TW201803805A - 使用自由浮動法處理大規模轉移的石墨烯片之方法 - Google Patents

使用自由浮動法處理大規模轉移的石墨烯片之方法 Download PDF

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TW201803805A
TW201803805A TW106112415A TW106112415A TW201803805A TW 201803805 A TW201803805 A TW 201803805A TW 106112415 A TW106112415 A TW 106112415A TW 106112415 A TW106112415 A TW 106112415A TW 201803805 A TW201803805 A TW 201803805A
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史考特 海斯
彼得 貝沃斯
傑考布 史威特
史帝芬 辛頓
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洛克希德馬汀公司
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/194—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/18—Acidic compositions for etching copper or alloys thereof

Abstract

一種從銅基材轉移石墨烯片至功能基材的方法包括使用化學蒸氣沉積使該石墨烯片形成在該銅基材上和使用寬束照射藉由多個氙離子照射配置在該銅基材上之該石墨烯片以形成經製備之石墨烯片。該經製備之石墨烯片對在該經製備之石墨烯片轉移至該功能基材期間所引起之形成非故意的缺陷呈現抗性。該方法另外包括使用蝕刻劑浴以自該經製備之石墨烯片移除該銅基材、使該經製備之石墨烯片在浮動浴中浮動、使該功能基材浸沒在該浮動浴中及降低該浮動浴之流體水平以使該經製備之石墨烯片下降至該功能基材上。

Description

使用自由浮動法處理大規模轉移的石墨烯片之方法
本發明關於使用自由浮動法處理大規模轉移的石墨烯片之方法。
石墨烯代表一種碳形式，其中碳原子處於六員晶格環之單一原子薄片內或於數個層合片(例如約20或更少個)內。製造高品質之大規模之石墨烯片(亦即1cm2或更大)的已知方法是透過化學蒸氣沉積(CVD)。在CVD期間，生長基材曝於一或多種氣態反應物，該氣態反應物反應以在該生長基材表面上沉積碳膜，該沉積產生石墨烯片。在生長後，該石墨烯片後續必須轉移至適合該石墨烯片之所要應用的功能基材。為轉移該石墨烯片至所要之基材需要使該石墨烯片與該生長基材分開，該分開尤其在大規模轉移(其中受損風險是高的)時可能在該石墨烯片中產生撕扯的、裂開的、或其他實質的缺陷。通常，可以使用 二種方法以促進該石墨烯片從該生長基材轉移：經載持之轉移方法和自由浮動轉移方法。
該載持的轉移方法一般包含使用載體聚合物諸如聚(甲基丙烯酸甲酯)(PMMA)或其他類似的聚合物。在此方法中，該石墨烯係以PMMA塗覆且後續下方的生長基材被蝕刻掉。該PMMA-石墨烯複合材料後續被轉移至該功能基材且安裝。一旦被安裝，該複合材料以溶劑清洗以移除該PMMA。因為此方法在轉移期間配備物理載體給石墨烯，令石墨烯片之大規模轉移成為可能。然而，該聚合物之使用在該石墨烯片之表面上留下污染物或殘留物。雖然可能移除該PMMA使得該污染物或殘留物少量存在，但即使少量也可能會影響該片之品質。此品質的影響即使多小在某些應用中也是明顯的。例如，該污染物或殘留物可影響可靠鑽孔該石墨烯片的能力。此外，移除該聚合物所需之溶劑可限制可被使用之功能基材的類型。例如，在移除PMMA時，一般使用丙酮。然而，此溶劑之使用可阻礙經徑跡蝕刻之聚碳酸酯作為功能基材的用途。
