TWI353391B - - Google Patents

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TWI353391B
TWI353391B TW96137299A TW96137299A TWI353391B TW I353391 B TWI353391 B TW I353391B TW 96137299 A TW96137299 A TW 96137299A TW 96137299 A TW96137299 A TW 96137299A TW I353391 B TWI353391 B TW I353391B
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Taiwan
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workpiece
filament
diamond film
stage
temperature
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TW96137299A
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Chinese (zh)
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TW200916600A (en
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Atomic Energy Council
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Description

1353391 < » 九、發明說明: 【發明所屬之技術領域】 本發明係有關於一種熱燈絲鑽石膜沉積裝置及其 方法,尤指一種利用熱燈絲高溫裂解氫氣及曱烷成自' 由基,並加入特殊前處理及電漿輔助以提升鑽石膜磨 潤性及附著力以增加其實用性能之熱燈絲鑽石膜沉積 裝置及其方法。 ' 【先前技術】 目前在工業上利用熱燈絲化學氣相法(H〇t1353391 < » IX DESCRIPTION OF THE INVENTION: Technical Field of the Invention The present invention relates to a hot filament diamond film deposition apparatus and method thereof, and more particularly to a method for pyrolyzing hydrogen and decane into a self-curing group by using a hot filament. A special filament filament diamond deposition apparatus and method for adding special pretreatment and plasma assist to enhance the wettability and adhesion of the diamond film to increase its practical performance. [Prior Art] Currently used in the industry by hot filament chemical vapor phase method (H〇t

Filament Chemical Vapor Deposition,HFCVD)於各刀 具工件上沉積鑽石膜係很常用之一種方式。該法係將 熱燈絲作為裂解氣體之熱能來源、,當氣氣(%)、甲院 (CH4)或其他如乙炔(阳2)及乙酸(阳⑺⑽) 等碳氫氣源在真空幾十托爾(τ〇ΓΓ)環境下,碰撞到 =⑽0〇C〜250〇〇c之高溫燈絲時’其氣體將裂解成各 種風原子(H)及甲烧基(CH3)等活性基原子或分子 Uad1C朴此類活性粒子其化學活性強,當甲烧與氫 軋(ch4/h2)氣體湲度在〇 5%〜6 %時大量之活性 ^ =在鑽石膜表面形成碳.咖),藉__ ㈣免㈣碳·碳魏之(c=c) 鑽f臈之品質。另外,碳⑹原子於沉積過 由於Μ子靠近碳氫鍵表面時,會將表面 風鍵打斷而形成氫氣,使表面碳原子形成空懸鍵 !353391 t 二成glln!B°'d)狀態’此時當該甲烧基靠近時’就 兮:件二Γ成軌域之鑽石結構’如此循環反應,在 m持_°c〜_c時,就會形成鑽石膜。 力強w歸於鑽石結構之碳.碳鍵(c%c)其化學鍵 田“ ·石臈與非碳類工件結合成長時其介面 之結合強度不僅不^ '、 杏且在加上鑽石硬度高及熱膨脹 ,田〃,屬工件在高溫成長後再降回常溫時,Filament Chemical Vapor Deposition (HFCVD) is a common method of depositing diamond film on each tool workpiece. The system uses hot filament as a source of thermal energy for cracking gas, when gas (%), Jiayuan (CH4) or other carbon and hydrogen sources such as acetylene (yang 2) and acetic acid (yang (7) (10)) in the vacuum dozens of tol (τ〇ΓΓ) environment, when colliding with the high temperature filament of =(10)0〇C~250〇〇c, the gas will be cleaved into various atomic atoms or molecules such as various wind atoms (H) and methyl group (CH3). The active particles of this kind have strong chemical activity. When the temperature of the gas burning and hydrogen rolling (ch4/h2) is 〇5%~6 %, a large amount of activity ^=carbon on the surface of the diamond film. __ (4) Free (four) carbon · carbon Wei (c = c) drill quality. In addition, carbon (6) atoms are deposited. Because the scorpion is close to the surface of the carbon-hydrogen bond, the surface wind bond is broken to form hydrogen gas, so that the surface carbon atoms form an empty dangling bond! 353391 t two into glln! B°'d) state 'At this time, when the nail base is close, 'the 钻石: the diamond structure of the two turns into the orbital domain' is thus cyclically reacted, and when m is held at _°c~_c, a diamond film is formed. The strength of w is attributed to the carbon of the diamond structure. The carbon bond (c%c) is chemically bonded to the field. · The combination strength of the interface between the stone and the non-carbon workpiece is not only ^', the apricot and the hardness of the diamond are high. Thermal expansion, Tian Hao, is a workpiece that falls back to normal temperature after it has grown at a high temperature.

=:=膜質有很高之應力存在,尤其在沉積 间厚度鑽石膜時更為明顯,因此易於導致該鑽石膜從 此工件上剝裂。 按目前有關熱燈絲沉積鑽石膜之專利,以美國專 利第5’833’753號之矩陣式燈絲及張力之設計,並雖可 沉積大面積’但具有高度之工件則無法均勾沉積;又 專利第G254312號及美國專利第6,細,652號其 皆有利用-柵極、—燈絲及—基台等三處相互之間加 偏壓,使該基台上方形成電漿,以作為輔助工件成核 及成長鑽石敵用H與前述相同,對於立體有 高度之工件皆係難以沉積,再者,上述各專利亦不以 金屬刀具為設言十縣。雖然其雙偏壓製程對石夕晶片及 石英等工件具辅助成核效果,唯其鑽石膜與工件之附 著力仍無法應付刀具之高速運轉,因此容易發生膜剝 落或斷刀等問題。 ' 目前常用之尺寸,如直徑3毫米(mm)〜〇1毫 米微銑刀或Μ鑽頭之材料都係使用碳化鶴(wc),其 1353391=:=The film quality has a high stress, especially when the thickness of the diamond film is deposited between the layers, so it is easy to cause the diamond film to peel off from the workpiece. According to the current patent on hot filament deposition diamond film, the design of the matrix filament and tension of U.S. Patent No. 5'833'753, and the deposition of a large area 'but the height of the workpiece can not be uniformly deposited; No. G254312 and U.S. Patent No. 6, detail No. 652, all of which use a grid--filament and a base to bias each other to form a plasma above the base to serve as an auxiliary workpiece. The nucleation and growth diamond enemy H is the same as the above, and it is difficult to deposit the workpieces with high height for three dimensions. Moreover, the above patents do not use the metal cutters as the ten counties. Although its double-biasing process has an auxiliary nucleating effect on workpieces such as Shixi wafer and quartz, the adhesion of the diamond film and the workpiece cannot cope with the high-speed operation of the tool, so it is easy to cause problems such as film peeling or broken knife. 'The current commonly used dimensions, such as the diameter of 3 mm (mm) ~ 〇 1 mm micro-milling or boring bit material are all using carbonized crane (wc), its 1353391

