TWI252913B - Probe device for atomic force microscopy and method for making same - Google Patents
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12529131252913
五、發明說明(1) 【發明所屬之技術領域 本發明係涉及一種原早七θ Μί·Ρτ^ 、刀热員微鏡(AtomicForceV. INSTRUCTION DESCRIPTION OF THE INVENTION (1) Technical Field The present invention relates to an original early seven θ Μί·Ρτ^, a knife-heater micro-mirror (AtomicForce)
Micr〇sc〇py,以下簡稱afm) 传、、牛芬 絲m * 、’十衣置及其製造方法,特只,| 加/步及一種採用奈米碳管作、 付別 及其製造方法。 次之原子力顯微鏡探針裝置 【先前技術】 近年來’隨著光盤、磁纟 化、高集成化,以夺米以下、半導祖等器件之高密度Micr〇sc〇py, hereinafter referred to as afm), 牛芬丝m*, 'ten clothes and its manufacturing method, special only, | plus/step and one using carbon nanotubes, farewell and its manufacturing method . The second atomic force microscope probe device [Prior Art] In recent years, with the high-density of devices such as the following, semi-conducting ancestors, etc.
之應用範圍日益擴展。1工2測定樣本表面形態之AFM 間力盥部雜沾彳六q 乍原理係利用其探針與樣本之 J刀興距r離的依賴關係來獲楫 的A F Μ女、# L 于物貝表面結構和性質。並型The scope of application is expanding. 1 work 2 to determine the surface morphology of the sample AFM inter-force 盥 杂 彳 彳 q q q q q q 乍 乍 乍 乍 乍 乍 乍 乍 乍 AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF AF Surface structure and properties. Conformity
WAFM有三種成像模式:接觸 貝/、I 針係AFM.之核心部件,價格昂責非接觸鸟式及輕敲式。而探 為探I!:奈米:管所具備之良好彈性及又尖貝端特性,以其作 α私針針尖之AFM早有報道。 告之筮r 戴宏杰等於2 0 0 2年2月12日公 ° <弟6, 346, 1 89號美國鼻利"& 管处播”士 J利用催化劑島製成之奈米碳 之;;中揭露一種糊用探針懸臂上形成奈米碳管針尖 ::。該方法步驟如下:提供一可用於afm之懸臂;於 劑if之自由端(Free End)沈積一催化劑顆粒;使該催化 顆;於高溫下接觸含碳氣氛以長出奈米碳管。 米/?,該方法直接酬之懸臂尖端生長用作針尖之奈 精i L所得之奈米碳管取向性差,勢必影響整個afm之 有鐘於此,提供一雜呈支仏, ^WAFM has three imaging modes: the core part of the contact shell/, I-pin AFM. The price is blameless for non-contact birds and tapping. And explore for I!: Nano: tube has good elasticity and tipping characteristics, with its A private needle tip AFM has been reported. Announced that 戴r Dai Hongjie is equal to February 12, 2002, and the younger brother, 6, 346, 1 89, American nose, "& A method for forming a carbon nanotube tip on a cantilever of a paste probe is as follows: The method is as follows: providing a cantilever for afm; depositing a catalyst particle at the free end of the agent if (Free End); Catalytic granules; contact with a carbon-containing atmosphere at a high temperature to grow a carbon nanotube. M/?, the direct weight of the cantilever tip is used as a tip of the nano-carbon nanotubes, which is poorly oriented, and is bound to affect the whole There is a clock in afm, which provides a miscellaneous support, ^
接私壯 種/、阿取向性奈米碳管針尖之AFM 咏針裝置及其製造方法實為必要。It is necessary to use the AFM needle device and the manufacturing method of the A-oriented carbon nanotube tip.
上述L IGA製程包括步驟:於該平面形成具預定圖案之 光阻材料層;蝕刻該平面以使其形成與光阻材料層相應之 預定圖案;去除光阻材料層。 上述採用化學氣相沈積法於該孔洞生長出與該平面基The above L IGA process includes the steps of: forming a photoresist layer having a predetermined pattern on the plane; etching the plane to form a predetermined pattern corresponding to the photoresist layer; and removing the photoresist layer. The above-mentioned chemical vapor deposition method is used to grow the hole and the plane base.