該自由浮動轉移方法一般需要使該石墨烯在溶液中浮動。在此方法的期間，該石墨烯生長的基材複合材料首先在含蝕刻掉該生長基材之蝕刻劑之蝕刻溶液中浮動，此浮動產生自由浮動之石墨烯片。該蝕刻溶液後續被洗出且改成以水為底質之溶液以令該石墨烯被浮動至所要基材上。因為該自由浮動轉移方法不包含使用二次聚合物材料以塗覆該石墨烯片，該自由浮動轉移方法比該經載持 之轉移方法合宜，因為減低導入污染物或留下殘留物在該石墨烯片上的風險。然而，使用此方法大規模轉移該石墨烯片是困難的，因為由於該轉移方法之未載持本質，撕扯或以其他方式破壞該片之風險是更高的。
根據一些具體例，一種從銅基材轉移石墨烯片至功能基材的方法可包括使用化學蒸氣沉積使該石墨烯片形成在該銅基材上和使用寬束照射藉由多個氙離子照射配置在該銅基材上之該石墨烯片以形成經製備之石墨烯片。該經製備之石墨烯片對在該經製備之石墨烯片轉移至該功能基材期間所引起之形成非故意的缺陷呈現抗性。該方法可另外包括使用蝕刻劑浴以自該經製備之石墨烯片移除該銅基材、使該經製備之石墨烯片在浮動浴中浮動、使該功能基材浸沒在該浮動浴中、及降低該浮動浴之流體水平以使該經製備之石墨烯片下降至該功能基材上。
根據一些具體例，該石墨烯片可包含1cm2或更大之面積。
根據一些具體例，該寬束照射可以是準直的。
根據一些具體例，該多個氙離子係在介於約100V至約1500V之電壓下被施加。
根據一些具體例，該多個氙離子係在介於約250V至約750V之電壓下被施加。
根據一些具體例，該多個氙離子係在約500V之電壓下被施加。
根據一些具體例，該方法可另外包括加熱在該銅基材上形成之石墨烯片至介於約50℃至約100℃的溫度。
根據一些具體例，該方法可另外包含加熱配置在該銅基材上之石墨烯片至約80℃的溫度。
根據一些具體例，該多個氙離子係在約6.24×1011Xe+/cm2/s至約6.24×1014Xe+/cm2/s之通量下被提供。
根據一些具體例，該多個氙離子係在約6.24×1012Xe+/cm2/s至約6.24×1013Xe+/cm2/s之通量下被提供。
根據一些具體例，該多個氙離子係在約3.75×1013Xe+/cm2/s之通量下被提供。
根據一些具體例，該形成在該銅基材上之石墨烯片以該多個氙離子照射一段接觸時間，該照射產生約6.24×1012Xe+/cm2至約2.5×1013Xe+/cm2之總累積通量。
根據一些具體例，該形成在該銅基材上之石墨烯片以該多個氙離子照射一段接觸時間，該照射產生約1.25×1013Xe+/cm2之總累積通量。
根據一些具體例，一種從銅基材轉移石墨烯片至功能基材的方法可包括使用化學蒸氣沉積使該石墨烯片形成在該銅基材上及使用寬束照射藉由多個氖離子照射 形成在該銅基材上之該石墨烯片以形成經製備之石墨烯片。該經製備之石墨烯片對在該經製備之石墨烯片轉移至該功能基材期間所引起之形成非故意的缺陷呈現抗性。該方法可另外包括使用蝕刻劑浴以自該經製備之石墨烯片移除該銅基材、使該經製備之石墨烯片在浮動浴中浮動、使該功能基材浸沒在該浮動浴中、及降低該浮動浴之流體水平以使該經製備之石墨烯片下降至該功能基材上。
根據一些具體例，該方法可包括加熱在該銅基材上形成之石墨烯片至約50℃至約100℃的溫度。
根據一些具體例，該形成在該銅基材上之石墨烯片以該多個氖離子照射一段接觸時間，該照射產生約6.24×1012離子/cm2至約7.5×1013離子/cm2之總累積通量。