• I 本身微硬度達2500 HV,常用在印刷電路板(Printed• I itself has a microhardness of 2500 HV and is commonly used on printed circuit boards (Printed

Circuit Board,PCB )加工使用。然而,由於不易在該 • 碳化鎢之工件上形成鑽石核種,因此其鑽石核密度並 . 不高,且膜附著力亦不強而易發生剝裂。雖然可利用 電漿促進成核以增強其膜之附著力,但其電漿中之粒 子能量較高,當碰撞該工件表面時,容易使碳碳鍵扭 曲或形成碳-碳雙鍵,其將使膜產生應力或石墨化,有 時更反而降低膜之附著力,因此亦達不到效果。目前 每1業上直徑3毫米以上銑刀沉積鑽石膜確實能達到數 倍使用壽命,但在此尺寸以下之銑刀一下刀,刀柄就 斷’顯然在講求高轉速加工之前提下,鑽石膜銳刀不 僅講究其膜附著力,且其刀刃之切削率或磨潤性亦同 時被要求。 綜上所述,由於習用技術無法克服鑽石膜之附著 力不佳、刀刀之i刀削率或膜之磨潤性低等問題,因此 ·#導致刀具斷刀,難以提升刀具之使用壽命。故,一 般習用者係無法符合使用者於實際使用時之所 【發明内容】 發明之主要目的係在於’可在一般刀具及微刀 儿積’尤其針對目前高轉速之印刷電路板微刀且 =石膜,且加入特殊前處理及電漿辅助可使該鑽 ,接近_伽結構,隸有高㈣力及良好之磨 潤性’能增強刀具之切削能力而不易斷刀,進而可提 1353391 . · 升刀具之使用壽命β 本發明之次要目的係在於’沉積有該鑽石膜之刀 具係可提高該印刷電路板之加工速率並降低其成本。 為達以上之目的’本發明係一種熱燈絲鑽石膜沉 積裝置及其方法’係至少包含一真空腔體、一真空機 械幫浦、一氣壓控制器、一平板狀之金屬柵極、—栅 極偏電壓電源'-平板狀之工件載台、一載台偏電壓 電源、數排平行燈絲、一燈絲電源、一溫度程式控制 器及一進氣管所構成。首先對一為刀具之工件表面進 行特殊前處理,以化學藥水浸蝕該工件,使气2件達 到表面粗化及拋掉鈷(Co)元素,並以一^粉 超音波振盪,接著將該工件置入該熱燈絲鑽石 裝置中’使該:M牛在氫電槳環境中拋掉雜質以達、、主 !門:==源之正電壓金屬栅極與接地極燈: = 以輔助且促進該工件表面鑽石核 =生最後再以向溫至低溫穩定遞減之溫度梯度方 成該鑽石膜之成長。 以積鑽石膜,進而完 【實施方式】 請參閱『第1圖〜第3 明之έ士爐-立国丄 Η』所不’係分別為本發 月之、,、。構不意圖、本發明之金屬栅 :: 發明之工件載台結構示意圖。如圖所示.太:圖及本 -種熱燈絲鑽石膜沉積裝發明係為 ,、万法,本發明之熱燈 9 1.353391 為直流或直流脈衝電壓。 該工件載台16係具有數排以直線排列且彼此並 排之透氣孔1 6 1及工件插孔i 6 2,且該工件載台 1 6邊緣處係有數個支撐孔,由下方腔壁之載台支撐 角座1 6 3支撐,並由該載台支撐角座丄6 3上之絕 緣套1 6 4將該工件載台1 6與該真空腔體1 1内壁 作電絕緣,其中,該工件載台工6之透氣孔工6 Μ 係為0.3毫米〜5毫米;該工件插孔1 6 2之排距係 與下述之燈絲1 8排距相同,且該工件插孔丄6 2直 徑係可從1毫米〜2〇毫米不等;該工件載台丄6之位 置高度係可依不同工件長度替換不同高度之絕緣墊片 調整;該工件載台i 6亦可為幾微米(μη〇或幾十 米金屬粒壓製之金屬透氣材質。 該載台偏電壓電源1 7係電性連接該工件載台工 6之一端,用以提供負幾十伏特〜一佰多伏特接ς偏 • I電源以產生電漿’其中’該載台偏電壓電源1 7係 可為直流或直流脈衝電壓。 ▲各排平行之燈絲1 8係設置於該金屬柵極i 4與 5亥工件載台1 6之間,分為上下兩層排列。各排平行 之燈絲1 8其兩端係由一以鉬(M〇)金屬或其它高熔 點金屬所製之燈絲電極座工8 la、丄8 lb固定,且 :端之燈絲電極座i 8 la係以—直立式燈絲座支樓 1 1 8 2支揮’由該燈絲錢樓桿i 8 2上之絕緣插 柃1 8 3將遠燈絲1 8與該真空腔體丄丄内壁作電絕 1353391Circuit Board, PCB) processing. However, since the diamond core species are not easily formed on the tungsten carbide workpiece, the diamond core density is not high, and the film adhesion is not strong and the cracking is liable to occur. Although plasma can be used to promote nucleation to enhance the adhesion of the membrane, the particles in the plasma have higher energy. When colliding with the surface of the workpiece, it is easy to twist the carbon-carbon bond or form a carbon-carbon double bond. Stress or graphitization of the film sometimes increases the adhesion of the film, and thus does not achieve an effect. At present, the diamond film deposited by milling cutters with a diameter of more than 3 mm per industry can achieve several times of service life, but the cutters below this size have a knife and the handle is broken. Obviously, it is lifted before the high-speed processing, diamond film Sharp knife not only pays attention to its film adhesion, but also the cutting rate or the grinding property of its cutting edge. In summary, since the conventional technology cannot overcome the problems of poor adhesion of the diamond film, low cutting rate of the knife, or low abrasion of the film, it is difficult to increase the service life of the tool by causing the tool to be broken. Therefore, the general practitioner can not meet the user's actual use. [The invention] The main purpose of the invention is to 'can be used in general tools and micro-knife', especially for the current high-speed printed circuit board micro-knife and = The stone film, with the addition of special pre-treatment and plasma assist, can make the drill, close to the _ gamma structure, with high (four) force and good grinding property 'can enhance the cutting ability of the tool and not easy to break the knife, and then can be raised 1353391. The service life of the liter tool is a secondary objective of the present invention in that the tool system in which the diamond film is deposited can increase the processing speed of the printed circuit board and reduce its cost. For the purpose of the above, the present invention relates to a hot filament diamond film deposition apparatus and method thereof, which comprises at least a vacuum chamber, a vacuum mechanical pump, a gas pressure controller, a flat metal gate, a gate The partial voltage power supply '- flat workpiece carrier, one stage bias voltage power supply, several rows of parallel filaments, one filament power supply, one temperature program controller and one intake pipe. Firstly, a special pre-treatment is performed on the surface of the workpiece of the tool, and the workpiece is etched with chemical syrup, so that the surface of the gas is roughened and the cobalt (Co) element is discarded, and the ultrasonic vibration is oscillated by a powder, and then the workpiece is pulverized. Placed in the hot filament diamond device 'make this: M cattle throw impurities in the hydrogen electric paddle environment to reach, main! Gate: == source positive voltage metal grid and grounding pole lamp: = to assist and promote The diamond nucleus on the surface of the workpiece is finally grown in a temperature gradient which is stable to decrease from warm to low temperature. In the case of the diamond film, it is completed. [Embodiment] Please refer to "1st to 3rd of the Gentleman's Furnace - Liguo 丄 Η". Not intended, the metal gate of the present invention :: The schematic diagram of the workpiece stage structure of the invention. As shown in the figure. Too: