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Currently, graphene synthesis involves several key factors need to be improved: (i) lengthy high-temperature annealing processes to increase the grain size of the metal catalyst used to form graphene; (ii) utilization of purified and compressed gases to offer a homogenous and controlled delivery of carbon source materials; and (iii) the use of lengthy vacuum operation to avoid the presence of any detrimental reactive oxygen species from air2,4. To overcome these problems, we have designed a thermal CVD process to produce graphene in an ambient-air environment that is completely free of compressed or purified gases and requires minimum processing time. The process is schematically illustrated in Fig. 1a, in which the precursor for graphene growth and a metal catalyst (for example, Ni foil) are placed close together inside the heating zone of a furnace, before heating the quartz tube. The quartz tube is then sealed and the temperature is increased. During the ramping stage, air inside the quartz tube is released through a valve to maintain atmospheric pressure. Once the annealing stage is complete, the sample is removed from the heating zone for rapid cooling. Raman spectra of the samples grown at 800 °C in the ambient-air process indicated the presence of single-to-few layer graphene films covering the surface of the growth substrate (Fig. 1b). In the standard operation, the catalyst is low-cost polycrystalline Ni foil. Graphene growth occurs by thermal reforming of a natural precursor, soybean oil, in a closed ambient-air environment. Unlike conventional CVD methods or conventional natural precursor methods for growing graphene, the technique does not require any purified gases8,9. Moreover, expensive vacuum processing is avoided. The natural precursors substituted for purified gases are cheaper and safer. By restricting the air flow into the quartz tube, the transformation of solid-state carbon into carbon dioxide or other gaseous species is prevented. By controlling the temperature, cooling rate and precursor amount, the process enables the growth of homogenous graphene films of good quality. A comparison of the method with other CVD processes is provided in Supplementary Tables 1 and 2. The parameters observed to control the quality of graphene include temperature, processing time, precursor, substrate and the ambient-air environment. Nickel acted as a good catalyst for the breakdown of precursor material (in this case, the soybean-oil molecules) into smaller building units that are essential for the synthesis of graphene12. To investigate how the transformation occurred in the process, we have analysed the chemical composition of the annealed soybean oils at different temperatures (Supplementary Fig. 1). During the early stages of the annealing process, for instance at 300 °C, the long carbon chains in the soybean oil precursor were thermally dissociated into gaseous carbon building units such as methyl and ethyl species (Supplementary Fig. 1a). Other gaseous species were also generated, including hydrogen, water, hydroxyls and carbon dioxide, as confirmed by mass spectrometry (Supplementary Fig. 1b and c). Traces of heavier hydrocarbons such as propane were also observed. Most of the oil was vapourized by about 425 °C and a rapid mass reduction of the oil was observed by thermogravimetric analysis below 500 °C (Supplementary Fig. 1d). These building units present in the vapour can diffuse through the tube during the heating stage. As the temperature gradually increases to 800 °C, these carbon building units begin to dissociate into carbon atoms and dissolve into the Ni bulk. The sample was annealed for 3 min at 800 °C to promote dissolution of carbon atoms in the Ni substrate. Finally, following