根據一些具體例，該形成在該銅基材上之石墨烯片以該多個氖離子照射一段接觸時間，該照射產生達至2×1014離子/cm2之總累積通量。
根據一些具體例，一種從生長基材轉移石墨烯片至功能基材的方法可包括使該石墨烯片形成在該生長基材上且藉由多個離子照射形成在該生長基材上之該石墨烯片以形成經製備之石墨烯片。該經製備之石墨烯片對在該經製備之石墨烯片轉移至該功能基材期間所引起之形成非故意的缺陷呈現抗性。該方法可另外包括使用蝕刻劑浴以自該經製備之石墨烯片移除該生長基材、使該經製備之石墨烯片在浮動浴中浮動、使該功能基材浸沒在該浮動浴 中、及降低該浮動浴之流體水平以使該經製備之石墨烯片下降至該功能基材上。
根據一些具體例，該石墨烯片可包含1cm2或更大之面積。
根據一些具體例，該生長基材可以是銅基材。
根據一些具體例，該生長基材可以是鎳基材。
根據一些具體例，該石墨烯片可以使用化學蒸氣沉積被形成在該銅基材上。
根據一些具體例，該石墨烯片可以使用化學蒸氣沉積被形成在該鎳基材上。
根據一些具體例，該多個離子可以包含惰性氣體離子。
根據一些具體例，該惰性氣體離子可以包含氙離子。
根據一些具體例，該惰性氣體離子可以包含氖離子。
根據一些具體例，該惰性氣體離子可以包含氬離子。
根據一些具體例，該多個離子可以使用寬束照射被施加至形成在該生長基材上之石墨烯片。
根據一些具體例，該寬束照射可以是準直的。
根據一些具體例，該多個離子可在約100V至約1500V之電壓下被施加至形成在該生長基材上之石墨烯片。
根據一些具體例，該多個離子可以約1nA/mm2至約1000nA/mm2的通量被施加。
根據一些具體例，該多個離子可以約10nA/mm2至約100nA/mm2的通量被施加。
根據一些具體例，該多個離子可以約40nA/mm2至約80nA/mm2的通量被施加。
根據一些具體例，該多個離子可以約60nA/mm2的通量被施加。
根據一些具體例，在該生長基材上所形成之石墨烯片可以該多個離子照射一段接觸時間，該照射產生約10nAs/mm2至約120nAs/mm2之總累積通量。
根據一些具體例，在該生長基材上所形成之石墨烯片可以該多個離子照射一段接觸時間，該照射產生約10nAs/mm2至約40nAs/mm2之總累積通量。
根據一些具體例，在該生長基材上所形成之石墨烯片可以該多個離子照射一段接觸時間，該照射產生約20nAs/mm2之總累積通量。
10‧‧‧生長基材
20‧‧‧石墨烯片
30‧‧‧蝕刻劑浴
35‧‧‧浮動浴
40‧‧‧功能基材
50‧‧‧離子
100‧‧‧轉移製備設備
圖1A是在根據本發明之具體例之石墨烯片的形成中使用的生長基材的概略透視圖。
圖1B是形成在圖1A之生長基材上之石墨烯片的概略透視圖。
圖2是製備用於自由浮動轉移之圖1B之石墨烯片的轉移製備設備的概略視圖。
圖3A是使用自由浮動轉移方法從圖2之該經製備之石墨烯片蝕刻該生長基材的步驟的概略透視圖。
圖3B是使用該自由浮動方法轉移圖2之該經製備之石墨烯片至功能基材的轉移步驟的概略透視圖。
圖4顯示在移除該生長基材後使用圖2之轉移製備設備所製備之大規模石墨烯片。
圖5顯示在使用該自由浮動轉移方法轉移至功能基材後之圖4的大規模的石墨烯片。
圖6是使用該自由浮動轉移方法轉移至功能基材的石墨烯片的掃描電子顯微鏡(SEM)的顯微照片。
圖7是圖6之SEM顯微照片的詳細視圖。
