TW202314008A - Manufacturing method of metal compound film - Google Patents
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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Abstract
Description
本發明涉及半導體製程領域,更具體地,涉及一種金屬化合物薄膜的製備方法。The invention relates to the field of semiconductor manufacturing process, and more specifically, to a method for preparing a metal compound thin film.
物理氣相沉積(Physical Vapor Deposition,簡稱PVD) 作為一種薄膜沉積技術,主要應用於各種功能薄膜的沉積,被廣泛應用於積體電路、太陽能電池、LED等的半導體領域。Physical vapor deposition (Physical Vapor Deposition, PVD for short), as a thin film deposition technology, is mainly used in the deposition of various functional thin films, and is widely used in semiconductor fields such as integrated circuits, solar cells, and LEDs.
氮化鋁(AlN)薄膜作為緩衝層或壓電層已廣泛應用在LED、微機電系統(Micro-Electro-Mechanical System,MEMS)、高電子遷移率電晶體(High Electron Mobility Transistor,HEMT)等的領域。理想狀況下,AlN薄膜的應力為零,如果AlN薄膜的應力過大,會造成薄膜受力彎曲,甚至脫落,影響器件的可靠性。AlN薄膜作為壓電層,主要沉積於Si襯底或者SiO 2襯底上,其在MEMS應用中要求應力在0±100Mpa範圍內,但是,現有的薄膜製備方法在對濺射功率、濺射溫度、濺射氣體、壓力等製程參數優化,並保持其它製程參數不變的情況下,AlN薄膜的應力基本不變,很難調整AlN(厚度為500nm~1500nm)的應力。 Aluminum nitride (AlN) thin films have been widely used as buffer layers or piezoelectric layers in LEDs, micro-electro-mechanical systems (Micro-Electro-Mechanical System, MEMS), high electron mobility transistors (High Electron Mobility Transistor, HEMT), etc. field. Ideally, the stress of the AlN film is zero. If the stress of the AlN film is too large, the film will be bent or even fall off due to force, which will affect the reliability of the device. As a piezoelectric layer, AlN films are mainly deposited on Si substrates or SiO 2 substrates. In MEMS applications, the stress is required to be within the range of 0±100Mpa. When the process parameters such as sputtering gas and pressure are optimized, and other process parameters are kept constant, the stress of the AlN film is basically unchanged, and it is difficult to adjust the stress of AlN (with a thickness of 500nm~1500nm).
因此,對於在Si襯底或者SiO 2襯底上沉積AlN薄膜來說,尋找一種新的應力可調的AlN薄膜製備方法至關重要。 Therefore, for the deposition of AlN thin films on Si substrates or SiO 2 substrates, it is very important to find a new stress-tunable AlN thin film preparation method.
本發明的目的是提出一種金屬化合物薄膜的製備方法,解決薄膜受力彎曲,甚至脫落的問題,進而提升了器件的可靠性,該製備方法包括:The purpose of the present invention is to propose a method for preparing a metal compound film, which solves the problem of bending or even falling off of the film under force, thereby improving the reliability of the device. The preparation method includes:
步驟1:將承載有待沉積薄膜的晶圓的托盤放入反應腔室中,且位於基座上方;Step 1: Put the tray carrying the wafer to be deposited into the reaction chamber and place it above the base;
步驟2:向該反應腔室內通入第一惰性氣體和製程氣體的第一混合氣體,對該反應腔室中的金屬靶材施加激勵功率,使該第一混合氣體形成等離子體,該等離子體轟擊該金屬靶材,以在該晶圓上形成金屬化合物薄膜;同時對該基座施加射頻偏壓功率,以調節該金屬化合物薄膜的應力。Step 2: Introduce the first mixed gas of the first inert gas and the process gas into the reaction chamber, apply excitation power to the metal target in the reaction chamber, and make the first mixed gas form plasma, and the plasma Bombarding the metal target to form a metal compound film on the wafer; at the same time applying radio frequency bias power to the base to adjust the stress of the metal compound film.
可選方案中,在該步驟2之後還包括:In an optional solution, after step 2, it also includes:
步驟3:向該反應腔室內通入第二惰性氣體,並對該基座施加射頻偏壓功率,使該第二惰性氣體形成等離子體,該第二惰性氣體形成的等離子體對該金屬化合物薄膜的表面進行蝕刻,以進一步調節該金屬化合物薄膜的應力。Step 3: Introduce a second inert gas into the reaction chamber, and apply radio frequency bias power to the susceptor, so that the second inert gas forms a plasma, and the plasma formed by the second inert gas forms a plasma on the metal compound film The surface is etched to further adjust the stress of the metal compound film.