12529131252913
五、發明說明(3) 本垂直,奈米碳管之步驟包括步驟: 於該平面沈積催化劑; 奈米= 於預定溫度與催化劑接觸使得 人呂由孔洞中基本垂直於該平面長出。 米碳ί=支二縣Τ採用LI!A製程處理需設置奈 結槿,涵_ 41 '·心# 使其末端頂部形成奈米孔洞 :於該縣臂末m ΐ: y模板效應"採用化學氣相沈積 管取向性好,從提板製得之奈米碳 精密性/ 確保卫如同使用该種探針之AFM儀器之 【實施方式】 , ::將結合附圖對本發明作進一步之詳細說明。 5月參閱第一圖,本發明所提供 括:-探針座50 · -固定于二木針裝置5,其包 末知54,設置於該懸臂末端54、用作針尖之夺: 其中,懸臂末端54之頂部56形成有_平二厌吕60。 於該平面57。 且暴本垂直 =本實施例中,孔洞58之孔徑優選為⑼〜丨 臂5 2可由氮化矽製成。 不未。懸 請參閱第二圖,本發明所提供之上述AFM 製造方法7,其包括步驟: 、’衣置5之 (2a)提供可用於AFM之懸臂52,,其具一需設置針+V. INSTRUCTIONS (3) The vertical, carbon nanotube step comprises the steps of: depositing a catalyst on the plane; nanometer = contacting the catalyst at a predetermined temperature such that the person grows substantially perpendicular to the plane from the hole.米碳 ί=支二县Τ Use LI!A process to set up Naijie 槿, 涵 _ 41 '·心# Make the end of the end form a nano hole: at the end of the county m ΐ: y template effect " The chemical vapor deposition tube has good orientation, and the nanocarbon precision obtained from the plate is ensured as the AFM instrument using the probe, and the following will be further described in detail with reference to the accompanying drawings. Description. Referring to the first figure in May, the present invention provides that: - the probe holder 50 is fixed to the two-wood needle device 5, and the end of the cannula 54 is disposed at the end of the cantilever 54 and used as a needle tip: wherein the cantilever The top 56 of the end 54 is formed with a flat plead 60. In this plane 57. And the vertical is vertical. In the present embodiment, the hole diameter of the hole 58 is preferably (9) ~ 臂 The arm 5 2 can be made of tantalum nitride. Not yet. The above-mentioned AFM manufacturing method 7 provided by the present invention includes the steps of:
第7頁 1252913___ 五、發明說明(4) 末端5 4 ’,該末端5 4 ’具,尖形頂部5 6,; (2b )可通過切割打磨等方式於該末端之頂部5 6,形成 一平面57’ ,; (2c)採用LIGA製程於該平面5了,形成一孔洞58,; (2 d )採用化學氣相沈積法於該孔洞5 8,生長出與該平 面57’基本垂直以用作針尖之奈米碳管60。 請參閱第三圖,所述之LIGA製程包括步驟如下: (3a)於平面57,塗敷一光阻材料層80(如聚曱基丙烯酸 曱醋、聚氣乙烯或聚碳酸酯等),再將一設有預定圖案之 光罩(圖气示)置於光阻材料層80上並於χ光中曝霖一 $日士 康性溶液為顯影劑採用濕式腐。; 丨且材枓層顯現預定圖案; , u (3b)採用反應性離子蝕刻法蝕 與光阻材料層80相應之預定圖案;】千面57以使其形成 (由劑如丙酮等去除光阻材料層8。。 田此於千面57形成孔洞58,。 ^ 另’採用L 1 GA法對物铲谁4十抖她从 芩考第6,245,849號、第479二j機械加工之具體製程可 國專利之相關内容。,472, 459號及第6, 455, 233號美 請參閱第四圖,利# 用作針尖之太丰π & e用化子虱相沈積法於孔洞58,生長 I大之奈未奴官60可採用步驟: (4a)於平面57,沈浐拙儿今, 或塗敷等方法將催化劑用電子束蒸鍵、藏射 形成4〜10奈米厚之催化孔:58’之平面57’,使其 J潯膜82,催化劑係選自鐵、鈷、Page 7 1252913___ V. Description of the invention (4) End 5 4 ', the end 5 4 ' has a pointed top 5 6; (2b ) can form a plane at the top 5 6 of the end by cutting and polishing 57', (2c) using the LIGA process in the plane 5 to form a hole 58; (2d) by chemical vapor deposition, the hole 508 is grown substantially perpendicular to the plane 57' for use as Needle tip carbon nanotube 60. Referring to the third figure, the LIGA process includes the following steps: (3a) applying a photoresist layer 80 (such as polyacrylic acid vinegar, polyethylene or