TWI487624B - 石墨箔黏合的裝置及其準備方法 - Google Patents

石墨箔黏合的裝置及其準備方法 Download PDF

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Publication number
TWI487624B
TWI487624B TW102115515A TW102115515A TWI487624B TW I487624 B TWI487624 B TW I487624B TW 102115515 A TW102115515 A TW 102115515A TW 102115515 A TW102115515 A TW 102115515A TW I487624 B TWI487624 B TW I487624B
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Taiwan
Prior art keywords
substrate
graphite foil
resin
graphite
composite
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TW102115515A
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English (en)
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TW201343411A (zh
Inventor
Chern Jiin Huey Lin
Chien Ping Ju
Kuo Jung Lee
Hsun Yu Lin
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Univ Nat Cheng Kung
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Publication of TW201343411A publication Critical patent/TW201343411A/zh
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Description

石墨箔黏合的裝置及其準備方法 相關申請案之相互參照
本案請求在2012年4月30日申請的前美國臨時申請案序號第61/640,109號的優先權。
本發明係關於具有金屬、陶瓷、碳質或聚合性基材及黏合於該基材表面的石墨箔的裝置，並且關於用於準備該裝置的方法，其包含將一可撓性石墨箔鋪疊於該基材表面上，其中該可撓性石墨箔包含多數與該基材表面平行的天然石墨薄片。
有人建議以熔融鹽反應器(MSR)作為有希望的第IV代核反應器，其使用熔融氟化物鹽作為燃料。第IV代國際論壇為了先進研究開發所挑選的這六個核反應器設當中，至少二者將使用熔融氟化物鹽作為主要冷卻劑。MSR的優點包括優越的安全性(沒有一直保持熔融核心的“中國症候群(China Syndrome)”)、消除核廢料的問題、滋生新核燃料而沒有核擴散的風險及把豐產且可實質再生的釷作為核燃料使用 得比鈾更有效率許多的能力。再者，MSR具有能以非常高的熱效率於氟化物鹽類的沸點(約1400℃)之溫度限制集下操作的可能性。
在核能產業中使用碳質材料已經有一段長的歷史。石墨及碳-碳(C/C)複合材料係用於各式各樣的高溫核反應器。由於其相對高的機械強度，已經有人把C/C複合材料研發用於包括達於1600℃的短期操作溫度之熔合及分裂應用。
由於C/C複合材料保持幾乎完全的機械強度到高溫(達於1400℃)的能力，使C/C複合材料可能搭配經熔融鹽冷卻的先進高溫反應器、熔融鹽反應器及熱核發電廠作為各式各樣核應用的高溫交換器、輸送管、容器等等的構成材料而引人注目。
石墨一般能抵抗氟化物鹽類的化學藥品攻擊。由於核能等級石墨的較低機械強度，所以很推薦把C/C複合材料用於以熔融氟化物鹽冷卻的反應器，而且由於C/C複合材料保持幾乎完全的機械強度到高溫(達於1400℃)的能力而作為供核應用用的熱交換器、輸送管、泵及容器中的高腐蝕性熔融氟化物鹽之結構圍阻體。
儘管其有優良的高溫機械性質及與熔融氟化物鹽的化學相容性，但是C/C複合材料的固有高孔隙率水平(導致對於該等熔融鹽的高可透性)是對於此材料之一主要挑戰。儘管化學氣相沉積(CVD)或化學氣相滲透(CVI)技術經常用以使該複合材料緻密化，但是卻無法完全解決C/C複合材料的孔隙率問題。再者，許多固有及/或高溫熱處理引發C/C複合 材料中的大裂縫及小裂縫極難以藉由習用方法例如CVD或CVI來密封。
WO 03/001133 A2揭示藉由下列方法準備的以石墨為底質的各向異性散熱件或熱導管，該方法包含形成包含多數含石墨烯層的可撓性石墨片的層疊體；及藉由施壓使該層疊體的石墨烯層定向對準。WO 03/001133 A2也揭示用於準備該可撓性石墨片的方法。
本發明揭示一種包含至少一片石墨箔的方法，其中該片石墨箔的至少一部分包含天然石墨薄片。本發明的裝置很能耐化學反應及/或高腐蝕性環境的滲透及/或透入，舉例來說，包含高溫熔融氟化物鹽的環境，該高溫熔融氟化物鹽包含LiF、NaF及/或KF。本發明也揭示一種用於準備該裝置的方法。本發明裝置的應用不限於用於熱交換器。任何需要下列性質的其他應用，例如高導熱性、高溫及/或高耐腐蝕性、高溫強度及/或模數、表面/次表面細孔密封等等也能得到本發明裝置的優點。本發明裝置也是當作熔合反應器的第一壁材料的可能候選物。該石墨箔的可撓性/柔軟性及氣密性/壓縮性石墨薄片也使本發明裝置成為當作不良環境中的密封材料/裝置例如螺帽、螺釘、螺絲、閥、接頭、連接器、填塞物等等的理想候選物。
根據本發明建構的複合材料包含一分層結構，該分層結構包含黏合於基材表面的石墨箔，其中該石墨箔包含 多數與該基材表面平行的天然石墨薄片的層疊體，其中該石墨箔及該基材表面直接透過擴散黏合作用(diffusion bonding)來黏合，或於其間以固化樹脂、固化柏油脂、碳化樹脂、碳化柏油脂、石墨化樹脂或石墨化柏油脂黏合，其中該石墨箔含有不低於95%，較佳99%，的碳。
較佳地，該基材係金屬或陶瓷基材，而且更佳為金屬基材，而且該石墨箔及該基材表面直接透過擴散黏合作用來黏合。
較佳地，該金屬基材係不銹鋼、鈦、鈦合金、超合金、銅、銅合金或鋁合金。
較佳地，該基材係金屬、陶瓷、碳質或聚合性基材，而且該石墨箔及該基材表面係於其間以固化樹脂、固化柏油脂、碳化樹脂、碳化柏油脂、石墨化樹脂或石墨化柏油脂黏合。