Fig. and this kind of hot filament diamond film deposition equipment invention, , Wanfa, the heat lamp of the invention 9 1.353391 is DC or DC pulse voltage. The workpiece stage 16 has a plurality of rows of vent holes 161 and workpiece jacks i 6 2 arranged in a line, and a plurality of support holes are formed at the edge of the workpiece stage 16 and are carried by the lower chamber wall. The support angle bracket 163 supports, and the workpiece carrier 16 is electrically insulated from the inner wall of the vacuum chamber 1 1 by the insulating sleeve 164 on the corner support 丄6 3 of the stage, wherein the workpiece The venting hole 6 of the stage worker 6 is 0.3 mm to 5 mm; the row spacing of the workpiece jack 162 is the same as that of the filament 8 8 described below, and the workpiece insertion hole 丄 6 2 diameter system It can be varied from 1 mm to 2 mm; the height of the workpiece stage 6 can be adjusted by replacing the insulation pads of different heights according to different workpiece lengths; the workpiece stage i 6 can also be several micrometers (μη〇 or The metal gas permeable material of tens of meters of metal particles is pressed. The stage bias voltage power source 17 is electrically connected to one end of the workpiece carrier 6 to provide a negative tens of volts to a volt volt. In order to generate a plasma 'where' the stage bias voltage source 17 can be a DC or DC pulse voltage. ▲ each row of parallel lights The wire 18 is disposed between the metal gate i 4 and the 5 sea workpiece carrier 16 and is divided into upper and lower layers. The rows of parallel filaments 18 are made of a molybdenum (M〇) metal. Or other high-melting-point metal filament electrode holder 8 la, 丄 8 lb fixed, and: the end of the filament electrode holder i 8 la with - vertical filament seat branch 1 1 8 2 branch swing 'by the filament money Insulation plug 1 8 3 on the pole i 8 2, the far filament 1 8 and the inner wall of the vacuum chamber are electrically insulated 1353391

緣;另一端之燈絲電極座i 8 lb則由一張力控制器 1 8 4施一張力在一燈絲座滑槽i 8 5上移動拉直各 排平行之燈絲1 8,其中,該燈絲1 8之材質係可為 鎢(W)、鉬、钽(Ta)及其合金,且該燈絲丄8係無 需事先碳化即可直接進行鍍膜;該燈絲座支撐桿丄8 2亦可進一步改為該柵極支撐角座丄4 2型式;各燈 絲1 8間之距離係在!公分(cm)〜2公分之間該 燈、’糸1 8與S亥金屬柵極1 4間之距離係在〇 5公分〜2 公分之間、及該燈絲i 8與該工件4間之距離係在〇 3 公分〜1公分之間,且以上係依微尺寸並為刀具之工 件4大小而定;該張力控制器工8 4之操作係包括掛 重物拉力、彈簧力或氣壓缸力。 該燈絲電源1 9係用以作為各燈絲i 8之加熱電 源,係將該燈絲1 8加熱至18〇〇〇c〜 25〇〇〇c之高严。 該溫度程式控制器2 0係以該工件4之溫:二 要數據。利用一在該工件載台2 6上可單支或多支插 入單一工件插孔1 6 2或不同位置之工件插孔i 6 2 之測溫棒2 0 1,由該測溫棒2 〇 i測出身旁之工件 4其溫度值後,回饋訊號傳至該溫度程式控制器 做計算,再送出- 0伏特⑺〜1〇伏特或4毫安培 (mA)〜20毫安培訊號給該燈絲電源玉9做功率輸 出,以達到由程式設定控制該燈絲電源丄9於 段加熱該工件4至設定之溫度值,其中,該溫度程式 控制器2 0之控溫方式亦可為可程式邏輯控制器 12 1353391 (Programmable Logic Controller,PLC )或電腦程式控 制’不僅不會受到電漿轟擊等因素干擾,且該控溫方 • 式更進一步包括溫度多點偵測及溫差程式化比較控 制’若某一溫度偵測點附近之燈絲1 8斷掉,則立即 由其他測溫點替代,係具有可防止影響整體溫度控制 之功能。 該進軋管2 1係以一根主管在該熱燈絲鑽石膜沉 積裝置1中心分給其它幅射狀支管,各支管上係含有 •複數個氣孔2 1 1,且各氣孔2 1 1孔距在該進氣管 2 1中心處較大,越往中心外圍洞距逐漸縮短,用以 將一反應氣體經由該進氣管2丄上各氣孔2 i丄向上 噴出,再均勻流向下方由該真空機械幫浦丄2抽出, 其中,該進氣管之型式係為T型、十字型及多方向型; 該反應氣體係包括氫氣(H2 )、曱烷(CH4)、乙炔 (C2H2 )、乙烷(c2H6 )、苯(c6H6)及酒精等含碳氫 % 化合物。以上所述,係構構一全新之熱燈絲鑽石膜沉 積裝置1。 請進一步參閱『第4圖及第5圖』所示,係分別 為本發明之沉積流程示意圖及本發明之製程溫度控制 不意圖。如圖所示:本發明係利用±述之熱燈絲鑽石 膜沉積裝置1對工件4進行沉積處理,且本發明用以 實驗之工件4係為微銑刀工件,其成長鑽石膜方法係 至少包含以下步驟: 1353391 ' · (A)工件表面前處理51:先配製一含有赤血 鹽鉀(K:3Fe(CN)6)、氫氧化鉀(K〇H)及去離子水之 化學藥水,藉此浸蝕該工件4達20分鐘,將該工件4 表面做化學拋光,待該工件4表面達粗化後,再浸入 一另外配製含有30%次硫酸(仏8〇2)及7〇%氣化氫 (HC1)之化學藥水達20秒’使該工件4拋掉表面鈷 (Co )元素以避免鑽石碳(c )元素被銅吸收,而影 響其附著力。接著再浸入一以粒徑小於1微米之鑽石 霉粉加上去離子水所成之溶液,由一超音波振盪2〇分 鐘,最後在將該工件4放入去離子水中以該超音波振 盪沖洗後取出並吹乾; (B )鼠電漿清潔5 2 :將表面處理後之工件4 放入該熱燈絲鑽石膜沉積裝置i中具透氣孔i 6丄之 工件載台16上之工件插孔1 62内,由該真空機械 幫浦1 2抽氣至最終氣壓後,以該進氣管2 1上之氣 • 孔211充入一氣體濃度為2%之曱烷/氫氣(ch4/h2) 氣體至该真空腔體11内,使該真空腔體11之真空 氣壓達20托爾(Torr)。當進行鍍膜時,鍍膜第一階 段係由該溫度程式控制器2 〇設定為30分鐘升溫時 間’並啟動該燈絲電源1 9加熱該工件4,使該工件 4溫度升至750°C〜800oC ;之後進入鑛膜第二階段, 於此階段中加上一正偏壓1〇〇伏特於該金屬柵極1 4,及一負偏壓-60伏特於該工件載台1 6,將該工件 4於此氫電漿環境中清潔10分鐘〜30分鐘,使該工 1353391 件4可拋掉雜質而達到表面清潔,同時該工件4溫度 亦從原本750°C〜800。(:間逐漸升至9〇〇〇c〜98〇〇c ; • ( C )雙偏壓鑽石核種成核5 3 :鍍膜第三階段 雙偏㈣核,其所需之雙偏壓值係分別為該金屬橋極 1 4正偏壓3G〜2GG伏特,及該工件載台16負偏壓 30 150伏特,且6玄工件4溫度仍維持9〇〇〜98〇〇c, 並另充入-氣體濃度為〇·5〜4%之曱烧/氮氣氣體至該 真空腔體11内,使該真空腔體工丄之真空氣壓達i • 〜30托爾。利用雙偏壓電源之正電愿金屬拇極丄核 接地極燈絲1 8之間放電產生電漿,當熱燈絲i 8在 高溫時發射出電子飛向該金屬栅極i 4時,會裂解該 氫氣及甲烧而離化產生一部份之氫離子(H+)及曱烧 基(CH/)等自由基,此等離子因具有能量可被負偏 壓之工件4所吸引而與該工件4發生碰撞反應,進而 可辅助且促進該工件4表面鑽石核種產生。在成核時 餳 間持續3分鐘〜3小時後,關掉此雙偏壓電源,該工 件4亦在數十分鐘内降溫至8〇〇〜880oC,其中,該甲 烷係可由乙炔、乙烷、苯及酒精等含碳氫化合物替代; 以及 (D)鑽石膜成長54 :於步驟(C)成核後, 進行鍍膜第四階段成長鑽石膜,在該鑽石膜成長過程 中’该金屬栅極1 4係接地,而該工件4採接地或浮 接’且該工件4溫度係由800〜880。(:間逐漸降至 780°C,並在同氣體濃度〇.5〜4%之甲烷/氫氣氣體下, 1353391 將該真空腔體1 1之真空氣壓提升為10〜50托爾。藉 由高溫至低溫穩定遞減之溫度梯度方式在該工件4表 面進行化學重組以沉積厚度1〜1〇微米鑽石膜,其成 長時間為5〜20小時,並在成長結束時關閉該甲烧氣 體,且於數十分鐘内待該工件4降至室溫後取出該工 件4,其中,該曱烷係可由乙炔、乙烷、苯及酒精等 含碳氫化合物替代。 上述步驟(D) 該工件4溫度亦可先由高溫 腎〜95〇。(:附近成長—段時間後,再以低溫請〜 780°C附近成長一段長時間。 藉此,在该工件溫度不超過i 〇〇〇〇C下,利用加入 特殊前處理及電漿輔助後,可使本發明製作之鑽石膜 接近類鑽碳膜結構,能提升該鑽石膜之磨潤性及附著 性,以增加其實用性及廣泛之工業應用性,不僅可降 低該鑽石臈應力、減低該工件表面摩擦力及增強該工 % 件磨/閏性’使刀具工件可在印刷電路板(Printed Circuit Board,PCB )之高轉速下正常工作而不易斷刀,並且, 尤其在直把1毫米碳化鎢(WC)銑刀經由沉積一層5 〜8微米厚度之鑽石膜後,其使用壽命更可達未鍍銑 刀6倍以上’明顯具有可提升使用壽命之優點。 良丁'上所述’本發明係一種熱燈絲鑽石膜沉積裝置 及其方法,可有效改善習用之種種缺點,利用加入特 殊刚處理及電漿辅助後,,可提升鑽石膜之磨潤性及附 著性’以增加其實用性及廣泛之工業應用性,不僅可 1353391 * · 降低該鑽石膜應力、減低工件表面摩擦力及增強該工 件磨潤性,且在一般刀具及微刀具上沉積之鑽石膜更 可提升該刀具之使用壽命,尤其對於印刷電路板之高 轉速下亦可正常工作而不易斷刀,係可提高其加工速 率,以降低成本,進而使本發明之産生能更進步、更 實用、更符合使用者之所須,確已符合發明專利申請 之要件,爰依法提出專利申請。 冬惟以上所述者,僅為本發明之較佳實施例而已, 田不忐以此限定本發明實施之範圍;故,凡依本發明 申明專利範圍及發明說明書内容所作之簡單的等效變 化與修飾’皆應仍屬本發明專利涵蓋之範圍内。