TW201817910A - Heater module, thin film deposition apparatus and method - Google Patents
Heater module, thin film deposition apparatus and method Download PDFInfo
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- TW201817910A TW201817910A TW105136954A TW105136954A TW201817910A TW 201817910 A TW201817910 A TW 201817910A TW 105136954 A TW105136954 A TW 105136954A TW 105136954 A TW105136954 A TW 105136954A TW 201817910 A TW201817910 A TW 201817910A
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- 238000000427 thin-film deposition Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims description 61
- 239000010408 film Substances 0.000 claims description 40
- 239000012495 reaction gas Substances 0.000 claims description 37
- 239000002243 precursor Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- 238000000151 deposition Methods 0.000 claims description 13
- 230000008021 deposition Effects 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 8
- 229910052714 tellurium Inorganic materials 0.000 claims description 7
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 7
- 238000007736 thin film deposition technique Methods 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 3
- 238000005755 formation reaction Methods 0.000 claims description 3
- 229910052711 selenium Inorganic materials 0.000 claims description 3
- 239000011669 selenium Substances 0.000 claims description 3
- 150000003623 transition metal compounds Chemical group 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 2
- 238000005424 photoluminescence Methods 0.000 description 7
- 239000012159 carrier gas Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910000410 antimony oxide Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 150000004771 selenides Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910016001 MoSe Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- CXRFFSKFQFGBOT-UHFFFAOYSA-N bis(selanylidene)niobium Chemical compound [Se]=[Nb]=[Se] CXRFFSKFQFGBOT-UHFFFAOYSA-N 0.000 description 1
- USWJSZNKYVUTIE-UHFFFAOYSA-N bis(sulfanylidene)rhenium Chemical compound S=[Re]=S USWJSZNKYVUTIE-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 150000001787 chalcogens Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- OMEPJWROJCQMMU-UHFFFAOYSA-N selanylidenebismuth;selenium Chemical compound [Se].[Bi]=[Se].[Bi]=[Se] OMEPJWROJCQMMU-UHFFFAOYSA-N 0.000 description 1
- NYPFJVOIAWPAAV-UHFFFAOYSA-N sulfanylideneniobium Chemical compound [Nb]=S NYPFJVOIAWPAAV-UHFFFAOYSA-N 0.000 description 1
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
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- Chemical Vapour Deposition (AREA)
Abstract
Description
本發明是關於一種加熱器模組,特別是關於一種使用加熱器模組製備高品質薄膜的薄膜沉積裝置及方法。 The present invention relates to a heater module, and more particularly to a thin film deposition apparatus and method for preparing a high quality film using a heater module.
化學氣相沉積(Chemical Vapor Deposition,CVD)裝置可分為熱壁式(hot-wall)沉積裝置及冷壁式(cold-wall)沉積裝置。由於冷壁式沉積裝置可藉由沉積時間的改變而調控薄膜成長的層數,且具有膜厚均勻性佳等優點,故相較於熱壁式沉積裝置更適合用來製備奈米尺度的二維層狀材料。然而,傳統的冷壁式沉積裝置僅對基板進行加熱,故不同管路的反應氣體需到達基板表面才有足夠的熱源進行化學反應。由於薄膜成長前的化學反應是影響薄膜品質的重要因素,因而於薄膜成長前,不同管路的反應氣體需維持於高溫狀態,以便進行充分的化學反應,進而提升沉積薄膜的品質。 Chemical Vapor Deposition (CVD) devices can be classified into hot-wall deposition devices and cold-wall deposition devices. Since the cold wall type deposition apparatus can adjust the number of layers of film growth by the change of deposition time, and has the advantages of good film thickness uniformity, it is more suitable for preparing the nanometer scale than the hot wall type deposition apparatus. Dimensional layered material. However, the conventional cold wall deposition apparatus only heats the substrate, so that the reaction gases of different pipelines need to reach the surface of the substrate to have sufficient heat source for chemical reaction. Since the chemical reaction before the film growth is an important factor affecting the quality of the film, the reaction gas of different pipelines needs to be maintained at a high temperature before the film grows, so as to carry out a sufficient chemical reaction, thereby improving the quality of the deposited film.