一些具體例提供一種處理石墨烯片的系統和方法，該石墨烯片在生長基材被移除且使用該自由浮動轉移方法使該石墨烯片轉移至功能基材之前在生長基材上成長。該處理提供具有甚少至沒有非故意之缺陷的未受污染(例如實質上無殘留物/污染物)的石墨烯片，其能在該自由浮動轉移方法之期間之轉移該片至功能基材時，在降低失敗風險(例如甚少撕扯、龜裂、或形成其他非所欲之缺陷 的風險)下從該生長基材轉移至功能基材。在一些具體例中，該石墨烯片在被配置在該生長基材的同時，透過能量施加至該石墨烯片而被改質，且因此被製備以供轉移。該能量之施加可以是寬束離子源形式，該寬束離子源經配置以利用離子(例如第18族之元素的離子)照射該石墨烯片，使得該石墨烯片在配置於該生長基材的同時被製備以供可靠的大規模轉移。因此，在本文中描述之某些該系統和方法消除輔助該石墨烯片轉移至該功能基材的二次塗覆材料(例如聚合物)之需要，因此消除石墨烯之品質透過藉由二次塗覆材料之使用所導入之污染物而降低的風險。因此，某些該等具體例之轉移製備方法令高品質石墨烯片之可靠轉移能使用該自由浮動轉移方法大規模(亦即1cm2或更大)進行。
圖1A-1B說明根據一些具體例之生長大規模石墨烯或以石墨烯為底質之片在生長基材上的方法。圖1A顯示製備用於石墨烯片之製造的生長基材10的第一步驟。該生長基材10可以是適合石墨烯之製造的任何生長基材。例如，在一些具體例中，該生長基材10是金屬觸媒，諸如銅或鎳。如圖1A中顯示的，該生長基材10是銅基材，其係藉由以溶劑清潔該表面且在高溫下使該基材10退火而製備。
在製備該生長基材10之後，石墨烯係在該生長基材10之上方和底部二表面上生長，該生長可透過化學蒸氣沉積(CVD)藉由使該生長基材10曝於氣態反應物直至形成石墨烯而完成。該CVD程序使石墨烯片皆在該生長基 材10之底部表面和該生長基材10之上方表面上合成。如圖1B中顯示的，在該底部表面上合成之石墨烯片被移除，同時在上方表面上合成之石墨烯片10被利用以供轉移至功能基材。在生長後，該石墨烯片10可具有碳質材料在其表面上，該碳質材料在一些情況中可能是該石墨烯片10在該銅基材上之生長的結果。該碳質材料可以是諸如非結晶碳、一或多種烴類、含氧之碳材料、含氮之碳材料、或其結合之材料。在圖1B顯示之具體例中，該石墨烯片10是在平面方向上具有至少1cm2或更大之橫截面積的大規模的片。
一旦該石墨烯片20沉積在該生長基材10之上方表面上，該石墨烯片20後續可被轉移至基材以供所要之應用。在圖2中顯示的，在該石墨烯片20從該生長基材10移除之前，製備該石墨烯片20以供使用轉移製備設備100來轉移。該轉移製備設備100被配置以將能量給予該石墨烯片20及生長基材10的結構。例如，該轉移製備設備100可被配置已將離子照射給予該石墨烯片20及生長基材10。如圖2中顯示的，該轉移製備設備100可以是經配置以供應多個離子50給該石墨烯片20的離子來源。
在某些具體例中，該轉移製備設備100可被配置以提供寬束離子照射至該石墨烯片20及該生長基材10。該寬束離子來源可以是準直的或實質準直的(例如與垂直差5度)。該多個離子50可包含帶單一電荷或多電荷的離子。在一些具體例中，該多個離子50可以是惰性氣體離子諸如週期表之第18族之元素的離子。在一些具體例中，該 多個離子50可以是有機離子或有機金屬離子。該有機或有機金屬離子可具有芳香族成分。此外，該有機或有機金屬離子之分子質量可在介於75至200或90至200。在一些具體例中，該多個離子50可包含Ne+離子、Ar+離子、托品鎓(tropylium)離子、及/或二茂鐵鎓(ferrocenium)離子。在某些具體例中，該多個離子50包含Xe+離子。
該離子源可以被配置以在介於約100V至約1500V的電壓下供應該多個離子50。在一些具體例中，該多個離子50可在介於約250V至約750V的電壓下被施加。在某些具體例中，該多個離子50(例如Xe+離子)可在約500V的電壓下被施加。
