薄膜層數進行檢測而進行一多頻譜色彩再現影像的檢測石墨烯薄膜層數之流程。The foregoing detection method comprises a process for establishing a graphene film layer spectrum database, which firstly constructs a low-layer graphene film spectrum database, and reconstructs an image by multi-spectral color according to the low-layer graphene film spectrum database. The process of detecting the number of layers of the graphene film by detecting the number of layers of the graphene film and performing a multi-spectral color reproduction image.
1、該石墨烯薄膜層數頻譜資料庫建立流程係包括:1. The process of establishing the graphene film layer spectrum database includes:
(1)頻譜分析步驟,其針對成長於不同基板之不同層數之低層數石墨烯薄膜進行頻譜分析以提供一頻譜分析結果:(1) A spectrum analysis step for performing spectrum analysis on a low number of graphene films grown in different layers of different substrates to provide a spectrum analysis result:
(1-a)齊備成長於不同基板低層數石墨烯薄膜。例如:於二氧化矽/矽基板或玻璃基板等不同基板成長低層數石墨烯薄膜。(1-a) A graphene film having a low number of layers grown on different substrates. For example, a low-layer graphene film is grown on a different substrate such as a cerium oxide/germanium substrate or a glass substrate.
(1-b)獲取該低層數石墨烯薄膜之影像。例如:以顯微鏡及相機等取像裝置拍攝該低層數石墨烯薄膜之影像。(1-b) Obtaining an image of the low-layer graphene film. For example, an image of the low-layer graphene film is imaged by an image capturing device such as a microscope or a camera.
(1-c)確認該低層數石墨烯薄膜之層數。例如:以拉曼頻譜分析、穿透頻譜分析或原子力顯微鏡等方法對於該低層數石墨烯薄膜之層數進行確認。(1-c) The number of layers of the low-layer graphene film was confirmed. For example, the number of layers of the low-layer graphene film is confirmed by Raman spectrum analysis, penetration spectrum analysis, or atomic force microscopy.
(1-d)以多頻譜影像技術就前述低層數石墨烯薄膜之影像求得不同基板、不同層數石墨烯薄膜之穿透頻譜,進 而提供頻譜分析結果。(1-d) Using multi-spectral imaging technology to obtain the penetration spectrum of different substrates and different number of graphene films for the image of the low-layer graphene film Provide spectrum analysis results.
(2)主軸成份分析步驟,其針對前述頻譜分析結果進行主軸成份分析以提供一判別式:(2) A spindle component analysis step for performing spindle component analysis on the aforementioned spectrum analysis results to provide a discriminant:
(2-a)對於不同基板、不同層數石墨烯薄膜之穿透頻譜進行主軸成分分析以獲取主軸成分分析結果。(2-a) Perform spindle component analysis on the breakthrough spectra of graphene films of different substrates and different layers to obtain spindle component analysis results.
(2-b)基於前述主軸成分分析結果,建立不同基板、不同層數石墨烯薄膜之判別式。例如,設第一主成分為y0、第二主成分為y1,則成長於玻璃基板上不同層數之石墨烯薄膜,分別具有如下表1所示之判別式:
(3)資料庫建立步驟:基於前述多頻譜影像技術之頻譜分析結果及主軸成分分析之判別式建立資料庫以提供石墨烯薄膜層數及判別式之對應關係之資料。(3) Database establishment step: based on the spectrum analysis result of the multi-spectral image technology and the discriminant of the spindle component analysis, a database is established to provide data on the correspondence between the number of layers of the graphene film and the discriminant.
2、前述多頻譜色彩再現影像之石墨烯薄膜層數檢測流程係包括:2. The graphene film layer number detection process of the multi-spectral color reproduction image includes:
(1)擷取影像步驟:獲取待測低層數石墨烯薄膜之影像。例如以顯微鏡及相機等取像裝置拍攝該低層數石墨烯薄膜之影像。(1) Step of capturing image: Obtain an image of the graphene film with a low number of layers to be tested. For example, an image of the low-layer graphene film is imaged by an image capturing device such as a microscope or a camera.