可選方案中,在該步驟1之後,且在該步驟2之前還包括:In an optional solution, after the
步驟101:將該托盤和該晶圓加熱至預設溫度,以去除該托盤和該晶圓的水氣以及附著在該晶圓表面的有機雜質。Step 101: heating the tray and the wafer to a preset temperature to remove moisture from the tray and the wafer and organic impurities attached to the surface of the wafer.
可選方案中,在該步驟101之後,且在該步驟2之前還包括:In an optional solution, after the step 101, and before the step 2, it also includes:
步驟102:向該反應腔室中通入第三惰性氣體,並對該基座施加射頻偏壓功率,使該第三惰性氣體形成等離子體,該第三惰性氣體形成的等離子體轟擊該晶圓的表面,以去除該晶圓表面上的雜質。Step 102: Flowing a third inert gas into the reaction chamber, and applying radio frequency bias power to the susceptor, so that the third inert gas forms a plasma, and the plasma formed by the third inert gas bombards the wafer surface to remove impurities on the wafer surface.
可選方案中,在該步驟102之後,且在該步驟2之前還包括:In an optional solution, after the step 102, and before the step 2, it also includes:
步驟103:將擋板移至遮蓋該晶圓的上方,向該反應腔室內通入第四惰性氣體和製程氣體的第二混合氣體,對該金屬靶材施加激勵功率,使該第二混合氣體形成等離子體,進行預濺射製程;待向該反應腔室通入的該第二混合氣體的氣體流量和該激勵功率穩定後,將該擋板從該晶圓的上方移開,並維持該激勵功率和該第二混合氣體的氣體流量不變。Step 103: Move the baffle to cover the wafer, introduce a second mixed gas of a fourth inert gas and a process gas into the reaction chamber, apply excitation power to the metal target, and make the second mixed gas forming plasma, and performing a pre-sputtering process; after the gas flow rate of the second mixed gas and the excitation power introduced into the reaction chamber are stabilized, the baffle is removed from above the wafer, and the The excitation power and the gas flow rate of the second mixed gas remain unchanged.
可選方案中,該第一惰性氣體的流量小於等於200sccm,該製程氣體的流量小於等於500sccm;該製程氣體和該第一惰性氣體的流量比值大於等於4,且小於等於10,對該金屬靶材施加的激勵功率小於等於10000W,對該基座施加的射頻偏壓功率小於等於1000W。In an optional solution, the flow rate of the first inert gas is less than or equal to 200 sccm, the flow rate of the process gas is less than or equal to 500 sccm; the flow rate ratio of the process gas to the first inert gas is greater than or equal to 4, and is less than or equal to 10, the metal target The excitation power applied to the base is less than or equal to 10000W, and the RF bias power applied to the base is less than or equal to 1000W.
可選方案中,在該步驟102中,該第三惰性氣體的流量小於等於200sccm;對該基座施加的射頻偏壓功率為大於等於40W,且小於等於100W;該反應腔室的壓力大於等於6mTorr,且小於等於15mTorr。Optionally, in step 102, the flow rate of the third inert gas is less than or equal to 200 sccm; the RF bias power applied to the susceptor is greater than or equal to 40W and less than or equal to 100W; the pressure of the reaction chamber is greater than or equal to 6mTorr, and less than or equal to 15mTorr.
可選方案中,在該步驟103中,該第四惰性氣體的流量小於等於200sccm,該製程氣體的流量小於等於500sccm;該製程氣體和該第四惰性氣體的流量比值大於等於4,且小於等於10,對該金屬靶材施加的激勵功率小於等於10000W。Optionally, in step 103, the flow rate of the fourth inert gas is less than or equal to 200 sccm, the flow rate of the process gas is less than or equal to 500 sccm; the flow ratio of the process gas to the fourth inert gas is greater than or equal to 4, and is less than or equal to 10. The excitation power applied to the metal target is less than or equal to 10000W.
可選方案中,在該步驟3中,該第二惰性氣體的流量小於等於200sccm,對該基座施加的射頻偏壓功率大於等於150W,且小於等於400W。In an optional solution, in the
可選方案中,該步驟1中,該反應腔室的真空度小於等於5×10
-6Torr;該基座的溫度大於等於400℃,且小於等於600℃。
In an optional solution, in
可選方案中,該金屬靶材包括鋁、鈦、鉿或鉭,或者包括鋁的化合物、鈦的化合物、鉿的化合物或鉭的化合物。In an optional solution, the metal target includes aluminum, titanium, hafnium or tantalum, or a compound of aluminum, titanium, hafnium or tantalum.
