TWI772285B - 限制擴散速率之熱化學氣相沉積塗層 - Google Patents
限制擴散速率之熱化學氣相沉積塗層 Download PDFInfo
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Abstract
在此揭示一種熱化學氣相沈積塗覆物件以及熱化學氣相沈積方法。該物件包括一基材以及在該基材上之一熱化學氣相沈積塗層。該熱化學氣相沈積塗層包括經由限制擴散速率之熱化學氣相沈積產生之特性。該熱化學氣相沈積方法包括將一氣態物種引入一容器，以及通過該氣態物種之限制擴散速率之反應，在該容器內之一物件上產生一熱化學氣相沈積塗層。
Description
本發明是針對一種熱化學氣相沈積。更具體地說，本發明是針對一種限制擴散速率之熱化學氣相沈積塗層。
限制反應速率之熱化學氣相沈積(“CVD”)能夠用於生產具有極佳特性之塗層，其可應用於各式的材料。然而，限制反應速率之熱CVD可能產生不合需要的視覺效果(cosmetic effects)和/或不一致。例如，加工珠之使用，是生產限制反應速率之熱CVD塗層之技術。此等珠可能導致厚度不一致，例如，產生珠點和/或不相似的著色。同樣的，高濃度的氣體在大於1000托的壓力下分解可導致類似不合需要的效應。
一些像是電漿增強化學氣相沈積(PECVD)和/或濺鍍之技術，產生額外的問題。此等技術可能會在塗層和/或基材上造成衝擊。此外，此等技術可能因加速離子的存在而造成材料的損壞或限制。同樣地，需要高熱(例如，高於700℃)的沈積技術，可能引起許多像是對基材的治金和/或結晶衝擊的問題。
取決於物種以及沈積技術，厚度亦可能產生問題。例如，在某些技術中，大厚度(例如，大於8,000埃、大於10,000埃或20,000埃)可能導致不希望有的塗層剝落。此種剝落可能遍布整個塗層，或在某些技術中可能局限在缺乏均一厚度的地方。
與先前技術相較之下顯示出一或多種改善之限制擴散速率之熱化學氣相沈積塗層，將是本技藝所需要的。
在一實施例中，一種物件包括一基材以及在該基材上之一熱化學氣相沈積塗層。該熱化學氣相沈積塗層包括經由限制擴散速率之熱化學氣相沈積產生之特性。
在另一實施例中，一種熱化學氣相沈積方法包括將一氣態物種引入一容器，以及通過該氣態物種之限制擴散速率之反應，於該容器內之一物件上產生一熱化學氣相沈積塗層。
依照下列更詳細的說明以及結合舉例說明本發明之原理之附圖，本發明之其它的特徵以及優點將顯而易見。
100:熱化學氣相沈積方法
101:熱CVD塗層
102:步驟
103:表面
105:容器
107:物件
109:基材
111:第一厚度
113:範圍
115:第二厚度
圖1是根據本發明之一實施例之限制擴散速率之熱化學氣相沈積塗覆方法之示意透視截面圖。
可能的話，在整個圖式中將使用相同的參
考符號來表示相同的部件。
所提供的是一種限制擴散速率之熱化學氣相沈積塗覆物件以及塗覆方法。本發明之實施例與例如無法包括在此所揭示之一或多個特徵之概念相比，增加塗層的一致性/重複性、厚度公差範圍窄(例如，從250埃至150埃)、改善美觀、容許在沒有使用珠之情況下實現方法、修飾膜的密度、允許低溫操作(例如，超過10%)、修飾微結構、修飾光學特性、修飾孔隙率、修飾耐腐蝕性、修飾光澤度、修飾表面特徵、允許更有效的生產塗層、允許塗覆各式各樣的幾何形狀(例如，窄通道/管、三維複雜幾何形狀和/或隱藏或非視距(non-line-of-site)幾何形狀，諸如針頭、管、探針、夾具、複雜的平面和/或非平面幾何形狀物件、簡單非平面和/或平面幾何物件以及其等之組合)、允許塗覆大量的物件或允許其等之組合。
參照圖1，熱化學氣相沈積(“CVD”)方法100包括使一或多種氣體在一容器105和/或室之一或二者內，於一或多個步驟中(步驟102)反應，在一物件107之一表面103上形成一熱CVD塗層101。圖1中所示之物件107是一管子，其亦作為容器105，其之內部是塗覆熱CVD塗層101之表面103。額外地或選擇性地，在其它實施例中，容器105和/或該室與要被塗覆之物件107是獨立的結構，像是熱爐室、獨立的容器結構或任何其它具有配置成可至少暫時封閉之有限體積之結構(相對於其它技術
中使用之流通配置)。