polycarbonate) to the surface 57, and then A photomask (illustrated) having a predetermined pattern is placed on the photoresist material layer 80 and exposed to sunlight. The Nisker's solution is a wet rot for the developer. And the material layer exhibits a predetermined pattern; u (3b) is etched by reactive ion etching to a predetermined pattern corresponding to the photoresist layer 80;] a thousand faces 57 are formed to form (removal of the photoresist by an agent such as acetone) Material layer 8. Tian is in the formation of a hole 58 in the thousand face 57. ^ Another 'using L 1 GA method for the object shovel who is 4 tweeting her from the reference to the sixth, 245, 849, the fourth process of the mechanical processing of the 479 The relevant content of the patent., 472, 459 and 6, 455, 233, please refer to the fourth figure, Li # used as the tip of the Taifeng π & e using the 虱 phase deposition method in the hole 58, growth I The procedure can be as follows: (4a) in the plane 57, sinking, or coating, etc., the catalyst is evaporated by electron beam, and the catalyst is formed to form a catalytic hole of 4 to 10 nm thick: 58' Plane 57', such that J 浔 film 82, the catalyst is selected from iron, cobalt,
第8頁 五、發明說明(5) 錄及其氧化物的一種或多種物質。 (4b)提供一碳源氣,並使其於預定溫度與催化 使得奈米碳管由孔洞58’中基本垂直於平面57 1妾:蜀 度3士00L500T:,空氣氣氛下,對催化劑薄膜82進行^皿 J τ退火處理,使其收縮為分離之奈米級顆粒(圖一 並將帶有催化劑顆粒之懸臂52,同時放進反應爐(不), 不);通入保護氣體(未標示)將空氣完全趕盡,同 爐、加熱至冗。,00。0 ;然後通入保護氣體與碳源氣(未 t ^),保護氣體可為.氬、氮或氦等,碳源氣可為乙^未 fin 70、乙許等;約15秒〜40分鐘後,高度一定的夺t俨其 ⑼於孔洞58,長出。 不木石反官 當然催化劑薄膜82亦可僅分布於孔洞U,中 不米碳管6 〇可以A 一太丰 μ 斤付之 限。 為不未妷e管束,不應以本實施例為 採用化學氣相沈積法於懸臂 體步驟及反應條件還可參考上 46 1 ;之具 之相關内容。、』^哼上这弟6’ 346’ 189唬吳國專利Page 8 V. INSTRUCTIONS (5) Record one or more substances of their oxides. (4b) providing a carbon source gas and catalyzing it at a predetermined temperature and catalyzing such that the carbon nanotubes are substantially perpendicular to the plane 57 1 from the hole 58': a temperature of 3 00 L500T: under the air atmosphere, the catalyst film 82 Annealing is carried out to shrink into nano-sized particles (Fig. 1 and the cantilever 52 with catalyst particles are placed in the reactor (not), no); protective gas is introduced (not labeled) ) completely exhaust the air, the same furnace, heating to redundancy. , 00. 0; then pass the shielding gas and carbon source gas (not t ^), the shielding gas may be argon, nitrogen or helium, etc., the carbon source gas may be 乙^fin 70, 乙许, etc.; about 15 seconds After ~40 minutes, the height is certain to take it (9) in the hole 58 and grow out. Of course, the catalyst film 82 can also be distributed only in the hole U, and the carbon nanotubes in the middle can be limited to A. In order to use the chemical vapor deposition method for the cantilever step and the reaction conditions, reference may be made to the above-mentioned contents. , 』^哼上弟6’ 346’ 189唬Wu Guo patent