本發明的有益效果在於:The beneficial effects of the present invention are:
本發明提供的金屬化合物薄膜的製備方法,在步驟2中,在利用由第一混合氣體形成的等離子體轟擊金屬靶材,同時對基座施加射頻偏壓功率,該射頻偏差功率會在基座上形成負偏壓,該偏壓可以優化等離子體中的離子的運動方向,以在晶圓上形成金屬化合物薄膜時調節金屬化合物薄膜的應力,使應力由張應力向壓應力轉變,促進薄膜向(002)生成晶向集中,解決了薄膜受力彎曲,甚至脫落的問題,進而提升了器件的可靠性。In the preparation method of the metal compound thin film provided by the present invention, in step 2, the plasma formed by the first mixed gas is used to bombard the metal target, and at the same time, the radio frequency bias power is applied to the base, and the radio frequency bias power will be generated on the base A negative bias voltage is formed on the surface, which can optimize the direction of movement of ions in the plasma, so as to adjust the stress of the metal compound film when the metal compound film is formed on the wafer, so that the stress changes from tensile stress to compressive stress, and promotes the film to (002) generates a concentration of crystal orientations, which solves the problem of bending or even falling off of the film under force, thereby improving the reliability of the device.
進一步地,金屬化合物薄膜濺射完成後,通過向反應腔室通入第二惰性氣體,對基座施加射頻偏壓功率,該第二惰性氣體產生的等離子體可以對金屬化合物薄膜的表面進行蝕刻,可以進一步使應力由張應力向壓應力轉變,以進一步調節金屬化合物薄膜的應力。Further, after the sputtering of the metal compound film is completed, a second inert gas is introduced into the reaction chamber, and a radio frequency bias power is applied to the susceptor, and the plasma generated by the second inert gas can etch the surface of the metal compound film , the stress can be further transformed from tensile stress to compressive stress to further adjust the stress of the metal compound film.
本發明的方法具有其它的特性和優點,這些特性和優點從併入本文中的附圖和隨後的具體實施方式中將是顯而易見的,或者將在併入本文中的附圖和隨後的具體實施方式中進行詳細陳述,這些附圖和具體實施方式共同用於解釋本發明的特定原理。The method of the present invention has other features and advantages that will be apparent from, or will be apparent from, the drawings and detailed description that follow, incorporated herein. Set forth in detail in the manner, these drawings and the detailed description together serve to explain certain principles of the present invention.
以下揭露提供用於實施本揭露之不同構件之許多不同實施例或實例。下文描述組件及配置之特定實例以簡化本揭露。當然,此等僅為實例且非意欲限制。舉例而言,在以下描述中之一第一構件形成於一第二構件上方或上可包含其中該第一構件及該第二構件經形成為直接接觸之實施例,且亦可包含其中額外構件可形成在該第一構件與該第二構件之間,使得該第一構件及該第二構件可不直接接觸之實施例。另外,本揭露可在各個實例中重複參考數字及/或字母。此重複出於簡化及清楚之目的且本身不指示所論述之各個實施例及/或組態之間的關係。The following disclosure provides many different embodiments, or examples, of different means for implementing the disclosure. Specific examples of components and configurations are described below to simplify the present disclosure. Of course, these are examples only and are not intended to be limiting. For example, in the following description a first member is formed over or on a second member may include embodiments in which the first member and the second member are formed in direct contact, and may also include embodiments in which additional members An embodiment may be formed between the first member and the second member so that the first member and the second member may not be in direct contact. Additionally, the present disclosure may repeat reference numerals and/or letters in various instances. This repetition is for simplicity and clarity and does not in itself indicate a relationship between the various embodiments and/or configurations discussed.
此外,為便於描述,諸如「下面」、「下方」、「下」、「上方」、「上」及類似者之空間相對術語可在本文中用於描述一個元件或構件與另一(些)元件或構件之關係,如圖中圖解說明。空間相對術語意欲涵蓋除在圖中描繪之定向以外之使用或操作中之裝置之不同定向。設備可以其他方式定向(旋轉90度或按其他定向)且因此可同樣解釋本文中使用之空間相對描述詞。In addition, for ease of description, spatially relative terms such as "below", "below", "under", "above", "upper" and the like may be used herein to describe the relationship between one element or member and another(s) The relationship between elements or components, as illustrated in the figure. Spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and thus the spatially relative descriptors used herein should be interpreted similarly.