較佳地，該樹脂係熱固性樹脂。
較佳地，該基材係碳質基材，而且更佳地，該碳質基材係以碳纖維強化的碳基質複合基材或石墨塊基材，而且最佳為以碳纖維強化的碳基質複合基材。
較佳地，該基材係呈輸送管或槽的形態而且該表面係該輸送管或槽的內壁。
依據本發明揭示的製造複合材料之方法包含把可撓性石墨箔置於金屬或陶瓷基材，較佳金屬基材，的表面上以形成一分層結構；及藉由於惰性氣氛中或在真空作用之下於200至1200℃，較佳300至1100℃，的溫度下壓縮該分 層結構而擴散黏合該可撓性石墨箔及該基材表面，其中該可撓性石墨箔包含多數與該基材表面平行的天然石墨薄片的層疊體，其中該可撓性石墨箔含有不低於90%，較佳95%，的碳。
依據本發明揭示的另一製造複合材料之方法包含提供基材及可撓性石墨箔，其中該基材、該可撓性石墨或該二者包含沉積於其表面上的樹脂或柏油脂；把可撓性石墨箔置於該基材表面上以形成一分層結構，其中該可撓性石墨箔包含多數與該基材表面平行的天然石墨薄片的層疊體，而且該可撓性石墨箔含有不低於90%，較佳95%，的碳；及於提高的溫度下壓縮該分層結構，使至少一部分樹脂或柏油脂軟化並且於該石墨箔和該基材之間流動。
較佳地，該基材係以樹脂或柏油脂沉積於其表面上，而且該可撓性石墨箔不包含樹脂或柏油脂。
較佳地，該壓縮係於50至300℃，較佳100至200℃，的溫度及1至100 MPa，較佳1至50 MPa，的壓力下進行1至1000分鐘，較佳1至100分鐘，的時期。
較佳地，該基材係碳質基材，而且較佳地，該碳質基材係以碳纖維強化的樹脂基質複合基材、以碳纖維強化的柏油脂基質複合基材、樹脂或柏油脂浸製以碳纖維強化的碳基質複合基材或樹脂或柏油脂浸製石墨塊基材。
較佳地，該基材係樹脂塗佈金屬基材。
較佳地，前述本發明的另一方法另外包含使該壓縮層結構中經至少部分固化的樹脂或柏油脂後固化。更佳 地，前述本發明的另一方法另外包含將該經後固化的樹脂或經後固化的柏油脂碳化，並且任意將該經後固化的樹脂或經後固化的柏油脂石墨化。
較佳地，其中在該可撓性石墨箔置於該基材表面上以前將該可撓性石墨箔或該基材的表面粗糙化。
圖1是本發明實施例1準備的石墨箔-C/C複合材料的截面SEM顯微照片。
圖2是本發明實施例2準備的石墨箔-C/C複合材料：(a)R/R；(b)R/P；(c)P/R；(d)P/P，的截面SEM顯微照片。
圖3是本發明實施例3準備的石墨箔-C/C複合材料的截面SEM顯微照片。
圖4是顯示(a)不含石墨箔的C/C複合材料；(b)工業用高密度石墨；及(c)本發明的石墨箔-C/C複合材料之水接觸角照片。
圖5是(a)本發明經氟化鋰鈉鉀鹽浸泡的石墨箔-C/C(R/R)複合材料，(b)其C分佈情形(C map)及(c)其F分佈情形的截面SEM形態學。
圖6是(a)本發明經氟化鋰鈉鉀鹽浸泡的石墨箔-C/C(R/R)複合材料，其具有如箭頭所強調之鑽過該石墨箔的0.5 mm直徑洞孔，(b)其C分佈情形及(c)其F分佈情形的截面SEM顯微照片。
圖7是本發明的石墨箔-C/C複合材料經過氟化鋰鈉鉀鹽浸泡試驗(a)之前及(b)之後的SEM顯微照片。
圖8是工業用的NBG-18石墨經過氟化鋰鈉鉀鹽浸泡試驗(a)之前及(b)之後的SEM顯微照片。
圖9是本發明的石墨箔-C/C複合材料經過氟化鋰鈉鉀鹽侵蝕試驗(a)之前及(b)之後的SEM顯微照片。
圖10是工業用的NBG-18石墨經過氟化鋰鈉鉀鹽侵蝕試驗(a)之前及(b)之後的SEM顯微照片。
圖11是本發明實施例9準備在不同加工階段之下的石墨箔-石墨複合材料的寬面((a)、(c)、(e))及截面((b)、(d)、(f))形態學。
圖12a是顯示發明性石墨箔-SS 304複合材料的擴散黏合行為的圖表。
圖12b顯示根據本發明於800℃擴散黏合1小時的石墨箔-SS 304複合材料之截面SEM顯微照片。
圖13a是顯示發明性石墨箔-SS 316複合材料的擴散黏合行為的圖表。
圖13b顯示根據本發明於800℃擴散黏合1小時的石墨箔-SS 316複合材料之截面SEM顯微照片。
圖14a是顯示發明性石墨箔-工業級純度Ti複合材料的擴散黏合行為的圖表。
圖14b顯示根據本發明於800℃擴散黏合5小時的石墨箔-工業級純度Ti複合材料之截面SEM顯微照片。
圖15a是顯示發明性石墨箔-Ti6-Al4-V複合材料的擴散 黏合行為的圖表。
圖15b顯示根據本發明於800℃擴散黏合5小時的石墨箔-Ti6-Al4-V複合材料之截面SEM顯微照片。
圖16a是顯示發明性石墨箔-800H超合金複合材料的擴散黏合行為的圖表。
圖16b顯示根據本發明於800℃擴散黏合1小時的石墨箔-800H超合金複合材料之截面SEM顯微照片。
圖17a是顯示發明性石墨箔-Hastelloy超合金複合材料的擴散黏合行為的圖表。
圖17b顯示根據本發明於800℃擴散黏合1小時的石墨箔-Hastelloy超合金複合材料之截面SEM顯微照片。
圖18a是顯示發明性石墨箔-銅複合材料的擴散黏合行為的圖表。
圖18b顯示根據本發明於800℃擴散黏合1小時的石墨箔-銅複合材料之截面SEM顯微照片。
圖19是顯示發明性石墨箔-黃銅複合材料的擴散黏合行為的圖表。
圖20a是顯示發明性石墨箔-磷青銅複合材料的擴散黏合行為的圖表。
圖20b顯示根據本發明於800℃擴散黏合1小時的石墨箔-磷青銅複合材料之截面SEM顯微照片。
用於本發明的措辭“石墨箔”是代表任何石墨層 的通稱，其包含天然石墨(較佳為天然石墨薄片)或任何從天然石墨加工得到的石墨片，其中使該等石墨薄片或石墨片以及裡面的基面高度對準而與該石墨箔的表面平行。其也可被稱作“石墨片”、“可撓性石墨片”、“石墨紙”、“Grafoil®”(市售商品)等等，並且可由此領域中眾所周知的不同程序及方法準備，舉例來說用於準備該“石墨箔”的適合方法包含把一定量的夾層型或層離型(intercalated and exfoliated)天然石墨壓縮或壓延成具有所欲厚度及密度的石墨箔片。
本發明的發明包括但不限於下列觀點：
(1)一種包含至少一片石墨箔之複合材料裝置，其中該石墨箔片的至少一部分包含天然石墨；而且前述石墨箔係黏合於基材上。
(2)如觀點(1)的裝置，其中前述天然石墨係呈天然石墨薄片的形態。
(3)如觀點(1)的裝置，其中前述石墨箔片係從天然石墨薄片加工得到的石墨片。
(4)如觀點(1)的裝置，其中該基材係由金屬材料、陶瓷材料、碳質材料或聚合性材料製造。
(5)如觀點(1)的裝置，其中前述石墨箔黏合於基材上係藉由擴散黏合作用、化學氣相滲透或聚合性黏膠進行。
(6)如觀點(4)的裝置，其中該金屬材料係不銹鋼、鈦或鈦合金、銅或銅合金、超合金或鋁合金。
