TWI675799B - 石墨片製造方法 - Google Patents

石墨片製造方法 Download PDF

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TWI675799B
TWI675799B TW107126560A TW107126560A TWI675799B TW I675799 B TWI675799 B TW I675799B TW 107126560 A TW107126560 A TW 107126560A TW 107126560 A TW107126560 A TW 107126560A TW I675799 B TWI675799 B TW I675799B
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substrate
graphite sheet
composite substrate
octadecyltrichlorosilane
manufacturing
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TW202007643A (zh
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謝淑貞
Shu Chen Hsieh
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國立中山大學
National Sun Yat-Sen University
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Abstract

一種石墨片製造方法，用以製造獲得與石墨烯具有類似特性的石墨片，其包含：於一基板上形成一十八烷基三氯矽烷層，得一複合基板；於250~400℃之溫度下，對該複合基板進行退火30~90分鐘，使該十八烷基三氯矽烷層中的十八烷基三氯矽烷自行組裝形成附著於該基板上的石墨片；及將經退火之複合基板浸入水中，在40KHz之頻率、200瓦之功率下，進行超音波震盪2分鐘，使該石墨片脫離該基板。

Description

石墨片製造方法
本發明係關於一種石墨片製造方法，尤其是一種與石墨烯具有類似特性的石墨片之石墨片製造方法。
石墨烯(graphene)係呈蜂巢狀晶格(honeycomb crystal lattice)之平面薄膜，為僅具有一個碳原子厚度(約為0.34nm)之二維材料，其具有高機械強度、熱傳導及高載子轉移率等優異特性，能夠應用於多種領域。
然而，石墨烯多以習知化學氣相層積法(chemical vapor deposition，CVD)製備而成，製備過程繁瑣。有鑑於此，若是能夠以簡單的製程即能夠製造獲得與石墨烯具有類似特性的石墨片，將對石墨烯的相關應用產業上帶來極大的助益。
為解決上述問題，本發明的目的是提供一種石墨片製造方法係用以製造獲得與石墨烯具有類似特性的石墨片者。
本發明的石墨片製造方法，包含：於一基板上形成一十八烷基三氯矽烷層，得一複合基板；於250~400℃之溫度下，對該複合基板進行退火30~90分鐘，使該十八烷基三氯矽烷層中的十八烷基三氯矽烷自行組裝形成附著於該基板上的石墨片；及將經退火之複合基板浸入水中，在40KHz 之頻率、200瓦之功率下，進行超音波震盪2分鐘，使該石墨片脫離該基板。
依據上述，藉由前述的石墨片製造方法，即能夠製造獲得與石墨烯具有類似特性的石墨片(晶格間距約為0.24nm、厚度約為0.34nm)，因此可以作為石墨烯的替代物，例如能夠作為表面增強拉曼散射活性基板使用，應用於分析一待測樣品中的雙酚A的濃度，為本發明之功效。
本發明的石墨片製造方法另包含：於該基板上形成該十八烷基三氯矽烷層包含：將該基板置入一十八烷基三氯矽烷溶液中，於25~35℃之溫度下靜置24小時，得一複合基板半成品；及於115℃之溫度下，對將該複合基板半成品進行退火10分鐘；如此有助於在該基板上形成厚度均一的十八烷基三氯矽烷層。
本發明的石墨片製造方法另包含：將十八烷基三氯矽烷溶於一溶劑中，以得該十八烷基三氯矽烷溶液，該溶劑為十六烷、甲苯、氯仿或二氯甲烷；如此能夠藉由該溶劑的選擇，使十八烷基三氯矽烷能夠均勻分布於該十八烷基三氯矽烷溶液中。
本發明的石墨片製造方法另包含：對該複合基板半成品進行退火前，以至少一潤洗液潤洗該複合基板半成品，以去除該複合基板半成品上的雜質及殘留物；較佳地，以該至少一潤洗液潤洗該複合基板半成品包含：依序以一第一潤洗液、一第二潤洗液及一第三潤洗液潤洗該複合基板半成品，該第一潤洗液、該第二潤洗液及該第三潤洗液分別為氯仿、異丙醇及去離子水；如此藉由該第一潤洗液、該第二潤洗液及該第三潤洗液的使用，可以去除該複合基板半成品上的雜質及殘留物，以避免該雜質及該殘留物對後續製程造成的影響。
本發明的石墨片製造方法中，該基板為一矽晶片；如此，藉由該矽晶片的平整表面，使該十八烷基三氯矽烷層中的十八烷基三氯矽烷能夠 形成矽氧鍵結(Si-O bond)，因而該矽晶片可以作為支撐所形成的石墨片之良好基板。
〔第1圖〕試驗(B)中各組待測樣品的拉曼光譜曲線。
〔第2圖〕試驗(C)中各組待測樣品的拉曼光譜曲線。
〔第3圖〕試驗(D)中各組待測樣品的拉曼光譜曲線。
〔第4圖〕試驗(E)中各組待測樣品的拉曼光譜曲線。
為讓本發明之上述及其他目的、特徵及優點能更明顯易懂，下文特舉本發明之較佳實施例，並配合所附圖式，作詳細說明如下：本發明之石墨片製造方法的一實施例中，係藉由形成於一基板上的十八烷基三氯矽烷(ocatadecyltrichlorosilane，簡稱OTS)層的自組裝作用，得以於該基板上成形一石墨片，該石墨片之晶格間距約為0.24nm，且厚度約為0.34nm，與石墨烯具有類似特性。
詳而言之，工者係可以藉由塗佈、噴灑等任何習知方式於該基板上形成該十八烷基三氯矽烷層。於本實施例中，係可以將作為該基板的一矽晶片置入一十八烷基三氯矽烷溶液(濃度為1M)中，並於25~35℃之溫度下靜置24小時，得一複合基板半成品，接著再於115℃之溫度下，對該複合基板半成品進行退火(annealing)10分鐘，得一複合基板，該複合基板包含該基板及形成於該基板上的該十八烷基三氯矽烷層。又，該十八烷基三氯矽烷溶液包含十八烷基三氯矽烷及一溶劑，該溶劑可以為十六烷 (hexadecane)、甲苯(tolune)、氯仿(chloroform)或二氯甲烷(dichloromethane)，使十八烷基三氯矽烷能夠均勻分布於該十八烷基三氯矽烷溶液中。