儘管陳述本揭露之寬泛範疇之數值範圍及參數係近似值,然儘可能精確地報告特定實例中陳述之數值。然而,任何數值固有地含有必然由於見於各自測試量測中之標準偏差所致之某些誤差。再者,如本文中使用,術語「大約」通常意謂在一給定值或範圍之10%、5%、1%或0.5%內。替代地,術語「大約」意謂在由此項技術之一般技術者考量時處於平均值之一可接受標準誤差內。除在操作/工作實例中以外,或除非以其他方式明確指定,否則諸如針對本文中揭露之材料之數量、時間之持續時間、溫度、操作條件、數量之比率及其類似者之全部數值範圍、數量、值及百分比應被理解為在全部例項中由術語「大約」修飾。相應地,除非相反地指示,否則本揭露及隨附發明申請專利範圍中陳述之數值參數係可根據需要變化之近似值。至少,應至少鑑於所報告有效數位之數目且藉由應用普通捨入技術解釋各數值參數。範圍可在本文中表達為從一個端點至另一端點或在兩個端點之間。本文中揭露之全部範圍包含端點,除非另有指定。Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the disclosure are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements. Furthermore, as used herein, the term "about" generally means within 10%, 5%, 1%, or 0.5% of a given value or range. Alternatively, the term "about" means within an acceptable standard error of the mean when considered by one of ordinary skill in the art. Except in operating/working examples, or unless expressly specified otherwise, all numerical ranges such as for amounts of materials disclosed herein, durations of time, temperatures, operating conditions, ratios of amounts, and the like, Amounts, values and percentages should be understood as being modified by the term "about" in all instances. Accordingly, unless indicated to the contrary, the numerical parameters set forth in this disclosure and the accompanying claims are approximations that may vary as desired. At a minimum, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques. Ranges can be expressed herein as from one endpoint to the other or as between two endpoints. All ranges disclosed herein are inclusive of endpoints unless otherwise specified.
圖1示出了本發明實施例採用的磁控濺射設備的結構圖。請參閱圖1,該磁控濺射設備包括反應腔室14,在該反應腔室14的頂部設置有靶材2,在靶材2的上方設置有真空腔體15,該真空腔體15中充滿去離子水,用於冷卻靶材2,防止濺射過程中由於放熱導致靶材2升溫。而且在真空腔體15中設置有可旋轉的磁控管1,該磁控管1包括具有相反極性的內、外磁極,用於在濺射製程中提高氣體的離化率,進而提高濺射沉積速率。在反應腔室14中且位於靶材2的下方設置有基座9,該基座9上設置有支柱13,用於支撐承載有晶圓的托盤8,以使托盤8位於基座9的上方;基座9上還設置有加熱管(圖中未示出),用於朝位於其上方的托盤8和晶圓輻射熱量,從而能夠將晶圓加熱至預設溫度。可選的,基座9中還設置有冷卻裝置,用於對晶圓進行冷卻。此外,基座9是可升降的,其可以從圖1所示的傳片位上升至製程位,在此過程中,基座9會將壓環5頂起,以使基座9、上內襯3和下內襯4圍成密閉的濺射環境。在反應腔室14的一側還設置有庫10,用於容置擋板7,該擋板7用於在進行預濺射製程時從庫10移出,並移動至遮擋晶圓的上方。另外,在反應腔室14的底部設置有真空泵系統12,用於對反應腔室14進行抽氣,使反應腔室14能夠達到較高的真空度,以滿足製程所需的真空條件。Fig. 1 shows a structural diagram of a magnetron sputtering device used in an embodiment of the present invention. Please refer to Fig. 1, this magnetron sputtering equipment comprises
上述靶材2為金屬靶材,該金屬靶材可以是純金屬,也可以是金屬化合物。靶材2與激勵電源電連接,激勵電源用於向靶材2載入激勵,使靶材2相對於接地的腔體(包含上內襯3和下內襯4)形成負偏壓,以使濺射氣體(包括N
2、Ar、O
2等)放電而產生等離子體,等離子體中帶正電的離子被吸引至靶材2,轟擊靶材2的表面,濺射出的金屬原子與等離子體中的原子(例如氮原子)反應形成金屬化合物沉積在晶圓表面形成金屬化合物薄膜。可選的,上述激勵電源例如為用於載入直流功率的直流電源、用於載入脈衝直流功率的脈衝直流電源,或者直流電源(或脈衝直流電源)與射頻電源的結合。
The above-mentioned target material 2 is a metal target material, and the metal target material may be a pure metal or a metal compound. The target 2 is electrically connected to the excitation power supply, and the excitation power is used to load the excitation to the target 2, so that the target 2 forms a negative bias voltage relative to the grounded cavity (including the
本發明第一實施例提供了一種金屬化合物薄膜的製備方法,請參考圖2,該金屬化合物薄膜的製備方法包括:The first embodiment of the present invention provides a method for preparing a metal compound film, please refer to Figure 2, the method for preparing the metal compound film includes:
步驟1:將承載有待沉積薄膜的晶圓的托盤放入反應腔室中,且位於基座上方;Step 1: Put the tray carrying the wafer to be deposited into the reaction chamber and place it above the base;
步驟2:向反應腔室內通入第一惰性氣體和製程氣體的第一混合氣體,對反應腔室中的金屬靶材施加激勵功率,使該第一混合氣體形成等離子體,該等離子體轟擊金屬靶材,以在晶圓上形成金屬化合物薄膜;同時對基座施加射頻偏壓功率,以調整金屬化合物薄膜的應力。Step 2: Introduce the first mixed gas of the first inert gas and the process gas into the reaction chamber, apply excitation power to the metal target in the reaction chamber, make the first mixed gas form plasma, and the plasma bombards the metal target material to form a metal compound film on the wafer; at the same time, RF bias power is applied to the base to adjust the stress of the metal compound film.
