TWI582268B - The cleaning method of the process chamber of the CVD reactor - Google Patents

The cleaning method of the process chamber of the CVD reactor Download PDF

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TWI582268B
TWI582268B TW102105962A TW102105962A TWI582268B TW I582268 B TWI582268 B TW I582268B TW 102105962 A TW102105962 A TW 102105962A TW 102105962 A TW102105962 A TW 102105962A TW I582268 B TWI582268 B TW I582268B
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process chamber
cleaning
gas
temperature
susceptor
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TW102105962A
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TW201343971A (en
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Olaf Rockenfeller
Holger Grube
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Aixtron Se
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/4401Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4405Cleaning of reactor or parts inside the reactor by using reactive gases

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Drying Of Semiconductors (AREA)

Description

CVD反應器之製程室的清洗方法 Cleaning method of process chamber of CVD reactor

本發明係關於一種清洗CVD(化學氣相沉積)-反應器製程室的方法,該製程室具有一個可由加熱裝置進行加熱的基座作為製程室底座和一個與製程室底座對置的製程室蓋罩,在CVD過程中在製程室底座和製程室蓋罩上形成的寄生覆層經由加熱裝置加熱底座和輸入腐蝕氣體在兩個連續的清洗過程中加以去除。 The present invention relates to a method of cleaning a CVD (Chemical Vapor Deposition)-reactor process chamber having a susceptor that can be heated by a heating device as a process chamber base and a process chamber cover opposite the process chamber base The cover, the parasitic coating formed on the process chamber base and the process chamber cover during the CVD process is heated by the heating means and the input etching gas is removed during two successive cleaning processes.

專利文獻DE 101 02 745 C2描述一種CVD-反應器和一種用於清洗CVD-反應器的方法,輸送含氟氣體至反應室內,在反應室內該氣體借經由等離子體進行電離。 The patent document DE 101 02 745 C2 describes a CVD-reactor and a method for cleaning a CVD-reactor, which delivers a fluorine-containing gas into a reaction chamber in which the gas is ionized by means of a plasma.

專利文獻DE 198 32 566 C2描述一種用於清洗CVD-反應器製程室的方法,在清洗過程中重複變化製程室的壓力和溫度。使用氯氟化合物作為腐蝕氣體。 The patent document DE 198 32 566 C2 describes a method for cleaning a CVD-reactor process chamber in which the pressure and temperature of the process chamber are repeatedly varied during the cleaning process. Chlorofluoride is used as an etching gas.

專利文獻DE 10 2006 018 515 A1描述一種方法,對於該方法而言,CVD-反應器的製程室經由輸入腐蝕氣體以進行清洗。由於在腐蝕時製程室蓋板會下降,製程室的高度因而降低,從而使得製程室的底座和蓋板可以同時透過腐蝕而加以清洗。 The patent document DE 10 2006 018 515 A1 describes a method for which the process chamber of a CVD reactor is cleaned by means of an input of corrosive gases. Since the process chamber cover is lowered during corrosion, the height of the process chamber is thus lowered, so that the base and the cover of the process chamber can be simultaneously cleaned by corrosion.

專利文獻DE 38 88 736 T2(EP 0 296 804 B1)描述一種CVD-反應器製程室的清洗方法。在基座放電後,將含氯化氫的腐蝕氣體的強氣流輸送至製程室中,以便對基座進行清洗。在基座清洗後, 氣體成分發生變化,整個反應器室上聚集的沉積物被清除。 A cleaning method for a CVD-reactor process chamber is described in the patent document DE 38 88 736 T2 (EP 0 296 804 B1). After the susceptor is discharged, a strong gas stream of corrosive gas containing hydrogen chloride is delivered to the process chamber to clean the susceptor. After the pedestal is cleaned, The composition of the gas changes and the accumulated deposits on the entire reactor chamber are removed.

專利文獻US 6,242,347 B1描述一種用於清洗製程室, 尤其是基座的兩階段腐蝕方法,對此在清洗過程中將「Placebo Wafer(安慰晶片)」置於基座上,以便在清洗過程中保護基座的表面。建議使用石英片作為安慰晶片。 Patent document US 6,242,347 B1 describes a process for cleaning a process chamber, In particular, the two-stage etching method of the susceptor is to place a "Placebo Wafer" on the susceptor during the cleaning process to protect the surface of the pedestal during the cleaning process. Quartz plates are recommended as a comfort chip.

專利文獻US 2005/0 242 061 A1描述一種CVD-反應 器的清洗方法,對此將清洗氣體輸入製程室中,並在製程室中形成等離子體。 A CVD-reaction is described in the patent document US 2005/0 242 061 A1 The cleaning method of the device, in which the cleaning gas is introduced into the process chamber, and a plasma is formed in the process chamber.

專利文獻US 5,812,403描述一種CVD-反應器和一種 經由腐蝕去除在塗覆過程中附著在製程室表面的塗層。使用和塗層反應的反應氣體。 No. 5,812,403 describes a CVD reactor and a The coating adhered to the surface of the process chamber during the coating process is removed by etching. The reaction gas reacted with the coating is used.