(7)如觀點(4)的裝置，其中該陶瓷材料係SiC、Si3 N4 、ZrO2 或Al2 O3 。
(8)如觀點(4)的裝置，其中該碳質材料係石墨。
(9)如觀點(4)的裝置，其中該碳質材料係以碳纖維強化的碳基質複合材料(C/C複合材料)。
(10)如觀點(4)的裝置，其中該聚合性材料係熱固性聚合物。
(11)如觀點(6)至(10)中任一觀點的裝置係呈輸送管或槽的形態，其中前述石墨箔係黏合於前述輸送管或槽的內壁。
(12)如觀點(9)的裝置，其係藉由包含下列步驟的方法準備：
(i)準備碳纖維或碳纖維預製件、碳基質(黏結劑)前驅物及任意某些想要的基質添加物；其中若有必要，該碳纖維或碳纖維預製件可預先與該碳基質前驅物合併形成預浸材；
(ii)準備包含天然石墨(較佳為天然石墨薄片)或任何從天然石墨加工得到的石墨片之石墨箔；
(iii)於一模子中將該纖維或纖維預製件、基質前驅物(或其預合併的預浸材)及該石墨箔堆疊在一起，形成具有所欲造形及鋪疊圖案的堆疊複合材料；
(iv)於該模子中，較佳地在約1至100 MPa的壓力下而且較佳地於約50至300℃的溫度下，熱壓該堆疊複合材料以形成石墨箔-C/C複合材料生坯；
(v)任意使該經熱壓的石墨箔-C/C複合材料生坯於較佳地約70至400℃的溫度下後固化；
(vi)於非氧化性氣氛中將該經熱壓的或經後固化的石墨箔-C/C複合材料物件較佳地碳化至約500至1500℃的溫度；
(vii)於非氧化性環境中任意地將該碳化石墨箔-C/C複合材料物件較佳地石墨化至約1500至3000℃的溫度；
(viii)任意藉由至少一另外的基質滲透/碳化緻密化循環使該碳化或石墨化C/C/石墨箔複合材料物件進一步緻密化；
(ix)任意藉由陶瓷，較佳為SiC，層來保護不含石墨箔的表面。
(x)任意在多重緻密化循環的途中進行前述步驟(iii)的石墨箔結合。
(xi)在最終緻密化循環之後任意進行前述步驟(iii)的石墨箔結合。
(12a)如觀點(9)的裝置(用於市售可得的C/C基材)，其係藉由包含下列步驟的方法準備：(i)準備C/C複合材料物件；任意將前述物件表面粗糙化及/或塗佈可固化樹脂；(ii)準備包含天然石墨(較佳為天然石墨薄片)或任何從天然石墨加工得到的石墨片之石墨箔；任意將前述C/C複合材料物件表面粗糙化及/或塗佈可固化樹脂；(iii)較佳於一模子中，將該石墨箔堆疊於前述C/C複合材料物件的至少一表面上，形成一堆疊複合材料；(iv)較佳於該模子中，較佳地在約1至100 MPa的壓力下 而且較佳地於約50至300℃的溫度下，熱壓該堆疊複合材料以形成複合材料生坯；(v)任意使該經熱壓的複合材料生坯於較佳地約70至400℃的溫度下後固化；(vi)於非氧化性氣氛中將該經熱壓的或經後固化的複合材料物件較佳地碳化至約500至1500℃的溫度；(vii)於非氧化性環境中任意地將該碳化複合材料物件較佳地石墨化至約1500至3000℃的溫度；(xii)任意藉由陶瓷，較佳為SiC，層來保護不含石墨箔的表面。
(13)如觀點(8)的裝置，其係藉由包含下列步驟的方法準備：(i)準備石墨基材；任意將前述石墨基材表面粗糙化及/或塗佈可固化樹脂；(ii)準備包含天然石墨(較佳為天然石墨薄片)或任何從天然石墨加工得到的石墨片之石墨箔；任意將前述石墨箔表面粗糙化及/或塗佈可固化樹脂；(iii)於一模子中將前述石墨基材及該石墨箔堆疊在一起，形成一堆疊複合材料；(iv)於該模子中，較佳地在約1至100 MPa的壓力下而且較佳地於約50至300℃的溫度下，熱壓該堆疊複合材料以形成石墨箔-石墨基材複合材料生坯；(v)任意使該經熱壓的複合材料生坯於較佳地約70至400℃的溫度下後固化； (vi)於非氧化性氣氛中將該經熱壓的或經後固化的複合材料物件較佳地碳化至約500至1500℃的溫度；(vii)於非氧化性環境中任意地將該碳化複合材料物件較佳地石墨化至約1500至3000℃的溫度；(viii)任意藉由陶瓷，較佳為SiC，層來保護不含石墨箔的表面。
(14)如觀點(6)或(7)的裝置，其係藉由包含下列步驟的方法準備：(i)準備金屬或陶瓷基材；任意將前述基材表面粗糙化及/或塗佈可固化樹脂；(ii)準備包含天然石墨(較佳為天然石墨薄片)或任何從天然石墨加工得到的石墨片之石墨箔；任意將前述石墨箔表面粗糙化及/或塗佈可固化樹脂；(iii)讓前述基材和前述石墨箔能緊密接觸以形成石墨箔/基材層疊體；(iv)加熱前述層疊體(較佳於真空或惰性氣氛中；較佳於高於200℃的溫度下；更佳約300至1200℃)以讓前述基材及前述石墨箔能擴散黏合。
(15)如觀點(11)的裝置，其中該裝置係呈輸送管的形態，而且該裝置係藉由包含下列步驟的方法準備：
(i)準備輸送管；任意地使前述輸送管的內表面粗糙化及/或塗佈可固化樹脂；
(ii)準備包含天然石墨(較佳為天然石墨薄片)或任何從天然石墨加工得到的石墨片之石墨箔；任意將前述石墨箔表面粗 糙化及/或塗佈可固化樹脂；
(iii)準備直徑稍微小於該輸送管內徑而且徑向的CTE(熱膨脹係數)不小於該輸送管的CTE之嵌入物(較佳由銅或銅合金構成)；
(iv)把前述石墨箔及前述嵌入物插入該輸送管內部以致於該石墨箔夾於輸送管和嵌入物之間；而且讓該石墨箔、該嵌入物及該輸送管的內壁緊密接觸；
(v)加熱該填充嵌入物/石墨箔的輸送管(較佳為在真空或惰性氣氛中)以讓輸送管內壁及石墨箔能擴散黏合。
(vi)從輸送管移除嵌入物。
本發明的裝置很能耐化學反應及/或高腐蝕性環境的滲透及/或透入，舉例來說，包含高溫熔融氟化物鹽的環境，該高溫熔融氟化物鹽包含LiF、NaF及/或KF。本發明的裝置可呈任何形態。若作為熱交換器，該基材較佳呈輸送管或細長管的形態，其中前述石墨箔係黏合於前述輸送管或細長管的內壁。
本發明的觀點(12)中揭示的方法之其他特徵包括：在步驟(i)中，該碳纖維，任意為長/連續纖維或短/人造短纖，較佳為PAN(聚丙烯腈)-為底質的纖維或柏油脂為底質的纖維。該預製件或預浸材中的短碳纖維可個別分佈(不規則地或按照預定圖案)或呈短切束(chopped bundle)形態。該預製件或預浸材中的長碳纖維可經單向、多向編織或針織。該基質前驅物較佳為樹脂或柏油脂。該基質添加物可 為石墨粉、中間相柏油脂粉末、碳黑、Si或陶瓷粉末例如SiC、奈米碳管(CNT)、石墨烯等等。