製程處理::ΓΓ所屬技術人員應明白’本發明提供之L: 體牛1¾ h Ζ ^端以及化學氣相沈積法生長奈来碳管^ 說明本發明,不應以具體實施例所 有兩個用;二;;用不同的固定位置日夺,探針懸她 -步驟Γ將;之末端。該製造方法7可進-步包 卩將所传之探針懸臂52’固定於AFM之探針座。 电明採用L IG A製程處理需設置奈米碳管針尖之A]Process treatment: ΓΓ The skilled person should understand that the invention provides L: body cattle 13⁄4 h Ζ ^ end and chemical vapor deposition method to grow carbon nanotubes ^ Description of the invention, should not be used in all embodiments ; two;; with different fixed positions, the probe hangs her - step Γ will; the end. The manufacturing method 7 can further secure the transmitted probe cantilever 52' to the probe holder of the AFM. The use of L IG A process for the installation of the carbon nanotube tip A]
1252913 五、發明說明(6) 探針懸臂,使其末端頂 洞結構之π模板效應π採 長奈米碳管。由於LIGA 度易控,使得以其為模 確保並提高使用該種探 綜上所述,本發明 出專利申請。惟,以上 舉凡熟悉本案技藝之人 效修飾或變化,皆應包 部形成奈米孔洞結構,再利用該孔 用化學氣相沈積法於該懸臂末端生 製程處理所得之孔洞直徑均勻且深 板製得之奈米碳管取向性好,從而 針之AFM儀器之精密性。 確已符合發明專利要件,爰依法提 所述者僅為本發明之較佳實施例, 士,於援依本案發明精神所作之等 含於以下之申請專利範圍内。1252913 V. INSTRUCTIONS (6) The probe cantilever has a π-template effect of its end-of-the-hole structure and a long-nano carbon nanotube. Since the LIGA degree is easy to control, it is exemplified to ensure and improve the use of the above-described invention, and the present invention is a patent application. However, all the above-mentioned human modifications or changes in the skill of the present invention should form a nanopore structure in the package, and then use the hole to form a hole with uniform diameter and deep plate by chemical vapor deposition at the end of the cantilever process. The carbon nanotubes have good orientation and thus the precision of the AFM instrument. It is true that the invention patents have been met, and the above is only a preferred embodiment of the present invention, and it is within the scope of the following patent application, which is based on the spirit of the invention.
苐]0頁 1252913 圖式簡單說明 第一圖係本發明之AFM探針裝置之示意圖; 第二圖係本發明之製造上述AF Μ探針裝置之方法之流 程示意圖; 第三圖係本發明提供之L I G Α製程於平面5 7 ’形成孔洞 5 8 ’之流程示意圖; 第四圖係本發明提供之化學氣相沈積法於孔洞5 8 ’生 長奈米碳管之流程示意圖。 【元件符號說明】 探針裝置 5 製造方法 7 探針座 50 懸臂 52, 52 末端 54, 54’ 頂部 56, 56 平面/ 5 7, 5 7’ 孔洞 1 58, 58 奈米碳管 60 光阻材料層 80 催化劑薄膜 82BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view showing the first embodiment of the AFM probe device of the present invention; the second drawing is a schematic flow chart of the method for manufacturing the above AF Μ probe device of the present invention; The schematic diagram of the LIG process for forming the hole 5 8 ' in the plane 5 7 '; the fourth picture is the flow chart of the chemical vapor deposition method provided by the present invention for the growth of the carbon nanotubes in the hole 5 8 '. [Explanation of component symbols] Probe device 5 Manufacturing method 7 Probe holder 50 Cantilever 52, 52 End 54, 54' Top 56, 56 Plane / 5 7, 5 7' Hole 1 58, 58 Carbon tube 60 Resistive material Layer 80 Catalyst Film 82
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