專利文獻US 6,042,654描述一種經由輸入氯氣對CVD -反應器的製程室進行清洗的過程,氯氣在熱分解過程中分解為自由基。 Patent document US 6,042,654 describes a CVD via input chlorine - The process of cleaning the process chamber of the reactor, the chlorine gas is decomposed into free radicals during thermal decomposition.

專利文獻EP 0 855 453 A1或者US5,348,587描述一種方 法,對於該方法而言,使用經由等離子體進行分解的含氯氣體作為腐蝕氣體,以便對CVD-反應器製程室的覆層和內壁加以清洗。 A patent is described in the patent document EP 0 855 453 A1 or US Pat. No. 5,348,587. For the method, a chlorine-containing gas decomposed by a plasma is used as an etching gas to clean the coating and the inner wall of the CVD-reactor process chamber.

專利文獻US 6,242,347 B1描述一種兩階段清洗方法, 可以對CVD-反應器製程室在塗覆過程中形成的覆層加以清洗。此處使用氯化合物作為腐蝕氣體。對於該清洗步驟而言,製程室必須加熱至比塗覆過程中之過程溫度更高的溫度。 Patent document US 6,242,347 B1 describes a two-stage cleaning method, The coating formed during the coating process of the CVD-reactor process chamber can be cleaned. A chlorine compound is used here as an etching gas. For this cleaning step, the process chamber must be heated to a temperature higher than the process temperature during the coating process.

專利文獻DE 38 88 736 T2描述一種矽之外延沉積物的 分離方法,在分離過程後製程室經由輸入腐蝕氣體以進行清洗。 DE 38 88 736 T2 describes a bismuth exfoliating deposit The separation method, after the separation process, the process chamber is cleaned by inputting a corrosive gas.

製程室包含一個製程室蓋板和一個用於支承待塗覆基 材的基座,該基座可以由下方進行加熱,專利文獻DE 10 2006 018515 A1、DE 10 2006 013801 A1和DE 102 17 806 A1對這一特徵作了說明。 在該裝置中,基材放置在基座上,經由輸送過程將氣體塗覆半導體塗層或者類似塗層。過程中氣體不僅會在基材的表面進行熱分解,而且也會對裸露、未被基材覆蓋的基座表面區域以及製程室蓋罩的表面進行熱分解。在實施一次或者多次塗覆過程後必須清除寄生的覆層。對此使用諸如氯化氫或者氯氣。此外,清洗過程的效率還取決於待清洗表面的表面溫度。經由在下方進行加熱,將基座表面溫度提高至進行腐蝕過程的600至650攝氏度。製程室蓋罩由基座的輻射熱量進行加熱,因此溫度稍低。為了更有效地實施腐蝕過程,上述現有技術建議減小製程室蓋罩和製程室底部之間的垂直距離,以便可以在輻射熱量傳遞的過程中製程室蓋罩可以獲得更高的溫度。此外,由於基座的特徵,尤其是基座表面的塗層,基座無法被加熱至超過特定的極限溫度,因此基座的可加熱性受限。 The process chamber includes a process chamber cover and a support for the substrate to be coated The pedestal of the material can be heated from below, and this feature is described in the patent documents DE 10 2006 018515 A1, DE 10 2006 013801 A1 and DE 102 17 806 A1. In this device, the substrate is placed on a susceptor and the gas is coated with a semiconductor coating or similar coating via a transport process. During the process, the gas not only thermally decomposes on the surface of the substrate, but also thermally decomposes the exposed surface area of the substrate that is not covered by the substrate and the surface of the process chamber cover. The parasitic coating must be removed after one or more coating processes have been performed. For this purpose, such as hydrogen chloride or chlorine. In addition, the efficiency of the cleaning process also depends on the surface temperature of the surface to be cleaned. The surface temperature of the susceptor is raised to 600 to 650 degrees Celsius for the etching process by heating underneath. The process chamber cover is heated by the radiant heat of the susceptor, so the temperature is slightly lower. In order to more effectively perform the etching process, the above prior art suggests reducing the vertical distance between the process chamber cover and the bottom of the process chamber so that the process chamber cover can achieve higher temperatures during radiant heat transfer. Furthermore, due to the characteristics of the pedestal, especially the coating on the surface of the pedestal, the susceptor cannot be heated above a certain extreme temperature, so the susceptibility of the susceptor is limited.

該發明的所要解決的技術問題在於更高效能地實施清洗過程。 The technical problem to be solved by the invention is to carry out the cleaning process with higher efficiency.