在該轉移製備程序之期間，該石墨烯片20和該生長基材30可被加熱至介於約50℃至約100℃的溫度。在一些具體例中，該石墨烯片20和該生長基材30可被加熱至約80℃之溫度。在其他具體例中，該石墨烯片20和該生長基材30可保持在室溫下。此外，該石墨烯片20和該生長基材30可曝於低於5×10-7Torr之壓力下。在一些具體例中，該石墨烯片20和該生長基材30可曝於1×10-7Torr至5×10-6Torr之壓力下。在一些具體例中，此程序可以被設定以進行數小時或過夜。
該離子源可被配置以在約1nA/mm2(6.24×1011離子/cm2/s)至約1000nA/mm2(6.24×1014離子/cm2/s)之通量下提供該多個離子50。在一些具體例中，該多個離子50係在約10nA/mm2(6.24×1012離子/cm2/s)至約 100nA/mm2(6.24×1013離子/cm2/s)之通量下被提供。在某些具體例中，該多個離子50係在約40nA/mm2(2.5×1013離子/cm2/s)至約80nA/mm2(5.0×1013離子/cm2/s)之通量下被提供。在某些具體例中，該多個離子50係在約60nA/mm2(3.75×1013離子/cm2/s)之通量下被提供。在該多個離子50包含Xe+離子的具體例中，該多個離子50可在約6.24×1011Xe+/cm2/s至約6.24×1014Xe+/cm2/s之通量下被提供。在其他具體例中，該多個離子50包含在約6.24×1012Xe+/cm2/s至約6.24×1013Xe+/cm2/s之通量下提供之Xe+離子。在其他具體例中，該多個離子50包含在約3.75×1013Xe+/cm2/s之通量下提供之Xe+離子。
該石墨烯片20和該生長基材30可曝露於該離子源一段接觸時間，該曝露產生約10nAs/mm2(6.24×1012離子/cm2)至約40nAs/mm2(2.5×1013離子/cm2)之總累積通量。在某些具體例中，該石墨烯片20和該生長基材30係曝露1秒以下，使得該總累積通量為20nAs/mm2(1.25×1013離子/cm2)。在該多個離子包含Xe+離子的具體例中，該石墨烯片20和該生長基材30可曝露一段接觸時間，該曝露產生約10nAs/mm2至約40nAs/mm2(或約6.24×1012Xe+/cm2至約2.5×1013Xe+/cm2)之總累積通量。在該多個離子50包含Xe+離子的某些具體例中，該總曝露時間產生約1.25×1013Xe+/cm2之總累積通量。用於該轉移製備程序之總累積通量的上限可隨著該多個離子50之原子數減少而增加。在一些具體例中，該總累積通量之上限可 以是約120nAs/mm2。在其他具體例中，該總累積通量之上限可以是約500nAs/mm2。在一些具體例中，該總累積通量之上限可以是約1000nAs/mm2。例如，在該多個離子包含Ne+離子的具體例中，該石墨烯片20和該生長基材30可曝露一段接觸時間，該曝露產生約10nAs/mm2(6.24×1012離子/cm2)至約120nAs/mm2(7.5×1013離子/cm2/s)之總累積通量。在一些具體例中，該石墨烯片20和該生長基材30可曝露於多個氖離子一段接觸時間，該曝露產生約10nAs/mm2至約500nAs/mm2之總累積通量。在其他具體例中，該石墨烯片20和該生長基材30可曝露於多個氖離子一段接觸時間，該曝露產生約10nAs/mm2至約1000nAs/mm2之總累積通量。在另外的其他具體例中，該石墨烯片20和該生長基材30可曝露於多個氖離子一段接觸時間，該曝露產生達到2×1014離子/cm2之總累積通量。