因此,如何提供一種加熱器模組,以提升沉積薄膜的品質,實為當前重要的課題之一。 Therefore, how to provide a heater module to improve the quality of deposited films is one of the most important issues at present.
有鑑於此,本發明之目的為提供一種加熱器模組、薄膜沉積裝置及方法,以提升沉積薄膜的品質。 In view of the above, an object of the present invention is to provide a heater module, a thin film deposition apparatus and a method for improving the quality of a deposited film.
為達上述目的,本發明提供一種加熱器模組,應用於一薄膜沉積裝置。加熱器模組包括一氣體混合室、一反應室以及一加熱器。氣體混合室包括至少一氣體分散板及一擋板,擋板設置於氣體分散板上方。反應室設置於氣體混合室下游,並與氣體混合室相連通。加熱器鄰設於氣體混合室。 To achieve the above object, the present invention provides a heater module for use in a thin film deposition apparatus. The heater module includes a gas mixing chamber, a reaction chamber, and a heater. The gas mixing chamber includes at least one gas dispersion plate and a baffle disposed above the gas dispersion plate. The reaction chamber is disposed downstream of the gas mixing chamber and is in communication with the gas mixing chamber. The heater is adjacent to the gas mixing chamber.
在一實施例中,氣體混合室更包括複數個進氣通道。 In an embodiment, the gas mixing chamber further includes a plurality of intake passages.
在一實施例中,氣體分散板具有複數個通孔。 In an embodiment, the gas dispersion plate has a plurality of through holes.
在一實施例中,加熱器是選自燈泡、燈管、加熱線圈其中之一或其組合。 In an embodiment, the heater is one selected from the group consisting of a bulb, a tube, a heating coil, or a combination thereof.
在一實施例中,擋板為石英板。 In an embodiment, the baffle is a quartz plate.
為達上述目的,本發明提供一種薄膜沉積裝置包括一製程腔室以及至少一氣體供應管路。製程腔室包括一基座及一前述的加熱器模組。至少一氣體供應管路與加熱器模組相連接。 To achieve the above object, the present invention provides a thin film deposition apparatus including a process chamber and at least one gas supply line. The process chamber includes a base and a heater module as described above. At least one gas supply line is connected to the heater module.
在一實施例中,薄膜沉積裝置為冷壁式化學氣相沉積裝置。 In one embodiment, the thin film deposition apparatus is a cold wall type chemical vapor deposition apparatus.
為達上述目的,本發明提供一種薄膜沉積方法,包括以下步驟:加熱一基板至一反應溫度;提供一第一反應氣體及一第二反應氣體;隔絕第一反應氣體及第二反應氣體;使第一反應氣體及第二反應氣體保持於一預熱溫度;於預熱溫度下,混合第一反應氣體及第二反應氣體以進行成膜反應;以及於基板上沉積一薄膜。 In order to achieve the above object, the present invention provides a thin film deposition method comprising the steps of: heating a substrate to a reaction temperature; providing a first reaction gas and a second reaction gas; isolating the first reaction gas and the second reaction gas; The first reaction gas and the second reaction gas are maintained at a preheating temperature; at the preheating temperature, the first reaction gas and the second reaction gas are mixed to perform a film formation reaction; and a film is deposited on the substrate.
在一實施例中,提供第一反應氣體及第二反應氣體的步驟更包括:加熱一第一前驅物至一第一溫度,以產生第一反應氣體;以及加熱一第二前驅物至一第二溫度,以產生第二反應氣體。 In one embodiment, the step of providing the first reactive gas and the second reactive gas further comprises: heating a first precursor to a first temperature to generate a first reactive gas; and heating a second precursor to a first Two temperatures to produce a second reactive gas.
在一實施例中,預熱溫度為500~800℃。 In one embodiment, the preheat temperature is between 500 and 800 °C.
