TW202342805A - Chemical vapor deposition device and method - Google Patents
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- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 239000010409 thin film Substances 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims description 92
- 238000006243 chemical reaction Methods 0.000 claims description 49
- 239000010408 film Substances 0.000 claims description 38
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 22
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 abstract 2
- 238000000151 deposition Methods 0.000 description 29
- 230000008021 deposition Effects 0.000 description 29
- 238000002474 experimental method Methods 0.000 description 26
- 238000009826 distribution Methods 0.000 description 17
- 239000002994 raw material Substances 0.000 description 11
- 238000010586 diagram Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000012495 reaction gas Substances 0.000 description 8
- 238000000427 thin-film deposition Methods 0.000 description 6
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- AZFVLHQDIIJLJG-UHFFFAOYSA-N chloromethylsilane Chemical compound [SiH3]CCl AZFVLHQDIIJLJG-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 125000003866 trichloromethyl group Chemical group ClC(Cl)(Cl)* 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
Description
本發明是有關於一種化學氣相沉積技術，且特別是有關於一種化學氣相沉積裝置及方法。The present invention relates to a chemical vapor deposition technology, and in particular to a chemical vapor deposition device and method.
以化學氣相沉積法（chemical vapor deposition，CVD）製作的碳化矽（CVD-SiC）憑藉其高純度及本身耐腐蝕、耐磨耗、耐熱衝擊等安定之化學特性，可提供用於半導體製造設備所需的零件耗材，或半導體製程的測試晶片（dummy wafer）之使用。Silicon carbide (CVD-SiC) produced by chemical vapor deposition (CVD) can be used in semiconductor manufacturing equipment due to its high purity and stable chemical properties such as corrosion resistance, wear resistance, and thermal shock resistance. Required parts and consumables, or the use of test wafers (dummy wafers) for semiconductor manufacturing processes.
一般使用化學氣相沉積法在大面積的基材上製做碳化矽薄膜時，常採用可以容納該當基材的反應器，並將其放置在反應器底部，藉由上方的氣體分散噴頭（shower head）將原料氣體導入反應器後加熱至約1000℃~1400℃使原料反應並在基材上形成碳化矽薄膜。這種類型的生產方式大部分都採用固定原料在反應器內的滯留時間，以獲得均勻的薄膜沉積。因此原料實際反應轉化成薄膜的莫耳轉化率一般較低，是目前生產成本過高的主要原因之一。When chemical vapor deposition is generally used to make silicon carbide thin films on large-area substrates, a reactor that can accommodate the substrate is often used, and is placed at the bottom of the reactor, using a gas dispersion nozzle (shower) above. head) introduces the raw material gas into the reactor and heats it to about 1000℃~1400℃ to react the raw material and form a silicon carbide film on the substrate. Most of this type of production methods use a fixed residence time of the feedstock in the reactor to obtain uniform film deposition. Therefore, the molar conversion rate of the actual reaction of raw materials into films is generally low, which is one of the main reasons for the current high production costs.
本發明提供一種化學氣相沉積裝置，透過使反應器中的氣體為對向流動狀態，得以提高原料轉化成薄膜的莫耳轉化率，又能獲得均勻的薄膜沉積。The present invention provides a chemical vapor deposition device, which can improve the molar conversion rate of converting raw materials into thin films by making the gas in the reactor be in a counter-flow state, and achieve uniform thin film deposition.
本發明另提供一種化學氣相沉積方法，透過上述化學氣相沉積裝置進行反應溫度以及氣體在反應器內的滯留時間的調控，得以提高原料轉化成薄膜的莫耳轉化率，又能獲得均勻的薄膜。The present invention also provides a chemical vapor deposition method. By controlling the reaction temperature and the residence time of gas in the reactor through the above chemical vapor deposition device, the molar conversion rate of raw materials into thin films can be improved, and a uniform film can be obtained. film.