the rapid cooling stage, carbon segregates from the bulk and crystallizes on the Ni surface forming graphene12,13. At elevated temperatures, long hydrocarbons in the oil decompose in the presence of O2 to form water vapour. In particular, water vapour can promote the etching of amorphous carbon deposits on the Ni surface14. As such, we did not observe the formation of amorphous carbons in our sample. This also helps maintain the catalytic activity of the Ni surface in breaking down the precursor material15. Moreover, we have conducted a detailed analysis on the consumption of oxygen in the reactor during the growth process (Supplementary Note 1). We found that the precursor amount was critical for the consumption of reactive oxygen species. In the optimal growth condition, a slight carbon excessive environment is used to promote the growth of graphene and deter the formation of amorphous carbon. On the other hand, an over-excessive amount of precursor material led to an oversaturation of deposited carbon in the bulk of Ni, and subsequently, the crystallization of graphite on the Ni surface. This may explain the resulting formation of thick graphene sheets as observed in Supplementary Fig. 2a. Moreover, in the case of an insufficient amount of precursor, oxygen species can be present in the as-grown product in the form of C–O amorphous carbons (Supplementary Fig. 2b), consistent with the aforementioned calculations of oxygen consumption (Supplementary Note 1)16. These experiments indicate the critical role of the thermally dissociated precursor materials (that is, hydrocarbons) in consuming the reactive oxygen species present in the ambient-air environment, which has a profound effect in controlling the quality of the as-grown graphene films.We have also noticed that a slow cooling can promote excessive carbon segregation from the Ni bulk, which may account for the observed formation of a graphite-like film (Supplementary Fig. 2c). Another parameter that significantly influences the growth of graphene in the ambient air environment is the annealing temperature. At an annealing temperature of 500 °C, an incomplete formation of the graphene film was observed (Supplementary Fig. 2d). This may be attributed to an insufficient amount of energy to dissociate and reform the precursor material (that is, hydrocarbon species) required for graphene formation. Conversely, at a higher annealing temperature of 900 °C, thicker graphene sheets were observed (Supplementary Fig. 2e). This may arise from the increased rate of carbon diffusion, segregation and graphitization as a result of the elevated temperature. Importantly, these parameters allow us to obtain graphene films with tuneable average thickness and optical transmission, as characterized by Raman spectroscopy and optical transmission (Supplementary Fig. 3). It is worth mentioning that graphene did not form on other growth substrate materials with significantly lower carbon solubility than Ni, such as the commonly used Cu foil. Moreover, we did not observe graphene formation on graphitic surfaces such as woven carbon cloth (Supplementary Fig. 4). This suggests that the use of Ni (through, for example, carbon solubility, carbon segregation ability, catalytic effect, possibility of formation of oxide in air) and its interaction with the precursor material play a critical role in enabling the growth of graphene films. We also investigated the possibility of transforming other types of renewable oil groups. In particular, we were able to demonstrate the ambient-air growth of similar graphene films from other types of triglyceride (carbon)-containing precursors such as butter (Supplementary Fig. 5). As such, this method is versatile and may be tailored to transform other renewable carbon-containing natural precursors into graphene films. |