(2)頻譜分析步驟:以多頻譜影像技術就待測低層數石墨烯薄膜之影像求得待測石墨烯薄膜之穿透頻譜。(2) Spectrum analysis step: The multi-spectral image technique is used to obtain the penetration spectrum of the graphene film to be tested with respect to the image of the low-layer graphene film to be tested.
(3)石墨烯薄膜層數分類步驟:藉由前述對於不同基板、不同層數石墨烯薄膜判別式所建立之資料庫,待測石墨烯薄膜之穿透頻譜加以分類獲取一判別結果。(3) Steps of classifying the number of layers of graphene film: by using the above-mentioned database for different substrate and different number of graphene film discriminants, the penetration spectrum of the graphene film to be tested is classified to obtain a discriminating result.
(4)色彩增益步驟:基於前述判別結果確認經分類之石墨烯薄膜層數之模擬頻譜。(4) Color gain step: confirm the analog spectrum of the number of layers of the graphene film classified based on the above discrimination result.
(5)色彩影像再現步驟:依前述判別結果所對應之模擬頻譜藉由多頻譜影像技術進行色彩影像再現。(5) Color image reproduction step: color image reproduction is performed by the multi-spectral image technology according to the analog spectrum corresponding to the discrimination result.
(6)石墨烯薄膜層數檢測步驟:基於經過色彩影像再現之影像,進行直觀快速之石墨烯薄膜層數檢測。(6) Graphene film layer number detecting step: based on the image reproduced by the color image, the intuitive and rapid graphene film layer number detection is performed.
較佳的是,該檢測方法係實施於前述多頻譜色彩影像再現模組30中,該多頻譜色彩影像再現模組30,係藉由擷取來自擷取單元23之經聚焦石墨烯薄膜樣本40的放大影像以實施前述擷取影像步驟,並對該影像進行頻譜分析步驟31、且配合前述資料庫進行石墨烯薄膜層數分類步驟以呈現一分類結果,其後依該分類結果進行色彩增益步驟32,以進而實施色彩影像再現步驟33,藉此,該多頻譜色彩影像再現模組30即能夠重新處理該擷取單元23所擷取的經過聚焦之石墨烯薄膜樣本40放大影像,以摸擬頻譜將之重建以提供使用者一色彩再現影像,以資實施石墨烯薄膜層數檢測步驟。Preferably, the detection method is implemented in the multi-spectral color image reproduction module 30, and the multi-spectral color image reproduction module 30 captures the focused graphene film sample 40 from the capture unit 23. Enlarging the image to perform the step of capturing the image, performing a spectrum analysis step 31 on the image, and performing a graphene film layer number sorting step with the data library to present a classification result, and then performing a color gain step according to the classification result. 32, to further implement the color image reproduction step 33, whereby the multi-spectral color image reproduction module 30 can reprocess the focused graphene film sample 40 captured by the capture unit 23 to magnify the image to simulate The spectrum is reconstructed to provide a user-color-reproduced image for the graphene film layer number detection step.
承上,以針對成長於玻璃基板上的五層石墨烯薄膜為例,若採用拉曼頻譜技術分析低層數石墨烯薄膜層數,需要長時間進行密集分析作業,因此無法快速而直觀 地確定真實石墨烯薄膜的層數。另如圖3及圖4所示,拉曼頻譜技術分析技術所得到的分析結果具有相當程度之模糊區域,因此難以明確地得到石墨烯薄膜層數檢測之結果。Taking the five-layer graphene film grown on a glass substrate as an example, if the low-layer graphene film layer is analyzed by Raman spectrum technology, it takes a long time to perform intensive analysis work, so it cannot be fast and intuitive. The number of layers of the real graphene film is determined. As shown in FIG. 3 and FIG. 4, the analysis results obtained by the Raman spectrum technique analysis technique have a considerable degree of blurring, so it is difficult to clearly obtain the result of the graphene layer number detection.