在以上處理之後，該石墨烯片20和該生長基材30可在該石墨烯片20轉移至該功能基材之前曝於約1atm之N2作為該程序之最後步驟。該製備程序之結果實際上是一種“堅韌化(toughened)”的石墨烯片20，其可以使用未載持之自由浮動轉移方法被可靠地轉移至功能基材，同時在該自由浮動轉移程序之期間對在該石墨烯片20中形成或造成非故意之缺陷(撕扯、龜裂、皺褶、非故意造成之孔)呈現抗性。該處理因此提供一種堅韌化的石墨烯片20，其能在該功能基材和乾淨的表面上提供高的覆蓋率(例如99%或更高之該功能基材被該石墨烯片覆蓋)以供其 他處理程序(例如鑽孔程序)之有效使用。雖然不限於任何特別之關於製備或堅韌化該用於轉移之石墨烯片20的機轉的理論，該堅韌化可藉由碳質材料之存在以及在該石墨烯片20與該銅生長基材10之介面之間的交互作用來促進。該離子束照射可提供足夠能量給該碳質材料以因在該石墨烯片20中及/或表面上存在之碳原子的濺射使該銅基材10上的該石墨烯片20重整成初始層。
一旦使用該轉移製備設備100製備該石墨烯片20，該石墨烯片20和該生長基材10的複合材料被放置在蝕刻劑浴30中，如圖3A中顯示的。該蝕刻劑浴30令該生長基材10能被蝕刻掉，使得維持乾淨之石墨烯片20。該蝕刻劑浴30可以是能從該石墨烯片20蝕刻掉該生長基材10的任何合適蝕刻劑。例如，對於以銅為底質之生長基材，該蝕刻劑浴30可包括氯化鐵、硝酸鐵、及/或過硫酸銨。在一些具體例中，該石墨烯片20和該生長基材10之複合材料可被放置在可包括相同或不同蝕刻劑之第二蝕刻劑浴30中，以進一步幫助該生長基材10從該石墨烯片20完全蝕刻掉。
如圖3B中顯示的，該蝕刻劑浴30後續逐漸被移除且代之以可充作浮動機轉之浮動浴35以將該石墨烯片20轉移至功能基材40。該浮動浴35可以是以水為底質之溶液諸如水(例如去離子水)或水和溶劑(例如異丙醇)的混合物。例如，在一些具體例中，該蝕刻劑浴30可藉由逐漸導入去離子水被移除，該去離子水然後可另外地以去離子水和異丙醇之混合物形式被導入。當該石墨烯片20在該浮動 浴35中浮動時，該功能基材40可被導入該石墨烯片20之底部表面的下方，如圖3B中顯示的。在一些具體例中，當該石墨烯片20在該溶液中浮動且後續被施加至該功能基材40時，浮動構架(未顯示)在此程序之期間可被配置在該石墨烯片20周圍以提供穩定性給該石墨烯片20。該浮動浴35然後逐漸地被移除，使得該流體水平減低以使該石墨烯片20降至該基材40上。一或多個已經製備以供使用該轉移製備設備100來轉移的另外石墨烯片20可視需要使用該自由浮動轉移方法被堆疊在該功能基材40。
圖4和5顯示藉由轉移製備設備之具體例所製備之供轉移的石墨烯片之影像，該轉移製備設備係經配置以供應使用Xe+離子之準直的寬束離子照射。圖4顯示在藉由化學蝕刻移除該銅生長基材之後所製備之石墨烯片。在圖4中顯示之經製備的石墨烯片是具有約9cm乘14cm的尺寸(或約126cm2之經擴大的平面面積)的大規模的片。在圖4中顯示之黑色圓形標記描繪該石墨烯片之邊界。
圖5顯示在經製備的石墨烯片已轉移至功能基材(在圖5中顯示的具體例中之聚合物薄膜基材)後，與圖4中顯示者類似之該經製備的石墨烯片。與圖4類似的，該經製備之石墨烯片是具有約9cm乘14cm的尺寸的大規模的片。如圖5中顯示的，該石墨烯片及功能基材之複合材料顯示沒有可見到之非故意的缺陷的石墨烯片。雖然因為在該片自由浮動時與該蝕刻劑浴槽之壁碰撞而沿著邊緣可能產生一些缺陷，該經製備之石墨烯片在沒有使用二次聚 合物載持材料下即使在該石墨烯片之自由浮動及降至該功能基材上之後，在該片的主體內不顯出任何可見的缺陷(例如可見的撕扯、龜裂或皺褶)。這指明：使用該轉移製備設備製備該石墨烯片的程序產生一種被韌化而對在該自由浮動轉移程序之期間可能引起之非故意的缺陷呈現抗性的石墨烯片。