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Currently, graphene synthesis involves several key factors need to be improved: (i) lengthy high-temperature annealing processes to increase the grain size of the metal catalyst used to form graphene; (ii) utilization of purified and compressed gases to offer a homogenous and controlled delivery of carbon source materials; and (iii) the use of lengthy vacuum operation to avoid the presence of any detrimental reactive oxygen species from air2,4. To overcome these problems, we have designed a thermal CVD process to produce graphene in an ambient-air environment that is completely free of compressed or purified gases and requires minimum processing time. 目前，石墨烯合成涉及多個(gè)需要改進(jìn)的關(guān)鍵因素：（i）冗長(zhǎng)的高溫退火過(guò)程增加用來(lái)形成石墨烯的金屬催化劑的晶粒尺寸；（ii）利用純化和壓縮氣體來(lái)提供碳源材料的均勻和受控的遞送；以及（iii）使用冗長(zhǎng)的真空操作來(lái)避免存在來(lái)自空氣的任何有害反應(yīng)性氧物質(zhì)。為了克服這些不足，我們?cè)O(shè)計(jì)了熱CVD工藝來(lái)在完全不含壓縮或純化氣體且需要極少加工時(shí)間的周圍空氣環(huán)境中制備石墨烯。 The process is schematically illustrated in Fig. 1a, in which the precursor for graphene growth and a metal catalyst (for example, Ni foil) are placed close together inside the heating zone of a furnace, before heating the quartz tube. The quartz tube is then sealed and the temperature is increased. During the ramping stage, air inside the quartz tube is released through a valve to maintain atmospheric pressure. Once the annealing stage is complete, the sample is removed from the heating zone for rapid cooling. Raman spectra of the samples grown at 800 °C in the ambient-air process indicated the presence of single-to-few layer graphene films covering the surface of the growth substrate (Fig. 1b). 這種熱CVD工藝如圖1a示意性顯示，其中將用于石墨烯生長(zhǎng)的前體和金屬催化劑（例如，Ni箔）一起靠近設(shè)置在爐子的熱區(qū)里面，然后加熱石英管。然后，密封石英管，增加溫度。在升溫階段，通過(guò)閥門來(lái)釋放石英管里面的空氣，以保持常壓。一旦退火階段完成，從熱區(qū)取出樣品用于快速冷卻。在周圍空氣工藝中在800℃下生長(zhǎng)的樣品的拉曼光譜表明存在覆蓋生長(zhǎng)襯底的單層石墨烯膜-到-幾層石墨烯膜（圖1b）。 |
3樓2017-02-10 21:24:11
2樓2017-02-06 21:25:26
【答案】應(yīng)助回帖
|
In the standard operation, the catalyst is low-cost polycrystalline Ni foil. Graphene growth occurs by thermal reforming of a natural precursor, soybean oil, in a closed ambient-air environment. Unlike conventional CVD methods or conventional natural precursor methods for growing graphene, the technique does not require any purified gases8,9. Moreover, expensive vacuum processing is avoided. The natural precursors substituted for purified gases are cheaper and safer. By restricting the air flow into the quartz tube, the transformation of solid-state carbon into carbon dioxide or other gaseous species is prevented. By controlling the temperature, cooling rate and precursor amount, the process enables the growth of homogenous graphene films of good quality. A comparison of the method with other CVD processes is provided in Supplementary Tables 1 and 2. 在標(biāo)準(zhǔn)操作中，催化劑是低成本多晶Ni箔。通過(guò)在密封周圍空氣環(huán)境中天然前體大豆油的熱重整來(lái)開始石墨烯生長(zhǎng)。與用于生長(zhǎng)石墨烯的常規(guī)CVD方法或常規(guī)天然前體方法不同，這種技術(shù)部需要任何純化的氣體。此外，避免了昂貴的真空加工。取代純化氣體的天然前體更便宜且更安全。通過(guò)限制進(jìn)入石英管的空氣流動(dòng)，阻止固態(tài)碳轉(zhuǎn)變成二氧化碳或其它氣體物質(zhì)。通過(guò)控制溫度、冷卻速率和前體量，該熱CVD工藝實(shí)現(xiàn)生長(zhǎng)具有良好質(zhì)量的均勻的石墨烯膜。在補(bǔ)充的表1和表2中，比較了該方法與其它CVD工藝。 The parameters observed to control the quality of graphene include temperature, processing time, precursor, substrate and the ambient-air environment. Nickel acted as a good catalyst for the breakdown of precursor material (in this case, the soybean-oil molecules) into smaller building units that are essential for the synthesis of graphene12. 觀察到控制石墨烯質(zhì)量的參數(shù)包括溫度、加工時(shí)間、前體、襯底和周圍空氣環(huán)境。鎳用作用于將前體材料（在這種情況下，大豆油分子）分解成對(duì)石墨烯的合成而言所必要的構(gòu)成單元。 