TW201331126A - Process for producing graphene with specific shape - Google Patents
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本發明係有關於一種石墨烯之製備方法，特別是關於一種產生特定形狀之石墨烯製作方法。The present invention relates to a method for preparing graphene, and more particularly to a method for producing graphene having a specific shape.
碳已知有四種結晶結構，包括鑽石、石墨、巴克球(fullerene)和碳奈米管，巴克球、奈米碳管和石墨被視為石墨烯的衍生物質。石墨烯的結構概念在很久前就已經存在，有些科學家從熱力學理論的觀點，認為單層原子的二維結構是不穩定的，主要因為熱擾動會使單層中的原子上下移動，造成原子間重新組合，而形成較穩定的三維結構。後來的實驗也顯示薄膜的熔點隨厚度變小而降低，這結果加強了單層原子結構不穩定的論點，因此二維平面原子層一直被視為是三維結構中的一部份，無法單獨穩定存在。石墨被視為由多層石墨烯所堆積組成的三維晶體；而碳六十和奈米碳管也被形容為是由石墨烯所捲曲而成的材料。Carbon is known to have four crystalline structures, including diamonds, graphite, fullerene, and carbon nanotubes, and buckyballs, carbon nanotubes, and graphite are considered derivatives of graphene. The structural concept of graphene has existed for a long time. Some scientists believe that the two-dimensional structure of a single layer of atoms is unstable from the viewpoint of thermodynamic theory, mainly because thermal perturbation causes atoms in a single layer to move up and down, resulting in interatomic Recombination to form a more stable three-dimensional structure. Subsequent experiments have also shown that the melting point of the film decreases with decreasing thickness, which strengthens the argument that the single-layer atomic structure is unstable. Therefore, the two-dimensional planar atomic layer has always been regarded as a part of the three-dimensional structure and cannot be stabilized alone. presence. Graphite is considered to be a three-dimensional crystal composed of a stack of graphene; and carbon sixty and nanocarbon tubes are also described as a material obtained by crimping graphene.
石墨烯是目前世界上最薄卻也是最堅硬的奈米材料，幾乎呈現完全透明，其熱傳導係數高達5300 W/m‧K，高於碳奈米管與金剛石，適用於製造導熱材料與熱界面材料。於室溫下，其電子遷移率(超過15000 cm2/V‧s)約為奈米碳管電子遷移率(約10000 cm2/V‧s)的1.5倍、矽晶電子遷移率(約1400 cm2/V‧s)的10倍以上速度，而其電阻率約為10-6 Ω‧cm，比銅或銀金屬低，為目前世界上具電阻率最小的材料。因其本身電阻率極低，故其電子移動的速度極快，因此被預期用來發展更薄、導電速度更快的新一代電子元件。另由於石墨烯幾乎完全透明且為良好的導體材料，也適用於製造透明觸控螢幕、光板、鋰電池、超級電容與太陽能電池。Graphene is currently the thinnest but hardest nano material in the world. It is almost completely transparent. Its thermal conductivity is up to 5300 W/m‧K, which is higher than that of carbon nanotubes and diamonds. It is suitable for the manufacture of thermal materials and thermal interfaces. material. At room temperature, its electron mobility (over 15000 cm2/V‧s) is about 1.5 times that of carbon nanotubes (about 10000 cm2/V‧s) and the mobility of twinned electrons (about 1400 cm2/ V‧s) is more than 10 times faster, and its resistivity is about 10-6 Ω‧cm, which is lower than copper or silver metal. It is the world's smallest resistivity material. Because of its extremely low resistivity, its electrons move extremely fast, so it is expected to develop a new generation of electronic components that are thinner and have faster conduction speeds. In addition, since graphene is almost completely transparent and is a good conductor material, it is also suitable for manufacturing transparent touch screens, light panels, lithium batteries, super capacitors and solar cells.
2004年英國曼徹斯特大學A. K. Geim教授的研究團隊將石墨薄片黏貼在一片膠布上，用另一片膠帶黏貼石墨薄片的另一面，再將兩片膠帶撕開時，會將石墨剝離成兩片更薄的石墨薄片，把這得到的石墨薄片再黏貼膠帶然後再撕開，重覆膠帶剝離步驟數次，可得到小片單層原子厚度的石墨烯。石墨烯經穿透式電子顯微鏡觀察，顯示石墨烯薄膜中的碳原子排列具高次序性。In 2004, the research team of Professor AK Geim of the University of Manchester in the United Kingdom glued the graphite sheet to a piece of tape and glued it to the other side of the graphite sheet with another piece of tape. When the two pieces of tape were torn open, the graphite was peeled off into two thinner pieces. The graphite flakes are further adhered to the tape and then peeled off, and the tape stripping step is repeated several times to obtain a small piece of single-layer atomic thickness graphene. Graphene was observed by a transmission electron microscope to show that the carbon atoms in the graphene film were aligned in a high order.