容器105和/或室之適合的尺寸包括，但不限於，具有大於5cm、大於10cm、大於20cm、大於30cm、大於100cm、大於300cm、大於1,000cm、介於10cm與100cm之間、介於100cm與300cm之間、介於100cm與1,000cm之間、介於300cm與1,000cm之間之最小寬度，任何其它能夠均勻或實質上均勻加熱之最小寬度，或其間之任何適合的組合、子組合、範圍或子範圍。
容器105和/或室之適合的體積包括，但不限於，至少1,000cm3、大於3,000cm3、大於5,000cm3、大於10,000cm3、大於20,000cm3、介於3,000cm3與5,000cm3之間、介於5,000cm3與10,000cm3之間、介於5,000cm3與20,000cm3之間、介於10,000cm3與20,000cm3之間，任何其它能夠均勻或實質上均勻加熱之體積，或其間之任何適合的組合、子組合、範圍或子範圍。
在此使用之短語"熱CVD"指的是一或多種氣體在，例如，飢餓(starved)反應器配置中之反應和/或分解，且不同於電漿輔助CVD、自由基引發的CVD和/或觸媒輔助CVD、濺鍍、原子層沈積(其每一周期限於單層分子沈積，相較之下能夠多於一層的分子沈積)和/或磊晶生長(例如，在大於700℃下生長)。
表面103是基材109上之層或基材109本身。在一實施例中，表面103是或包括不鏽鋼表面(馬氏
體或奥氏體)、鎳基合金、金屬表面、含金屬表面(鐵或非鐵的；回火或非回火的；和/或等軸、定向凝固或單晶的)、陶瓷表面、陶瓷基質複合表面、玻璃表面、陶瓷基質複合表面、複合金屬表面、塗覆表面、纖維表面、箔表面、薄膜、聚合物表面(諸如，聚醚醚酮)和/或任何其它能夠耐受熱化學氣相沈積方法100之操作條件之適合的表面。
在一實施例中，表面103是經處理的。適合的處理包括，但不限於，曝露於水(單獨、具零級空氣或具非活性氣體)、氧(例如，至少50重量%之濃度)、空氣(例如，單獨、不是單獨和/或為零級空氣)、一氧化氮、臭氧、過氧化物、高溫或其等之組合。在此使用之術語"零級空氣"意指具有低於0.1ppm之總烴之大氣空氣。術語“空氣”一般意指以重量計，其中大部分為氮，氧為第二高濃度的物種之氣態流體。例如，在一實施例中，氮存在之濃度為至少70重量%(例如，介於75%與76%之間)，氧存在之濃度為至少20重量%(例如，介於23%與24%之間)。
在一實施例中，處理表面103(以及基材105)之高溫高於200℃、高於300℃、高於350℃、高於370℃、高於380℃、高於390℃、高於400℃、高於410℃、高於420℃、高於430℃、高於440℃、高於450℃、介於300℃與450℃之間、介於350℃與450℃之間、介於380℃與450℃之間，或其間之任何適合的組
合、子組合、範圍或子範圍。
在一實施例中，表面103是由矽烷基材料形成，例如，由氫化矽、矽烷、二甲基矽烷(例如，氣態形式)、三甲基矽烷、非燃物種(例如，二烷基甲矽烷基二氫化物和/或烷基甲矽烷基三氫化物)、熱反應材料(例如，碳矽烷和/或羧基矽烷，諸如非晶形碳矽烷和/或非晶形羧矽烷)、能夠重組碳甲矽烷基之物種(二甲矽烷基或三甲矽烷基片段)和/或任何其它適合的矽烷基材料形成。額外地或選擇性地，在一實施例中，表面103是由熱反應材料，諸如氫化矽、氮化矽、乙烯或其等之組合形成。此等矽烷基材料和/或熱反應材料能夠迭代地施用和/或於其間加上例如用非活性氣體(諸如，氮、氦和/或氬，作為分壓稀釋劑)淨化。
在一實施例中，用於施塗熱CVD塗層101之一或多種氣體之反應(步驟102)，包括使用選自於由下列所構成之群組之氣體：矽烷、氫化矽、二甲基矽烷(例如，氣態形式)、三甲基矽烷、二烷基甲矽烷基二氫化物、烷基甲矽烷基三氫化物、非自燃物種(例如，二烷基甲矽烷基二氫化物/或烷基甲矽烷基三氫化物)、熱反應材料(例如，碳矽氧和/或羧基矽烷，諸如非晶形碳矽烷和/或非晶形羧基矽烷)、能夠重組碳甲矽烷基之物種(二甲矽烷基或三甲矽烷基片段)、甲基三甲氧矽烷、甲基三乙氧矽烷、二甲基二甲氧矽烷、二甲基二乙氧矽烷、三甲基甲氧矽烷、三甲基乙氧矽烷、一或多種含氮物種(例如，
氨、氮、肼、三甲矽烷基胺(亦稱作TSA；矽烷胺；N,N-二甲矽烷基-二矽氮烷；2-甲矽烷基-；矽烷、次氮基三；或3SA)、雙(叔-丁基胺)矽烷、1,2-雙(二甲基胺基)四甲基二矽烷和/或二氯矽烷、六氯二矽烷)以及其等之組合。在需引入超過一種物種之實施例中，該等物種可同時(預混合或現場混合)或依序(先引入其中一種物種)引入。