To investigate how the transformation occurred in the process, we have analysed the chemical composition of the annealed soybean oils at different temperatures (Supplementary Fig. 1). During the early stages of the annealing process, for instance at 300 °C, the long carbon chains in the soybean oil precursor were thermally dissociated into gaseous carbon building units such as methyl and ethyl species (Supplementary Fig. 1a). Other gaseous species were also generated, including hydrogen, water, hydroxyls and carbon dioxide, as confirmed by mass spectrometry (Supplementary Fig. 1b and c). Traces of heavier hydrocarbons such as propane were also observed. Most of the oil was vapourized by about 425 °C and a rapid mass reduction of the oil was observed by thermogravimetric analysis below 500 °C (Supplementary Fig. 1d). These building units present in the vapour can diffuse through the tube during the heating stage. As the temperature gradually increases to 800 °C, these carbon building units begin to dissociate into carbon atoms and dissolve into the Ni bulk. The sample was annealed for 3 min at 800 °C to promote dissolution of carbon atoms in the Ni substrate. Finally, following the rapid cooling stage, carbon segregates from the bulk and crystallizes on the Ni surface forming graphene12,13. 為了研究在這個(gè)工藝中轉(zhuǎn)變是如何進(jìn)行的，我們分析了在不同溫度下的退火的大豆油的化學(xué)組成（補(bǔ)充圖1）。在退火過(guò)程的早期階段，例如在300℃下，大豆油前體的長(zhǎng)碳鏈熱解離成氣態(tài)碳構(gòu)成單元例如甲基和乙基物質(zhì)（補(bǔ)充圖1a）。還產(chǎn)生其他氣態(tài)物質(zhì)，包括氫氣、水、羥基和二氧化碳，如通過(guò)質(zhì)譜所確認(rèn)（補(bǔ)充圖1b和1c）。還觀察到痕量的更重的烴，例如丙烷。大多數(shù)的油到約425℃時(shí)蒸發(fā)，通過(guò)熱重分析在500℃以下觀察到油的快速的質(zhì)量下降（補(bǔ)充圖1d）。在加熱階段過(guò)程中，在蒸氣中存在的構(gòu)成單元可擴(kuò)散通過(guò)管。隨著溫度逐漸增加到800℃，這些碳構(gòu)成單元開始解離成碳原子，并溶解進(jìn)入Ni本體。將樣品在800℃下退火3分鐘，以促進(jìn)碳原子在Ni襯底中的溶解。最后，在快速冷卻階段之后，碳從本體分離，且在Ni表面上結(jié)晶，這形成石墨烯。 |
4樓2017-02-10 21:48:37
【答案】應(yīng)助回帖
|
At elevated temperatures, long hydrocarbons in the oil decompose in the presence of O2 to form water vapour. In particular, water vapour can promote the etching of amorphous carbon deposits on the Ni surface14. As such, we did not observe the formation of amorphous carbons in our sample. This also helps maintain the catalytic activity of the Ni surface in breaking down the precursor material15. Moreover, we have conducted a detailed analysis on the consumption of oxygen in the reactor during the growth process (Supplementary Note 1). We found that the precursor amount was critical for the consumption of reactive oxygen species. In the optimal growth condition, a slight carbon excessive environment is used to promote the growth of graphene and deter the formation of amorphous carbon. On the other hand, an over-excessive amount of precursor material led to an oversaturation of deposited carbon in the bulk of Ni, and subsequently, the crystallization of graphite on the Ni surface. This may explain the resulting formation of thick graphene sheets as observed in Supplementary Fig. 2a. 在升高的溫度下，油中的長(zhǎng)烴在O2的存在下分解，以形成水蒸汽。具體地，水蒸汽可促進(jìn)沉積在Ni表面上的無(wú)定形碳的蝕刻。這樣，在我們的樣品中，我們沒(méi)有觀察到形成無(wú)定形碳。這也有助于保持Ni表面在分解前體材料時(shí)的催化活性。此外，我們還對(duì)生長(zhǎng)過(guò)程指南反應(yīng)器中氧氣的消耗進(jìn)行了詳細(xì)的分析（補(bǔ)充注釋1）。我們發(fā)現(xiàn)前體量對(duì)于反應(yīng)性氧物質(zhì)的消耗是關(guān)鍵的。在優(yōu)化的生長(zhǎng)條件下，使用稍微碳過(guò)量的環(huán)境來(lái)促進(jìn)石墨烯的生長(zhǎng)，且阻止形成無(wú)定形碳。另一方面，過(guò)度過(guò)量的前體材料導(dǎo)致Ni本體中沉積的碳的過(guò)飽和，且隨后導(dǎo)致在Ni表面上石墨的結(jié)晶。這可解釋導(dǎo)致形成如補(bǔ)充圖2a中所觀察到的較厚的石墨烯片。 明天繼續(xù)吧！ |
5樓2017-02-10 22:01:46
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[考研]
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[考研] 0703 化學(xué) 求調(diào)劑，一志愿山東大學(xué) 342 分 +7 | Shern—- 2026-03-28 | 7/350 |
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[考研] 290求調(diào)劑 +3 | dfffsar 2026-03-29 | 3/150 |
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[考研] 275求調(diào)劑 +15 | Micky11223 2026-03-25 | 20/1000 |
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