本發明的化學氣相沉積裝置包括反應器、氣體供應槽以及抽氣系統，所述反應器為管狀且具有沿著軸向相對設置的第一開口以及第二開口，所述氣體供應槽透過第一控制閥連接所述第一開口，以及透過第二控制閥連接所述第二開口，以提供氣體至所述反應器。所述抽氣系統透過第三控制閥連接所述第二開口，以及透過第四控制閥連接所述第一開口，以將提供至所述反應器中的所述氣體抽出。所述第一控制閥與所述第三控制閥開啟期間，關閉所述第二控制閥與所述第四控制閥，使所述氣體由所述第一開口流入所述反應器並從所述第二開口流出。所述第二控制閥與所述第四控制閥開啟期間，關閉所述第一控制閥與所述第三控制閥，使所述氣體由所述第二開口流入所述反應器並從所述第一開口流出，使得所述反應器中的所述氣體為對向流動狀態。The chemical vapor deposition device of the present invention includes a reactor, a gas supply tank and a gas extraction system. The reactor is tubular and has a first opening and a second opening oppositely arranged along the axial direction. The gas supply tank passes through the third opening. A control valve is connected to the first opening, and a second control valve is connected to the second opening to provide gas to the reactor. The gas extraction system is connected to the second opening through a third control valve and connected to the first opening through a fourth control valve to extract the gas provided into the reactor. While the first control valve and the third control valve are open, the second control valve and the fourth control valve are closed to allow the gas to flow into the reactor from the first opening and from the The second opening flows out. While the second control valve and the fourth control valve are open, the first control valve and the third control valve are closed to allow the gas to flow into the reactor from the second opening and from the The first opening flows out, so that the gas in the reactor is in a counter-flow state.
在本發明的一實施例中，上述反應器的長度與直徑的比例在1~20之間。In an embodiment of the present invention, the ratio of the length to the diameter of the reactor is between 1 and 20.
在本發明的一實施例中，上述化學氣相沉積裝置還包括加熱板，沿著上述反應器的管壁內設置。In an embodiment of the present invention, the chemical vapor deposition device further includes a heating plate, which is disposed along the tube wall of the reactor.
在本發明的一實施例中，上述化學氣相沉積裝置還包括流量控制器，設置於上述氣體供應槽與上述反應器之間，控制上述氣體提供至上述反應器的流量。In one embodiment of the present invention, the chemical vapor deposition device further includes a flow controller disposed between the gas supply tank and the reactor to control the flow rate of the gas supplied to the reactor.
在本發明的一實施例中，上述化學氣相沉積裝置還包括第一壓力感測裝置，設置於上述反應器中，以測量上述反應器內的壓力。In an embodiment of the present invention, the above-mentioned chemical vapor deposition device further includes a first pressure sensing device disposed in the above-mentioned reactor to measure the pressure in the above-mentioned reactor.
在本發明的一實施例中，上述化學氣相沉積裝置還包括第二壓力感測裝置，設置於上述氣體供應槽與上述反應器之間，以測量上述氣體供應槽提供的上述氣體的壓力。In an embodiment of the present invention, the chemical vapor deposition device further includes a second pressure sensing device disposed between the gas supply tank and the reactor to measure the pressure of the gas provided by the gas supply tank.
本發明的化學氣相沉積的方法包括將基板放置於如上述的化學氣相沉積裝置的反應器中，以及由氣體供應槽提供氣體至所述反應器進行反應，以於所述基板上形成薄膜。The chemical vapor deposition method of the present invention includes placing a substrate in a reactor of a chemical vapor deposition device as described above, and providing gas from a gas supply tank to the reactor for reaction to form a thin film on the substrate. .
在本發明的另一實施例中，進行上述反應的方法包括加熱上述反應器。In another embodiment of the present invention, the method of performing the above reaction includes heating the above reactor.