The other end of the filament electrode holder i 8 lb is moved by a force controller 1 8 4 on a filament holder chute i 8 5 to straighten the rows of parallel filaments 18 , wherein the filament 1 8 The material may be tungsten (W), molybdenum, tantalum (Ta) and alloys thereof, and the filament crucible 8 may be directly coated without prior carbonization; the filament holder support rod 8 2 may be further changed to the grid Extremely supported corner seat 丄 4 2 type; the distance between each filament is 18! The distance between the centimeters (cm) and 2 cm between the lamp, '糸18 and the S-metal gate 14 is between 公5 cm and 2 cm, and the distance between the filament i8 and the workpiece 4. The system is between 公3 cm and 1 cm, and the above is dependent on the micro-size and the size of the workpiece 4 of the tool; the tension controller 8-4 operation includes the weight pulling force, the spring force or the pneumatic cylinder force. The filament power source 19 is used as a heating power source for each of the filaments i 8 , and the filaments 18 are heated to a high temperature of 18 〇〇〇 c 25 〇〇〇 c. The temperature program controller 20 is based on the temperature of the workpiece 4: two data. By using a temperature measuring rod 2 0 1 on the workpiece stage 26 that can be inserted into a single workpiece socket 116 or a different position of the workpiece socket i 6 2 on the workpiece stage 26, the temperature measuring rod 2 〇i After measuring the temperature value of the workpiece 4 next to the body, the feedback signal is transmitted to the temperature program controller for calculation, and then sent - 0 volt (7) ~ 1 volt volt or 4 milliamperes (mA) ~ 20 mA signal to the filament power supply jade 9 is used for power output, so that the filament power supply 丄9 is programmed to heat the workpiece 4 to a set temperature value, wherein the temperature control mode of the temperature program controller 20 can also be a programmable logic controller 12 1353391 (Programmable Logic Controller, PLC) or computer program control 'not only will not be interfered by factors such as plasma bombardment, and the temperature control method further includes temperature multi-point detection and temperature difference stylization comparison control 'if a certain temperature When the filament near the detection point is broken, it is immediately replaced by other temperature measurement points, which has the function of preventing the overall temperature control from being affected. The inlet tube 2 1 is distributed to the other radiation branch pipe at the center of the hot filament diamond film deposition device 1 , and each branch tube includes a plurality of pores 2 1 1 and a pore distance of 2 1 1 The center of the intake pipe 2 1 is larger, and the distance from the center to the center is gradually shortened, so as to spray a reaction gas upward through the air holes 2 i丄 of the intake pipe 2, and then uniformly flow downward to the vacuum. The mechanical pump is extracted 2, wherein the type of the intake pipe is T-shaped, cross-shaped and multi-directional; the reaction gas system includes hydrogen (H2), decane (CH4), acetylene (C2H2), ethane A hydrocarbon-containing compound such as (c2H6), benzene (c6H6) or alcohol. As described above, a new hot filament diamond film deposition apparatus 1 is constructed. Please refer to the "Fig. 4 and Fig. 5" for further description of the deposition process of the present invention and the process temperature control of the present invention. As shown in the figure: the present invention utilizes the hot filament diamond film deposition apparatus 1 described above to deposit the workpiece 4, and the workpiece 4 used in the experiment is a micro-milling workpiece, and the method for growing the diamond film includes at least The following steps: 1353391 ' (A) Surface preparation of the workpiece 51: First prepare a chemical solution containing potassium salt of red blood (K: 3Fe (CN) 6), potassium hydroxide (K 〇 H) and deionized water, borrow The workpiece 4 is etched for 20 minutes, and the surface of the workpiece 4 is chemically polished. After the surface of the workpiece 4 is roughened, it is further immersed in an additional formulation containing 30% sulfoxylic acid (仏8〇2) and 7〇% gasification. Hydrogen (HC1) chemical syrup for 20 seconds' causes the workpiece 4 to throw off the surface cobalt (Co) element to prevent the diamond carbon (c) element from being absorbed by the copper, which affects its adhesion. Then, a solution of diamond dust powder with a particle diameter of less than 1 micrometer and deionized water is immersed, and the ultrasonic wave is oscillated for 2 minutes, and finally the workpiece 4 is placed in deionized water and washed with the ultrasonic wave. (B) Mouse plasma cleaning 5 2: The surface-treated workpiece 4 is placed in the workpiece socket 1 of the workpiece stage 16 having the vent hole i 6 in the hot filament diamond film deposition device i In the 62, after the vacuum mechanical pump 12 is evacuated to the final air pressure, the gas/hole 211 on the intake pipe 2 is filled with a gas having a gas concentration of 2% of decane/hydrogen gas (ch4/h2). To the inside of the vacuum chamber 11, the vacuum pressure of the vacuum chamber 11 is 20 Torr. When the coating is performed, the first stage of the coating is set by the temperature program controller 2 为 to a 30-minute heating time ′ and the filament power supply is activated to heat the workpiece 4 to