目前製備石墨烯的方法約為四種：(1)以機械剝離方式，從石墨材料製備出石墨烯，此方式可簡易快速獲得單層或多層的石墨烯，但只能小量製造；(2)以化學氣相沉積法或磊晶成長法製備石墨烯，利用通入熱裂解的碳氫化合物氣源並沉積在鎳片或銅片上，其特色為可製備出大面積單層或多層石墨烯，但其缺點為均勻性與厚度難以控制；(3)於絕緣體基材上生長石墨烯，例如於碳化矽表面可生長極薄的石墨烯，其缺點為價格昂貴且難以製備大面積；(4)利用有機酸性溶劑進行插層製備出氧化石墨烯(GO)，再經由還原程序得到石墨烯，其缺點為處理時間長，且還原後之石墨烯容易變形與翹曲，使得石墨烯品質良莠不齊。At present, there are about four methods for preparing graphene: (1) preparing graphene from a graphite material by mechanical stripping, which can easily and quickly obtain single-layer or multi-layer graphene, but can only be manufactured in a small amount; Preparing graphene by chemical vapor deposition or epitaxial growth method, using a hydrocarbon gas source that is passed through a pyrolysis and depositing on a nickel sheet or a copper sheet, which is characterized in that a large-area single-layer or multi-layer graphene can be prepared. However, the disadvantage is that the uniformity and thickness are difficult to control; (3) the growth of graphene on the insulator substrate, for example, the growth of extremely thin graphene on the surface of the tantalum carbide, which is disadvantageous in that it is expensive and difficult to prepare a large area; Graphene oxide (GO) is prepared by intercalation with an organic acidic solvent, and graphene is obtained through a reduction procedure. The disadvantage is that the treatment time is long, and the graphene after reduction is easily deformed and warped, so that the quality of graphene is uneven.
上述各項技術大都是以高純度粉體狀之天然石墨、價格昂貴之片狀單晶天然石墨為原始材料，利用化學酸插層處理製程來製備石墨烯，製程時間非常冗長，且須經還原製程處理，才可獲得高品質石墨烯，但仍不易具有均勻型狀的石墨烯薄片，也不易運用於大量生產。因此，目前業界極需發展出一種高效率、易控制且具有高經濟效應之一種產生特定形狀之石墨烯製作方法，如此一來，方能同時兼具成本與時效，有效產出均勻型狀的石墨烯薄片。Most of the above technologies are made of high-purity powder-like natural graphite and expensive sheet-like single crystal natural graphite. The chemical acid intercalation process is used to prepare graphene. The process time is very long and must be reduced. High-quality graphene can be obtained by process treatment, but it is still difficult to have a uniform shape of graphene sheets, and it is not easy to be used for mass production. Therefore, at present, it is extremely necessary for the industry to develop a method for producing graphene having a specific shape with high efficiency, easy control, and high economic effect, so that the cost and the time effect can be simultaneously combined, and the uniform shape can be effectively produced. Graphene sheets.
鑒於上述習知技術之缺點，本發明之主要目的在於提供一種產生特定形狀之石墨烯製作方法，整合一人造排列方向石墨之初始材料、一成型製程、一電化學製程等，以製備出高效率、高品質且具有特定形狀之石墨烯薄片。In view of the above disadvantages of the prior art, the main object of the present invention is to provide a method for producing graphene having a specific shape, integrating an initial material of an artificial alignment direction graphite, a molding process, an electrochemical process, etc., to prepare high efficiency. High quality and graphene sheets of a specific shape.