在步驟(ii)中，該包含天然石墨(較佳為天然石墨薄片)或任何從天然石墨加工得到的石墨片之石墨箔可藉由任何此領域中眾所周知的技術製造，舉例來說，利用或不用黏結劑壓縮或輾壓層離型天然石墨的各向異性層。為了提高“z軸”(與該箔的寬面垂直)的熱傳導度，該石墨箔可包含添加物例如石墨粉、中間相柏油脂粉末、碳黑、奈米碳管(CNT)、石墨烯等等。這些添加物可與天然石墨薄片混合，緊接著利用或不用黏結劑將該混合物壓縮或輾壓成薄可撓性石墨片。另一提高該“z軸”熱傳導度的方式是該等石墨薄片的至少一部分(及因此在裡面的基面)與該石墨箔表面成一角度對準。這可藉由與該等石墨薄片成一角度切削/研磨正常石墨片達成，以致於該等石墨薄片將不會與該石墨箔表面完全平行。另一提高該“z軸”熱傳導度的方式是準備一非平坦石墨箔表面。此非平坦石墨箔表面可藉由將該石墨箔/C/C複合材料熱壓至模子中而準備，其中該頂部及/或底部內表面不平坦。
在步驟(iii)中，該石墨箔(任意為單層狀或多層狀)可結合於該堆疊複合材料的任何地方，但是較佳為結合於外表面(黏合於該C/C複合材料表面)，所以該石墨箔將會直接接觸該等高度腐蝕性熔融鹽(擔任“第一壁”材料的角色)，由此密封/保護底下的C/C結構。
儘管有諸多不同技術，舉例來說，加硼硬化(needling)或化學氣相滲透(CVI)/化學氣相沉積(CVD)，可用以 將該石墨箔黏合於該C/C結構，但是所有這些技術都有高風險的滲漏及/或微龜裂現象，尤其是在高溫加工的加熱及/或冷卻(舉例來說，碳化或石墨化)的期間。
令人驚訝的是有人發現，在熱壓的期間，該基質材料(舉例來說，酚樹脂或柏油脂)變軟並且會流入介於該石墨箔與該C/C層疊體之間的薄空間。扮作像黏膠的角色，填充該界面空間的基質材料以附著方式將該二部分黏合在一起。又更令人驚訝的是有人發現，經過該高溫石墨化處理之後，該界面層維持的非常緻密而且該黏合維持得非常堅牢而沒留意到該界面區中有任何脫層或微龜裂。由於其缺乏液體流動階段，所以CVI碳不能作為主要/初始基質(將乾燥纖維預製件填滿/緻密化)。然而，等到已經形成牢固的黏合之後CVI可用於碳化多孔性基質的進一步緻密化。
該石墨箔可於初期加工階段裝設，舉例來說，如上所述，在熱壓之前。該石墨箔也可於最終階段裝設，舉例來說，等到最終緻密化循環之後。於最終階段裝設該石墨箔之一優點是，如果這樣做，由於有更多自由表面(開啟通道)可以利用使該等緻密化循環更有效率。當該石墨箔於初期階段裝設時，儘管該石墨箔與C/C基材之間的黏合可能更牢固，該石墨箔的存在總會有點妨礙到碳化引發的氣體之釋放。或者，該石墨箔可於指定的數個緻密化循環的途中裝設。該石墨箔可裝設於基本上市售可得或不可得的任何類型的複合材料上。
為了提高該複合材料的熱傳導度，高傳導性材 料，例如奈米碳管(CNT)、石墨烯等等可任意加於該基質中。
在步驟(iv)中，用於熱壓的模子(在步驟(iii)中也用於堆疊)可為任何造形及幾何形狀，取決於用途。作為熱交換器，較佳為管狀。該熱壓可於空氣、惰性氣氛或在真空之下，舉例來說，使用高壓釜進行。
在步驟(v)中，該後固化可於沒有壓力，或在降低樣品(尤其是由二維編織的預製件)膨脹的壓力之下的爐中進行。
在步驟(vi)中，該非氧化性環境可為碳的氧化反應可以忽略的任何環境。供碳氧化用的二常見來源是氧及水蒸氣。氮、惰性氣體或真空均可作為該碳化環境。
碳化的加熱速率可在廣大範圍中，舉例來說，約1℃/min至約1000℃/min。
或者，為了降低孔隙率，低速(例如約1℃/min至約10℃/min)碳化處理可在該最終階段期間應用，而高速碳化處理係於初期循環期間運用。
或者，於較低加熱速率下的預碳化處理可在該碳化處理以前運用。
在步驟(vii)中，該石墨化可於真空或惰性氣氛，舉例來說，氬或氦，中進行。由於其與碳質材料高溫反應性，氮氣，儘管常被當碳化氣氛使用，可能不適合用於碳的石墨化，尤其是於高溫下進行的石墨化(舉例來說，>2000℃)。於較低加熱溫度下的預石墨化處理可任意在該石墨化處理以前運用。
在步驟(viii)中，可依據所欲的密度及性質進行額外的基質滲透、碳化及任意石墨化的循環。CVI可任意用於這些額外的緻密化循環，只要該石墨箔及該C/C結構之間已經使用本發明的方法確立順利黏合即可。
在步驟(ix)中，為達氧化防護的目的，該表面(較佳地，但不限於，與直接接觸熔融鹽的表面於相反側的非熔融鹽接觸面)另外藉由SiC層來保護。該SiC層可藉由化學氣相沉積(CVD)或與液態或固態含矽材料的表面反應準備。
本發明的觀點(13)中揭示的方法之其他特徵包括：在步驟(i)中，該石墨可為任何習用石墨。關於作為核反應器中的熱交換器之用途，較佳為核能級石墨。
步驟(ii)中的特徵與觀點(12)中揭示的方法之步驟(ii)中列舉的特徵相同。
在步驟(iv)至(vii)中，把該石墨箔(任意為單層或多層)黏合於該石墨基材表面，所以該石墨箔將會直接接觸到該等高度腐蝕性熔融鹽(擔任“第一壁”材料的角色)，由此密封/保護底下的石墨結構。
儘管有諸多不同技術，舉例來說，CVI/CVD，可用以將該石墨箔黏合於該石墨基材，但是還是推薦前述用於將石墨箔黏合於C/C基材的方法(熱壓、後固化、碳化等等)。
在步驟(viii)中，為達氧化防護的目的，該表面(較佳地，但不限於，與直接接觸熔融鹽的表面於相反側的非熔融鹽接觸面)另外藉由SiC層來保護。該SiC層可藉由化學氣 相沉積(CVD)或與液態或固態含矽材料的表面反應準備。
本發明的觀點(14)中揭示的方法之其他特徵包括：在步驟(i)中，該金屬材料可為任何金屬工程材料。該金屬材料較佳為鈦合金、超合金或鋁合金。該陶瓷材料可為任何陶瓷工程材料。該陶瓷材料較佳為SiC、Si3 N4 、ZrO2 或Al2 O3 。
步驟(ii)中的特徵與以上步驟(ii)中的特徵相同。
在步驟(iii)中，前述緊密接觸可藉由任何習用方法達成，例如拍打、黏牢、釘固、膠黏等等。
在步驟(iv)中，前述加熱可藉由任何習用方法，例如電阻加熱、導電加熱等等，而且在任何習用環境中，較佳在真空或惰性氣氛中進行。
本發明的觀點(15)中揭示的方法之其他特徵包括：在步驟(i)中，前述輸送管可由金屬材料、陶瓷材料、碳質材料或聚合性材料構成。該輸送管的截面可依照任何形狀，較佳為圓形或矩形。
步驟(ii)中的特徵與以上步驟(ii)中的特徵相同。
在步驟(iii)中，前述嵌入物可由任何習用材料構成，較佳由不會與石墨於高溫下嚴重化學反應的材料構成，舉例來說，銅或銅合金。該等嵌入物可為實心或中空。該嵌入物的徑向較佳具有比該輸送管更大的熱膨脹係數(CTE)，以致於，當受熱時，該嵌入物會推動該石墨箔抵住該輸送管的 內壁，如步驟(v)所述，有助於該擴散黏合方法。
在步驟(iv)中，為了使該石墨箔、該嵌入物及該輸送管的內壁能緊密接觸，該嵌入物的直徑應該稍微小於該輸送管的內徑。該石墨箔可以先包裹於該嵌入物表面上，接著把該石墨箔包裹的嵌入物滑入該輸送管中，或該石墨箔可先施於該輸送管的內壁上，接著把該嵌入物滑入該“石墨箔輸送管”中。