反觀本案發明之技術手段能夠快速判別待測石墨烯薄膜之穿透頻譜並進行色彩影像再現,因此如圖5及圖6所示,本案發明能夠在短時間確認石墨烯薄膜之層數,顯能有效改善既有技術之缺點,提供具有極佳效率之低層數石墨烯薄膜層數檢測效果。In contrast, the technical means of the invention of the present invention can quickly discriminate the penetration spectrum of the graphene film to be tested and perform color image reproduction. Therefore, as shown in FIG. 5 and FIG. 6, the invention can confirm the number of layers of the graphene film in a short time, and display the energy. Effectively improve the shortcomings of the existing technology, and provide a layer layer graphene film with excellent efficiency.
以下配合實施例進一步說明本發明之實施態樣:The embodiments of the present invention are further described below in conjunction with the embodiments:
本實施例係關於低層數石墨烯薄膜之製備。This example relates to the preparation of a low layer graphene film.
本實施例使用銅箔作為觸媒,以成長較大面積之單層石墨烯薄膜,並使用甲烷(CH4)作為碳源,於低壓下成長石墨烯薄膜,再配合高分子覆蓋膜(PMMA)將石墨烯薄膜轉移至諸如二氧化矽/矽基板或玻璃基板等不同基板上。由於石墨烯薄膜之製備屬既有技術,茲略其細節不予贅述。In this embodiment, a copper foil is used as a catalyst to grow a large-area single-layer graphene film, and methane (CH4) is used as a carbon source, and a graphene film is grown at a low pressure, and then a polymer cover film (PMMA) is used. The graphene film is transferred to a different substrate such as a ceria/iridium substrate or a glass substrate. Since the preparation of the graphene film is a prior art, the details thereof will not be described.
在本實施例中,係如圖7所示於二氧化矽/矽基板上成長三層石墨烯薄膜,其於該二氧化矽/矽基板上形成有零層(即基板未為石墨烯薄膜所覆蓋)、一層、二層及三層之結構,並分別標示為「0L」、「1L」、「2L」及「3L」。復如圖8所示,本實施例於玻璃基板上成長五層石墨烯薄膜,其呈現極難以光學顯微鏡直接觀察判別石墨烯薄膜層數之形態。如圖9所示,在本實施例中,該成長於玻璃基 板上之五層石墨烯薄膜之結構呈現層數自兩側向中間遞增之形態。為便於分析,爰如圖10所示將玻璃基板加以劃分,從而得以如圖11所示藉由該分區選取不同區域進行分析。In this embodiment, as shown in FIG. 7, a three-layer graphene film is grown on the ceria/germanium substrate, and a zero layer is formed on the ceria/germanium substrate (ie, the substrate is not a graphene film). Covered, one, two and three layers are marked as "0L", "1L", "2L" and "3L" respectively. As shown in FIG. 8, in this embodiment, a five-layer graphene film is grown on a glass substrate, which is extremely difficult to directly observe and discriminate the number of graphene film layers by an optical microscope. As shown in FIG. 9, in the present embodiment, the growth is based on a glass base. The structure of the five-layer graphene film on the plate exhibits a form in which the number of layers increases from both sides toward the middle. For the purpose of analysis, the glass substrate is divided as shown in FIG. 10, so that different regions can be selected for analysis by the partition as shown in FIG.
本實施例係關於低層數石墨烯薄膜多頻譜再現技術之中,頻譜儀與取像裝置間之轉換矩陣(即「關係矩陣」)。本實施例所採用之取像裝置係設於光學顯微鏡之感光耦合元件攝影機。This embodiment relates to a conversion matrix (ie, "relationship matrix") between a spectrum analyzer and an image capturing device in a low-layer graphene film multi-spectral reproduction technique. The image pickup device used in this embodiment is a photocoupler camera of an optical microscope.
本實施例利用多頻譜影像系統與色彩再現技術,使用Ocean Optics公司所生產之型號QE65000頻譜儀,將其頻譜的範圍設在可見光的波段(波長:380 nm至780 nm),在光學顯微鏡的環境下量測Macbeth ColorChecker色表所列24色塊之穿透頻譜。In this embodiment, the multi-spectral image system and the color reproduction technology are used, and the model QE65000 spectrum analyzer produced by Ocean Optics is used to set the spectrum in the visible light band (wavelength: 380 nm to 780 nm) in the environment of the optical microscope. The measurement of the penetration spectrum of the 24 color blocks listed in the Macbeth ColorChecker color table is measured.