為了達到上述目的，根據本發明所提出之一方案，提供一種特定形狀之石墨烯製作方法，其步驟包括：(A)首先提供一人造排列方向石墨之初始材料，將該人造排列方向石墨之初始材料進行一成型製程而得一壓合材料；(B)接著利用一電化學法處理該壓合材料，其中該電化學法包含一電解液；(C)利用過濾該電解液而得一特定形狀之石墨烯薄片。In order to achieve the above object, according to one aspect of the present invention, a method for fabricating graphene of a specific shape is provided, the steps comprising: (A) first providing an initial material of an artificial alignment direction graphite, and initializing the artificial alignment direction graphite The material is subjected to a molding process to obtain a pressure-bonding material; (B) the electrochemical material is then treated by an electrochemical method, wherein the electrochemical method comprises an electrolyte; (C) the electrolyte is filtered to obtain a specific shape. Graphene sheets.
步驟(A)中的人造排列方向石墨之初始材料包含輻射狀之石墨結晶排列的碳纖維、輻射狀之石墨纖維、平行排列之碳纖維、平行排列石墨纖維、平行排列纖維塊材、平行排列纖維石墨片、同軸排列方向之石墨奈米結晶材料、沿軸向平行排列之氣相成長碳纖維、沿軸向平行排列之氣相成長石墨纖維、杯狀堆疊排列之氣相成長碳纖維、杯狀堆疊排列之氣相成長石墨纖維等材料。The artificial material of the artificial alignment direction in the step (A) comprises a radial graphite crystal carbon fiber, a radial graphite fiber, parallel carbon fibers, parallel aligned graphite fibers, parallel aligned fiber blocks, and parallel aligned fiber graphite sheets. Graphite nanocrystalline material in a coaxial alignment direction, vapor-grown carbon fiber arranged in parallel along the axial direction, vapor-grown graphite fiber arranged in parallel in the axial direction, vapor-grown carbon fiber arranged in a cup-shaped stack, gas arranged in a cup-like stack Phase growth graphite fiber and other materials.
步驟(A)中另包含一成型製程，該成型製程包含油壓、模壓、熱壓、擠出、押出、射出、紡出、熔紡等製程其中之一或利用上述製程任意組合來進行成型製程。成型製程主要的功用係利用上述的不同手段達到對材料的加壓，利用壓力提高該壓合材料的密度。The step (A) further comprises a molding process comprising one of oil pressure, molding, hot pressing, extrusion, extrusion, injection, spinning, melt spinning, or the like, or any combination of the above processes for forming the molding process . The main function of the forming process is to use the different means described above to achieve pressurization of the material, and the pressure is used to increase the density of the pressed material.
以上之概述與接下來的詳細說明及附圖，皆是為了能進一步說明本發明為達成預定目的所採取的方式、手段及功效。而有關本發明的其他目的及優點，將在後續的說明及圖示中加以闡述。The above summary, the following detailed description and the accompanying drawings are intended to further illustrate the manner, the Other objects and advantages of the present invention will be described in the following description and drawings.
以下係藉由特定的具體實例說明本發明之實施方式，熟悉此技藝之人士可由本說明書所揭示之內容輕易地瞭解本發明之其他優點與功效。The embodiments of the present invention are described below by way of specific examples, and those skilled in the art can readily appreciate other advantages and functions of the present invention from the disclosure herein.
請參考第一圖，為一種產生特定形狀之石墨烯製作方法流程示意圖。如圖所示，本發明提供一種產生特定形狀之石墨烯製作方法，其步驟如下：首先，如步驟(A)提供一人造排列方向石墨之初始材料，將該人造排列方向石墨之初始材料進行一成型製程而得一壓合材料S101。在本發明中，人造排列方向石墨之初始材料選用輻射狀之石墨結晶排列的碳纖維、輻射狀之石墨纖維、平行排列之碳纖維、平行排列石墨纖維、平行排列纖維塊材、平行排列纖維石墨片、同軸排列方向之石墨奈米結晶材料(多壁奈米碳管、單壁奈米碳管、雙壁奈米碳管、氣相成長碳纖維)時，利用一成型製程，可將該人造排列方向石墨之初始材料轉換成一壓合材料，該成型製程可包含油壓、模壓、熱壓、擠出、押出、射出、紡出、熔紡等製程其中之一或利用上述製程任意組合來進行成型製程。成型製程主要的功用係利用上述的不同手段達到對材料的加壓，利用壓力提高該壓合材料的密度。Please refer to the first figure for a schematic diagram of a method for producing a graphene having a specific shape. As shown in the figure, the present invention provides a method for producing graphene of a specific shape, the steps of which are as follows: First, as shown in step (A), an initial material of graphite in an artificial alignment direction is provided, and the initial material of the artificial alignment direction graphite is subjected to a A molding process S101 is obtained by the molding process. In the present invention, the initial material of the artificial alignment direction graphite is selected from a radial graphite crystal carbon fiber, a radial graphite fiber, a parallel arrangement of carbon fibers, a parallel arrangement of graphite fibers, a parallel arrangement of fiber blocks, a parallel arrangement of fiber graphite sheets, When the graphite nanocrystalline material (multi-walled carbon nanotube, single-walled carbon nanotube, double-walled carbon nanotube, vapor-grown carbon fiber) is coaxially arranged, the artificial alignment direction graphite can be formed by a molding process. The initial material is converted into a press-bonding material, and the forming process may include one of oil pressure, molding, hot pressing, extrusion, extrusion, injection, spinning, melt spinning, or the like, or any combination of the above processes may be used for the molding process. The main function of the forming process is to use the different means described above to achieve pressurization of the material, and the pressure is used to increase the density of the pressed material.