在一實施例中,第一前驅物是選自過渡金屬化合物。 In an embodiment, the first precursor is selected from the group consisting of transition metal compounds.
在一實施例中,第二前驅物是選自硫、硒、碲等硫族元素其中之一。 In one embodiment, the second precursor is one selected from the group consisting of sulfur, selenium, tellurium and the like.
承上所述,本發明藉由在薄膜沉積裝置中增設加熱器模組,使第一反應氣體及第二反應氣體在混合前先進行預熱的步驟,並確保第一反應氣體及第二反應氣體可於高溫狀態下進行混合反應,以使薄膜成長前的化學反應更完全,改善了習知技術中只對基板加熱的缺點,故本發明的加熱器模組、薄膜沉積裝置及方法可達成製備高品質薄膜的功效。 As described above, the present invention provides a step of preheating the first reaction gas and the second reaction gas before mixing, by adding a heater module to the thin film deposition apparatus, and ensuring the first reaction gas and the second reaction. The gas can be mixed at a high temperature to complete the chemical reaction before the film grows, and the disadvantages of heating only the substrate in the prior art are improved, so the heater module, the film deposition device and the method of the present invention can be achieved. The efficacy of preparing high quality films.
1‧‧‧第一前驅物 1‧‧‧First Precursor
1a‧‧‧第一反應氣體 1a‧‧‧First reaction gas
2‧‧‧第二前驅物 2‧‧‧Second precursor
2a‧‧‧第二反應氣體 2a‧‧‧second reaction gas
3‧‧‧製程腔室 3‧‧‧Processing chamber
4‧‧‧基座 4‧‧‧Base
5‧‧‧基板 5‧‧‧Substrate
6‧‧‧第二加熱源 6‧‧‧second heating source
7‧‧‧第一加熱源 7‧‧‧First heating source
8‧‧‧第一載流氣體 8‧‧‧First carrier gas
9‧‧‧第二載流氣體 9‧‧‧Second carrier gas
10a‧‧‧第二氣體供應管路 10a‧‧‧Second gas supply line
10b‧‧‧第一氣體供應管路 10b‧‧‧First gas supply line
11‧‧‧加熱器模組 11‧‧‧heater module
100‧‧‧薄膜沉積裝置 100‧‧‧film deposition apparatus
111‧‧‧反應室 111‧‧‧Reaction room
112‧‧‧氣體分散板 112‧‧‧ gas dispersion board
113‧‧‧氣體混合室 113‧‧‧Gas mixing room
114‧‧‧擋板 114‧‧‧Baffle
115‧‧‧加熱器 115‧‧‧heater
1121‧‧‧通孔 1121‧‧‧through hole
1131、1132、1133、1134‧‧‧進氣通道 Insulated passages 1131, 1132, 1133, 1134‧‧
S10~S15‧‧‧方法步驟 S10~S15‧‧‧ method steps
G‧‧‧氣體 G‧‧‧ gas
圖1為本發明一實施例中薄膜沉積裝置的示意圖。 1 is a schematic view of a thin film deposition apparatus in accordance with an embodiment of the present invention.
圖2A為本發明一實施例中加熱器模組的側視圖。 2A is a side elevational view of a heater module in accordance with an embodiment of the present invention.
圖2B至圖2F為圖2A中各元件的俯視圖。 2B to 2F are top views of the components of Fig. 2A.
圖3為本發明一實施例中成長MoS2薄膜的溫度與時間關係圖。 3 is a graph showing temperature versus time of a grown MoS 2 film in accordance with an embodiment of the present invention.
圖4為本發明一實施例中MoS2薄膜的拉曼光譜圖。 4 is a Raman spectrum diagram of a MoS 2 film according to an embodiment of the present invention.
圖5A為本發明一實施例中於MoS2薄膜上不同量測位置的示意圖。 FIG. 5A is a schematic diagram of different measurement positions on a MoS 2 film according to an embodiment of the invention. FIG.
圖5B為圖5A中各量測位置的光激螢光(PL)光譜圖。 Fig. 5B is a photoluminescence (PL) spectrum diagram of each measurement position in Fig. 5A.