在步驟(v)中，前述加熱可藉由任何習用方法，例如電阻加熱、導電加熱等等，而且在任何習用環境中，較佳在真空或惰性氣氛中進行。
在步驟(vi)中，為了易於從該輸送管移除該嵌入物，該嵌入物理應不得與石墨於高溫下發生嚴重的化學反應。
實施例1. 發明性石墨箔-C/C複合材料的製造
碳纖維預製件：PAN為底質的二維織布(日本，Toray公司的Torayca T300-2x2斜紋布)
基質前驅物：可溶性酚醛樹脂(Resole)型酚樹脂(台灣，長春塑料有限公司，PF-650)
鋪疊並且針軋(punch-needled)五片PAN為底質的二維織布(日本，Toray公司的Torayca T300-2x2斜紋布)。在針軋的期間，291支針打在該織布1500次。針軋的面積是直徑11 cm的圓。該針織毛氈藉由真空浸製法以可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)於25至30℃的溫度下浸製，緊接著於70℃的烘箱中加熱6小時以從該樹 脂並且從PAN/酚系預浸材除去溶劑。把該預浸材切成長度11 cm的方塊。把一張石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA)形塑成長度11 cm的方塊，配合20 psi的壓力噴砂1秒而粗糙化，並且鋪疊(堆疊)於該預浸材頂部上，緊接著於160℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔-C/C複合材料生坯。
使該經熱壓的複合材料生坯於230℃的空氣循環烘箱中後固化歷經8小時。使該經後固化的石墨箔-C/C複合材料於10℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化(初次碳化)1小時。使該碳化複合材料在帶有氬氣氛的爐中於1900℃下石墨化1小時。經過該石墨化處理之後，藉由可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)於25至30℃的溫度下之真空浸製使該複合材料緻密化，緊接著於180℃下固化2小時並且於1100℃下配合1000℃/min的加熱速率於帶有氮氣氛的爐中碳化3分鐘。這樣的浸製/固化/碳化循環重複進行4次以獲得所欲的密度。經過該緻密化程序之後，對試片施以於1100℃下配合10℃/min的加熱速率於帶有氮氣氛的爐中的預石墨化處理60分鐘及於1900℃下於帶有氬氣氛的爐中的最終石墨化處理60分鐘。(注意：對於許多案例C/C複合材料的製造並不需要此最終石墨化處理)。
圖1是顯示由此準備的石墨箔-C/C複合材料的截面之典型掃描式電子顯微鏡(SEM)。值得注意的是該石墨箔-C/C界面非常堅牢而且該石墨箔本身的結構非常緻密。
實施例2. 發明性石墨箔-C/C複合材料的密度、孔隙率及三點彎折性質
碳纖維預製件：針軋毛氈(日本，Toray公司的Torayca T300-2x2斜紋布)
預浸時的基質前驅物：可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)或石油柏油脂(美國，Ashland公司的A240)
緻密化/浸製時的基質前驅物：可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)或石油柏油脂(美國，Ashland公司的A240)
依循實施例1指定的通用順序搭配如表1列舉的不同材料及加工細節製造一系列石墨箔-C/C複合材料。表2中列舉不同樣品名稱。表3中列舉由此準備的複合材料的密度、孔隙率及三點彎折性質。
使用根據ASTM C830標準的水飽和法測定密度及孔隙率值。
根據ASTM D790使用SHIMADZU AGS-500D廣用測試器測定三點彎折強度及韌度值。於0.5 mm/min的十字頭速度下進行彎折。樣品的支撐件跨距-厚度比為16。圖2中顯示各種不同彎折-破裂石墨箔-C/C複合材料樣品的截面掃描式電子顯微照片。令人吃驚的是注意到，無論所用的基質的類型(樹脂或柏油脂)為何，在全部四個不同樣品中的石墨箔-C/C界面保持非常堅牢而且該石墨箔本身的結構非常緻密 (甚至毗鄰高應力的破裂帶)，即使所有複合材料均經歷過2次於1900℃的高溫處理、4次快速冷卻及最終彎折到破裂。
實施例3. 發明性石墨箔-C/C複合材料搭配低加熱速率碳化的密度、孔隙率及三點彎折性質
碳纖維預製件：PAN為底質的二維織布(日本，Toray公司的Torayca T300-2x2斜紋布)
基質前驅物：可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)及石油柏油脂(美國，Ashland公司的A240)
鋪疊並且針軋五片PAN為底質的二維織布(日本，Toray公司的Torayca T300-2x2斜紋布)。在針軋的期間， 171支針打在該織布500次。針軋的面積是長度5 cm的方塊。該針織毛氈藉由真空浸製法以可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)於25至30℃的溫度下或石油柏油脂(美國，Ashland公司的A240)於250至300℃的溫度下浸製。
該樹脂浸製的織布於70℃的烘箱中烘烤6小時以從該樹脂並且從PAN/樹脂為底質的預浸材除去溶劑。把該PAN/樹脂為底質的預浸材切成長度5 cm的方塊。把一張石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA)形塑成長度5 cm的方塊，配合20 psi的壓力噴砂1秒而粗糙化，並且鋪疊(堆疊)於該預浸材頂部上，緊接著於160℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔-C/C複合材料生坯。使該經熱壓的複合材料生坯於230℃的空氣循環烘箱中後固化歷經8小時。使該經後固化的石墨箔-C/C複合材料於1℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化(初次碳化)1小時。使該碳化複合材料在帶有氬氣氛的爐中於1900℃下石墨化1小時。
該柏油脂浸製的織布於50℃的烘箱中烘烤6小時以從該柏油脂並且從PAN/柏油脂為底質的預浸材除去溶劑。把該PAN/柏油脂為底質的預浸材切成長度5 cm的方塊。把一張石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA)形塑成長度5 cm的方塊，配合20 psi的壓力噴砂1秒而粗糙化，並且鋪疊(堆疊)於該預浸材頂部上，緊接著於120℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔 -C/C複合材料生坯。