raise the temperature of the workpiece 4 to 750 ° C to 800 ° C; After entering the second stage of the mineral film, a positive bias voltage of 1 volt is applied to the metal gate 14 in this stage, and a negative bias voltage of -60 volts is applied to the workpiece stage 16. The cleaning in the hydrogen plasma environment for 10 minutes to 30 minutes, so that the work 1353391 piece 4 can throw away impurities to achieve surface cleaning, and the temperature of the workpiece 4 is also from 750 ° C ~ 800. (: gradually increased to 9〇〇〇c~98〇〇c; • (C) double-biased diamond nuclear nucleation 5 3 : coating the third stage of the double-biased (four) core, the required double bias value is The metal bridge pole 14 is positively biased by 3G~2GG volts, and the workpiece stage 16 is negatively biased by 30 150 volts, and the temperature of the 6 phantom workpiece 4 is maintained at 9 〇〇 to 98 〇〇 c, and is additionally charged - The gas concentration is 5·5~4% of the argon/nitrogen gas into the vacuum chamber 11, so that the vacuum pressure of the vacuum chamber is up to ~30 Torr. The use of the double bias power supply is positive. The discharge between the metal thumb nucleus grounding filaments of the metal produces a plasma. When the hot filament i 8 emits electrons to the metal gate i 4 at a high temperature, the hydrogen and the sulphur are cracked and the ionization is generated. a part of radicals such as hydrogen ions (H+) and cesium-based groups (CH/), which are attracted to the workpiece 4 by the workpiece 4 having energy that can be negatively biased, thereby assisting and promoting the The diamond core of the workpiece 4 is produced. When the sugar is nucleated for 3 minutes to 3 hours, the double bias power supply is turned off, and the workpiece 4 is also cooled in tens of minutes. 8〇〇~880oC, wherein the methane can be replaced by hydrocarbons such as acetylene, ethane, benzene and alcohol; and (D) diamond film growth 54: after the nucleation in step (C), the fourth stage of coating Growing the diamond film, during the growth of the diamond film, the metal gate 14 is grounded, and the workpiece 4 is grounded or floated, and the temperature of the workpiece 4 is from 800 to 880. (: gradually decreases to 780°) C, and under the same gas concentration 〇.5~4% of methane/hydrogen gas, 1353391, the vacuum pressure of the vacuum chamber 1 is raised to 10~50 Torr. The temperature gradient is stabilized by high temperature to low temperature. Chemically recombining on the surface of the workpiece 4 to deposit a diamond film having a thickness of 1 to 1 〇 micron, which has a growth time of 5 to 20 hours, and is turned off at the end of growth, and the workpiece 4 is lowered in several tens of minutes. After the temperature is reached, the workpiece 4 is taken out, wherein the decane can be replaced by a hydrocarbon-containing compound such as acetylene, ethane, benzene or alcohol. In the above step (D), the temperature of the workpiece 4 can also be from high temperature kidney to 95 〇. (: Growing up nearby - after a period of time, please use low temperature ~ 780 °C The growth of the diamond film produced by the present invention is close to the diamond-like carbon film structure by adding special pre-treatment and plasma assisting under the temperature of the workpiece not exceeding i 〇〇〇〇C. Improve the grinding and adhesion of the diamond film to increase its practicability and wide industrial applicability, not only reduce the stress of the diamond, reduce the surface friction of the workpiece and enhance the grinding/smoothing of the workpiece. The tool workpiece can work normally at high speeds of the Printed Circuit Board (PCB) without breaking the knife, and especially by depositing a 1 mm to 8 μm thick diamond by straightening a 1 mm tungsten carbide (WC) cutter. After the film, its service life is more than 6 times that of the unplated milling cutter, which obviously has the advantage of improving the service life. The present invention is a hot filament diamond film deposition device and a method thereof, which can effectively improve various disadvantages of the conventional use, and can improve the abrasion resistance of the diamond film by adding special treatment and plasma assist. Adhesion' to increase its practicability and wide industrial applicability, not only 1353391 * · Reduce the diamond film stress, reduce the surface friction of the workpiece and enhance the grinding of the workpiece, and deposit diamonds on general tools and micro-tools The film can further improve the service life of the tool, especially for the high speed of the printed circuit board, and can work normally without breaking the knife, thereby increasing the processing rate and reducing the cost, thereby making the invention more progressive and more Practical and more in line with the needs of users, it has indeed met the requirements of the invention patent application, and filed a patent application according to law. The above is only the preferred embodiment of the present invention, and the scope of the present invention is limited by the scope of the present invention; therefore, the simple equivalent change made by the scope of the invention and the contents of the invention description according to the present invention And the modifications 'should be within the scope of the invention patent.