首先,建議在第一個清洗步驟中於第一個清洗溫度下主要對製程室底部進行清洗。該清洗步驟可以在一個低於基座最大可負載溫度的溫度下進行。在該清洗步驟下,製程室蓋罩的表面溫度低於製程室底部的表面溫度,因此在第一清洗步驟中主要、必要時僅對製程室底部進行清洗。在實施第一清洗步驟後,製程室冷卻至較低的溫度。將基座從製程室中移除。然後在第二清洗溫度下於第二清洗步驟中對製程室蓋罩進行清洗。在第二清洗步驟中主要對製程室蓋罩,或 者僅對製程室蓋罩進行清洗。在第二個清洗步驟中可以將在第一個清洗步驟中清洗過的基座替換為具有如此性能的輔助基座,即能夠使得製程室蓋罩的表面溫度加熱至高於在第一清洗步驟中達到的製程室蓋罩溫度,且該溫度足夠確保對蓋罩實施高效能的清洗。第二清洗溫度可以高於第一清洗溫度。製程室蓋罩在第二清洗過程中至少擁有比第一清洗步驟更高的清洗溫度。輔助基座可以是一種適用第二清洗步驟而生產的、並且其結構與此相關地進行過優化的固體。但也可以使用之前多次已進行塗覆過程的廢舊基座。較佳使用鹵素化合物,例如氯化氫和氯氣作為腐蝕氣體。但在相對應的高溫下也可以僅使用氫氣作為腐蝕氣體。在第一個清洗步驟中,基座較佳加熱至600至650攝氏度的溫度。輔助基座在第二清洗過程中加熱至明顯更高的溫度,例如800至1000攝氏度。也可以超過1000攝氏度,例如如果使用氫氣作為腐蝕氣體,可加熱至超過1200攝氏度的溫度。第一和/或第二清洗步驟可以包含多個子週期,對此多個週期經由所使用的腐蝕氣體和/或清洗溫度加以區分。塗覆步驟係在清洗步驟之前。該塗覆步驟是一種MOCVD(金屬有機化合物化學氣相沉積)-方法,在該方法中,將第III或者第II主族金屬有機化合物和同時或者與之交替地將第V或者第VI主族元素的氫化物以及必要時與惰性氣體一起輸送至製程室中。過程氣體在製程室中發生熱分解,並在基座上的一個或者多個基材上離析出單晶半導體塗層。使用TMAI、TMGa和/或者TMIn作為過程氣體。為形成InGaAs、AlN、AlGaN,金屬有機成分和AsH3、PH3或者NH3一起或者與AsH3、PH3或者NH3交替地輸送至製程室中。輸送過程係藉由氣體輸入裝置來進行,經由該裝置也可以在該清洗步驟中將腐蝕氣體輸送至製程室中。過程氣體或者清洗氣體經由氣體排出裝置 從製程室中重新排出。在塗覆過程或者清洗過程中,過程氣體或者清洗氣體在製程室內流動。不管是塗覆過程還是清洗過程,均較佳使用額外的載氣,該氣體可以是氫氣、氮氣,也可以是惰性氣體。塗覆過程或者腐蝕過程也可以在不同的總壓力下進行。在塗覆過程或者清洗過程中,製程室中的氣體總壓力介於100至900mbar之間。在一種特佳使用的腐蝕方法中,在沉積過程和從製程室中取出晶片後,首先在600至800攝氏度的溫度下進行低溫腐蝕步驟,在該步驟中使用氯氣作為腐蝕氣體。在一個或者多個借助氮氣或者氯氣從製程室去除腐蝕物的沖洗步驟後,將底座或者製程室加熱至1100攝氏度以上。然後在該溫度下經由輸入氫氣進行第二個清洗步驟。在製程室冷卻後可以重新放入待塗覆基材。如果使用輔助底座,則需要更換為可放置基材或者已經放置有待塗覆基材的基座。 First, it is recommended to clean the bottom of the process chamber primarily at the first cleaning temperature in the first cleaning step. The cleaning step can be carried out at a temperature below the maximum loadable temperature of the susceptor. In the cleaning step, the surface temperature of the process chamber cover is lower than the surface temperature of the bottom of the process chamber, so that only the bottom of the process chamber is cleaned mainly, if necessary, in the first cleaning step. After the first cleaning step is performed, the process chamber is cooled to a lower temperature. Remove the pedestal from the process chamber. The process chamber cover is then cleaned in a second cleaning step at a second cleaning temperature. In the second cleaning step, the process chamber cover is mainly used, or only the process chamber cover is cleaned. In the second cleaning step, the susceptor cleaned in the first cleaning step can be replaced with an auxiliary susceptor having such a property that the surface temperature of the process chamber cover can be heated higher than in the first cleaning step. The process chamber cover temperature is reached and is sufficient to ensure efficient cleaning of the cover. The second cleaning temperature can be higher than the first cleaning temperature. The process chamber cover has at least a higher cleaning temperature than the first cleaning step during the second cleaning process. The auxiliary base may be a solid that is produced using a second cleaning step and whose structure is optimized in relation thereto. However, it is also possible to use a used base that has been subjected to a coating process many times before. Halogen compounds such as hydrogen chloride and chlorine are preferably used as the etching gas. However, it is also possible to use only hydrogen as the corrosive gas at the corresponding high temperature. In the first cleaning step, the susceptor is preferably heated to a temperature of 600 to 650 degrees Celsius. The auxiliary susceptor is heated to a significantly higher temperature during the second cleaning process, for example 800 to 1000 degrees Celsius. It can also exceed 1000 degrees Celsius, for example if hydrogen is used as the corrosive gas, it can be heated to temperatures in excess of 1200 degrees Celsius. The first and/or second cleaning step may comprise a plurality of sub-cycles, the plurality of cycles being distinguished by the corrosive gases and/or cleaning temperatures used. The coating step is prior to the washing step. The coating step is an MOCVD (Metal Organic Compound Chemical Vapor Deposition)-method in which a Group III or Group II organometallic compound is simultaneously or alternatively substituted with a Vth or VIth main group The hydride of the element and, if necessary, the inert gas are delivered to the process chamber. The process gas thermally decomposes in the process chamber and separates the single crystal semiconductor coating from one or more substrates on the susceptor. Use TMAI, TMGa and/or TMIn as process gases. To form InGaAs, AlN, AlGaN, and a metal organic component AsH 3, PH 3 or AsH NH 3 together with or delivered to the process chamber 3, PH 3 or NH 3 alternately. The conveying process is carried out by means of a gas input device, via which the corrosive gas can also be supplied to the process chamber. The process gas or purge gas is re-discharged from the process chamber via a gas discharge device. Process gas or purge gas flows within the process chamber during the coating process or cleaning process. Whether it is a coating process or a cleaning process, it is preferred to use an additional carrier gas, which may be hydrogen, nitrogen, or an inert gas. The coating process or the etching process can also be carried out at different total pressures. The total gas pressure in the process chamber is between 100 and 900 mbar during the coating or cleaning process. In a particularly preferred etching method, after the deposition process and removal of the wafer from the process chamber, a low temperature etching step is first performed at a temperature of 600 to 800 degrees Celsius, in which chlorine gas is used as the etching gas. After the rinsing step of removing corrosives from the process chamber by means of nitrogen or chlorine, the base or process chamber is heated to above 1100 degrees Celsius. A second cleaning step is then carried out via the input of hydrogen at this temperature. The substrate to be coated can be re-applied after the process chamber has cooled. If an auxiliary base is used, it needs to be replaced with a base on which the substrate can be placed or where the substrate to be coated has been placed.