使該經熱壓的複合材料生坯於120℃的空氣循環烘箱中後固化歷經8小時。使該經後固化的石墨箔-C/C複合材料於1℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化(初次碳化)1小時。使該碳化複合材料在帶有氬氣氛的爐中於1900℃下石墨化1小時。
經過石墨化處理之後，藉由可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)於25至30℃的溫度下之真空浸製使該PAN/樹脂為底質的及PAN/柏油脂為底質的複合材料緻密化，緊接著於180℃下固化2小時並且於1100℃下配合3℃/min的加熱速率於帶有氮氣氛的爐中碳化1小時。這樣的浸製/固化/碳化循環重複進行4次以獲得所欲的密度。經過該緻密化程序之後，對試片施以於1900℃下於帶有氬氣氛的爐中的最終石墨化處理60分鐘。
該PAN/樹脂為底質的預浸材及PAN/柏油脂為底質的預浸材得到的石墨箔-C/C複合材料樣品分別取名為"R/R-R3"及"P/R-R3"。關於密度、孔隙率及三點彎折性質的試驗方法與實施例2所述的相同。表4顯示PAN/樹脂為底質的預浸材得到的石墨箔-C/C複合材料具有比PAN/柏油脂為底質的預浸材得到的石墨箔-C/C複合材料更低的孔隙率、更高的撓曲強度及更低的撓曲韌度值。
實施例4. 搭配不同石墨箔裝設時機製造發明性石墨箔-C/C複合材料
本實施例顯示發明性石墨箔-C/C複合材料的石墨箔裝設時機。於3個不同製造步驟時裝設一張石墨箔。一者於熱壓時，另一者於第三浸製/烘烤/碳化循環時，而且最後一者於最終石墨化(第二次石墨化)時(表5)。
按照下列方式製造G(O)PR及G(3D)PR石墨箔-C/C複合材料：
G(O)PR
鋪疊並且針軋五片PAN為底質的二維織布(日本，Mitsubishi Rayon公司的TR3523M)。在針軋的期間，171支針打在該織布500次。針軋的面積是長度5 cm的方塊。該針織毛氈藉由真空浸製法以石油柏油脂(美國，Ashland公司的A240)於250至300℃的溫度下浸製。該柏油脂浸製的織布於50℃的烘箱中烘烤6小時以從該柏油脂並且從PAN/柏 油脂為底質的預浸材除去溶劑。把該PAN/柏油脂為底質的預浸材切成長度5 cm的方塊，緊接著於120℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔-C/C複合材料生坯。
在該熱壓以前，把一張石墨箔裝設於C/C預浸材上。把那一張石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA)形塑成長度5 cm的方塊，配合20 psi的壓力噴砂1秒而粗糙化，並且鋪疊(堆疊)於該預浸材頂部上。
使該經熱壓的複合材料生坯於120℃的空氣 循環烘箱中後固化歷經8小時。使該經後固化的石墨箔-C/C複合材料於10℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化(初次碳化)1小時。使該碳化複合材料在帶有氬氣氛的爐中於1900℃下石墨化1小時。經過該石墨化處理之後，藉由可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)於25至30℃的溫度下之真空浸製使該PAN/柏油脂為底質的複合材料緻密化，緊接著於180℃下固化2小時並且於1100℃下配合1000℃/min的加熱速率於帶有氮氣氛的爐中碳化3分鐘。這樣的浸製/固化/碳化循環重複進行4次以獲得所欲的密度。
G(3D)PR
經過第三次浸製/固化/碳化循環之後，把一張石墨箔裝設於經過第三個循環的緻密化C/C複合材料上。該樹脂浸製的C/C於70℃的烘箱中烘烤6小時以從該樹脂除去 溶劑。把那一張石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA)形塑成長度5 cm的方塊，配合20 psi的壓力噴砂1秒而粗糙化，並且鋪疊(堆疊)於該樹脂浸製的C/C複合材料頂部上，緊接著於160℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔-C/C複合材料。使該經熱壓的複合材料生坯於230℃的空氣循環烘箱中後固化歷經8小時。使該經後固化的石墨箔-C/C複合材料於10℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化(初次碳化)1小時。等到石墨箔裝設之後，重複進行第四次浸製/固化/碳化循環。把獲得的產物名為G(3D)PR。
經過該緻密化程序之後，對試片施以10℃/min的加熱速率在氮氣氛中於1100℃下的爐中的預石墨化處理60分鐘及在帶有氬氣氛的爐中於1900℃下的最終石墨化60分鐘。
按照下列方式製造G(2G)PR-R3石墨箔-C/C複合材料：
鋪疊並且針軋五片PAN為底質的二維織布(日本，Mitsubishi Rayon公司的TR3523M)。在針軋的期間，171支針打在該織布500次。針軋的面積是長度5 cm的方塊。該針織毛氈藉由真空浸製法以石油柏油脂(美國，Ashland公司的A240)於250至300℃的溫度下浸製。該柏油脂浸製的織布於50℃的烘箱中烘烤6小時以從該柏油脂並且從PAN/柏油脂為底質的預浸材除去溶劑。把該PAN/柏油脂為底質的預浸材切成長度5 cm的方塊，緊接著於120℃的不銹鋼模中在 5 MPa的壓力之下熱壓30分鐘而形成石墨箔-C/C複合材料生坯。使該經熱壓的複合材料生坯於120℃的空氣循環烘箱中後固化歷經8小時。使該經後固化的石墨箔-C/C複合材料於1℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化(初次碳化)1小時。使該碳化複合材料在帶有氬氣氛的爐中於1900℃下石墨化1小時。經過該石墨化處理之後，藉由可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)於25至30℃的溫度下之真空浸製使該PAN/柏油脂為底質的複合材料緻密化，緊接著於180℃下固化2小時並且於1100℃下配合3℃/min的加熱速率於帶有氮氣氛的爐中碳化1小時。這樣的浸製/固化/碳化循環重複進行4次以獲得所欲的密度。經過該緻密化程序之後，對試片施以在帶有氬氣氛的爐中於1900℃下的最終石墨化處理(第二次石墨化)60分鐘。