圖6為本發明一實施例中薄膜沉積方法的流程示意圖。 FIG. 6 is a schematic flow chart of a thin film deposition method according to an embodiment of the present invention.
以下將參照相關圖式,說明依據本發明具體實施例的加熱器模組、薄膜沉積裝置及方法,其中相同的元件將以相同的元件符號加以說明,所附圖式僅為說明用途,並非用於侷限本發明。 Hereinafter, a heater module, a film deposition apparatus, and a method according to an embodiment of the present invention will be described with reference to the accompanying drawings, wherein the same elements will be described with the same reference numerals. This invention is limited.
關於本文中所使用之「連接」的用詞,除了包括元件與元件直接的相連,亦包括元件與元件間接的相連,例如二元件之間可能另包括介質或其他元件。其中,部分已知的元件可能會省略以避免模糊本發明的概念。 The term "connected" as used herein is used in addition to the direct connection of the elements to the elements, and the indirect connection of the elements to the elements. For example, a medium or other element may be included between the two elements. Some of the known elements may be omitted to avoid obscuring the concepts of the present invention.
圖1為本發明一實施例中薄膜沉積裝置的示意圖。請參閱圖1所示,本發明提供一種薄膜沉積裝置100,包括一製程腔室3、一第一氣體供應管路10b以及一第二氣體供應管路10a。製程腔室3包括一基座4及一加熱器模組11。基座4可隨製程需要升降以調整基板5與加熱器模組11之距離,第一氣體供應管路10b及第二氣體供應管路10a分別與加熱器模組11相連接,其中薄膜沉積裝置100可以是冷壁式化學氣相沉積裝置。此外,第一氣體供應管路10b及第二氣體供應管路10a的周圍設置有一第一加熱源7,以對第一前驅物1及第二前驅物2進行加熱。基座4可承載一基板5,並設置有一第二加熱源6,以對基板5進行加熱。 1 is a schematic view of a thin film deposition apparatus in accordance with an embodiment of the present invention. Referring to FIG. 1, the present invention provides a thin film deposition apparatus 100 including a process chamber 3, a first gas supply line 10b, and a second gas supply line 10a. The process chamber 3 includes a base 4 and a heater module 11. The susceptor 4 can be lifted and lowered according to the process to adjust the distance between the substrate 5 and the heater module 11. The first gas supply line 10b and the second gas supply line 10a are respectively connected to the heater module 11, wherein the thin film deposition device 100 may be a cold wall type chemical vapor deposition apparatus. Further, a first heating source 7 is disposed around the first gas supply line 10b and the second gas supply line 10a to heat the first precursor 1 and the second precursor 2. The susceptor 4 can carry a substrate 5 and is provided with a second heating source 6 for heating the substrate 5.
圖2A為本發明一實施例中加熱器模組的側視圖。請參閱圖2A所示,本發明提供一種加熱器模組11,可裝設於圖1的薄膜沉積裝置100內。加熱器模組11包括一氣體混合室113、一反應室111以及一加熱器115。氣體混合室113包括至少一氣體分散板112及一擋板114。圖2B至2F為圖2A中各元件的俯視圖。請參閱圖2A至2F所示,氣體混合室113 可包括複數個進氣通道(1131、1132、1133、1134),以供不同管路的氣體進氣,而氣體分散板112具有複數個通孔1121,可均勻分散進入反應室的氣體。圖2D所繪示的4個進氣通道(1131、1132、1133、1134)僅為示意圖,本發明並未限制進氣通道的數量。 2A is a side elevational view of a heater module in accordance with an embodiment of the present invention. Referring to FIG. 2A, the present invention provides a heater module 11 that can be mounted in the thin film deposition apparatus 100 of FIG. The heater module 11 includes a gas mixing chamber 113, a reaction chamber 111, and a heater 115. The gas mixing chamber 113 includes at least one gas dispersion plate 112 and a baffle 114. 2B to 2F are top views of the components of Fig. 2A. Referring to FIGS. 2A to 2F, the gas mixing chamber 113 may include a plurality of intake passages (1131, 1132, 1133, 1134) for gas intake of different pipelines, and the gas dispersion plate 112 has a plurality of through holes. 1121, the gas entering the reaction chamber can be uniformly dispersed. The four intake passages (1131, 1132, 1133, 1134) illustrated in FIG. 2D are only schematic views, and the present invention does not limit the number of intake passages.