此外，為了去除附著於該複合基板半成品上的雜質及殘留物，進而防止該雜質及殘留物影響後續的製程效率，可以在對該複合基板半成品進行退火前，以至少一潤洗液潤洗該複合基板半成品。於本實施例中，係依許使用一第一潤洗液、一第二潤洗液及一第三潤洗液潤洗該複合基板半成品，該第一潤洗液、該第二潤洗液及該第三潤洗液分別為氯仿、異丙醇(isopropanol)及去離子水(deionized water)。
接著於高溫下對該複合基板進行退火，使該十八烷基三氯矽烷層中的十八烷基三氯矽烷能夠進行該自組裝作用。於本實施例中，係於250~400℃之溫度下，對該複合基板進行退火30~90分鐘，此時該十八烷基三氯矽烷層中的十八烷基三氯矽烷即能夠進行該自組裝作用，進而形成附著於該基板上的石墨片。
進一步，工者即可以自該基板上分離該石墨片。於本實施例中，係將經退火之複合基板浸泡於水中，在40KHz之頻率、200瓦之功率下，進行超音波震盪2分鐘，即可以使該石墨片脫離該基板，取得該石墨片。
為證實經該石墨片製造方法所製造獲得的石墨片確實與石墨烯具有類似特性，且可以作為表面增強拉曼散射活性基板(surface-enhanced Raman spectroscopy active substrate)使用，應用於分析待測樣品中的雙酚A的濃度，遂進行以下試驗：
(A)石墨片的特性分析
依據穿透式電子顯微鏡(transmission electron microscopy，簡稱TEM)及高解析場發射穿透式電子顯微鏡(high-resolution transmission electron microscopy，簡稱HRTEM)的分析結果可以得知，經該石墨片製造方法所製造獲得的石墨片具有0.24nm的晶格間距(lattice spacing)，與石墨烯的晶格常數(lattice constant)相同。另依據原子力顯微鏡(atomic force microscopy，簡稱AFM)的表面形貌分析(surface topography)結果顯示，該石墨片的厚度約為0.34nm，與石墨烯的層間距(interlayer spacing)相當。依據上述，該石墨片確實具有與石墨烯類似的特性。
(B)石墨片作為表面增強拉曼散射活性基板的使用
本試驗係以雙酚A(bisphenol A，簡稱BPA)作為待測樣品，將雙酚A溶解於乙醇(即，95%的乙醇水溶液)中，以形成0.1M的雙酚A溶液，將2μL的雙酚A溶液滴在該石墨片(第B1組)或該矽晶片(第B2組)上，使該雙酚A溶液於室溫下乾燥後，進行拉曼光譜的分析，使用波長為532nm的雷射光，其功率為21.9mW。本試驗另以該石墨片(第B3組)及該矽晶片(第B4組)作為比較。
請參照第1圖所示，第B3組的拉曼光譜曲線僅於1341cm-1及1602cm-1處具有波峰，而第B1及B2組的拉曼光譜曲線則於1121cm-1、1188cm-1、1240cm-1、1269cm-1、1621cm-1及3072cm-1處具有波峰，然而比較第B1及B2組的拉曼光譜曲線可以得知，儘管以第B1組的石墨片或以第B2組的矽晶片均可以測得雙酚A的訊號，惟以B1組的石墨片所測得的強度明顯優於以第B2組的矽晶片所測得者，顯示該石墨片確實能夠作為表面增強拉曼散射活性基板使用。
(C)對雙酚A的靈敏度
本試驗係分別將濃度為10-1M(第C1組)、10-2M(第C2組)、10-3M(第C3組)、10-4M(第C4組)、10-5M(第C5組)及10-6M(第C6組)的雙酚A溶液作為待測樣品，續進行拉曼光譜的分析。
請參照第2圖所示，縱使針對濃度僅為10-6M的雙酚A溶液(第C6組)，藉由該石墨片的使用仍能夠有效測得雙酚A的訊號，且該濃度已遠低於歐盟對雙酚A的遷移限制(specific migration limit，簡稱SML)，即遷移至每公斤食物中的雙酚A不得高於0.6mg(經換算約為2.6μM)。
(D)各種塑膠用品的雙酚A之遷移量
本試驗係將兩種不同的塑膠湯匙(第D1、D2組)、嬰兒奶瓶(第D3組)、可重複使用的夾鏈袋(第D4組)及密封食品容器(第D5組)作為待測樣品，將各組待測樣品與80℃之熱水接觸1小時，再進行拉曼光譜的分析。本試驗另以濃度為10-4M的雙酚A溶液(第D6組)作為比較。
請參照第3圖所示，依據鄰近1121cm-1處的波峰(即，第3圖星號處)之波峰面積進行換算的結果，可以得知各組的待測樣品的雙酚A之遷移量約分別為1×10-5、3.2×10-6、2×10-5、1×10-6及6.3×10-7M。
(E)鹽類濃度對偵測效果的影響
本試驗係以濃度為10-3M的雙酚A溶液作為待測樣品，並於其中加入氯化鈉溶液，使各組待測樣品的氯化鈉濃度分別為0M(第E1組)、0.025M(第E2組)、0.05M(第E3組)、0.1M(第E4組)、0.25M(第E5組)、0.5M(第E6組)、1M(第E7組)及2M(第E8組)，續進行拉曼光譜的分析。
請參照第4圖所示，隨著氯化鈉濃度的升高，雙酚A的訊號強度有逐漸降低的現象，然而在與人類血清樣品與人類尿液樣品相似的氯化鈉離子強度(人類血清樣品與人類尿液樣品的氯化鈉離子強度分別為0.14M及0.17M)下，仍可以清楚地測得雙酚A的訊號強度，顯示該石墨片不僅能夠適用於檢測含鹽溶液中的雙酚A，亦適用於檢測體液(如，血清或尿液)中的雙酚A。
綜上所述，藉由前述的石墨片製造方法，即能夠製造獲得與石墨烯具有類似特性的石墨片(晶格間距約為0.24nm、厚度約為0.34nm)，因此可以作為石墨烯的替代物，例如能夠作為表面增強拉曼散射活性基板使用，應用於分析待測樣品中的雙酚A的濃度，為本發明之功效。
雖然本發明已利用上述較佳實施例揭示，然其並非用以限定本發明，任何熟習此技藝者在不脫離本發明之精神和範圍之內，相對上述實施例進行各種更動與修改仍屬本發明所保護之技術範疇，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。