在一實施例中，在該反應(步驟102)中所使用之一或多種氣體，是包括熱反應氣體與非活性氣體之氣態混合物之一部分。該熱反應氣體之適合的濃度，以體積計，介於10%與20%之間、介於10%與15%之間、介於12%與14%之間、介於10%與100%之間、介於30%與70%之間、介於500%與80%之間、介於70%與100%之間、介於80%與90%之間、介於84%與86%，或其間之任何適合的組合、子組合、範圍或子範圍。
該氣體之適合的分壓介於10托與150托之間、介於10托與30托之間、介於20托與40托之間、介於30托與50托之間、介於60托與80托之間、介於50托與100托之間、介於50托與150托之間、介於100托與150托之間、小於150托、小於100托、小於50托、小於30托，或其間之任何適合的組合、子組合、範圍或子範圍。
在一實施例中，透過控制流量引入該一或多種氣體至容器105和/或該室中，達到限制擴散速率之熱化學氣相沈積。此控制可透過任何適合的技術和/或配置，例如，透過流量限制器(諸如，墊圈從20微米收縮至
5微米、從20微米至10微米、從10微米至5微米，或其間之任何適合的組合、子組合、範圍或子範圍)、質量流量控制器、脈衝、閥、燒結墊片、限流器或其等之組合。
在另一實施例中，控制/調整壓力和/或溫度，以達到限制擴散速率之熱化學氣相沈積。該一或多種氣體之反應(步驟102)是在使該氣體熱反應以及促進沈積至表面103上之溫度範圍內進行。適合的溫度包括，但不限於，介於100℃與700℃之間、介於100℃與450℃之間、介於100℃與300℃之間、介於200℃與500℃之間、介於300℃與600℃之間、介於450℃與700℃、700℃、450℃、100℃、介於200℃與600℃之間、介於300℃與600℃之間、介於400℃與500℃之間、300℃、400℃、500℃、600℃，或其間之任何適合的組合、子組合、範圍或子範圍。
該一或多種氣體之反應(步驟102)是在促進該熱反應之壓力範圍內進行。適合的壓力包括，但不限於，介於0.01psia與200psia之間、介於1.0psia與100psia之間、介於5psia與40psia之間、介於20psia與25psia之間、1.0psia、5psia、20psia、23psia、25psia、40psia、100psia、200psia，或其間之任何適合的組合、子組合、範圍或子範圍。
該一或多種氣體之反應(步驟102)是在促進期望的表面103覆蓋所需之時間內進行。適合的期間包括，但不限於，至少2個小時、至少3個小時、至少4個小
時、至少5個小時、至少7個小時、介於4與10個小時之間、介於6與8個小時之間，或其間之任何適合的組合、子組合、範圍或子範圍。
根據本發明，與限制反應速率之熱CVD相反，經熱CVD方法100塗覆之物件107具有經由限制擴散速率之熱CVD所產生之特性。透過限制擴散速率之熱CVD能夠產生的特性包括，但不限於，可與經由限制反應速率之熱CVD所產生之薄膜密度區別之薄膜密度、可與經由限制反應速率之熱CVD所產生的區別之厚度、可與經由限制反應速率之熱CVD所產生的區別之在一定厚度以上之耐剝落性、比經由限制反應速率之熱CVD所產生的窄之波長範圍、與經由限制反應速率之熱CVD所產生的不同之波長、可與經由限制反應速率之熱CVD所產生之電子阻抗光譜測量值區別之電子阻抗光譜測量值、與經由限制反應速率之熱CVD所產生的不同之微結構(例如，主要是非晶形的、實質上完全非晶形的或完全非晶形的)，或其等之組合。
在一實施例中，該限制擴散速率之熱CVD施塗該熱CVD塗層101之厚度範圍在一適合的範圍113內，該範圍113取決於第一厚度111與第二厚度115間之差距，其等個別和/或共同抵抗剝落。適合的範圍包括，但不限於，1,000埃、500埃、300埃、200埃、150埃、100埃、80埃、50埃或其間之任何適合的組合、子組合、範圍或子範圍。
在一些具體例中，該限制擴散速率之熱CVD施塗該熱CVD塗層101之第一厚度111和/或第二厚度113之厚度介在5,000埃與30,000埃之間、介在5,000埃與20,000埃之間、介在5,000埃與10,000埃之間、介在10,000埃與20,000埃之間、介在10,000埃與15,000埃之間、介在15,000埃與20,000埃之間、8,000埃、12,000埃、16,000埃、19,000埃，或其間之任何適合的組合、子組合、範圍或子範圍。