承上所述,本實施例中的反應室111是由石英管所構成,並設置於氣體混合室113下游。反應室111的上端與氣體混合室113相連通,而反應室111的下端可直接架設於薄膜沉積裝置100內的製程腔室3上,故基板5可隔絕於反應室111內。此外,加熱器115鄰設於氣體混合室113,以使氣體混合室113保持於高溫狀態。於本實施例中,加熱器115設置於氣體混合室113上方僅為舉例說明,加熱器115亦可設置於氣體混合室113兩側或設置於氣體混合室113周圍的任何地方。擋板114設置於氣體分散板112上方,可隔離加熱器115與氣體混合室113內的反應氣體,以防止反應氣體吸附於加熱器115表面。本實施例中是採用石英板做為擋板114,因此不會影響加熱器115的熱傳遞,又能夠避免反應氣體汙染加熱器115。 As described above, the reaction chamber 111 in this embodiment is composed of a quartz tube and is disposed downstream of the gas mixing chamber 113. The upper end of the reaction chamber 111 communicates with the gas mixing chamber 113, and the lower end of the reaction chamber 111 can be directly mounted on the processing chamber 3 in the thin film deposition apparatus 100, so that the substrate 5 can be isolated from the reaction chamber 111. Further, the heater 115 is disposed adjacent to the gas mixing chamber 113 to maintain the gas mixing chamber 113 at a high temperature. In the present embodiment, the heater 115 is disposed above the gas mixing chamber 113. For example, the heater 115 may be disposed on both sides of the gas mixing chamber 113 or anywhere around the gas mixing chamber 113. The baffle 114 is disposed above the gas dispersion plate 112 to isolate the reaction gas between the heater 115 and the gas mixing chamber 113 to prevent the reaction gas from being adsorbed on the surface of the heater 115. In the present embodiment, the quartz plate is used as the baffle 114, so that the heat transfer of the heater 115 is not affected, and the reaction gas is prevented from contaminating the heater 115.
於上述實施例中,是以6個燈泡做為加熱器115的熱源,加熱器115亦可選自燈管或加熱線圈,或是燈泡、燈管及加熱線圈的任一組合。此外,加熱器115的操作溫度範圍為50~800℃,較佳為500~800℃,操作溫度的選擇是依據所欲成長的薄膜種類而定。 In the above embodiment, six bulbs are used as the heat source of the heater 115, and the heater 115 may also be selected from a lamp tube or a heating coil, or any combination of a bulb, a tube and a heating coil. Further, the operating temperature range of the heater 115 is 50 to 800 ° C, preferably 500 to 800 ° C, and the operating temperature is selected depending on the type of film to be grown.