經過第二次石墨化處理之後，把一張石墨箔裝設於經第二次石墨化的C/C複合材料上。該經第二次石墨化的C/C複合材料藉由真空浸製法以可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)於25至30℃的溫度下浸製。該經樹脂浸製的C/C於70℃的烘箱中烘烤6小時以從該樹脂除去溶劑。把那一張石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA可撓性石墨箔)形塑成長度5 cm的方塊，配合20 psi的壓力噴砂1秒而粗糙化，並且鋪疊(堆疊)於該該經樹脂浸製的C/C複合材料頂部上，緊接著於160℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔-C/C複合材料。使該石墨箔-C/C複合材料於230℃的空氣循 環烘箱中後固化歷經8小時。使該經後固化的石墨箔-C/C複合材料於10℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化1小時。
關於截面的SEM檢查，把樣品切割並且安裝於環氧樹脂中，緊接著使用SiC砂紙來拋光。
該截面的掃描式電子顯微照片(圖3)顯示該石墨箔-C/C界面堅牢而且該石墨箔本身於所有樣品中均為緻密的。
實施例5. 水接觸角測量
測量並且比較三不同碳質材料，包括缺乏石墨箔的C/C複合材料、工業用的高密度石墨(日本，Tokai Carbon有限公司的G348)(密度為1.78)及根據實施例1指定的方法準備的發明性石墨箔-C/C複合材料，的水接觸角。結果顯示於表4中。除了沒用石墨箔製造以外，該C/C複合材料樣品係藉由與用於準備發明性石墨箔-C/C複合材料的相同方法準備。
能清楚見到的是，此三材料當中，本發明的 石墨箔-C/C複合材料具有最大的水接觸角，昱示最小的水可透性。此結果能藉由水接觸到的發明性石墨箔-C/C複合材料中的石墨箔之緻密結構及高度對準基面(與該複合材料表面平行)來解釋。
實施例6. 發明性石墨箔-C/C複合材料在氟化鋰鈉鉀鹽(Flinak)中的腐蝕及氣密行為
研究發明性石墨箔-C/C複合材料在“氟化鋰鈉鉀鹽”熔融氟化物鹽類(LiF、NaF及KF鹽的混合物)中的腐蝕及氣密行為。此發明性石墨箔-C/C複合材料係依循實施例2指定的相同程序製造並且名為R/R。此實施例使用的氟化鋰鈉鉀鹽係藉由乾燥混合按照重量比29.3：11.7：59.0的適當量的LiF(氟化鋰98.5%，Alfa Aesar，USA)、NaF(氟化鈉99%，Alfa Aesar，USA)及KF(氟化鉀98.5%，Alfa Aesar，USA)鹽類，緊接著於氬氣氛中在石墨坩堝中加熱至500℃歷經3小時而準備。為了易於解釋浸泡試驗數據，除了一表面(寬面)暴露於熔融的氟化鋰鈉鉀鹽以外，該石墨箔-C/C複合材料樣品係覆以石墨箔(德國，SGL集團的SIGRAFLEX® C)。作比較用，從另一石墨箔-C/C複合材料樣品的表面，通過該石墨箔帶鑽出一0.5 mm直徑的洞孔以便使在此洞孔內下面的C/C結構在浸泡的期間暴露於該熔融鹽。接著指這兩個樣品(有及沒有洞孔)浸入在氬氣氛中加熱至800℃的溫度的氟化鋰鈉鉀鹽熔融鹽中歷經1小時。
圖5中顯示R/R型複合材料樣品的截面掃描 式電子顯微照片及C和F的EDS元素分佈情形(elemental mapping)。值得注意的是，在圖5(a)中，等到暴露於高溫、高度腐蝕性環境之後該石墨箔及下面的C/C結構二者實質上原封不動。該石墨箔-C/C界面，同樣地，保持得非常牢固。圖5(b)及圖5(c)分別顯示同一區域的C和F的EDS“點圖”。
圖6中顯示R/R型複合材料樣品的截面掃描式電子顯微照片及C和F的EDS元素分佈情形。在圖6(a)中清楚可見氟化物鹽透入通過箭頭所指的洞孔嚴重攻擊C/C結構。結果清楚指出固有多孔性C/C結構本身易受熔融的氟化鋰鈉鉀鹽攻擊。然而，即使是一層石墨箔的保護，也能戲劇性地改善其耐腐蝕性及氣密性能。
實施例7. 發明性複合材料及核能級石墨的氟化鋰鈉鉀鹽浸泡試驗
研究發明性石墨箔-C/C複合材料及核能級石墨(德國，SGL集團的NBG-18)在氟化鋰鈉鉀鹽熔融氟化物鹽(LiF、NaF及KF鹽的混合物)中的腐蝕行為。此發明性石墨箔-C/C複合材料係依循實施例3指定的相同程序製造並且名為R/R-R3。此實施例使用的氟化鋰鈉鉀鹽係藉由乾燥混合按照重量比29.3：11.7：59.0的適當量的LiF(氟化鋰98.5%，Alfa Aesar，USA)、NaF(氟化鈉99%，Alfa Aesar，USA)及KF(氟化鉀98.5%，Alfa Aesar，USA)鹽類，緊接著於氬氣氛中在石墨坩堝中加熱至500℃歷經3小時而準備。把所有樣品浸入在氬氣氛中加熱至800℃的氟化鋰鈉鉀鹽熔融鹽中歷經90小 時。經過浸泡試驗之後，該樣品藉由浸入300℃的Al(NO3 )3 (氮化鋁98+%，Alfa Aesar，USA)的1 M水溶液中以移除該樣品中的氟化鋰鈉鉀鹽而獲得清潔。
圖7清楚證實該發明性石墨箔-C/C複合材料於800℃的氟化鋰鈉鉀鹽中的優良耐腐蝕性。另一方面，如圖8所示，未受保護的NBG-18核能級石墨容易受到該高度腐蝕性熔融鹽的攻擊。
實施例8，發明性複合材料及核能級石墨的氟化鋰鈉鉀鹽侵蝕-腐蝕試驗
侵蝕-腐蝕試驗係藉由相同種類的樣品在與實施例7所述的相同氟化鋰鈉鉀鹽熔融鹽中進行。研究發明性石墨箔-C/C複合材料(在實施例3名為R/R-R3)及核能級石墨(德國，SGL集團的NBG-18)在該氟化鋰鈉鉀鹽熔融氟化物鹽中的侵蝕-腐蝕行為。該侵蝕-腐蝕試驗係利用自製的侵蝕測試系統進行，其中把待侵蝕的樣品表面設計成與夾持該樣品的輪軸呈45度角。等到該熔融鹽於氬氣氛中被加熱至750℃歷經1小時之後，使樣品沉入該熔融鹽。配合150 rpm的轉速於750℃下進行侵蝕試驗歷經24小時。經過侵蝕-腐蝕試驗之後，該樣品藉由浸入300℃的Al(NO3 )3 (氮化鋁98+%，Alfa Aesar，USA)的1 M水溶液中以移除該樣品中的氟化鋰鈉鉀鹽而獲得清潔。
圖9清楚證實該發明性石墨箔-C/C複合材料於800℃的氟化鋰鈉鉀鹽中的優良耐腐蝕性。另一方面，如 圖10所示，未受保護的NBG-18核能級石墨容易受到該高度腐蝕性熔融鹽的攻擊。
實施例9. 發明性石墨箔-石墨複合材料的製造