在本發明的另一實施例中，上述薄膜的材料為碳化矽，則加熱上述反應器的溫度為950℃至1050℃之間。In another embodiment of the present invention, the material of the thin film is silicon carbide, and the temperature for heating the reactor is between 950°C and 1050°C.
在本發明的另一實施例中，上述氣體於上述反應器中的滯留時間為0.27至0.50秒之間。In another embodiment of the present invention, the residence time of the gas in the reactor is between 0.27 and 0.50 seconds.
在本發明的另一實施例中，於上述基板上形成上述薄膜後，還包括進行退火製程。In another embodiment of the present invention, after forming the thin film on the substrate, an annealing process is also performed.
在本發明的另一實施例中，進行上述反應的方法包括同時提高上述氣體的流速或增加上述反應器中的壓力。In another embodiment of the present invention, the method for carrying out the above reaction includes simultaneously increasing the flow rate of the above gas or increasing the pressure in the above reactor.
在本發明的另一實施例中，上述薄膜的材料為碳化矽，則上述反應器中的壓力為1~30 Torr。In another embodiment of the present invention, the material of the film is silicon carbide, and the pressure in the reactor is 1 to 30 Torr.
在本發明的另一實施例中，上述薄膜的材料為碳化矽，則上述氣體包括三氯甲基矽烷、氫氣以及氬氣，且所述氫氣對三氯甲基矽烷的流量比為6.4:1至30:1之間。In another embodiment of the present invention, the material of the above-mentioned film is silicon carbide, the above-mentioned gases include trichloromethylsilane, hydrogen and argon, and the flow ratio of the hydrogen to trichloromethylsilane is 6.4:1 to 30:1.
基於上述，本發明的化學氣相沉積裝置透過反應器中的氣體為對向流動狀態，提高原料轉化成薄膜的莫耳轉化率，並獲得均勻的薄膜沉積。此外，本發明的化學氣相沉積方法透過上述化學氣相沉積裝置進行反應溫度以及氣體在反應器內滯留時間的調控，來提高原料轉化成薄膜的莫耳轉化率，並獲得均勻的薄膜沉積。Based on the above, the gas in the chemical vapor deposition device of the present invention is in a counter-flow state through the reactor, which improves the molar conversion rate of converting raw materials into thin films and obtains uniform thin film deposition. In addition, the chemical vapor deposition method of the present invention uses the above-mentioned chemical vapor deposition device to control the reaction temperature and the gas residence time in the reactor to improve the molar conversion rate of raw materials into thin films and obtain uniform thin film deposition.
為讓本發明的上述特徵和優點能更明顯易懂，下文特舉實施例，並配合所附圖式做詳細說明如下。In order to make the above-mentioned features and advantages of the present invention more obvious and easy to understand, embodiments are given below and described in detail with reference to the accompanying drawings.
以下內容提供許多不同的實施方式或實施例，用於實施本發明的不同特徵。而且，這些實施例僅為示範例，並不用來限制本發明的範圍與應用。再者，為了清楚起見，各區域或結構元件的相對尺寸（如長度、厚度、間距等）及相對位置可能縮小或放大。另外，在各圖式中使用相似或相同的元件符號表示相似或相同元件或特徵。The following provides many different implementations or examples for implementing different features of the invention. Moreover, these embodiments are only exemplary examples and are not intended to limit the scope and application of the present invention. Furthermore, the relative dimensions (such as length, thickness, spacing, etc.) and relative positions of various regions or structural elements may be reduced or exaggerated for clarity. In addition, similar or identical reference symbols are used in the various drawings to represent similar or identical elements or features.
圖1是依照本發明一實施例的一種化學氣相沉積裝置的示意圖，圖2是圖1中的反應器的放大示意圖。FIG. 1 is a schematic diagram of a chemical vapor deposition device according to an embodiment of the present invention, and FIG. 2 is an enlarged schematic diagram of the reactor in FIG. 1 .