得到穿透頻譜之後,藉多頻譜技術以所測得之穿透頻譜建立模組,能夠如圖12所示,計算出模擬色塊與取像裝置色塊之間的色差,再以其模擬出取像裝置影像之頻譜,找到頻譜儀之穿透頻譜與取像裝置之影像之間的關係,分析不同層數石墨烯薄膜之穿透頻譜之差異性。After obtaining the penetration spectrum, the multi-spectrum technique is used to build the module with the measured penetration spectrum, and as shown in FIG. 12, the color difference between the analog color block and the image capturing device color block can be calculated, and then simulated. The spectrum of the image of the imager is taken to find the relationship between the spectrum of the spectrum analyzer and the image of the image capturing device, and the difference in the penetration spectrum of the graphene films of different layers is analyzed.
在本實施例中,係採用如圖13所示之計算流程,找出穿透頻譜與取像裝置影像之間的轉換矩陣,以得到每張影像中每個畫素的穿透頻譜。In this embodiment, the calculation flow shown in FIG. 13 is used to find the conversion matrix between the penetration spectrum and the image of the image capturing device to obtain the penetration spectrum of each pixel in each image.
為便於分析,在本實施例中,係將這些穿透頻譜整理成一個401*24之矩陣。該401*24矩陣之每一列為 波長所對應的強度值,每一行則代表色塊的數目。For ease of analysis, in the present embodiment, these penetration spectra are organized into a matrix of 401*24. Each column of the 401*24 matrix is The intensity value corresponding to the wavelength, and each row represents the number of patches.
再經過如圖14所示之計算流程可求得模擬頻譜,並藉由特徵系統以及主成分分析,求得六組特徵向量(6*401)所對應之六組特徵值(6*24),如下數學式1所示:【數學式1】[α ] T =[D ] T pinv [E ]After the calculation process shown in Figure 14, the simulated spectrum can be obtained, and the six sets of eigenvalues (6*24) corresponding to the six sets of eigenvectors (6*401) are obtained by the feature system and principal component analysis. The following mathematical formula 1: [Math 1] [ α ] T = [ D ] T pinv [ E ]
其中pinv是偽逆矩陣。這些色塊同時在光學顯微鏡的環境下被取像裝置所獲取而輸出格式為sRGB之JPEG影像資料。藉由電腦的計算,可以得到每個影像資料之色片中的R、G、B值(0~255),並進而轉換到尺度更小的範圍(0~1)而得到R srgb 、G srgb 、B srgb 。藉由下列數學式2至4,將前述RGB值將轉換為CIE規範之三次激值X 、Y 、Z 。Where pinv is a pseudo inverse matrix. These color patches are simultaneously acquired by the image capture device in an optical microscope environment and output JPEG image data in the format of sRGB. By computer calculation, the R, G, and B values (0~255) in the color patches of each image data can be obtained, and then converted to a smaller scale (0~1) to obtain R srgb , G srgb . , B srgb . The aforementioned RGB values will be converted to the three-magnitude X , Y , Z of the CIE specification by the following mathematical formulas 2 to 4.
其中:
由於sRGB空間中的標準白為D65光源下的參考白,其有異於頻譜儀在鹵素燈光源下所量到之反射頻譜的參考白。從而該RGB值需藉色適應轉換進行修正。為準確估計色塊的頻譜值,則須校正取像裝置。Since the standard white in the sRGB space is the reference white under the D65 source, it is different from the reference white of the reflected spectrum measured by the spectrum analyzer under the halogen light source. Therefore, the RGB value needs to be corrected by the color adaptation conversion. In order to accurately estimate the spectral value of the patch, the imaging device must be corrected.
同樣的,頻譜儀所量測的反射頻譜亦以下列數學式5至8轉換成CIE規範之三次激值X 、Y 、Z 。其中S (λ )為鹵素燈的光源頻譜,R (λ )為每個色塊的反射頻譜,而(λ )、(λ )、及(λ )為配色函數。Similarly, the reflectance spectrum measured by the spectrum analyzer is also converted into the three-magnitude X , Y , Z of the CIE specification by the following mathematical formulas 5 to 8. Where S ( λ ) is the spectrum of the source of the halogen lamp, and R ( λ ) is the reflection spectrum of each patch, and ( λ ), ( λ ), and ( λ ) is a color matching function.