在一實施例中，該限制擴散速率之熱CVD施塗該熱CVD塗層101，以便具有一波長範圍小於10nm、小於20nm、小於30nm、小於40nm、小於50nm、小於100nm或其間之任何適合的組合、子組合、範圍或子範圍。受該波長範圍的限制之適合的波長包括，但不限於，400nm、450nm、500nm、550nm、600nm、650nm、700nm或其間之任何適合的組合、子組合、範圍或子範圍。
雖然無意受理論之約束，但在一實施例中，該限制擴散速率之熱CVD是建立在至表面之通量(J1)、反應通量(J2)、氣體濃度(Cg)、在該表面上之濃度(Cs)、氣相傳質係數(hg)以及表面反應速率(ks)上。在另一實施例中，關係由以下方程式表示：
根據此實施例，該氣相傳質係數(hg)遠小於表面反應速率(ks)，產生限制擴散速率之熱CVD。例如，在甚至又另一實施例中，該氣相傳質係數(hg)小於該表面反應速率(ks)至少100倍、200倍、300倍、400倍、500倍、600倍、700倍、800倍、900倍、1,000倍或其間之任何適合的組合、子組合、範圍或子範圍。
雖然參考一或多個實施例說明本發明，但是熟悉此技藝人士應理解，在不逸離本發明之範疇的情況下，可以進行各種改變並且可以用等同物替換其元件。此外，可在不逸離本發明的基本範圍的情況下進行許多修改，以便使特別的情況或材料適應本發明之教示。因此，本發明不限於作為實施本發明的最佳模式揭露的特定實施例，而是本發明將包括落在所附申請專利範圍之範疇內的所有實施例。此外，在詳細描述中識別的所有數值，應當被解釋為如同明確地識別精確和近似值二者。
100‧‧‧熱化學氣相沈積方法
101‧‧‧熱CVD塗層
102‧‧‧步驟
103‧‧‧表面
105‧‧‧容器
107‧‧‧物件
109‧‧‧基材
111‧‧‧第一厚度
113‧‧‧範圍
115‧‧‧第二厚度
Claims (19)
- 一種具一致的表面塗層之物件，其包含：一基材；以及在該基材上之一熱化學氣相沈積塗層；其中該熱化學氣相沈積塗層包括經由限制擴散速率之熱化學氣相沈積產生之特性；且其中該限制擴散速率之熱化學氣相沈積是建立在至表面之通量(J1)、反應通量(J2)、氣體濃度(Cg)、在該表面上之濃度(Cs)、氣相傳質係數(hg)以及表面反應速率(ks)上，關係由以下方程式表示：
- 如請求項1之物件，其中該特性包括一薄膜密度。
- 如請求項1之物件，其中該特性包括1,000埃或更小之一厚度差距範圍。
- 如請求項1之物件，其中該熱化學氣相沈積塗層具有大於8,000埃之一厚度且沒有剝落。
- 如請求項1之物件，其中該熱化學氣相沈 積塗層具有大於12,000埃之一厚度且沒有剝落。
- 如請求項1之物件，其中該熱化學氣相沈積塗層具有大於16,000埃之一厚度且沒有剝落。
- 如請求項1之物件，其中該熱化學氣相沈積塗層具有大於19,000埃之一厚度且沒有剝落。
- 如請求項1之物件，其中該特性包括可用電子阻抗光譜測量之一阻抗。
- 如請求項1之物件，其中該特性包括一主要是非晶形的結構。
- 如請求項1之物件，其中該特性包括一實質上完全非晶形的結構。
- 如請求項1之物件，其中該特性包括不是單層生長之生長。
- 如請求項1之物件，其中該特性包括沒有珠點。
- 如請求項1之物件，其中該基材包括金屬。
- 如請求項1之物件，其中該基材包括一金屬合金。
- 如請求項1之物件，其中該基材已經過至少380℃之溫度的處理。
- 如請求項1之物件，其中該基材已經過至少430℃之溫度的處理。
- 如請求項1之物件，其中該基材已經過至 少440℃之溫度的處理。
- 一種熱化學氣相沈積方法，其包含：將一氣態物種引入一容器中；以及經由在熱化學氣相沈積方法中該氣態物種之限制擴散速率反應，在該容器內之一物件上產生一一致的表面塗層。
- 如請求項18之方法，其中該氣態物種是一含矽烷之物種，以體積計，其包括濃度介於10%與20%之間之矽烷以及一非活性氣體。
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|---|---|