1‧‧‧反應器外殼 1‧‧‧reactor housing

2‧‧‧氣體輸入裝置 2‧‧‧ gas input device

3‧‧‧製程室蓋罩 3‧‧‧Processing room cover

4‧‧‧製程室 4‧‧‧Processing Room

5‧‧‧製程室底部 5‧‧‧Processing room bottom

6‧‧‧基座 6‧‧‧Base

7‧‧‧加熱裝置 7‧‧‧ heating device

8‧‧‧氣體輸出裝置 8‧‧‧ gas output device

9‧‧‧氣體輸送管 9‧‧‧ gas delivery tube

10‧‧‧氣體輸出開口 10‧‧‧ gas output opening

11‧‧‧冷卻管道 11‧‧‧Cooling pipe

12‧‧‧基材支架 12‧‧‧Substrate support

13‧‧‧支架 13‧‧‧ bracket

14‧‧‧軸線 14‧‧‧ axis

該發明的實施例在下文中結合附圖並加以說明。在附圖中:圖1示出CVD-反應器橫截面,其基本原理由專利文獻DE 10 2006 013801 A1已知,圖2示出根據圖1所示的CVD-反應器,其中基座6替換為輔助底座6’,圖3示出本發明的第二個實施例,CVD-反應器基本原理由專利文獻DE 10 2006 018515 A1已知,圖4示出根據圖3所示的CVD-反應器,其中基座6更換為輔助基座6’。 Embodiments of the invention are described below in conjunction with the drawings. In the drawings: Figure 1 shows a cross-section of a CVD reactor, the basic principle of which is known from the patent document DE 10 2006 013 801 A1, which shows a CVD reactor according to Figure 1, in which the susceptor 6 is replaced FIG. 3 shows a second embodiment of the invention, the basic principle of the CVD reactor is known from the patent document DE 10 2006 018515 A1, and FIG. 4 shows the CVD reactor according to FIG. , in which the base 6 is replaced with an auxiliary base 6'.

圖1和2所描述的反應器的結構和作用原理係引用專利文獻DE 10 2006 013801 A1,其公開內容已經全部在該申請中作了說明。在一個相對於外部氣密地密封的反應器外殼1中存在製程室4。製程室4之蓋罩3由氣體輸入裝置2的下端組成,該氣體輸入裝置為噴頭狀。經由輸送管9將過程氣體或者清洗氣體輸送至氣體輸送裝置2的內部。過程氣體或者清洗氣體經由氣體輸送裝置2的下端離開其內部,在該下端處具有大量的氣體排出開口10。在該結構實施例中,如果在塗覆過程中應對製程室蓋罩3進行冷卻,則氣體輸入裝置的下端具有流淌有冷卻液體的冷卻管道11。 The structure and principle of operation of the reactors described in Figures 1 and 2 are cited in the patent document DE 10 2006 013 801 A1, the disclosure of which is hereby incorporated by reference in its entirety. The process chamber 4 is present in a reactor housing 1 that is hermetically sealed from the outside. The cover 3 of the process chamber 4 is composed of the lower end of the gas input device 2, which is in the shape of a showerhead. The process gas or the purge gas is delivered to the inside of the gas delivery device 2 via a transfer pipe 9. The process gas or purge gas leaves its interior via the lower end of the gas delivery device 2, with a large number of gas discharge openings 10 at the lower end. In this structural embodiment, if the process chamber cover 3 is to be cooled during the coating process, the lower end of the gas input device has a cooling duct 11 through which a cooling liquid flows.