可選的,上述第一惰性氣體例如包括氬氣、氪氣等;製程氣體例如包括氧氣、氮氣等。在實際應用中,第一惰性氣體和製程氣體可以通過流量計連接到反應腔室。Optionally, the above-mentioned first inert gas includes, for example, argon, krypton, etc.; the process gas includes, for example, oxygen, nitrogen, and the like. In practical applications, the first inert gas and the process gas can be connected to the reaction chamber through flow meters.
在上述步驟2中,在對反應腔室中的金屬靶材施加激勵功率時,高壓條件下,使第一惰性氣體和製程氣體電離放電而產生帶正電的等離子體,帶正電的等離子體被金屬靶材吸引並轟擊金屬靶材。當等離子體的能量足夠高時,會使金屬靶材表面的原子逸出並沉積在晶圓上,以實現對晶圓表面的薄膜沉積。隨著靶材表面逸出的金屬原子和製程氣體中的原子結合形成金屬化合物沉積在晶圓表面並在晶圓表面發生遷移,同時向基座施加的射頻偏壓功率可以促進金屬化合物在晶圓表面向一定的方向遷移,射頻偏壓功率使基座表面形成的負偏壓可以優化等離子體中的離子的運動方向,以在晶圓上形成金屬化合物薄膜時調節金屬化合物薄膜的應力,使應力由張應力向壓應力轉變,促進薄膜向(002)生成晶向集中,解決了薄膜受力彎曲,甚至脫落的問題,進而提升了器件的可靠性。In the above step 2, when the excitation power is applied to the metal target in the reaction chamber, under high pressure conditions, the first inert gas and the process gas are ionized and discharged to generate positively charged plasma, and the positively charged plasma Attracted by and bombards the metal target. When the energy of the plasma is high enough, the atoms on the surface of the metal target will escape and be deposited on the wafer, so as to achieve thin film deposition on the wafer surface. As the metal atoms escaping from the surface of the target combine with the atoms in the process gas to form a metal compound that deposits on the wafer surface and migrates on the wafer surface, at the same time, the RF bias power applied to the susceptor can promote the metal compound on the wafer. The surface migrates to a certain direction, and the negative bias voltage formed on the surface of the base by the RF bias power can optimize the movement direction of the ions in the plasma, so as to adjust the stress of the metal compound film when the metal compound film is formed on the wafer, so that the stress The transition from tensile stress to compressive stress promotes the concentration of the film to the (002) crystal orientation, which solves the problem of bending or even falling off of the film under force, thereby improving the reliability of the device.
第二實施例second embodiment
請參考圖3,本發明第二實施例提供的金屬化合物薄膜的製備方法,其是在上述第一實施例基礎上所做的改進,具體地,該金屬化合物薄膜的製備方法同樣包括步驟1和步驟2,二者與上述第一實施例相同,在此不再重複描述。Please refer to Fig. 3, the preparation method of the metal compound thin film provided by the second embodiment of the present invention is an improvement made on the basis of the first embodiment above, specifically, the preparation method of the metal compound thin film also includes
在上述步驟2之後,製備方法還包括:After the above step 2, the preparation method also includes:
步驟3、向反應腔室內通入第二惰性氣體,並對基座施加射頻偏壓功率,使該第二惰性氣體形成等離子體,該第二惰性氣體形成的等離子體對金屬化合物薄膜的表面進行蝕刻,以進一步調節金屬化合物薄膜的應力。Step 3: Introduce a second inert gas into the reaction chamber, and apply radio frequency bias power to the susceptor, so that the second inert gas forms a plasma, and the plasma formed by the second inert gas conducts the surface of the metal compound film Etching to further adjust the stress of the metal compound film.
通過向反應腔室通入第二惰性氣體,對基座施加射頻偏壓功率,該第二惰性氣體產生的等離子體可以對金屬化合物薄膜的表面進行蝕刻,以蝕刻去除薄膜表面上品質較差的部分,同時可以進一步使應力由張應力向壓應力轉變,以進一步調節金屬化合物薄膜的應力。By feeding a second inert gas into the reaction chamber and applying radio frequency bias power to the base, the plasma generated by the second inert gas can etch the surface of the metal compound film to etch and remove the poor quality part on the film surface , and at the same time, the stress can be further transformed from tensile stress to compressive stress to further adjust the stress of the metal compound film.