其中:【數學式8】
色適應轉換後,經過前述數學式2至4之計算將相機的RGB值轉換為新的XYZ值,並將之設為矩陣[A ]。透過RGB之三階多項式回歸,即可求出頻譜儀與相機間之轉換關係。以下數學式9為三階多項式回歸的矩陣:【數學式9】[C ]=[A ]pinv [B ]After the color adaptation is converted, the RGB value of the camera is converted into a new XYZ value by the calculation of the aforementioned Mathematical Formulas 2 to 4, and is set as a matrix [ A ]. Through the third-order polynomial regression of RGB, the conversion relationship between the spectrum analyzer and the camera can be obtained. The following mathematical formula 9 is a matrix of third-order polynomial regression: [Math 9] [ C ]=[ A ] pinv [ B ]
其中:【數學式10】[B ]=[1,R ,G ,B ,RG ,GB ,BR ,R 2 ,G 2 ,B 2 ,RGB ,R 3 ,G 3 ,B3 ,RG 2 ,RB 2 ,GR 2 ,GB 2 ,BR 2 ,BG 2 ] T Where: [Math 10] [ B ]=[1, R , G , B , RG , GB , BR , R 2 , G 2 , B 2 , RGB , R 3 , G 3 , B 3 , RG 2 , RB 2 , GR 2 , GB 2 , BR 2 , BG 2 ] T
其中「R」、「G」、「B」為取像裝置所獲取對應於各色塊之RGB值。將色塊經RGB校正後轉為CIE三次激值XYZ設為[β ],則頻譜儀與取像裝置的轉換矩陣[M ]可由下列數學式11求得:【數學式11】[M ]=[α ]pinv [β ]Among them, "R", "G", and "B" are RGB values obtained by the image capturing device corresponding to the respective color patches. After the color block is corrected by RGB and converted to CIE three-time excitation value XYZ is set to [ β ], the conversion matrix [ M ] of the spectrum analyzer and the image capturing device can be obtained by the following mathematical expression 11: [Math 11] [ M ]= [ α ] pinv [ β ]
本實施例係關於以模擬頻譜進行色彩再現。This embodiment relates to color reproduction in an analog spectrum.
取像裝置所獲取影像之各畫素,可分別藉由RGB的相乘得到線性回歸矩陣[C
]並透過數學式2至4的計算得到相對應的XYZ值。各色塊的模擬頻譜(波段由380 nm到780 nm)可藉下列數學式12求得:
藉由本發明之技術手段,將頻譜儀量測鹵素燈之頻譜,除以原本取像場景之光源頻譜並乘上新的置換光源頻譜,即能夠於該置換光源再現色彩。從而於不同光源皆能再現色彩。By means of the technical means of the invention, the spectrum of the halogen lamp is measured by the spectrometer, divided by the spectrum of the source of the original image capturing scene and multiplied by the spectrum of the new replacement source, that is, the color can be reproduced in the replacement light source. Thus, the color can be reproduced by different light sources.
為了證實色彩再現的可行性,本實施例以色差公式評估實際頻譜與模擬頻譜之間的誤差。色差的計算流程如下所示:In order to confirm the feasibility of color reproduction, the present embodiment evaluates the error between the actual spectrum and the analog spectrum by the color difference formula. The calculation process of the color difference is as follows:
(一)將兩儀器所量到的三次激值XYZ轉成CIE 1976空間中的色度座標值(L*,a*,b*),其中:
(二)計算CIE 1976色度座標中兩點之歐基里德距離(即兩點之色差):
前述24色塊之各色塊的色差值如圖12所示。該24個色塊之平均色差為4.21。本實施例之結果顯示本發明之技術手段能夠達到色彩再現之效果,從而得以應用於影像之顏色表現。The color difference values of the respective color patches of the aforementioned 24 color patches are as shown in FIG. The average color difference of the 24 color patches is 4.21. The results of this embodiment show that the technical means of the present invention can achieve the effect of color reproduction, thereby being applied to the color representation of an image.