製程室4的底部5由和氣體輸入裝置2對置的基座6上端構成。基座6可以是由石墨、鉬或者其他合適的材料製成的固體。基本上呈圓盤狀的製程室由環狀的氣體排出裝置8所包圍。 The bottom 5 of the process chamber 4 is constituted by the upper end of the susceptor 6 opposed to the gas input device 2. The susceptor 6 can be a solid made of graphite, molybdenum or other suitable material. The substantially disk-shaped process chamber is surrounded by an annular gas discharge device 8.

在基座6的下方是以附圖標記7表示加熱裝置,該加熱裝置配備有紅外輻射器或者RF-加熱器。借助該加熱裝置,基座6可以加熱至過程溫度或者清洗溫度。在塗覆過程中,在基座6上放置一個或者多個基材(參見專利文獻DE 10 2006 013801 A1)。在按規定使用CVD-反應器時,經由氣體輸送管9或者多個為了簡化此處而未作說明的其他氣體輸送管將一種或者多種過程氣體輸送至氣體輸入裝置2中,並經由氣體排出開口10進入製程室4內。過程氣體可以使用AsH3、PH3、NH3、或者TMAl、TMGa或者TMIn。過程氣體隨同載氣,例如氫氣或者氮氣輸送至製程室4中。基座6在塗覆時加熱至過程溫度,在該溫度下,過程氣體進行熱分解,從而使得基材上離析出InGaAs、AlN和/或者AlGaN塗層。 Below the pedestal 6, the heating means is indicated by reference numeral 7, which is equipped with an infrared radiator or an RF-heater. With this heating device, the susceptor 6 can be heated to a process temperature or a cleaning temperature. During the coating process, one or more substrates are placed on the base 6 (see patent document DE 10 2006 013 801 A1). When the CVD reactor is used as intended, one or more process gases are delivered to the gas input device 2 via the gas delivery tube 9 or a plurality of other gas delivery tubes not illustrated herein for simplification and via the gas discharge opening 10 enters the process chamber 4. The process gas may use AsH 3 , PH 3 , NH 3 , or TMAl, TMGa or TMIn. The process gas is delivered to the process chamber 4 along with a carrier gas, such as hydrogen or nitrogen. The susceptor 6 is heated to the process temperature during coating, at which temperature the process gas undergoes thermal decomposition, thereby causing the InGaAs, AlN and/or AlGaN coating to be separated on the substrate.

在一個或者多個這一類的塗層離析步驟(在這些步驟中 一種或者多種塗層在基材上在不同的過程參數下進行離析)後,將已塗覆的基材從製程室取出。 One or more coating separation steps in this category (in these steps) After the one or more coatings are separated on the substrate under different process parameters, the coated substrate is removed from the process chamber.

在塗覆過程中,在製程室蓋罩3或者在製程室底部5上 未被基材覆蓋到的區域形成覆層。該覆層在根據該發明的清洗步驟(腐蝕步驟)中加以去除。 During the coating process, on the process chamber cover 3 or on the bottom 5 of the process chamber The area not covered by the substrate forms a coating. The coating is removed in a cleaning step (corrosion step) according to the invention.

在第一個清洗步驟中,在第一清洗溫度下主要對製程室 底部5進行清洗。對此,通過氣體輸送管9將腐蝕氣體,例如氯化氫或者氯氣輸送至氣體輸入裝置2中。該輸入過程和載氣,例如氫氣或者氮氣一起進行。氣體混合物經由氣體排出開口10進入製程室4中。 在第一個清洗步驟中,底座6,也就是製程室底部5,其被加熱至大約600至650攝氏度。在該溫度下,腐蝕氣體和覆層發生反應。該反應過程為乾式腐蝕過程,在化學反應的過程中,覆層轉變為氣態。氣狀覆層反應產物由載氣輸送至氣體排出裝置8中,並經由該排出裝置離開製程室4。在第一個清洗步驟中,將製程室蓋罩3輻射加熱至較低的溫度。該溫度不足以讓製程室蓋罩3經由乾式腐蝕而進行有效的清洗。 In the first cleaning step, at the first cleaning temperature, mainly to the process chamber The bottom 5 is cleaned. In this regard, an etching gas such as hydrogen chloride or chlorine gas is supplied to the gas input device 2 through the gas delivery pipe 9. This input process is carried out with a carrier gas such as hydrogen or nitrogen. The gas mixture enters the process chamber 4 via the gas discharge opening 10. In the first cleaning step, the base 6, which is the process chamber bottom 5, is heated to approximately 600 to 650 degrees Celsius. At this temperature, the etching gas reacts with the coating. The reaction process is a dry etching process in which the coating is transformed into a gaseous state. The gas-clad reaction product is transported by the carrier gas into the gas discharge device 8 and exits the process chamber 4 via the discharge device. In the first cleaning step, the process chamber cover 3 is radiantly heated to a lower temperature. This temperature is not sufficient to allow the process chamber cover 3 to be effectively cleaned by dry etching.