17 (S ) 1353391 【圖式簡單說明】 第1圖,係本發明之結構示意圖。 第2圖,係本發明之金屬柵極結構示意圖。 - 第3圖,係本發明之工件載台結構示意圖。 第4圖,係本發明之沉積流程示意圖。 第5圖,係本發明之製程溫度控制示意圖。 【主要元件符號說明】 I 熱燈絲鑽石膜沉積裝置1 真空腔體1 1 真空機械幫浦1 2 氣壓控制器1 3 金屬柵極1 4 透氣孔141 •I 棚極支撐角座1 4 2 絕緣套1 4 3 柵極偏電壓電源1 5 工件載台1 6 透氣孔161 工件插孔1 6 2 載台支撐角座1 6 3 1.353391 絕緣套1 6 4 載台偏電壓電源1 7 燈絲1 8 燈絲電極座1 8 1 a、1 8 1 b 燈絲座支撐桿1 8 2 絕緣插桿1 8 3 張力控制器1 8 4 燈絲座滑槽1 8 5 燈絲電源1 9 溫度程式控制器2 0 測溫棒2 0 1 進氣管2 1 氣孔2 1 1 真空抽氣閥門2 壓力計3 工件4 步驟(A)工件表面前處理5 1 步驟(B )氫電漿清潔5 2 步驟(C )雙偏壓鑽石核種成核5 3 步驟(D)鑽石膜成長5 4 (S ) 1917 (S) 1353391 [Simple description of the drawings] Fig. 1 is a schematic view showing the structure of the present invention. Fig. 2 is a schematic view showing the structure of a metal gate of the present invention. - Figure 3 is a schematic view of the structure of the workpiece stage of the present invention. Figure 4 is a schematic view of the deposition process of the present invention. Figure 5 is a schematic diagram of process temperature control of the present invention. [Main component symbol description] I Hot filament diamond film deposition device 1 Vacuum chamber 1 1 Vacuum mechanical pump 1 2 Air pressure controller 1 3 Metal grid 1 4 Ventilation hole 141 • I shed pole support seat 1 4 2 Insulation sleeve 1 4 3 Gate bias voltage supply 1 5 Workpiece stage 1 6 Ventilation hole 161 Workpiece socket 1 6 2 Stage support angle seat 1 6 3 1.353391 Insulation sleeve 1 6 4 Stage bias voltage supply 1 7 Filament 1 8 Filament electrode Block 1 8 1 a, 1 8 1 b Filament holder support rod 1 8 2 Insulation plunger 1 8 3 Tension controller 1 8 4 Filament holder chute 1 8 5 Filament power supply 1 9 Temperature program controller 2 0 Thermometer 2 0 1 Intake pipe 2 1 Pore 2 1 1 Vacuum suction valve 2 Pressure gauge 3 Workpiece 4 Step (A) Workpiece surface pretreatment 5 1 Step (B) Hydrogen plasma cleaning 5 2 Step (C) Double bias diamond seed Nucleation 5 3 Step (D) Diamond film growth 5 4 (S ) 19

Claims (1)

1353391 十、申請專利範圍: 1 ·熱燈絲鑽石膜沉積裝置,係至少包含: 一真空腔體,該真空腔體係為一外殼水冷及可 氣壓控制之腔體; 一真空機械幫浦,該真空機械幫浦係用以抽吸 該真空腔體之真空度;1353391 X. Patent application scope: 1 · The hot filament diamond film deposition device comprises at least: a vacuum chamber, which is a water-cooled and air-controllable cavity; a vacuum mechanical pump, the vacuum machine a vacuum for pumping the vacuum chamber; 一氣壓控制器,該氣壓控制器係用以控制一真 空抽氣閥門之開啟程度,藉另一端連結之壓力計達 到預定真空度; 一平板狀之金屬柵極,該金屬柵極係於中央區 具有複數個透氣孔,且該金屬柵極邊緣處係有數個 支撐孔,由下方腔壁之柵極支撐角座支撐,並由該 柵極支撐角座上之絕緣套將該金屬柵極與該真空 腔體内壁作電絕緣; 一柵極偏電壓電源,該柵極偏電壓電源係電性 連接該金屬栅極之一端,用以提供偏壓電源以產生 電漿; 一平板狀之工件載台,該工件載台係具有數排 以直線排列且彼此並排之透氣孔及工件插孔,且該 工件載台邊緣處係有數個支撐孔,由下方腔壁之載 台支撐角座支撐,並由該載台支撐角座上之絕緣套 將該工件載台與該真空腔體内壁作電絕緣; 一載台偏電壓電源,該載台偏電壓電源係電性 20 連接該工件載台之一端,用以提供偏壓電源以產生 電漿; 數排平行燈絲’各排平行之燈絲係設置於該金 屬栅極與該工件載台之間,分為上下兩層排列。各 排平行之燈絲其兩端係由一燈絲電極座固定,且一 端之燈絲電極座係以一直立式燈絲座支撐桿支 撐,由該燈絲座支撐桿上之絕緣插桿將該燈絲與該 真空腔體内壁作電絕緣;另一端之燈絲電極座則由 一張力控制器施一張力在一燈絲座滑槽上移動拉 直各排平行之燈絲; 一燈絲電源’該燈絲電源係用以作為各燈絲之 加熱電源; 一溫度程式控制器,該溫度程式控制器係用以 程式設定控制該燈絲電源於不同時段加熱一工件 至設定之溫度值;以及 一進氣管’該進氣管係以一根主氣管在該熱燈 絲鑽石膜沉積裝置中心分給其它幅射狀支管,各支 管上係含有複數個氣孔,且各氣孔孔距在該進氣管 中心處較大’越往中心外圍洞距逐漸縮短,用以將 一反應氣體經由各氣孔向上喷出,再均勻流向下方 由該真空機械幫浦抽出。 依據申請專利範圍第i項所述之熱燈絲鑽石膜沉積 1353391a pressure controller for controlling the opening degree of a vacuum pumping valve, and the pressure gauge connected to the other end reaches a predetermined degree of vacuum; a flat metal gate, the metal grid is tied to the central area Having a plurality of venting holes, and a plurality of supporting holes are formed at the edge of the metal gate, supported by a gate supporting angle seat of the lower cavity wall, and the metal gate is insulated by the insulating sleeve on the gate supporting corner seat The inner wall of the vacuum chamber is electrically insulated; a gate bias voltage source is electrically connected to one end of the metal gate for providing a bias power source to generate plasma; a flat workpiece stage The workpiece stage has a plurality of rows of vent holes and workpiece insertion holes arranged in a line and arranged side by side, and a plurality of support holes are arranged at the edge of the workpiece stage, supported by the stage support angle seat of the lower chamber wall, and An insulating sleeve on the support base of the stage electrically insulates the workpiece stage from the inner wall of the vacuum chamber; a stage bias voltage power supply, the stage bias voltage power supply is electrically connected to one end of the workpiece stage, To provide bias power to generate a plasma; filament number of parallel rows of 'filament lines parallel rows of metal disposed in the stage between the gate electrode and the workpiece, is divided into upper and lower layers are arranged. Each row of parallel filaments is fixed at both ends by a filament electrode holder, and the filament electrode holder at one end is supported by a vertical filament holder support rod, and the filament is insulated from the vacuum by the insulating rod on the filament holder support rod The inner wall of the cavity is electrically insulated; the filament electrode holder at the other end is biased by a force