圖3為本發明一實施例中成長MoS2薄膜的溫度與時間關係圖。圖6為本發明一實施例中薄膜沉積方法的流程示意圖。請同時參閱圖1、圖2A、圖3及圖6所示,以下將以成長二硫化鉬(MoS2)薄膜為例,說明本發明所提供的薄膜沉積方法。首先,於步驟S10中,將薄膜沉積裝置100內的基板5加熱至約850~950℃的反應溫度,並使製程腔室3保持於約10~30Torr的壓力。於步驟S11中,將一第一前驅物1加熱至約65~75℃的溫度,使第一前驅物1蒸發而形成一第一反應氣體1a,並將一第二前驅物2加熱至約190℃的溫度,使第二前驅物2蒸發而形成一第二反應氣體2a,於此實施例中,第一前驅物1為六羰基鉬(Mo(CO)6),第二前驅物2為硫粉(Sulfur)。 3 is a graph showing temperature versus time of a grown MoS 2 film in accordance with an embodiment of the present invention. FIG. 6 is a schematic flow chart of a thin film deposition method according to an embodiment of the present invention. Referring to FIG. 1 , FIG. 2A , FIG. 3 and FIG. 6 , the film deposition method provided by the present invention will be described below by taking a molybdenum disulfide (MoS 2 ) film as an example. First, in step S10, the substrate 5 in the thin film deposition apparatus 100 is heated to a reaction temperature of about 850 to 950 ° C, and the process chamber 3 is maintained at a pressure of about 10 to 30 Torr. In step S11, a first precursor 1 is heated to a temperature of about 65 to 75 ° C, the first precursor 1 is evaporated to form a first reactive gas 1a, and a second precursor 2 is heated to about 190. The temperature of °C causes the second precursor 2 to evaporate to form a second reaction gas 2a. In this embodiment, the first precursor 1 is hexacarbonyl molybdenum (Mo(CO) 6 ), and the second precursor 2 is sulfur. Powder (Sulfur).
於步驟S12中,分別藉由第一載流氣體8及第二載流氣體9 將第一反應氣體1a及第二反應氣體2a帶入加熱器模組11內,此時可藉由閥門的控制使第一反應氣體1a及第二反應氣體2a相互隔絕,於此實施例中,第一載流氣體8及第二載流氣體9均為氬氣(Ar)。於步驟S13中,以加熱器115為熱源使第一反應氣體1a及第二反應氣體2a保持於約500~800℃的預熱溫度,此過程約持續10分鐘,於此實施例中,較佳的預熱溫度可為650℃、700℃或750℃。於步驟S14中,藉由氬氣將第一反應氣體1a帶至第二反應氣體2a所在位置,並於約500~800℃的溫度下混合第一反應氣體1a及第二反應氣體2a,以便進行後續的成膜反應。於步驟S15中,沉積MoS2薄膜於基板5。 In step S12, the first reactant gas 1a and the second reactant gas 2a are brought into the heater module 11 by the first carrier gas 8 and the second carrier gas 9, respectively, and can be controlled by the valve at this time. The first reaction gas 1a and the second reaction gas 2a are isolated from each other. In this embodiment, the first carrier gas 8 and the second carrier gas 9 are both argon (Ar). In step S13, the first reaction gas 1a and the second reaction gas 2a are maintained at a preheating temperature of about 500 to 800 ° C by using the heater 115 as a heat source. The process lasts for about 10 minutes. In this embodiment, preferably. The preheating temperature can be 650 ° C, 700 ° C or 750 ° C. In step S14, the first reaction gas 1a is brought to the position of the second reaction gas 2a by argon gas, and the first reaction gas 1a and the second reaction gas 2a are mixed at a temperature of about 500 to 800 ° C for the purpose of performing Subsequent film formation reaction. In step S15, a MoS 2 film is deposited on the substrate 5.
承上所述,本發明所提供的薄膜沉積裝置及方法亦可用來製備其他種類的二維層狀硫族化合物。例如:硫化鉬(MoS2)、硒化鉬(MoSe2)、碲化鉬(MoTe2)、硫化鉿(HfS2)、硒化鉿(HfSe2)、碲化鉿(HfTe2)、硫化鎢(WS2)、硒化鎢(WSe2)、碲化鎢(WTe2)、硫化鈮(NbS2)、硒化鈮(NbSe2)、碲化鈮(NbTe2)、硫化錸(ReS2)、硒化錸(ReSe2)、碲化錸(ReTe2)等。其中,第一前驅物可選自過渡金屬化合物,例如是氧化鉬(MoO3)、氧化鎢(WO3)、氧化鈮(Nb2O5)、氧化錸(ReO3)、氧化鉿(HfO2)等過渡金屬氧化物,而第二前驅物可選自硫族元素其中之一或其化合物,硫族元素例如為硫、硒、碲…等等。 As described above, the thin film deposition apparatus and method provided by the present invention can also be used to prepare other kinds of two-dimensional layered chalcogenides. For example: molybdenum sulfide (MoS 2), molybdenum selenide (MoSe 2), tellurium molybdenum (MoTe 2), sulfide, hafnium (HfS 2), selenide hafnium (HfSe 2), tellurium hafnium (HfTe 2), tungsten sulfide (WS 2), selenide, tungsten (WSe 2), tellurium tungsten (WTe 2), niobium sulfide (NbS 2), niobium selenide (NbSe 2), tellurium niobium (NbTe 2), rhenium sulfide (ReS 2) , bismuth selenide (ReSe 2 ), bismuth telluride (ReTe 2 ), and the like. Wherein, the first precursor may be selected from transition metal compounds such as molybdenum oxide (MoO 3 ), tungsten oxide (WO 3 ), niobium oxide (Nb 2 O 5 ), antimony oxide (ReO 3 ), antimony oxide (HfO 2 ) a transition metal oxide, and the second precursor may be selected from one of the chalcogen elements or a compound thereof, such as sulfur, selenium, tellurium, and the like.