在結束第一個清洗步驟後,製程室經由惰性氣體,例如 氮氣或者氫氣進行沖洗和冷卻,直至基座6達到允許將其從反應器外殼1中移除的溫度。在該實施例中,基座6被替換為輔助基座6’。輔助基座6’可以是一個單獨針對第二清洗步驟生產的物體。例如與基座6相比,該輔助基座可以為具有更小的橫截面,並具有更高的耐熱性。 在一種較佳的變型例中,基座6僅更換為不再用於塗覆過程的廢舊基座,儘管其表面可能在溫度負載下出現損傷,但由於該基座不再用於塗覆過程,因此可以接受該情況。 After the end of the first cleaning step, the process chamber is passed through an inert gas, for example Nitrogen or hydrogen is flushed and cooled until the susceptor 6 reaches a temperature that allows it to be removed from the reactor housing 1. In this embodiment, the base 6 is replaced with an auxiliary base 6'. The auxiliary base 6' may be an object produced separately for the second cleaning step. For example, the auxiliary base may have a smaller cross section and have higher heat resistance than the base 6. In a preferred variant, the base 6 is only replaced with a waste base that is no longer used in the coating process, although its surface may be damaged under temperature loading, since the base is no longer used in the coating process. So you can accept the situation.

在安裝輔助基座6’(參見附圖2)或者在更換基座(參見附 圖1)後,製程室經由更大的加熱功率並藉由加熱裝置7加熱至比第一清洗過程更高的溫度。基座6或者輔助基座6’達到最高1000攝氏度或者超過1000攝氏度的溫度。在該溫度下,製程室蓋罩3被加熱至超過600攝氏度的溫度,因此可以經由輸送腐蝕氣體對製程室蓋罩3上的覆層進行有效清除。 Install the auxiliary base 6' (see Figure 2) or replace the base (see attached After Figure 1), the process chamber is heated by a greater heating power and by a heating device 7 to a higher temperature than the first cleaning process. The susceptor 6 or the auxiliary pedestal 6' reaches a temperature of up to 1000 degrees Celsius or more than 1000 degrees Celsius. At this temperature, the process chamber cover 3 is heated to a temperature in excess of 600 degrees Celsius, so that the coating on the process chamber cover 3 can be effectively removed by transporting corrosive gases.

取代鹵素氣體,尤其是含氯腐蝕氣體,也可以使用在高溫下具有腐蝕作用的純氫氣,尤其用於去除製程室蓋罩3上的鎵或鋁。在該清洗步驟中,冷卻管道內無冷卻劑。 Instead of a halogen gas, especially a chlorine-containing corrosive gas, it is also possible to use pure hydrogen having a corrosive action at a high temperature, in particular for removing gallium or aluminum on the process chamber cover 3. In this cleaning step, there is no coolant in the cooling duct.

附圖3和4所示的結構實施例是一種在專利文獻DE 10 2006 018515 A1中描述過的MOCVD-反應器。因此可以完全引用該文獻公開內容。 The structural embodiment shown in Figures 3 and 4 is an MOCVD-reactor described in the patent document DE 10 2006 018 515 A1. The disclosure of this document can therefore be fully cited.

同附圖1和2所示的反應器,附圖3和4所示的反應器擁有一個對稱軸14,基座6圍繞該軸進行旋轉驅動。在附圖3和4所示的實施例中,氣體輸入裝置2位於製程室4的中心位置。基座6環狀包圍氣體輸入裝置。製程室4擁有一個製程室蓋罩3,在塗覆過程中,製程室蓋罩藉由安裝在製程室蓋罩3上方的冷卻裝置而進行冷卻。 In the reactor shown in Figures 1 and 2, the reactor shown in Figures 3 and 4 has an axis of symmetry 14 around which the susceptor 6 is rotationally driven. In the embodiment shown in Figures 3 and 4, the gas input device 2 is located at the center of the process chamber 4. The base 6 is annularly surrounding the gas input device. The process chamber 4 has a process chamber cover 3 which is cooled by a cooling device mounted above the process chamber cover 3 during the coating process.

製程室4的底部5由基座6構成,該基座可以是帶塗層的石墨、鉬或者其他合適材料製成的固體。待塗層基材放置在旋轉驅動的基材支架12上,該支架位於基座6的卡槽中。平放在支架13上的基座在下方使用加熱裝置7進行加熱。該加熱過程也可以以IR或者RF的方式進行。 The bottom 5 of the process chamber 4 is constructed of a susceptor 6, which may be a solid of coated graphite, molybdenum or other suitable material. The substrate to be coated is placed on a rotationally driven substrate holder 12 which is located in the card slot of the base 6. The base that is placed flat on the bracket 13 is heated using a heating device 7 below. This heating process can also be carried out in IR or RF.

在塗覆過程結束並將一個或者多個基材從基材支架12上取下後,第一個清洗步驟中的氯氣或者氯化氫經由氣體輸入裝置2和載氣一起輸送至加熱到第一清洗溫度的製程室4中。在第一清洗步 驟中,製程室底部5,也就是基座6的表面或者基材支架12的表面擁有一個清洗溫度,在該溫度下覆層和腐蝕氣體發生反應,進而形成可離開製程室4的揮發性反應產物。對於該實施例而言,尚未冷卻的製程室蓋罩3僅受到輻射加熱且僅可達到在第一清洗步驟中的表面溫度,在該表面溫度下腐蝕過程完全無法進行或者僅可低效率進行。 After the coating process is completed and one or more substrates are removed from the substrate holder 12, the chlorine or hydrogen chloride in the first cleaning step is transported via the gas input device 2 together with the carrier gas to the first cleaning temperature. In the process chamber 4. In the first cleaning step In the step, the bottom of the process chamber 5, that is, the surface of the susceptor 6 or the surface of the substrate holder 12 has a cleaning temperature at which the coating reacts with the corrosive gas to form a volatile reaction which can leave the process chamber 4. product. For this embodiment, the process chamber cover 3 that has not been cooled is only subjected to radiant heating and can only reach the surface temperature in the first cleaning step, at which the etching process is completely impossible or can only be carried out with low efficiency.