controller to move a pair of parallel filaments on a filament seat chute; a filament power supply is used as a a heating power supply for the filament; a temperature program controller for programming to control the filament power to heat a workpiece to a set temperature value at different times; and an intake pipe 'the intake pipe system The root main gas pipe is distributed to other radiation-shaped branch pipes at the center of the hot filament diamond film deposition device, and each branch pipe has a plurality of air holes, and the distance of each air hole is larger at the center of the air intake pipe. It is gradually shortened to eject a reactive gas upward through the respective pores, and then uniformly flow downward to be withdrawn by the vacuum mechanical pump. Hot filament diamond film deposition according to item i of the patent application scope 1353391 裝置’其中,該反應氣體係包括氫氣(h2)、曱烷 (ch4)、乙炔(c2h2)、乙烷(c2h6)、苯(c6h6) 及酒精之含碳氫化合物,且該曱烷亦可由乙炔、乙 烷、苯及酒精之含碳氫化合物替代。 3·依據申凊專利範圍第1項所述之熱燈絲鑽石膜沉積 裝置,其中,該進氣管之型式係為τ型、十字型及 多方向型。 4.依據申凊專利範圍第1項所述之熱燈絲鑽石膜沉積 裝置’其中’該燈絲之材質係可為鎢(w)、鉬(Mo)、 钽(Ta)及其合金。 5 .依據申清專利範圍第1項所述之熱燈絲鑽石膜沉積 裝置,其中,該燈絲座支撐桿亦可改為該柵極支撐 角座型式。 6 ·依據申凊專利範圍第1項所述之熱燈絲鐵石膜沉積 編•裝置,其中,該燈絲間之距離係在!〜2公分(cm ) 之間、該燈絲與該金屬柵極間之距離係在〇5〜2 公分之間、及該燈絲與該工件間之距離係在0.3〜1 公分之間。 7 ·依據申請專利範圍第1項所述之熱燈絲鑽石膜沉積 裝置,其中,該金屬柵極與該工件載台之透氣孔孔 徑係為0.3〜5毫米(mm),且該金屬栅極在近其 中心區其透氣孔孔距係較外圍區大。 22 1353391 ^ °e?Wm 8 ·依據申請專利範圍第i項所述之熱燈絲鑽石膜沉積 裝置,其中,該工件載台亦可為幾微米(μπι)或 幾十微米金屬粒壓製之金屬透氣材質。 9 .依據申凊專利範圍第1項所述之熱燈絲鑽石膜沉積 裝置,其中,該工件載台之位置高度係可依不同工 件長度替換不同高度之絕緣墊片調整。 10依據申明專利範圍第1項所述之熱燈絲鑽石膜沉 積裝置,其中,該測溫棒係可單支或多支***該工 件載台上單一工件插孔或不同位置之工件插孔,或 用紅外線測溫器在爐外測溫方式,可回饋訊號至該 溫度程式控制器做.計算,再由該溫度程式控制器送 出一訊號給該燈絲電源做功率輸出。The apparatus of the present invention includes hydrogen (h2), decane (ch4), acetylene (c2h2), ethane (c2h6), benzene (c6h6), and an alcohol-containing hydrocarbon, and the decane may also be derived from acetylene. , hydrocarbon, benzene, benzene and alcohol are replaced by hydrocarbons. 3. The hot filament diamond film deposition apparatus according to claim 1, wherein the type of the intake pipe is a τ type, a cross type, and a multidirectional type. 4. The hot filament diamond film deposition apparatus according to claim 1 of the invention, wherein the material of the filament is tungsten (w), molybdenum (Mo), tantalum (Ta) and alloys thereof. 5. The hot filament diamond film deposition apparatus according to claim 1, wherein the filament holder support rod is also changed to the grid support angle seat type. 6 · The hot filament film deposition device according to item 1 of the patent application scope, wherein the distance between the filaments is tied! Between ~2 cm (cm), the distance between the filament and the metal gate is between 〜5 and 2 cm, and the distance between the filament and the workpiece is between 0.3 and 1 cm. The hot filament diamond film deposition apparatus according to claim 1, wherein the metal grid and the workpiece carrier have a vent hole diameter of 0.3 to 5 mm (mm), and the metal grid is Near its central area, its venting hole spacing is larger than the peripheral area. 22 1353391 ^ °e? Wm 8 · The hot filament diamond film deposition apparatus according to the scope of claim i, wherein the workpiece stage can also be ventilated by a metal of several micrometers (μπι) or several tens of micrometers of metal particles Material. 9. The hot filament diamond film deposition apparatus according to claim 1, wherein the position height of the workpiece stage can be adjusted by replacing the insulation spacers of different heights according to different workpiece lengths. The hot filament diamond film deposition apparatus according to claim 1, wherein the temperature measuring rod can be inserted into a single workpiece insertion hole or a workpiece insertion hole of a different position on the workpiece stage, or Using the infrared thermometer to measure the temperature outside the furnace, the signal can be fed back to the temperature program controller for calculation, and then the temperature program controller sends a signal to the filament power source for power output. 1 ·依據申请專利範圍第1項所述之熱燈絲鑽石膜沉 積裝置’其中’該工件插孔排距與該燈絲排距相 同’且該工件插孔直徑係可從1〜2〇毫米不等。 2 .依據申請專利範圍第1項所述之熱燈絲鑽石膜沉 積裝置’其中’該柵極偏電壓電源與該載台偏電壓 電源係可為直流或直流脈衝電壓。 1 3 ·依據申請專利範圍第1項所述之熱燈絲鑽石膜沉 積裝置’其中’該溫度程式控制器之控溫方式亦可 為可程式邏輯控制器(pr〇grammable Logic Controller,PLC)或電腦程式控制,且進一步包括 23 1353391 WO: '57' 07Γ—1 年月日修正##胃 溫度多點偵測及溫差程式化比較控制。 -- 1 4 · 一種熱燈絲鑽石膜沉積方法,其至少包含以下步 驟: (A)先對一工件表面進行特殊前處理,以化 學藥水浸兹該工件’使該工件達到表面粗化及拋掉 鈷(Co)元素,並以一鑽石粉進行超音波振盪; (B )將該工件置入一熱燈絲鑽石膜沉積裝置 中,並充入一甲烷/氫氣氣體。在鍍臈第一階段進 行升溫,啟動一燈絲電源加熱該工件,之後進入鍍 膜第一階段’於此階段中加上正負偏壓於一金屬栅 極及一工件載台,使該工件於氫電漿環境中拋掉雜 質以達清潔; (C) 鍍膜第三階段雙偏壓成核,在正負之雙 偏壓值下,另充入一甲烷/氫氣氣體,利用雙偏壓 電源之正電壓金屬柵極與接地極燈絲之間放電產 生電漿,以辅助該工件表面鑽石核種產生,之後關 掉該雙偏壓電源;以及 (D) 進行鍍膜第四階段成長鑽石膜,藉由高 溫至低溫穩定遞減之溫度梯度方式在該工件表面 進行化學重組以沉積鑽石膜,並在成長結束時關閉 該甲烷氣體,且於數十分鐘内待該工件降至室温後 取出該工件。 5 ·依據申請專利範圍第1 4項所述之熱燈絲鑽石膜 24 '儿積方法’其中’該步驟(A)中用以粗化及拋銅 之化學藥水係分別為赤血鹽鉀(K3Fe(CN)6)與氫 氧化鉀(K0H)及次硫酸(H2S02)與氯化氫( HC1)。 1 6依據申请專利範圍第1 4項所述之熱燈絲鑽石膜 '儿積方法’其該超音波振盪之鑽石粉其粒徑係 小於1微米。 