圖4為本發明一實施例中MoS2薄膜的拉曼光譜圖。請參閱圖4所示,拉曼光譜中顯示出383.5cm-1及405.6cm-1兩個特徵峰,故可判斷所製備的薄膜為多層結構的MoS2薄膜。 4 is a Raman spectrum diagram of a MoS 2 film according to an embodiment of the present invention. Referring to FIG. 4, two characteristic peaks of 383.5 cm-1 and 405.6 cm-1 are shown in the Raman spectrum, so that the prepared film is a multilayered MoS 2 film.
圖5A為本發明一實施例中於MoS2薄膜上不同量測位置的示意圖。圖5B為圖5A中各量測位置的光激螢光(PL)光譜圖。請同時參閱圖5A-5B所示,本實施例中,是將MoS2薄膜成長於藍寶石(sapphire)基板上,並於MoS2薄膜上任取9個點進行光激螢光(PL)分析。如圖5B所示,MoS2薄膜的PL強度於各量測位置上均遠大於基板的PL強度,故在薄膜沉積裝置中加裝本發明的加熱器模組有助於製備高品質的MoS2薄膜。 FIG. 5A is a schematic diagram of different measurement positions on a MoS 2 film according to an embodiment of the invention. FIG. Fig. 5B is a photoluminescence (PL) spectrum diagram of each measurement position in Fig. 5A. Referring to FIG. 5A-5B at the same time, in this embodiment, the MoS 2 film is grown on a sapphire substrate, and 9 points are taken on the MoS 2 film for photoexcitation fluorescence (PL) analysis. As shown in FIG. 5B, the PL intensity of the MoS 2 film is much larger than the PL intensity of the substrate at each measurement position, so the addition of the heater module of the present invention to the thin film deposition apparatus contributes to the preparation of high quality MoS 2 . film.
綜上所述,本發明藉由在薄膜沉積裝置中增設加熱器模組,使第一反應氣體及第二反應氣體在混合前先進行預熱的步驟,並確保第一 反應氣體及第二反應氣體可於高溫狀態下進行混合反應,以使薄膜成長前的化學反應更完全,改善了習知技術中只對基板加熱的缺點,故本發明的加熱器模組、薄膜沉積裝置及方法可達成製備高品質薄膜的功效。 In summary, the present invention adds a heater module to the thin film deposition apparatus to preheat the first reaction gas and the second reaction gas before mixing, and ensures the first reaction gas and the second reaction. The gas can be mixed at a high temperature to complete the chemical reaction before the film grows, and the disadvantages of heating only the substrate in the prior art are improved, so the heater module, the film deposition device and the method of the present invention can be achieved. The efficacy of preparing high quality films.
上述實施例並非用以限定本發明,任何熟悉此技藝者,在未脫離本發明之精神與範疇內,而對其進行之等效修改或變更,均應包含於後附之申請專利範圍中。 The above-mentioned embodiments are not intended to limit the invention, and any equivalent modifications and variations of the present invention are intended to be included within the scope of the appended claims.
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