本實施例係藉由主軸成分分析進行主成分得點的運算,分別將成長於二氧化矽/矽基板之三層石墨烯薄膜之頻譜與成長於玻璃基板之五層石墨烯薄膜之頻譜進行分 類。In this embodiment, the main component points are calculated by the spindle component analysis, and the spectrum of the three-layer graphene film grown on the ceria/germanium substrate and the spectrum of the five-layer graphene film grown on the glass substrate are respectively divided. class.
如圖15及圖16所示。主成分得點可將高維度資料簡化為較低維度資料,並投影於特徵向量空間以利資料分析。主成分得點之公式如下列數學式18所示:
其中x 1i 、x 2i ...x pi 為第一個、第二個...第p個波長下對應的頻譜強度值。、...為第一個、第二個...第p個波長下的平均頻譜強度值。a j 1 、a j 2 ...a jp 為頻譜取共變異矩陣後的特徵向量的係數。Where x 1 i , x 2 i ... x pi are the corresponding spectral intensity values at the first, second ... p-th wavelength. , ... The average spectral intensity value at the pth wavelength of the first, second, .... a j 1 , a j 2 ... a jp are the coefficients of the eigenvectors after the spectrum takes the covariation matrix.
就主軸成分分析法而言,第一主成分呈現原資料中最多的資訊,可視為綜合性指標。第二主成分以及第三主成分亦呈現原資料部分資訊,可用以將各群組進行分類。為瞭解資料分布的情形,對於個別群組資料再進行一次主成分分析,將群組的範圍以橢圓表示。橢圓的方程式如下數學式19所示:
其中a 1 、b 1 、a 2 、b 2 為群組的逆共變異矩陣的特徵向量係數,其物理意義為座標軸的旋轉;c 1 、c 2 為群組 資料值的平均值,因群組於主成分分析時就所有點資料進行平移,故須將橢圓的圓心移回原空間;d 1 以及d 2 為共變異矩陣之特徵值,其物理意義代表橢圓的長軸以及短軸之一半。Where a 1 , b 1 , a 2 , b 2 are the eigenvector coefficients of the inverse co-mutation matrix of the group, the physical meaning of which is the rotation of the coordinate axis; c 1 and c 2 are the average values of the group data values, due to the group In the principal component analysis, all the point data are translated, so the center of the ellipse must be moved back to the original space; d 1 and d 2 are the eigenvalues of the covariation matrix, and the physical meaning represents the long axis and one half of the short axis of the ellipse.
本實施例係藉由拉曼頻譜儀分析驗證本發明之效果。This embodiment demonstrates the effect of the present invention by analysis by a Raman spectrometer.
拉曼效應可用以研究分子結構、分子振動能級與轉動能級,確定分子中各種功能基或化學鍵位置,以及對於複雜混合分子進行定量分析。拉曼散射係因介質分子本身振動或轉動,造成入射光子及介質分子之間能量交換,使反射後之散射光頻率發生轉變。The Raman effect can be used to study the molecular structure, molecular vibrational energy levels and rotational energy levels, determine the various functional or chemical bond positions in the molecule, and quantitatively analyze complex hybrid molecules. The Raman scattering system causes the energy exchange between the incident photons and the dielectric molecules due to the vibration or rotation of the dielectric molecules themselves, so that the frequency of the scattered light after the reflection changes.
本實施例使用顯微拉曼頻譜儀(Renishaw公司所生產之Invia 1000 system),其係將雷射光透過光學顯微鏡聚焦於試片,並使散射光線透過相同之顯微鏡進入頻譜儀轉成待分析之光譜。This embodiment uses a micro-Raman spectrometer (Invia 1000 system manufactured by Renishaw Co., Ltd.), which focuses the laser light through an optical microscope on the test piece, and transmits the scattered light through the same microscope into the spectrum analyzer to be analyzed. spectrum.
本實施例藉由前述拉曼頻譜儀,採用功率為8.6 mw之633 nm紅光雷射,以40倍物鏡量測拉曼訊號。In this embodiment, the Raman signal is measured by a 40-fold objective lens by using the aforementioned Raman spectrometer with a 633 nm red laser with a power of 8.6 mW.