圖6和7顯示藉由經配置以使用Xe+離子供應準直寬束離子照射的轉移製備設備的具體例所製備之用於轉移的經製備的石墨烯片的SEM影像。在製備後，使用如上述之自由浮動轉移方法，使該經製備之石墨烯片轉移至功能基材，其呈具有多個孔之經徑跡蝕刻的聚合物基材形式。在該圖顯示的具體例中，該多個孔具有範圍在介於350nm至450nm的標稱孔尺寸。在圖6中顯示之總視野是約0.036mm2(約225μm×160μm)，同時圖7顯示在圖6中顯示之石墨烯片之左上象限的精細區域。
在該聚合物基材中存在之被該經製備之石墨烯片覆蓋的孔在圖6和7中顯示為中等的灰色。在由於轉移程序所製備之石墨烯片中所存在之非故意的缺陷而未受覆蓋的孔被顯示成黑色。如在圖6和7中顯示的，多於99%之該基材的孔被該經製備之石墨烯片覆蓋，此指明在該聚合物基材上高的該經製備之石墨烯片的覆蓋面積。
在特別引用較佳具體例下，一些具體例已詳細地被描述，但在此技藝中的技術人員會了解：在該申請專利範圍之精神和範圍內進行變化和改良。
10‧‧‧生長基材
20‧‧‧石墨烯片
30‧‧‧蝕刻劑浴
35‧‧‧浮動浴
40‧‧‧功能基材

Claims (37)

  1. 一種從銅基材轉移石墨烯片至功能基材之方法，其包含：使用化學蒸氣沉積使該石墨烯片形成在該銅基材上；使用寬束照射藉由多個氙離子照射形成在該銅基材上之該石墨烯片以形成經製備之石墨烯片，其中該經製備之石墨烯片對在該經製備之石墨烯片轉移至該功能基材期間所引起之形成非故意的缺陷呈現抗性；使用蝕刻劑浴以由該經製備之石墨烯片移除該銅基材；使該經製備之石墨烯片在浮動浴中浮動；使該功能基材浸沒在該浮動浴中；及降低該浮動浴之流體水平以使該經製備之石墨烯片下降至該功能基材上。
  2. 如申請專利範圍第1項之方法，其中該石墨烯片包含1cm2或更大之面積。
  3. 如申請專利範圍第1項之方法，其中該寬束照射是準直的。
  4. 如申請專利範圍第1項之方法，其中該多個氙離子係在介於約100V至約1500V範圍內之電壓下被施加。
  5. 如申請專利範圍第1項之方法，其中該多個氙離子係在介於約250V至約750V範圍內之電壓下被施加。
  6. 如申請專利範圍第1項之方法，其中該多個氙離子係在約500V之電壓下被施加。
  7. 如申請專利範圍第1項之方法，其另外包含加熱在該銅基材上形成之石墨烯片至介於約50℃至約100℃的溫度。
  8. 如申請專利範圍第1項之方法，其另外包含加熱配置在該銅基材上之石墨烯片至約80℃的溫度。
  9. 如申請專利範圍第1項之方法，其中該多個氙離子係在約6.24×1011Xe+/cm2/s至約6.24×1014Xe+/cm2/s之通量下被提供。
  10. 如申請專利範圍第1項之方法，其中該多個氙離子係在約6.24×1012Xe+/cm2/s至約6.24×1013Xe+/cm2/s之通量下被提供。
  11. 如申請專利範圍第1項之方法，其中該多個氙離子係在約3.75×1013Xe+/cm2/s之通量下被提供。
  12. 如申請專利範圍第1項之方法，其中形成在該銅基材上之石墨烯片以該多個氙離子照射一段接觸時間，該照射產生約6.24×1012Xe+/cm2至約2.5×1013Xe+/cm2之總累積通量。
  13. 如申請專利範圍第1項之方法，其中形成在該銅基材上之石墨烯片以該多個氙離子照射一段接觸時間，該照射產生約1.25×1013Xe+/cm2之總累積通量。
  14. 一種從銅基材轉移石墨烯片至功能基材之方法，其包含：使用化學蒸氣沉積使該石墨烯片形成在該銅基材上；使用寬束照射藉由多個氖離子照射形成在該銅基材上之該石墨烯片以形成經製備之石墨烯片，其中該經製備之石墨烯片對在該經製備之石墨烯片轉移至該功能基材期間所引起之形成非故意的缺陷呈現抗性；使用蝕刻劑浴以自該經製備之石墨烯片移除該銅基材；使該經製備之石墨烯片在浮動浴中浮動；使該功能基材浸沒在該浮動浴中；及降低該浮動浴之流體水平以使該經製備之石墨烯片下降至該功能基材上。