以在晶圓表面沉積氮化鋁薄膜為例,上述步驟2之後,上述步驟3具體包括:可以停止載入激勵功率和射頻偏壓功率,並停止惰性氣體和製程氣體的通入,維持加熱溫度和基座位置(製程位)不變;向反應腔室通入第二惰性氣體(例如Ar),第二惰性氣體的流量小於等於200sccm,優選大於等於100sccm,且小於等於200sccm。真空泵系統中的冷泵門閥處於全開狀態,以確保能夠將反應腔室中的雜質氣體排出。對基座施加射頻偏壓功率,可選的,對上述基座施加的射頻偏壓功率大於等於150W,且小於等於400W。Taking the deposition of aluminum nitride film on the surface of the wafer as an example, after the above step 2, the
第三實施例third embodiment
請參考圖4,本發明第二實施例提供的金屬化合物薄膜的製備方法,其是在上述第二實施例基礎上所做的改進,具體地,該金屬化合物薄膜的製備方法同樣包括步驟1、步驟2和步驟3,三者與上述第二實施例相同,在此不再重複描述。Please refer to Fig. 4, the method for preparing a metal compound thin film provided in the second embodiment of the present invention is an improvement made on the basis of the second embodiment above, specifically, the method for preparing a metal compound thin film also includes
在此基礎上,製備方法還包括步驟101、步驟102和步驟103中的至少一者。下面以在晶圓表面沉積氮化鋁薄膜,且製備方法在包括步驟1、步驟2和步驟3的基礎上,還包括步驟101、步驟102和步驟103為例,對製備方法進行詳細說明。On this basis, the preparation method further includes at least one of step 101, step 102 and step 103. The preparation method will be described in detail below by taking the deposition of an aluminum nitride film on the surface of the wafer, and the preparation
具體地,根據沉積的薄膜不同,對反應腔室設定適合的製程條件,將承載有待沉積薄膜的晶圓(如矽或二氧化矽)的托盤放入反應腔室中,且位於基座上方,即,放置於基座上的支柱頂端;將基座的溫度調節至製程所需的溫度,例如在沉積氮化鋁薄膜時,反應腔室的真空度小於5×10 -6Torr;基座的溫度大於等於400℃,且小於等於600℃,如為500℃。可選的,在沉積諸如氮化鋁薄膜等的不導電薄膜時,向靶材載入的激勵功率可以為脈衝直流功率,這可以避免因載入直流功率而容易在金屬靶材表面形成金屬氮化物,影響金屬靶材的金屬原子逸出。 Specifically, according to the different deposited films, set suitable process conditions for the reaction chamber, put the tray carrying the wafer (such as silicon or silicon dioxide) to be deposited into the reaction chamber, and place it on the base, That is, the top of the pillar placed on the base; the temperature of the base is adjusted to the temperature required by the process, for example, when depositing aluminum nitride film, the vacuum degree of the reaction chamber is less than 5×10 -6 Torr; The temperature is greater than or equal to 400°C and less than or equal to 600°C, such as 500°C. Optionally, when depositing non-conductive films such as aluminum nitride films, the excitation power loaded to the target can be pulsed DC power, which can avoid the formation of metal nitrogen on the surface of the metal target due to the loading of DC power. Compounds, which affect the escape of metal atoms from the metal target.
本實施例中,在步驟1之後,且在步驟2之前還包括:In this embodiment, after
步驟101:將托盤和晶圓加熱至預設溫度,以去除托盤和晶圓的水氣以及附著在晶圓表面的有機雜質。Step 101: heating the tray and the wafer to a preset temperature to remove moisture from the tray and the wafer and organic impurities attached to the surface of the wafer.
具體可以為,利用基座上的加熱管對托盤和晶圓進行加熱,以使其緩慢升溫至預設溫度,該預設溫度例如大於等於300℃,且小於等於1000℃,優選為大於等於450℃,且小於等於800℃,並維持10s~200s,優選為20s~60s。通過將托盤和晶圓加熱至預設溫度,可以在高溫條件下去除托盤和晶圓的水氣及附著晶圓表面的有機雜質。Specifically, the tray and the wafer can be heated by the heating tube on the base to slowly raise the temperature to a preset temperature, the preset temperature is, for example, greater than or equal to 300° C. and less than or equal to 1000° C., preferably greater than or equal to 450° C. °C, and less than or equal to 800 °C, and maintained for 10s~200s, preferably 20s~60s. By heating the tray and wafer to a preset temperature, the water vapor of the tray and wafer and the organic impurities attached to the surface of the wafer can be removed under high temperature conditions.
本實施例中,在步驟101之後,且在步驟2之前還包括:In this embodiment, after step 101 and before step 2, it also includes:
步驟102:向反應腔室中通入第三惰性氣體,並對基座施加射頻偏壓功率,使該第三惰性氣體形成等離子體,該第三惰性氣體形成的等離子體轟擊晶圓的表面,以去除晶圓表面上的雜質。Step 102: injecting a third inert gas into the reaction chamber, and applying radio frequency bias power to the susceptor, so that the third inert gas forms plasma, and the plasma formed by the third inert gas bombards the surface of the wafer, To remove impurities on the wafer surface.