在結束第一個清洗步驟且基座6冷卻後,將基座6移 除,並更換為舊的、不再用於塗覆過程的基座6(附圖3)或者更換為單獨針對第二清洗過程生產的輔助基座6’(見附圖4)。 After the first cleaning step is completed and the susceptor 6 is cooled, the pedestal 6 is moved In addition, and replaced with the old base 6 (Fig. 3) which is no longer used for the coating process or replaced with the auxiliary base 6' produced separately for the second cleaning process (see Fig. 4).

這一類裝配有輔助基座6、6’的製程室4同樣使用加熱裝置7進行加熱。但輔助基座6、6’加熱至比第一清洗步驟更高的溫度。在第二清洗步驟中,輔助基座6、6’的表面溫度應夠高,從而使得尚未冷卻的製程室蓋罩3加熱至可以有效進行腐蝕過程的溫度。在第二清洗步驟中同樣使用氯化氫、氯氣或者其他合適的氣體作為腐蝕氣體。也可以藉由氫氣進行表面腐蝕。 This type of process chamber 4 equipped with auxiliary pedestals 6, 6' is also heated using a heating device 7. However, the auxiliary susceptors 6, 6' are heated to a higher temperature than the first cleaning step. In the second washing step, the surface temperature of the auxiliary susceptor 6, 6' should be high enough to heat the process chamber cover 3 which has not been cooled to a temperature at which the etching process can be effectively performed. Hydrogen chloride, chlorine or other suitable gas is also used as the etching gas in the second washing step. Surface etching can also be carried out by hydrogen gas.

如果製程室蓋罩是使用冷卻劑冷卻的製程室蓋罩,可以在第二清洗步驟中關閉冷卻裝置,從而停止冷卻。 If the process chamber cover is a process chamber cover that is cooled with coolant, the cooling device can be turned off during the second cleaning step to stop cooling.

在腐蝕後,輔助基座6’重新更換為實施塗覆過程之過程基座6。 After the etching, the auxiliary base 6' is replaced with the process base 6 which performs the coating process.

在使用氯氣或者氯化氫作為清洗氣體時,金屬覆層轉化為揮發性氯化物。在第一清洗步驟中,基座6得到清洗,在第二清洗步驟中,製程室蓋罩3或者其他遠離基座6的表面獲得清洗。在接下來的第三清洗過程中,使用氫氣作為腐蝕氣體,以便將反應器壁上吸附的氯化物,尤其是吸附的氯經由轉化為氯化氫並加以去除。 When chlorine or hydrogen chloride is used as the purge gas, the metal coating is converted to volatile chloride. In the first cleaning step, the susceptor 6 is cleaned, and in the second cleaning step, the process chamber cover 3 or other surface remote from the susceptor 6 is cleaned. In the next third cleaning process, hydrogen is used as the etching gas in order to convert the adsorbed chloride, especially the adsorbed chlorine, to hydrogen chloride and remove it.

所有已經公開的特徵(個體)都是本發明的實質內容。在 該申請的公開內容中,相關/附帶的優先性資料(在先申請副本)的公開內容被完全引用,對於這些資料的目的、特徵也被包含在本發明的申請專利範圍中。申請專利範圍中的附屬項係能夠在其任選並列的技術方案中獨立地刻畫現有技術之具有創造性的擴展設計,尤其可以基於這些申請專利範圍進行分割案申請。 All features (individuals) that have been disclosed are essential to the invention. in In the disclosure of the application, the disclosure of the relevant/attached priority material (copy of the prior application) is fully cited, and the purpose and features of the material are also included in the scope of the patent application of the present invention. The sub-items in the scope of the patent application are capable of independently portraying the inventive extensions of the prior art in their optional technical solutions, and in particular, the divisional application can be made based on the scope of these patent applications.

1‧‧‧反應器外殼 1‧‧‧reactor housing

2‧‧‧氣體輸入裝置 2‧‧‧ gas input device

3‧‧‧製程室蓋罩 3‧‧‧Processing room cover

4‧‧‧製程室 4‧‧‧Processing Room

5‧‧‧製程室底部 5‧‧‧Processing room bottom

6‧‧‧基座 6‧‧‧Base

7‧‧‧加熱裝置 7‧‧‧ heating device

8‧‧‧氣體輸出裝置 8‧‧‧ gas output device

9‧‧‧氣體輸送管 9‧‧‧ gas delivery tube

10‧‧‧氣體輸出開口 10‧‧‧ gas output opening

11‧‧‧冷卻管道 11‧‧‧Cooling pipe

14‧‧‧軸線 14‧‧‧ axis

Claims (14)