1 7依據申請專利範圍第1 4項所述之熱燈絲鑽石膜 ’儿積方法,其中,該步驟(C)中成核之操作條件 係I括甲烧/虱氣氣體之濃度為0.5〜4%、金屬栅極 正偏壓為30〜200伏特、工件載台負偏壓為_3〇〜 -150伏特、成核溫度為900〜980。〇真空氣壓為1 • 〜30托爾及成核時間為3分鐘〜3小時。 1 8 ·依據申請專利範圍第1 4項所述之熱燈絲鑽石膜 沉積方法,其中,該步驟(D )中成長鑽石膜之操 % 作條件係包括甲烷/氫氣氣體之濃度為0.5〜4%、金 屬柵極接地、工件之電極採接地或浮接、工件溫度 降至780。〇真空氣壓為10〜50托爾及沉積5〜2〇 小時。 9 ·依據申請專利範圍第1 4項所述之熱燈絲鑽石膜 沉積方法,其中,該步驟(D)中該工件之溫度亦 可先由高溫1000〜950〇c附近成長—段時間後,再 以低溫830〜780。(1!附近成長一段長時間。 25 1353391 1ΘΘ;**8:· θ 4 — 「年月日修正替換頁丨 2 ◦·依據#請專利範圍第1 4項所述之熱燈絲鑽石膜 沉積方法,其中,該鑽石膜厚度係為5〜8微米。1) The hot filament diamond film deposition apparatus according to item 1 of the patent application scope, wherein the workpiece jack has the same row spacing as the filament row, and the workpiece jack diameter may range from 1 to 2 mm. . 2. The hot filament diamond film deposition apparatus according to claim 1, wherein the gate bias voltage source and the stage bias voltage source are DC or DC pulse voltages. 1 3 · The hot filament diamond film deposition device according to claim 1 of the patent application scope, wherein the temperature control mode of the temperature program controller may also be a programmable logic controller (PLC) or a computer Program control, and further includes 23 1353391 WO: '57' 07Γ-1 year and month correction ## stomach temperature multi-point detection and temperature difference stylized comparison control. - 1 4 · A hot filament diamond film deposition method comprising at least the following steps: (A) first special pre-treatment of a workpiece surface, immersing the workpiece with a chemical syrup to make the workpiece rough and throw away Cobalt (Co) element and ultrasonically oscillate with a diamond powder; (B) The workpiece is placed in a hot filament diamond film deposition apparatus and filled with a methane/hydrogen gas. In the first stage of the ruthenium plating, the temperature is raised, a filament power source is started to heat the workpiece, and then enters the first stage of the coating process. In this stage, a positive and negative bias voltage is applied to a metal grid and a workpiece stage, so that the workpiece is hydrogen-charged. (3) The third stage of the coating is double-biased nucleation. Under the positive and negative double bias values, another methane/hydrogen gas is charged, and the positive voltage metal of the double bias power source is used. A discharge between the gate and the grounding filament generates a plasma to assist the generation of the diamond core on the workpiece surface, and then the dual bias power supply is turned off; and (D) a fourth stage diamond film is formed, which is stabilized by high temperature to low temperature. A decreasing temperature gradient mode chemically recombines the surface of the workpiece to deposit a diamond film, and the methane gas is turned off at the end of growth, and the workpiece is taken out after the workpiece is cooled to room temperature within tens of minutes. 5 · According to the patent application scope of the fifteenth item of the thermal filament diamond film 24 'child accumulation method', 'the chemical base system used in this step (A) for roughening and throwing copper is respectively red blood potassium salt (K3Fe (CN) 6) with potassium hydroxide (K0H) and hyposulfuric acid (H2S02) and hydrogen chloride (HC1). 1 6 The hot filament diamond film 'child' method according to claim 14 of the patent application scope, wherein the ultrasonically oscillated diamond powder has a particle size of less than 1 micrometer. 1 7 according to the hot filament diamond film 'integration method according to claim 14 of the patent application scope, wherein the operating condition of the nucleation in the step (C) is the concentration of the ketone/helium gas of 0.5 to 4 %, the metal grid positive bias is 30~200 volts, the workpiece stage negative bias is _3 〇~-150 volts, and the nucleation temperature is 900~980. 〇 Vacuum pressure is 1 • 〜30 Torr and nucleation time is 3 minutes to 3 hours. 1 8 The hot filament diamond film deposition method according to claim 14, wherein the operating condition of the diamond film in the step (D) comprises a concentration of methane/hydrogen gas of 0.5 to 4%. The metal gate is grounded, the electrode of the workpiece is grounded or floated, and the workpiece temperature is reduced to 780. 〇 Vacuum pressure is 10~50 Torr and deposition is 5~2 〇 hours. 9. The hot filament diamond film deposition method according to claim 14, wherein the temperature of the workpiece in the step (D) may first be grown from a high temperature of 1000 to 950 — c after a period of time, and then Take low temperature 830~780. (1! It has been growing for a long time. 25 1353391 1ΘΘ; **8:· θ 4 — "The year of the year, the replacement of the page 丨 2 ◦ · According to the patent scope of the patent, the thermal filament silk film deposition method Wherein, the thickness of the diamond film is 5 to 8 microns. 2626
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Publication number Priority date Publication date Assignee Title
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