| US (1) | US20170211180A1 (zh) |
| EP (1) | EP3196335A1 (zh) |
| JP (1) | JP2017150068A (zh) |
| KR (1) | KR20170088307A (zh) |
| CN (1) | CN107267955A (zh) |
| AU (1) | AU2017200337A1 (zh) |
| SG (1) | SG10201700441SA (zh) |
| TW (1) | TWI772285B (zh) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102018100686A1 (de) * | 2018-01-12 | 2018-03-01 | Peter Lell | Elektrisches Unterbrechungsschaltglied mit Reaktivbeschichtung in der Reaktionskammer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102741452A (zh) * | 2009-10-27 | 2012-10-17 | 西尔科特克公司 | 化学气相沉积涂层、制品和方法 |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4579752A (en) * | 1984-10-29 | 1986-04-01 | At&T Bell Laboratories | Enhanced corrosion resistance of metal surfaces |
| US4792460A (en) * | 1986-07-15 | 1988-12-20 | Electric Power Research Institute, Inc. | Method for production of polysilanes and polygermanes, and deposition of hydrogenated amorphous silicon, alloys thereof, or hydrogenated amorphous germanium |
| US4684542A (en) * | 1986-08-11 | 1987-08-04 | International Business Machines Corporation | Low pressure chemical vapor deposition of tungsten silicide |
| GB2195663B (en) * | 1986-08-15 | 1990-08-22 | Nippon Telegraph & Telephone | Chemical vapour deposition method and apparatus therefor |
| WO1993002468A1 (fr) * | 1991-07-16 | 1993-02-04 | Seiko Epson Corporation | Appareil de deposition en phase vapeur par procede chimique, procede de formation de films semi-conducteurs et procede de production de dispositifs semi-conducteurs a mince film |
| US5299731A (en) * | 1993-02-22 | 1994-04-05 | L'air Liquide | Corrosion resistant welding of stainless steel |
| JPH10321819A (ja) * | 1997-05-22 | 1998-12-04 | Toshiba Corp | 半導体素子の製造方法 |
| JP2001345379A (ja) * | 2000-05-30 | 2001-12-14 | Fujitsu Ltd | 半導体装置およびその製造方法 |