請參考圖1及圖2，化學氣相沉積裝置100包括反應器110、氣體供應槽120以及抽氣系統130。反應器110為管狀且具有沿著軸向相對設置的第一開口111以及第二開口112。氣體供應槽120透過第一控制閥101連接第一開口111，以及透過第二控制閥102連接第二開口112，以提供氣體至反應器110。抽氣系統130透過第三控制閥103連接第二開口112，以及透過第四控制閥104連接第一開口111，以將提供至反應器110中的氣體抽出，其中第一控制閥101與第三控制閥103開啟期間，關閉第二控制閥102與第四控制閥104，使氣體由第一開口111流入反應器110並從第二開口112流出，其中第二控制閥102與第四控制閥104開啟期間，關閉第一控制閥101與第三控制閥103，使氣體由第二開口112流入反應器110並從第一開口111流出，使得反應器110中的氣體為對向流動狀態。Referring to FIGS. 1 and 2 , the chemical vapor deposition apparatus 100 includes a
請參考圖2，反應器110的長度L與直徑R的比例在1~20之間。在一實施例中，反應器110的直徑R為2.2公分，長度L為30公分，長度L與直徑R的比例為約13.6，然而，本發明並不限於此，反應器110的直徑R與長度L可依比例放大，惟反應器110內薄膜沉積場域的表面積對體積比在1.8~10 cm
-1之間。
Please refer to Figure 2. The ratio of the length L to the diameter R of the
化學氣相沉積裝置100還包括加熱板160（如圖2所示），沿著反應器110的管壁內設置，在一實施例中，環狀加熱板160設置於反應器110的內管壁，以均勻地加熱反應器110。The chemical vapor deposition apparatus 100 further includes a heating plate 160 (as shown in FIG. 2 ), which is disposed along the inner tube wall of the
請繼續參考圖1，化學氣相沉積裝置100還包括多個流量控制器140，設置於氣體供應槽120與反應器110之間，控制氣體提供至反應器110的流量。在一實施例中，氣體供應槽120包括反應氣體槽，如三氯甲基矽烷供應槽121、氫氣氣體供應槽122以及氬氣氣體供應槽123，其中三氯甲基矽烷供應槽121例如三氯甲基矽烷（MTS）的蒸氣供給之蒸發罐（bubbler），而氬氣氣體供應槽123是用作載氣來帶出蒸發罐內的三氯甲基矽烷蒸氣，及用以調節反應氣體的濃度或流量。然而，本發明並不限於此，氣體供應槽120可包括供應其他化學氣相沉積的反應氣體，且氬氣氣體供應槽123可以改為供應其他的惰性氣體。在一實施例中，數個流量控制器140分別設置於氫氣氣體供應槽122與反應器110之間、氬氣氣體供應槽123與反應器110之間以及氬氣氣體供應槽123與三氯甲基矽烷供應槽121之間，用以控制氫氣以及氬氣提供至反應器110中的流量。Please continue to refer to FIG. 1 . The chemical vapor deposition apparatus 100 further includes a plurality of flow controllers 140 , which are disposed between the gas supply tank 120 and the
化學氣相沉積裝置100還包括第一壓力感測裝置151以及第二壓力感測裝置152。第一壓力感測裝置151設置於反應器110中，以測量反應器110內的壓力。第二壓力感測裝置152設置於三氯甲基矽烷供應槽121與反應器110之間，以測量三氯甲基矽烷供應槽121的出口氣體壓力，藉此計算出被氬氣帶出來的三氯甲基矽烷蒸氣的流量。在一實施例中，第二壓力感測裝置152控制為400毫米汞柱，其中三氯甲基矽烷（MTS）的分壓最大值為167毫米汞柱（即三氯甲基矽烷供應槽121保持在25℃恆溫下的三氯甲基矽烷（MTS）飽和蒸汽壓），而流經三氯甲基矽烷供應槽121的氬氣分壓為233毫米汞柱。此時流經三氯甲基矽烷供應槽121的氬氣流量由流量控制器140讀得為每分鐘8.8標準毫升，依分配比例可計算得到三氯甲基矽烷供應槽121所提供的三氯甲基矽烷氣體流量為每分鐘2.6標準毫升。若與氫氣氣體供應槽122提供的氫氣流量為每分鐘16.8標準毫升相比時，可得氫氣對三氯甲基矽烷的流量比為6.4:1。The chemical vapor deposition apparatus 100 further includes a first pressure sensing device 151 and a second pressure sensing device 152 . The first pressure sensing device 151 is disposed in the