如參考文獻22所述,石墨烯薄膜之拉曼位移主要呈現於座落在1582 cm-1 之G-band與座落在2676 cm-1 之2D-band。圖17所示者為成長於二氧化矽/矽基板之三層石墨烯薄膜之拉曼頻譜分析圖表,圖18所示者為成長於玻璃基板之五層石墨烯薄膜之拉曼頻譜分析圖表,藉之可看出不同層數之石墨烯薄膜呈現相異之拉曼位移,其G-band 之訊號強度隨著層數增加而遞增,而2D-band之訊號強度則隨層數增加而發生位移。As described in reference 22, the Raman shift of the graphene film is mainly exhibited by a G-band located at 1582 cm -1 and a 2D-band seated at 2676 cm -1 . 17 is a Raman spectrum analysis chart of a three-layer graphene film grown on a ceria/germanium substrate, and FIG. 18 is a Raman spectrum analysis chart of a five-layer graphene film grown on a glass substrate. It can be seen that the graphene films of different layers exhibit different Raman shifts, the signal intensity of G-band increases with the number of layers, and the signal intensity of 2D-band shifts with the increase of the number of layers. .
在本實施例中所驗證二氧化矽/矽基板上成長之三層石墨烯薄膜已如圖7所示。藉由如圖17之拉曼頻譜分析,可驗證本發明技術之三層石墨烯薄膜層數檢測結果確實與既有拉曼頻譜分析之結果相符。The three-layer graphene film grown on the ceria/ruthenium substrate verified in this example has been shown in FIG. By Raman spectrum analysis as shown in Fig. 17, it can be verified that the three-layer graphene film layer number detection result of the present invention is indeed consistent with the results of the existing Raman spectrum analysis.
另針對如圖8至11所示成長於玻璃基板之五層石墨烯薄膜,以本發明技術進行層數檢測結果,亦與圖18及圖19所示之拉曼頻譜分析其2D-band與G-band之比值結果相符,另就圖20所示,以拉曼頻譜對於該成長於玻璃基板之五層石墨烯薄膜不同部位之分析也同樣呈現與本發明技術進行層數檢測相符合之結果,配合前述圖3及4與圖5及6之比較,更能進一步確認本發明技術確實得以快速直觀地進行檢測,提供優於既有拉曼頻譜分析技術之發明效果。Further, for the five-layer graphene film grown on the glass substrate as shown in FIGS. 8 to 11, the layer number detection result is performed by the technique of the present invention, and the 2D-band and G are also analyzed with the Raman spectrum shown in FIGS. 18 and 19. The ratio of -band is consistent, and as shown in Fig. 20, the Raman spectrum also shows the results of the layer detection of the five layers of graphene film grown on the glass substrate. Compared with the foregoing Figures 3 and 4 and Figures 5 and 6, it can be further confirmed that the technique of the present invention can be quickly and intuitively detected, providing an effect of the invention superior to the existing Raman spectrum analysis technique.
本實施例係藉由穿透頻譜儀分析驗證本發明之效果。This embodiment demonstrates the effects of the present invention by analyzing the spectrum analyzer.
紫外-可見分光光度法(Ultraviolet-visible spectroscopy,UV-Vis,又稱紫外-可見分子吸收光譜法),係以紫外線-可見光區域電磁波連續光譜作為光源照射樣品,研究物質分子對光吸收的相對強度之方法。Ultraviolet-visible spectroscopy (UV-Vis, also known as ultraviolet-visible molecular absorption spectroscopy), which uses a continuous spectrum of ultraviolet-visible region electromagnetic waves as a light source to study the relative intensity of light absorption of matter molecules. The method.
藉由分子紫外-可見分子吸收光譜法,可進行定性分析,並可依據朗伯-比爾定律進行定量分析。當光之 波長減小至一定數值時,溶劑將對其產生強烈之吸收,即「端吸收」,從而樣品測試係於該「端吸收」之透明界限內為之。Qualitative analysis can be performed by molecular ultraviolet-visible molecular absorption spectroscopy and quantitative analysis can be performed according to Lambert-Beer law. When the light When the wavelength is reduced to a certain value, the solvent will strongly absorb it, that is, "end absorption", so that the sample test is within the transparent limit of the "end absorption".