一種用於清洗CVD-反應器(1)的製程室(4)的方法,該製程室具有由加熱裝置(7)加熱的基座(6)作為製程室底部(5)和與製程室底部(5)對置的製程室蓋罩(3),在CVD過程中在製程室底部(5)和製程室蓋罩(3)上形成的寄生覆層經由加熱裝置(7)加熱基座(6)並在兩個相繼的清洗步驟中輸入腐蝕氣體加以清除,其特徵在於,在第一清洗步驟中並於第一清洗溫度下主要對製程室底部(5)進行清洗,接著將基座(6)從製程室中取出,然後在第二清洗步驟中並於第二清洗溫度下清洗製程室蓋罩(3)。 A method for cleaning a process chamber (4) of a CVD reactor (1) having a susceptor (6) heated by a heating device (7) as a process chamber bottom (5) and a process chamber bottom ( 5) The opposite process chamber cover (3), the parasitic coating formed on the bottom of the process chamber (5) and the process chamber cover (3) during the CVD process is heated by the heating device (7) (6) And removing the etching gas in two successive cleaning steps to remove, characterized in that in the first cleaning step and at the first cleaning temperature, the bottom of the process chamber (5) is mainly cleaned, and then the base (6) Remove from the process chamber and then clean the process chamber cover (3) in the second cleaning step and at the second cleaning temperature. 如申請專利範圍第1項之方法,其中,基座(6)在第一個清洗步驟後和第二個清洗步驟前被輔助基座(6’)更換。 The method of claim 1, wherein the susceptor (6) is replaced by the auxiliary pedestal (6') after the first cleaning step and before the second cleaning step. 如申請專利範圍第2項之方法,其中,第一清洗溫度低於第二清洗溫度。 The method of claim 2, wherein the first cleaning temperature is lower than the second cleaning temperature. 如申請專利範圍第2項之方法,其中,輔助基座(6’)是之前多次用於塗覆過程的廢舊基座(6)。 The method of claim 2, wherein the auxiliary base (6') is a used base (6) previously used for the coating process multiple times. 如申請專利範圍第2項之方法,其中,輔助基座(6’)具有比基座(6)更高的耐熱性。 The method of claim 2, wherein the auxiliary base (6') has higher heat resistance than the base (6). 如申請專利範圍第2項之方法,其中,在不同的清洗步驟中使用不同的清洗氣體。 The method of claim 2, wherein different cleaning gases are used in different cleaning steps. 如申請專利範圍第2項之方法,其中,第二清洗步驟包含多個在不同的溫度下和使用不同的腐蝕氣體進行實施的子清洗步驟。 The method of claim 2, wherein the second cleaning step comprises a plurality of sub-cleaning steps performed at different temperatures and using different etching gases. 如申請專利範圍第2項之方法,其中,在清洗步驟前的塗覆過程為MOCVD-過程,在該過程中,安放在基座(6)上的基材被塗覆塗層,其中,將第III或者第II主族元素的金屬有機化合物以及第V或者 第VI主族元素的氫化物作為過程氣體輸入製程室中。 The method of claim 2, wherein the coating process before the cleaning step is an MOCVD-process, in which the substrate placed on the susceptor (6) is coated, wherein Metal organic compounds of the III or II main group elements and the Vth The hydride of the Group VI main element is fed as a process gas into the process chamber. 如申請專利範圍第2項之方法,其中,在該清洗步驟之一中,腐蝕氣體和載氣一起輸送至製程室中。 The method of claim 2, wherein in one of the cleaning steps, the etching gas and the carrier gas are delivered together into the process chamber. 如申請專利範圍第2項之方法,其中,使用鹵素化合物,尤其是氯氣(Cl2)和/或氯化氫(HCl)或者也可使用氫氣(H2)作為腐蝕氣體。 The method of claim 2, wherein a halogen compound, in particular chlorine (Cl 2 ) and/or hydrogen chloride (HCl) or hydrogen (H 2 ) can also be used as the etching gas. 如申請專利範圍第1項之方法,其中,第一清洗溫度低於第二清洗溫度。 The method of claim 1, wherein the first cleaning temperature is lower than the second cleaning temperature. 如申請專利範圍第1項之方法,其中,在不同的清洗步驟中使用不同的清洗氣體。 The method of claim 1, wherein the different cleaning gases are used in different cleaning steps. 如申請專利範圍第1項之方法,其中,在清洗步驟前的塗覆過程為MOCVD-過程,在該過程中,安放在基座(6)上的基材被塗覆塗層,其中,將第III或者第II主族元素的金屬有機化合物以及第V或者第VI主族元素的氫化物作為過程氣體輸入製程室中。 The method of claim 1, wherein the coating process before the cleaning step is an MOCVD-process, in which the substrate placed on the susceptor (6) is coated, wherein The metal organic compound of the III or II main group element and the hydride of the V or VI main group element are introduced as process gases into the process chamber. 如申請專利範圍第3或11項之方法,其中,第一清洗溫度係介於600至650攝氏度之間,以及第二清洗溫度係高於800攝氏度。 The method of claim 3, wherein the first cleaning temperature is between 600 and 650 degrees Celsius and the second cleaning temperature is greater than 800 degrees Celsius.
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