接著如步驟(B)利用一電化學法處理該壓合材料，其中該電化學法包含一電解液S102。在本發明中，使用一種電化學法處理該壓合材料，其裝置包含有一電解槽含有電解液、兩個對電極、一個施加偏壓之電源供應器。其中電解液是硫酸與氫氧化鉀等離子溶液以比例來混合，其pH值範圍可以在1-14的範圍，而最佳製程pH值範圍在12-14。而對電極可以一邊為金屬電極(如鉑、金等)，另一邊為石墨初始原料，亦可以兩邊電極皆為石墨初始原料。而電化學製程中的施加電壓可以是一直流電壓電源、交流電壓電源、直流電流電源、或交流電流電源。The press material is then treated by an electrochemical process as in step (B), wherein the electrochemical process comprises an electrolyte S102. In the present invention, the press material is treated by an electrochemical method, the apparatus comprising an electrolytic cell containing an electrolyte, two counter electrodes, and a biasing power supply. The electrolyte is mixed with a solution of sulfuric acid and potassium hydroxide, and the pH range can be in the range of 1-14, and the optimum process pH range is 12-14. The counter electrode may be a metal electrode (such as platinum, gold, etc.) on one side, and a graphite starting material on the other side, or both of the electrodes may be graphite starting materials. The applied voltage in the electrochemical process may be a DC voltage source, an AC voltage source, a DC current source, or an AC current source.
然後，如步驟(C)利用過濾該電解液而得一特定形狀之石墨烯薄片S103，其中，該特定形狀之石墨烯薄片係為一長條狀之石墨烯薄片，其長寬之比值大於三，厚度小於30nm。Then, in step (C), the electrolyte is filtered to obtain a graphene sheet S103 of a specific shape, wherein the graphene sheet of the specific shape is a long strip of graphene sheet having a ratio of length to width greater than three The thickness is less than 30 nm.
為更加說明本發明，以實施例說明之。在上述材料中，使用輻射狀石墨結晶排列的碳纖維為人造排列方向石墨之初始材料，以熱壓方式將該輻射狀石墨結晶排列的碳纖維壓製作成壓合材料，再以電化學法處理該壓合材料，其製程參數為以固定直流電壓-10~+10 V，施加於兩對電極且作正負極性切換(週期10秒)，進行電化學法快速剝離該初始材料，其中電解液的選擇為硫酸混合氫氧化鉀(混合後pH值約13)。最後再利用過濾該電解液及可得一長條狀之石墨烯薄片，其拉曼分析結果顯示請參考第二圖，第二圖為一種長條狀石墨烯薄片之拉曼光譜圖，所獲得的石墨烯薄片為具備規則形狀之長條狀，其長寬比值約為3/1~5/1，同時參考其拉曼光譜圖時可發現其缺陷密度特徵峰(D模)，僅略高於初始材料的高石墨化結晶特性，且其2D模形成對稱且較低的半高寬，顯示所獲得的石墨烯為高品質且為寡層石墨烯。另外，請參考第三圖，一種長條狀石墨烯薄片之厚度量測圖，顯示石墨烯薄片的長條狀之厚度約為雙層石墨烯的結構(厚度~1.6 nm)。To further illustrate the invention, it is illustrated by the examples. In the above materials, the carbon fiber arranged by the radial graphite crystal is an initial material of the artificial alignment direction graphite, and the carbon fiber arranged by arranging the radial graphite crystal is pressed into a pressing material by hot pressing, and the pressing is electrochemically treated. The material has a process parameter of fixed DC voltage -10~+10 V, applied to two pairs of electrodes and switched between positive and negative polarity (period of 10 seconds), and electrochemically stripped the starting material, wherein the electrolyte is selected as sulfuric acid. Mix potassium hydroxide (pH about 13 after mixing). Finally, the electrolyte is filtered and a long strip of graphene sheet is obtained. The Raman analysis results show that the second graph is shown. The second graph is a Raman spectrum of a long strip of graphene sheet. The graphene sheet has a long strip shape with a regular shape and an aspect ratio of about 3/1 to 5/1, and the defect density characteristic peak (D mode) can be found only when referring to the Raman spectrum thereof, which is only slightly higher. The high graphitization crystallization characteristics of the starting material, and its 2D mode formation symmetry and lower full width at half maximum, show that the obtained graphene is of high quality and is oligo-layer graphene. In addition, please refer to the third figure, a thickness measurement diagram of a long strip of graphene sheet, showing that the strip-like thickness of the graphene sheet is about the structure of the double-layer graphene (thickness ~1.6 nm).