具體可以為:維持步驟101中採用的加熱溫度不變,向反應腔室內通入第三惰性氣體,如氬氣(Ar),可選的,第三惰性氣體的流量小於等於200sccm,優選大於等於100sccm,且小於等於200sccm。將腔室壓力維持在較高的壓力範圍,例如大於等於6mTorr,且小於等於15mTorr。對基座施加射頻偏壓功率,該射頻偏壓功率採用較低的功率範圍,以使第三惰性氣體形成的等離子體中的離子能夠轟擊晶圓表面,以去除晶圓表面上的雜質和氧化物,減少晶圓表面缺陷,增加晶圓表面的活性。可選的,對基座施加的射頻偏壓功率為大於等於40W,且小於等於100W。另外,在對基座施加的射頻偏壓功率穩定後,可以將製程壓力(即,腔室壓力)降低至原來的二分之一左右(如大於等於3mTorr,且小於等於8mTorr),開始正式進行預清洗處理製程(即,步驟102)。Specifically, the heating temperature adopted in step 101 can be kept constant, and a third inert gas, such as argon (Ar), is introduced into the reaction chamber. Optionally, the flow rate of the third inert gas is less than or equal to 200 sccm, preferably greater than or equal to 100sccm, and less than or equal to 200sccm. The chamber pressure is maintained in a relatively high pressure range, for example greater than or equal to 6 mTorr and less than or equal to 15 mTorr. Applying radio frequency bias power to the susceptor, the radio frequency bias power adopts a lower power range, so that ions in the plasma formed by the third inert gas can bombard the wafer surface to remove impurities and oxidation on the wafer surface substances, reduce wafer surface defects, and increase wafer surface activity. Optionally, the RF bias power applied to the base is greater than or equal to 40W and less than or equal to 100W. In addition, after the RF bias power applied to the susceptor is stabilized, the process pressure (that is, the chamber pressure) can be reduced to about half of the original (such as greater than or equal to 3mTorr, and less than or equal to 8mTorr), and the formal process can be started. Pre-cleaning treatment process (ie, step 102 ).
本實施例中,在步驟102之後,且在步驟2之前還包括步驟103:In this embodiment, after step 102, step 103 is also included before step 2:
將擋板移至遮蓋晶圓的上方,向反應腔室內通入第四惰性氣體和製程氣體的第二混合氣體,對金屬靶材施加激勵功率,使該第二混合氣體形成等離子體,進行預濺射製程;待向反應腔室通入的該第二混合氣體的氣體流量和激勵功率穩定後(穩定的指標為氣體流量的波動範圍不大於±0.1%;激勵功率的波動範圍不大於±0.1%),將擋板從晶圓的上方移開,並維持該激勵功率和該第二混合氣體的氣體流量不變。Move the baffle to the top of the covering wafer, introduce the second mixed gas of the fourth inert gas and the process gas into the reaction chamber, apply excitation power to the metal target, make the second mixed gas form plasma, and perform a preliminary Sputtering process; after the gas flow and excitation power of the second mixed gas fed into the reaction chamber are stabilized (the stable index is that the fluctuation range of the gas flow is not greater than ±0.1%; the fluctuation range of the excitation power is not greater than ±0.1% %), remove the baffle from above the wafer, and keep the excitation power and the gas flow rate of the second mixed gas constant.
上述步驟103為預濺射製程。具體可以為,停止通入第三惰性氣體,關閉對基座施加的射頻偏壓功率,將基座調整至預濺射工位,將擋板移入反應腔室,並移至遮蓋晶圓的上方;向反應腔室中通入第四惰性氣體(如Ar)和製程氣體(如N 2)的第二混合氣體,其中第四惰性氣體的流量小於等於200sccm,優選大於等於15sccm,且小於等於45sccm,製程氣體的流量小於等於500sccm,優選為大於等於90sccm,且小於等於300sccm,製程氣體和第四惰性氣體的流量比值大於等於4,且小於等於10,對金屬靶材施加的激勵功率小於等於10000W,優選大於等於5000W,且小於等於9000W,並維持20s左右。待反應腔室的反應濺射環境穩定後,維持激勵功率和氣體流量不變,維持真空泵系統中的冷泵門閥處於全開狀態,將擋板從晶圓上移開,並維持1s左右。由於反應腔室濺射初期功率和氣體流量不穩定,形成的金屬化合物薄膜品質不佳,借助上述步驟103,可以使晶圓上形成的金屬化合物薄膜在初始階段也滿足較高的品質要求。 The above step 103 is a pre-sputtering process. Specifically, stop feeding the third inert gas, turn off the RF bias power applied to the base, adjust the base to the pre-sputtering station, move the baffle into the reaction chamber, and move it to cover the wafer ; Introducing a second mixed gas of a fourth inert gas (such as Ar) and a process gas (such as N 2 ) into the reaction chamber, wherein the flow rate of the fourth inert gas is less than or equal to 200 sccm, preferably greater than or equal to 15 sccm, and less than or equal to 45 sccm , the flow rate of the process gas is less than or equal to 500 sccm, preferably greater than or equal to 90 sccm, and less than or equal to 300 sccm, the flow ratio of the process gas to the fourth inert gas is greater than or equal to 4, and less than or equal to 10, and the excitation power applied to the metal target is less than or equal to 10000W , preferably greater than or equal to 5000W, and less than or equal to 9000W, and maintain it for about 20s. After the reactive sputtering environment in the reaction chamber is stable, keep the excitation power and gas flow constant, keep the cold pump valve in the vacuum pump system fully open, remove the baffle from the wafer, and keep it for about 1s. Since the initial power and gas flow rate of the reaction chamber are not stable during sputtering, the quality of the formed metal compound film is poor. With the help of the above step 103, the metal compound film formed on the wafer can also meet higher quality requirements at the initial stage.