| JP4484185B2 (ja) * | 2000-08-29 | 2010-06-16 | コバレントマテリアル株式会社 | シリコン半導体基板の化学的気相薄膜成長方法 |
| EP1421607A2 (en) * | 2001-02-12 | 2004-05-26 | ASM America, Inc. | Improved process for deposition of semiconductor films |
| US7175713B2 (en) * | 2002-01-25 | 2007-02-13 | Applied Materials, Inc. | Apparatus for cyclical deposition of thin films |
| GB2395492A (en) * | 2002-11-25 | 2004-05-26 | Thermo Electron Corp | Improvements in deposition methods for the production of semiconductors |
| CN101066842A (zh) * | 2007-06-05 | 2007-11-07 | 浙江大学 | 制备非晶氢硅薄膜的方法及装置 |
| WO2014123084A1 (ja) * | 2013-02-07 | 2014-08-14 | ピーエスフォー ルクスコ エスエイアールエル | 半導体装置およびその製造方法 |
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2016
- 2016-01-22 US US15/004,455 patent/US20170211180A1/en not_active Abandoned
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2017
- 2017-01-18 AU AU2017200337A patent/AU2017200337A1/en not_active Abandoned
- 2017-01-19 SG SG10201700441SA patent/SG10201700441SA/en unknown
- 2017-01-20 KR KR1020170009675A patent/KR20170088307A/ko not_active Ceased
- 2017-01-20 EP EP17152489.5A patent/EP3196335A1/en not_active Ceased
- 2017-01-20 TW TW106102096A patent/TWI772285B/zh active
- 2017-01-22 CN CN201710053666.7A patent/CN107267955A/zh active Pending
- 2017-01-23 JP JP2017009186A patent/JP2017150068A/ja active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102741452A (zh) * | 2009-10-27 | 2012-10-17 | 西尔科特克公司 | 化学气相沉积涂层、制品和方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3196335A1 (en) | 2017-07-26 |
| US20170211180A1 (en) | 2017-07-27 |
| AU2017200337A1 (en) | 2017-08-10 |
| KR20170088307A (ko) | 2017-08-01 |
| JP2017150068A (ja) | 2017-08-31 |
| CN107267955A (zh) | 2017-10-20 |
| SG10201700441SA (en) | 2017-08-30 |
| TW201739950A (zh) | 2017-11-16 |
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