如圖21及圖24所示,使用穿透頻譜儀佐證石墨烯薄膜層數時,不同基板上不同層數之石墨烯薄膜呈現出相異之穿透頻譜。其中,圖21及圖22所示針對成長於二氧化矽/矽基板之三層石墨烯薄膜之穿透頻譜分析結果,與本發明對於該成長於二氧化矽/矽基板之三層石墨烯薄膜之檢測結果具有一致性。若以圖23之反射頻譜分析結果觀之,其亦與本發明對於該成長於二氧化矽/矽基板之三層石墨烯薄膜之檢測結果具有一致性。As shown in FIG. 21 and FIG. 24, when a penetrating spectrum analyzer is used to prove the number of graphene film layers, the graphene films of different layers on different substrates exhibit different penetration spectra. 21 and 22 show the results of the penetration spectrum analysis of the three-layer graphene film grown on the ceria/germanium substrate, and the three-layer graphene film grown on the ceria/germanium substrate according to the present invention. The test results are consistent. According to the results of the reflection spectrum analysis of FIG. 23, it is also consistent with the detection result of the present invention for the three-layer graphene film grown on the ceria/germanium substrate.
另如圖24所示,針對成長於玻璃基板之五層石墨烯薄膜之穿透頻譜分析結果,與本發明對於該成長於玻璃基板之五層石墨烯薄膜之檢測結果同樣具有一致性;其如圖25所示之反射頻譜分析結果,亦與本發明對於該成長於玻璃基板之五層石墨烯薄膜之檢測結果具有一致性。As shown in FIG. 24, the results of the penetration spectrum analysis of the five-layer graphene film grown on the glass substrate are consistent with the detection results of the five-layer graphene film grown on the glass substrate of the present invention; The results of the reflection spectrum analysis shown in Fig. 25 are also consistent with the detection results of the five-layer graphene film grown on the glass substrate of the present invention.
綜上所述,本發明之技術藉由多頻譜技術配合主軸成分分析法快速地藉由光學顯微鏡所得到影像檢測石墨烯薄膜層數,其檢測結果經既有技術驗證,確實與諸如特定波段隨著層數增加反射率遞增之驗證結果相符,其與拉曼頻譜分析結果之間亦呈現一致性。從而本發明確實能夠藉由搭配顯微鏡與感光耦合元件等取像裝置,以低成本、高效率之方式直觀而迅速地檢測出石墨烯薄膜層數。In summary, the technique of the present invention rapidly detects the number of graphene film layers by optical microscopy by using multi-spectral technology and spindle component analysis method, and the detection result is verified by existing techniques, and is indeed related to, for example, a specific band. The verification result of increasing the number of layers and increasing the reflectivity is consistent, and it is consistent with the Raman spectrum analysis results. Therefore, the present invention can accurately and quickly detect the number of graphene thin film layers in a low cost and high efficiency by using an image pickup device such as a microscope and a photosensitive coupling element.
下列參考文獻被引用為構成本發明之發明說明之部分:The following references are cited as part of the description of the invention that constitutes the invention:
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10‧‧‧觀察模組10‧‧‧Observation module
11‧‧‧載臺單元11‧‧‧stage unit
12‧‧‧照明單元12‧‧‧Lighting unit
13‧‧‧影像放大單元13‧‧‧Image magnification unit
14‧‧‧濾光單元14‧‧‧ Filter unit
20‧‧‧取像模組20‧‧‧Image capture module
21‧‧‧透鏡單元21‧‧‧ lens unit
22‧‧‧感光耦合單元22‧‧‧Photosensitive coupling unit
23‧‧‧擷取單元23‧‧‧Capture unit
30‧‧‧多頻譜色彩影像再現模組30‧‧‧Multi-spectral color image reproduction module
31‧‧‧頻譜分析步驟31‧‧‧ Spectrum analysis steps
32‧‧‧色彩增益步驟32‧‧‧Color gain step
33‧‧‧色彩影像再現步驟33‧‧‧Color image reproduction steps
40‧‧‧石墨烯薄膜樣本40‧‧‧ Graphene film samples
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