一張高密度石墨板(日本，Tokai Carbon有限公司的G348)係真空浸製並且塗佈一層可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)，緊接著於80℃的烘箱中烘烤6小時以從該樹脂除去溶劑。把該烘烤過的經樹脂塗佈的石墨板夾於兩張經噴砂(表面粗糙化)的石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA)之間，緊接著於160℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔-石墨複合材料。使該經熱壓的複合材料於230℃的空氣循環烘箱中後固化歷經8小時，緊接著於10℃/min的加熱速率下在氮氣氛中於1100℃下的爐中碳化處理1小時並且利用氬氣氛於1900℃下石墨化處理1小時。
圖11清楚顯示，即使是經過該高溫石墨化處理之後，該石墨箔牢固地黏附於該石墨基材。
實施例10. 藉由擴散黏合作用製造發明性石墨箔-金屬複合材料
將石墨箔擴散黏合於一系列普遍使用的工業用金屬，包括不銹鋼(台灣，燁聯鋼鐵股份有限公司的SS304、及台灣，燁聯鋼鐵股份有限公司的SS316)、工業級純度鈦(中鋼，工業級純度Ti(c.p.Ti))，2級)、鈦合金(中鋼，Ti-6Al-4V)、 超合金(台灣，中鋼股份有限公司的Alloy 800(H)及美國，Haynes國際有限公司的Hastelloy® X)、銅(台灣，第一銅科技有限公司的C1100)及銅合金(台灣，第一銅科技有限公司的黃銅C2680及台灣，名佳利金屬工業有限公司的青銅C5191)。把一張石墨箔(美國，Graftech國際有限公司的GRAFOIL® GTA)夾於兩張金屬之間。為了增進黏合作用，藉由SiC砂紙將該金屬表面粗糙化。藉由二螺絲以機械方式固定此堆疊的夾層，二螺絲各自接近該夾層的一角。擴散黏合處理係於被加熱至300至1100℃的溫度之充滿氬的爐中進行。藉由研磨切斷輪把該經擴散黏合的石墨箔-金屬複合材料樣品切開。檢查該等複合材料樣品的截面以評估該石墨箔-金屬基材黏合行為。圖12至20中的結果指出，在一定的熱處理(擴散黏合)條件之下，所有研究的基材金屬均能有黏附力地黏合於該石墨箔以順利形成該等發明性石墨箔-金屬複合材料。
實施例11. 藉由熱壓製造發明性石墨箔-金屬複合材料
把金屬板噴砂，清潔，並且浸於可溶性酚醛樹脂型酚樹脂(台灣，長春塑料有限公司，PF-650)歷經10分鐘。該經樹脂塗佈的金屬於80℃的烘箱中烘烤6小時以從該樹脂除去溶劑。一張石墨箔鋪疊於該經樹脂塗佈的金屬上，緊接著於160℃的不銹鋼模中在5 MPa的壓力之下熱壓30分鐘而形成石墨箔-金屬複合材料。使該經熱壓的複合材料於230℃的空氣循環烘箱中後固化歷經8小時。藉由研磨切斷輪把該經熱壓黏合的石墨箔-金屬複合材料樣品切開。檢查該等 複合材料樣品的截面以評估該石墨箔-金屬基材黏合行為。結果指出所有研究的基材金屬均能有黏附力地熱壓黏合於該石墨箔以順利形成該等發明性石墨箔-金屬複合材料。該等經後固化的石墨箔-金屬複合材料樣品均可任意進一步碳化以供用於高溫應用。
從以上的描述，熟悉此技藝者能輕易確定本發明的基本特徵，並且能在不悖離其精神和範疇的情況之下完成本發明的各種不同變化及修飾使其適於各種不同用法及條件。因此，其他具體實施例也在申請專利範圍所及的範圍以內。

Claims (20)

  1. 一種包含分層結構之複合材料，該分層結構包含黏合於基材表面的石墨箔，其中該石墨箔包含多數與該基材表面平行的天然石墨薄片的層疊體，其中該石墨箔及該基材表面間以碳化樹脂、碳化柏油脂、石墨化樹脂或石墨化柏油脂黏合，其中該石墨箔含有不低於95%的碳。
  2. 如申請專利範圍第1項之複合材料，其中該基材係金屬或陶瓷基材。
  3. 如申請專利範圍第1項之複合材料，其中該基材係金屬基材，且該金屬基材係不銹鋼、鈦、鈦合金、超合金、銅、銅合金或鋁合金。
  4. 如申請專利範圍第1項之複合材料，其中該基材係碳質或聚合性基材。
  5. 如申請專利範圍第4項之複合材料，其中該基材係碳質基材。
  6. 如申請專利範圍第5項之複合材料，其中該碳質基材係碳纖維強化的碳基質複合基材或石墨塊基材。
  7. 如申請專利範圍第6項之複合材料，其中該碳質基材係該 碳纖維強化的碳基質複合基材。
  8. 如申請專利範圍第1項之複合材料，其中該基材係呈輸送管或槽的形態而且該表面係該輸送管或槽的內壁。
  9. 一種製造複合材料之方法，其包含提供基材及可撓性石墨箔，其中該基材、該可撓性石墨或該二者包含沉積於其表面上的樹脂或柏油脂；把可撓性石墨箔置於該基材表面上以形成一分層結構，其中該可撓性石墨箔包含多數與該基材表面平行的天然石墨薄片的層疊體，而且該可撓性石墨箔含有不低於90%的碳；於提高的溫度下壓縮該分層結構，使至少一部分樹脂或柏油脂軟化並且於該石墨箔和該基材之間流動；及將該被壓縮的分層結構中的樹脂或柏油脂固化及碳化。
  10. 如申請專利範圍第9項之方法，其中該基材係以樹脂或柏油脂沉積於其表面上，而且該可撓性石墨箔不包含樹脂或柏油脂。
  11. 如申請專利範圍第9項之方法，其中該壓縮係於50至300℃的溫度及1至100MPa的壓力下進行1至1000分鐘的時期。
  12. 如申請專利範圍第9項之方法，其中該樹脂係熱固性樹 脂，而且該基材係金屬或陶瓷基材。
  13. 如申請專利範圍第9項之方法，其中該樹脂係熱固性樹脂，而且該基材係金屬基材，及該金屬基材係不銹鋼、鈦、鈦合金、超合金、銅、銅合金或鋁合金。
  14. 如申請專利範圍第9項之方法，其中該樹脂係熱固性樹脂，而且該基材係碳質或聚合性基材。
  15. 如申請專利範圍第10項之方法，其中該基材係碳質基材，而且該碳質基材係碳纖維強化的樹脂基質複合基材、碳纖維強化的柏油脂基質複合基材、樹脂或柏油脂浸製之碳纖維強化的碳基質複合基材、或樹脂或柏油脂浸製之石墨塊基材。
  16. 如申請專利範圍第10項之方法，其中該基材係樹脂塗佈金屬基材，且該金屬基材係不銹鋼、鈦、鈦合金、超合金、銅、銅合金或鋁合金。
  17. 如申請專利範圍第9項之方法，其另外包含於該碳化之前，將該被壓縮的分層結構中被固化的樹脂或柏油脂後固化。
  18. 如申請專利範圍第9或17項之方法，其另外包含於該碳化 之後，將該被碳化的樹脂或柏油脂石墨化。
  19. 如申請專利範圍第9項之方法，其中在該可撓性石墨箔被置於該基材表面上以前將該可撓性石墨箔或該基材的表面粗糙化。
  20. 如申請專利範圍第9項之方法，其中該基材係呈輸送管或槽的形態而且該表面係該輸送管或槽的內壁。
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