Claims (6)

  1. 一種石墨片製造方法，包含：於一基板上形成一十八烷基三氯矽烷層，得一複合基板；於250~400℃之溫度下，對該複合基板進行退火30~90分鐘，使該十八烷基三氯矽烷層中的十八烷基三氯矽烷自行組裝形成附著於該基板上的石墨片；及將經退火之複合基板浸入水中，在40KHz之頻率、200瓦之功率下，進行超音波震盪2分鐘，使該石墨片脫離該基板。
  2. 如申請專利範圍第1項所述之石墨片製造方法，其中，於該基板上形成該十八烷基三氯矽烷層包含：將該基板置入一十八烷基三氯矽烷溶液中，於25~35℃之溫度下靜置24小時，得一複合基板半成品；及於115℃之溫度下，對將該複合基板半成品進行退火10分鐘。
  3. 如申請專利範圍第2項所述之石墨片製造方法，另包含：將十八烷基三氯矽烷溶於一溶劑中，以得該十八烷基三氯矽烷溶液，該溶劑為十六烷、甲苯、氯仿或二氯甲烷。
  4. 如申請專利範圍第2項所述之石墨片製造方法，另包含：對該複合基板半成品進行退火前，以至少一潤洗液潤洗該複合基板半成品，以去除該複合基板半成品上的雜質及殘留物。
  5. 如申請專利範圍第4項所述之石墨片製造方法，其中，以該至少一潤洗液潤洗該複合基板半成品包含：依序以一第一潤洗液、一第二潤洗液及一第三潤洗液潤洗該複合基板半成品，該第一潤洗液、該第二潤洗液及該第三潤洗液分別為氯仿、異丙醇及去離子水。
  6. 如申請專利範圍第1~5項中任一項所述之石墨片製造方法，其中，該基板為一矽晶片。
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