當使用沿軸向平行排列之氣相成長碳纖維、沿軸向平行排列之氣相成長石墨纖維為人造排列方向石墨之初始材料時，利用上述實施例步驟，可得一圓板狀之石墨烯薄片，其直徑小於1微米，厚度小於30nm。When a vapor-grown carbon fiber arranged in parallel in the axial direction and a vapor-grown graphite fiber arranged in parallel in the axial direction are used as an initial material of the artificial alignment direction graphite, a disk-shaped graphene sheet can be obtained by using the steps of the above embodiment. It has a diameter of less than 1 micron and a thickness of less than 30 nm.
當使用杯狀堆疊排列之氣相成長碳纖維、杯狀堆疊排列之氣相成長石墨纖維為人造排列方向石墨之初始材料時，利用上述實施例步驟，可得一圓板狀之石墨烯薄片，其直徑大於100nm，厚度小於30nm。When the gas-phase-growth carbon fiber arranged in a cup-shaped stack and the vapor-grown graphite fiber arranged in a cup-like stack are used as the starting material of the artificial alignment direction graphite, a disk-shaped graphene sheet having a diameter can be obtained by using the steps of the above embodiment. It is larger than 100 nm and has a thickness of less than 30 nm.
上述之實施例僅為例示性說明本發明之特點及其功效，而非用於限制本發明之實質技術內容的範圍。任何熟習此技藝之人士均可在不違背本發明之精神及範疇下，對上述實施例進行修飾與變化。因此，本發明之權利保護範圍，應如後述之申請專利範圍所列。The above-described embodiments are merely illustrative of the features and functions of the present invention, and are not intended to limit the scope of the technical scope of the present invention. Modifications and variations of the above-described embodiments can be made by those skilled in the art without departing from the spirit and scope of the invention. Therefore, the scope of protection of the present invention should be as set forth in the scope of the claims described below.
S101-S103．．．步驟S101-S103. . . step
第一圖係為本發明一種產生特定形狀之石墨烯製作方法流程示意圖；The first figure is a schematic flow chart of a method for producing graphene having a specific shape according to the present invention;
第二圖係為本發明一種長條狀石墨烯薄片之拉曼光譜圖；The second figure is a Raman spectrum of a long strip of graphene sheet of the present invention;
第三圖係為本發明一種長條狀石墨烯薄片之厚度量測圖。The third figure is a thickness measurement diagram of a long strip of graphene sheet of the present invention.
S101-S103．．．步驟S101-S103. . . step
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103879998A (en) * | 2013-12-27 | 2014-06-25 | 杭州金马能源科技有限公司 | Device for preparing graphene through large-scale electrochemical efficient stripping |
| CN114447269A (en) * | 2021-12-28 | 2022-05-06 | 华为数字能源技术有限公司 | Positive electrode conductive agent, preparation method thereof, positive electrode piece and battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103879998A (en) * | 2013-12-27 | 2014-06-25 | 杭州金马能源科技有限公司 | Device for preparing graphene through large-scale electrochemical efficient stripping |
| CN114447269A (en) * | 2021-12-28 | 2022-05-06 | 华为数字能源技术有限公司 | Positive electrode conductive agent, preparation method thereof, positive electrode piece and battery |
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