化學氣相沉積的方法，包括將基板200（如圖2所示）放置於如上述的化學氣相沉積裝置100的反應器110中，以及由氣體供應槽120提供氣體至反應器110進行反應，以於基板200上形成薄膜。在一實施例中，進行反應的方法包括藉由加熱板160對通入反應器110的氣體進行加熱，並且於基板200上形成薄膜後，還包括進行退火製程，以進一步改善薄膜的品質。反應氣體在反應器110內的滯留時間若是太短或太長皆可能會影響薄膜的均勻度，所以在一實施例中，氣體於反應器110中的滯留時間為0.27至0.50秒之間，但本發明並不限於此。在另一實施例中，在進行反應時藉由提高加熱板160的溫度同時縮短氣體於反應器110的滯留時間，可提高原料轉化成薄膜的莫耳轉化率，也可保持薄膜厚度分布的均勻度。The chemical vapor deposition method includes placing the substrate 200 (as shown in FIG. 2 ) in the
下文將藉由實驗來更具體地描述本發明的特徵。雖然描述了以下實驗，但是在不逾越本發明範疇之情況下，可適當地改變所用材料、其量及比率、處理細節以及處理流程等等。因此，不應由下文所述之實驗對本發明作出限制性地解釋。 ＜實驗1＞ The features of the present invention will be described in more detail below through experiments. Although the following experiments are described, the materials used, their amounts and ratios, processing details, processing procedures, etc. may be appropriately changed without exceeding the scope of the present invention. Therefore, the present invention should not be interpreted restrictively from the experiments described below. ＜Experiment 1＞
將基板200放置於如圖1所示的化學氣相沉積裝置100的反應器110中，反應器110的直徑R為2.2公分且總長度L為40公分，由氣體供應槽120提供三氯甲基矽烷、氫氣以及氬氣至反應器110進行反應，以於基板200上形成碳化矽薄膜，其中反應氣體氫氣對三氯甲基矽烷的流量比（H
2:MTS）固定為6.4:1，且反應器110內總壓力保持在13 Torr，藉由加熱板160加熱反應器110分別至900℃、950℃、1000℃以及1050℃，經由伸入熱電偶測量反應器110內的溫度分布，其結果示於圖3。圖3中的反應氣體滯留時間為對照圖2在反應器110中的滯留時間位置，滯留時間為0.0秒時的位置為反應器110中距離第一開口111為5 cm處，滯留時間為0.5秒時的位置為反應器110中距離第一開口111為35 cm處，亦即基板200的兩端分別位於距離第一開口111為5 cm處以及35 cm處。
The
從圖3的內容可知，溫度為900℃~1050℃時，除了靠近第一開口111的位置以及遠離第一開口111的位置約35至40公分處（相當於第二開口112的位置）具有較大的溫度變化，反應氣流在進入反應器110後的5公分以後到35公分之間的30公分區域內，在反應器110中間的位置其溫度變化趨近穩定，視為均溫區域。藉由對三氯甲基矽烷在氫氣下的薄膜沉積動力得知，原料氣體三氯甲基矽烷的分解反應乃依循連續反應（consecutive reactions）模式，即在氣相中隨滯留時間的增加，三氯甲基矽烷會進行一系列脫除氯原子基的分解反應，並貢獻到碳化矽的薄膜沉積。因此在反應器110的均溫區域內薄膜沉積速率呈現先上升後下降的趨勢，即具有一波峰的薄膜沉積分布。
＜實驗2＞
It can be seen from the content of Figure 3 that when the temperature is 900°C to 1050°C, except for the position close to the
除了使得反應器110的溫度為975℃，並且控制氣體的流速為0.6 公尺/秒，以與實驗1相同的方式，分別量測以由上而下氣流（top-down flow）、由下而上氣流（bottom-up flow）與對向流（countercurrent flow）方式所沉積的薄膜沉積速率（厚度除以沉積時間）分布，其結果顯示於圖4。由上而下氣流表示氣體固定由第一開口111流入反應器110並從第二開口112流出。由下而上氣流表示氣體固定由第二開口112流入反應器110並從第一開口111流出。Except that the temperature of the