  15. 如申請專利範圍第14項之方法，其另外包含加熱在該銅基材上形成之石墨烯片至介於約50℃至約100℃的溫度。
  16. 如申請專利範圍第14項之方法，其中形成在該銅基材上之石墨烯片以該多個氖離子照射一段接觸時間，該照射產生約6.24×1012離子/cm2至約7.5×1013離子/cm2之總累積通量。
  17. 如申請專利範圍第14項之方法，其中形成在該銅基材上之石墨烯片以該多個氖離子照射一段接觸時間，該照射產生多達2×1014離子/cm2之總累積通量。
  18. 一種從生長基材轉移石墨烯片至功能基材之方法，其包含：使該石墨烯片形成在該生長基材上；藉由多個離子照射形成在該生長基材上之該石墨烯片以形成經製備之石墨烯片，其中該經製備之石墨烯片對在該經製備之石墨烯片轉移至該功能基材期間所引起之形成非故意的缺陷呈現抗性；使用蝕刻劑浴以自該經製備之石墨烯片移除該生長基材；使該經製備之石墨烯片在浮動浴中浮動；使該功能基材浸沒在該浮動浴中；及 降低該浮動浴之流體水平以使該經製備之石墨烯片下降至該功能基材上。
  19. 如申請專利範圍第18項之方法，其中該石墨烯片包含1cm2或更大之面積。
  20. 如申請專利範圍第18項之方法，其中該生長基材是銅基材。
  21. 如申請專利範圍第18項之方法，其中該生長基材是鎳基材。
  22. 如申請專利範圍第20項之方法，其中該石墨烯片經使用化學蒸氣沉積被形成在該銅基材上。
  23. 如申請專利範圍第21項之方法，其中該石墨烯片經使用化學蒸氣沉積被形成在該鎳基材上。
  24. 如申請專利範圍第18項之方法，其中該多個離子包含惰性氣體離子。
  25. 如申請專利範圍第24項之方法，其中該惰性氣體離子包含氙離子。
  26. 如申請專利範圍第24項之方法，其中該惰性氣體離子包含氖離子。
  27. 如申請專利範圍第24項之方法，其中該惰性氣體離子包含氬離子。
  28. 如申請專利範圍第18項之方法，其中該多個離子經使用寬束照射被施加至形成在該生長基材上之石墨烯片。
  29. 如申請專利範圍第28項之方法，其中該寬束照射是準直的。
  30. 如申請專利範圍第18項之方法，其中該多個離子係在約100V至約1500V之電壓下被施加至形成在該生長基材上之石墨烯片。
  31. 如申請專利範圍第18項之方法，其中該多個離子係以約1nA/mm2至約1000nA/mm2的通量被施加。
  32. 如申請專利範圍第18項之方法，其中該多個離子係以約10nA/mm2至約100nA/mm2的通量被施加。
  33. 如申請專利範圍第18項之方法，其中該多個離子係以約40nA/mm2至約80nA/mm2的通量被施加。
  34. 如申請專利範圍第18項之方法，其中該多個離子係以約60nA/mm2的通量被施加。
  35. 如申請專利範圍第18項之方法，其中在該生長基材上所形成之石墨烯片以該多個離子照射一段接觸時間，該照射產生約10nAs/mm2至約120nAs/mm2之總累積通量。
  36. 如申請專利範圍第18項之方法，其中在該生長基材上所形成之石墨烯片以該多個離子照射一段接觸時間，該照射產生約10nAs/mm2至約40nAs/mm2之總累積通量。
  37. 如申請專利範圍第18項之方法，其中在該生長基材上所形成之石墨烯片以該多個離子照射一段接觸時間，該照射產生約20nAs/mm2之總累積通量。
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SG11201808962RA (en) 2018-11-29
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