從圖4的內容可知，對於由上而下氣流及由下而上氣流而言，在縮短反應均溫區域為18cm(此時滯留時間為0.3 秒)，將此區域內的碳化矽薄膜沉積總量除以三氯甲基矽烷的供給量可得到總共約40%的薄膜成長莫耳轉化率。在經由對向流沉積疊加後的沉積速率分布顯示均勻沉積區域的碳化矽薄膜成長轉化率佔比約22%。 ＜實驗3＞ It can be seen from the content of Figure 4 that for top-down airflow and bottom-up airflow, the shortened reaction average temperature area is 18cm (at this time the residence time is 0.3 seconds), and the total silicon carbide film deposition in this area is The amount divided by the supply amount of trichloromethylsilane gives a total molar conversion of film growth of approximately 40%. The deposition rate distribution after superposition through counterflow deposition shows that the silicon carbide film growth conversion rate in the uniform deposition area accounts for about 22%. ＜Experiment 3＞
除了使得反應器110的溫度改為1000℃，並且控制氣體的流速為0.6公尺/秒，使得氣體於反應器110的滯留時間改為0.5秒，以與實驗2相同的方式，量測其薄膜沉積速率分布，其結果顯示於圖5。Except that the temperature of the
從圖5的內容可知，當反應器110溫度提升至1000℃且滯留時間改為0.5秒時，其三氯甲基矽烷轉化為碳化矽的總莫耳轉化率提升至83%。經由對向流沉積疊加後的沉積速率分布顯示均勻沉積區域的轉化率提升至54%的佔比。
＜實驗4＞
It can be seen from the content of Figure 5 that when the temperature of the
除了使得反應器110的溫度改為1025℃，並且控制氣體的流速為0.6公尺/秒，並縮短反應均溫區域為18cm使得氣體於反應器的滯留時間改為0.3秒，以與實驗2相同的方式，量測其薄膜沉積速率分布，其結果示於圖6。Except that the temperature of the
從圖6的內容可知，當反應器110溫度提升至1025℃且滯留時間縮短為0.3秒時，其三氯甲基矽烷轉化為碳化矽的總莫耳轉化率可達81%。經由對向流沉積疊加後的沉積速率分布顯示沉積速率均勻的區域仍可保持約50%的轉化率佔比。
＜實驗5＞
It can be seen from the content of Figure 6 that when the temperature of the
除了使得反應器110的溫度改為1050℃，並且控制氣體的流速為0.6公尺/秒，並縮短反應均溫區域為16cm使得氣體於反應器的滯留時間改為0.27秒，採用與實驗2相同的方式，量測其薄膜沉積速率分布，其結果示於圖7。Except that the temperature of the
從圖7的內容可知，當反應器110溫度提升至1050℃且滯留時間改為0.27秒時，其三氯甲基矽烷轉化為碳化矽的總莫耳轉化率提升至96%。經由對向流沉積疊加後的沉積速率分布顯示沉積速率均勻的區域仍可保持約52%的轉化率佔比。即升高反應溫度時，藉由縮短反應滯留時間可有效率地提高三氯甲基矽烷原料轉化成碳化矽薄膜的轉化率，同時亦可保有到約5成轉化率的均勻沉積區域。
＜實驗6＞
It can be seen from the content of Figure 7 that when the temperature of the
利用掃描式電子顯微鏡觀測實驗3所形成的碳化矽薄膜，其影像示於圖8A及圖8B，其中圖8A為反應滯留時間為0.13秒的位置，圖8B為反應滯留時間為0.35秒的位置。The silicon carbide film formed in Experiment 3 was observed using a scanning electron microscope. The images are shown in Figures 8A and 8B. Figure 8A shows the position where the reaction residence time is 0.13 seconds, and Figure 8B shows the position where the reaction residence time is 0.35 seconds.
從圖8A及圖8B的內容可知，在不同的反應滯留時間位置，其薄膜的厚度皆為均勻。顯示無論在反應氣流的上下游位置皆可獲得緻密薄膜的沉積。 ＜實驗7＞ It can be seen from the contents of Figure 8A and Figure 8B that the thickness of the film is uniform at different reaction residence time positions. It shows that the deposition of dense films can be obtained regardless of the upstream and downstream positions of the reaction gas flow. ＜Experiment 7＞
與實驗3具有相同的條件，量測不同反應滯留時間位置沉積的碳化矽薄膜中C/Si組成比變化，其結果示於圖9。從圖9的內容可知，上述反應條件下沉積的薄膜經X光繞射觀察皆顯示β晶相的碳化矽特徵繞射峰，又沉積薄膜內的碳矽原子組成比大致呈現當量組成，並不因反應氣流上下游位置不同而有改變。 ＜實驗8＞ Under the same conditions as Experiment 3, the changes in the C/Si composition ratio in the silicon carbide films deposited at different reaction residence time positions were measured. The results are shown in Figure 9. It can be seen from the content of Figure 9 that X-ray diffraction observations of the films deposited under the above reaction conditions all show the characteristic diffraction peak of silicon carbide in the β crystal phase, and the carbon-silicon atomic composition ratio in the deposited film roughly shows an equivalent composition, and does not It changes due to different upstream and downstream positions of the reaction gas flow. ＜Experiment 8＞
除了將反應器110的溫度分別改為950℃、975℃、1000℃以及1025℃，以與實驗7相同的方式，量測在同一反應器110位置沉積的碳化矽薄膜中C/Si組成比變化，其結果示於圖10。從圖10的內容可知，在該當反應溫度範圍（950℃~1025℃）沉積的薄膜，其碳矽原子組成比不會隨溫度變化而有大幅改變（幾乎為當量組成）。Except that the temperatures of the
綜上所述，本發明的化學氣相沉積裝置透過使反應器中的氣體為對向流動狀態，可以在較高反應溫度下提升薄膜成長的莫耳轉化率的同時，獲得厚度均勻的大面積薄膜沉積。此外，本發明的化學氣相沉積方法透過上述化學氣相沉積裝置進行反應並調控氣體的滯留時間，提高反應原料轉化成薄膜的莫耳轉化率，同時獲得均勻的薄膜沉積形態。To sum up, the chemical vapor deposition device of the present invention can achieve a large area with uniform thickness while improving the molar conversion rate of film growth at a higher reaction temperature by making the gas in the reactor be in a counter-flow state. Thin film deposition. In addition, the chemical vapor deposition method of the present invention uses the above-mentioned chemical vapor deposition device to react and regulate the residence time of the gas, thereby improving the molar conversion rate of the reaction raw materials into the film and obtaining a uniform film deposition morphology.
雖然本發明已以實施例揭露如上，然其並非用以限定本發明，任何所屬技術領域中具有通常知識者，在不脫離本發明的精神和範圍內，當可作些許的更動與潤飾，故本發明的保護範圍當視後附的申請專利範圍所界定者為準。Although the present invention has been disclosed above through embodiments, they are not intended to limit the present invention. Anyone with ordinary knowledge in the technical field may make some modifications and modifications without departing from the spirit and scope of the present invention. Therefore, The protection scope of the present invention shall be determined by the appended patent application scope.
100:化學氣相沉積裝置 101:第一控制閥 102:第二控制閥 103:第三控制閥 104:第四控制閥 110:反應器 111:第一開口 112:第二開口 120:氣體供應槽 121:三氯甲基矽烷供應槽 122:氫氣氣體供應槽 123:氬氣氣體供應槽 130:抽氣系統 140:流量控制器 151:第一壓力感測裝置 152:第二壓力感測裝置 200:基板 L:長度 R:直徑 100: Chemical vapor deposition device 101: First control valve 102: Second control valve 103:Third control valve 104:Fourth control valve 110:Reactor 111:First opening 112:Second opening 120:Gas supply tank 121:Trichloromethylsilane supply tank 122:Hydrogen gas supply tank 123: Argon gas supply tank 130: Air extraction system 140:Flow controller 151: First pressure sensing device 152: Second pressure sensing device 200:Substrate L: length R: diameter
圖1是依照本發明一實施例的一種化學氣相沉積裝置的示意圖。 圖2是圖1中的反應器的放大示意圖。 圖3是本發明的實驗1的反應器中的溫度分布圖。 圖4是本發明的實驗2的薄膜沉積速率分布圖。 圖5是本發明的實驗3的薄膜沉積速率分布圖。 圖6是本發明的實驗4的薄膜沉積速率分布圖。 圖7是本發明的實驗5的薄膜沉積速率分布圖。 圖8A及圖8B是本發明的實驗6的薄膜在不同的反應滯留時間之剖面的掃描式電子顯微鏡影像。 圖9是本發明的實驗7在不同反應滯留時間的C/Si組成比變化關係圖。 圖10是本發明的實驗8在不同反應溫度的C/Si組成比變化關係圖。 FIG. 1 is a schematic diagram of a chemical vapor deposition device according to an embodiment of the present invention. Figure 2 is an enlarged schematic view of the reactor in Figure 1. Fig. 3 is a temperature distribution diagram in the reactor in Experiment 1 of the present invention. Figure 4 is a film deposition rate distribution diagram of Experiment 2 of the present invention. Figure 5 is a film deposition rate distribution diagram of Experiment 3 of the present invention. Figure 6 is a film deposition rate distribution diagram of Experiment 4 of the present invention. Figure 7 is a film deposition rate distribution diagram of Experiment 5 of the present invention. 8A and 8B are scanning electron microscope images of cross-sections of the thin film in Experiment 6 of the present invention at different reaction residence times. Figure 9 is a graph showing the change relationship of the C/Si composition ratio at different reaction residence times in Experiment 7 of the present invention. Figure 10 is a graph showing the change relationship of the C/Si composition ratio at different reaction temperatures in Experiment 8 of the present invention.
100:化學氣相沉積裝置 100: Chemical vapor deposition device
101:第一控制閥 101: First control valve
102:第二控制閥 102: Second control valve
103:第三控制閥 103:Third control valve
104:第四控制閥 104:Fourth control valve
110:反應器 110:Reactor
120:氣體供應槽 120:Gas supply tank
121:三氯甲基矽烷供應槽 121:Trichloromethylsilane supply tank
122:氫氣氣體供應槽 122:Hydrogen gas supply tank
123:氬氣氣體供應槽 123: Argon gas supply tank
130:抽氣系統 130: Air extraction system
140:流量控制器 140:Flow controller
151:第一壓力感測裝置 151: First pressure sensing device
152:第二壓力感測裝置 152: Second pressure sensing device
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