待反應腔室反應濺射環境穩定後,開始執行上述步驟2。具體地,維持激勵功率,溫度和製程氣氛不變,將基座升至製程位。晶圓與靶材之間的距離例如大於等於30mm,且小於等於80mm,優選大於等於40mm,且小於等於60mm,這樣,既可以保證薄膜的高生長速率,又可以保證金屬化合物薄膜的結晶品質。After the reactive sputtering environment in the reaction chamber is stable, the above step 2 is started. Specifically, the excitation power is maintained, the temperature and the process atmosphere are kept constant, and the susceptor is raised to the process position. The distance between the wafer and the target is, for example, greater than or equal to 30 mm and less than or equal to 80 mm, preferably greater than or equal to 40 mm and less than or equal to 60 mm. In this way, both the high growth rate of the film and the crystallization quality of the metal compound film can be guaranteed.
對基座施加小於等於1000W的射頻偏壓功率,優選大於等於50W,且小於等於300W,載入的射頻偏壓功率越高,薄膜的應力由張應力向壓應力轉變的趨勢越大,基於此,當生成的金屬化合物薄膜張應力較大時,可以通過提高射頻偏壓功率來降低張應力,當生成的金屬化合物薄膜的張應力較小時,可以通過降低射頻偏壓功率來提高張應力。與此同時,結合使用基座中加熱管對晶圓進行加熱,可以維持較高的製程溫度,保證了金屬化合物薄膜的結晶品質。該金屬化合物薄膜的結晶品質與製程溫度呈正向變化,同時製程溫度越高,金屬化合物薄膜的張應力越大,這就需要更高的射頻偏壓功率進行應力的調節,使其向壓應力轉變。隨著靶材表面逸出的金屬原子(例如Al原子)和製程氣體形成的等離子體中的原子(例如N原子)結合,沉積在晶圓表面並在晶圓表面發生遷移,基座施加射頻偏壓功率可以促進金屬化合物在晶圓表面向一定的方向遷移,射頻偏壓功率使基座表面形成的負偏壓促進金屬化合物向(002)生長晶向集中,從而調整金屬化合物薄膜的應力由張應力向壓應力轉變。金屬化合物薄膜在晶向(002)的結晶品質更優。(002)是固體物理中材料內部原子結構的排列取向。Apply a radio frequency bias power of less than or equal to 1000W to the base, preferably greater than or equal to 50W, and less than or equal to 300W, the higher the loaded radio frequency bias power, the greater the tendency of the stress of the film to change from tensile stress to compressive stress, based on this , when the tensile stress of the generated metal compound film is large, the tensile stress can be reduced by increasing the RF bias power, and when the tensile stress of the generated metal compound film is small, the tensile stress can be increased by reducing the RF bias power. At the same time, combined with the use of heating tubes in the susceptor to heat the wafer, a relatively high process temperature can be maintained to ensure the crystallization quality of the metal compound film. The crystallization quality of the metal compound film is positively changed with the process temperature. At the same time, the higher the process temperature, the greater the tensile stress of the metal compound film, which requires higher RF bias power to adjust the stress to transform it to compressive stress. . As the metal atoms (such as Al atoms) escaped from the target surface combine with the atoms (such as N atoms) in the plasma formed by the process gas, they are deposited on the wafer surface and migrate on the wafer surface, and the base applies RF bias. The voltage power can promote the metal compound to migrate in a certain direction on the wafer surface, and the RF bias power makes the negative bias formed on the surface of the susceptor promote the concentration of the metal compound to the (002) growth crystal direction, thereby adjusting the stress of the metal compound film from tension Stress changes to compressive stress. The crystallization quality of the metal compound film is better in the crystal direction (002). (002) is the arrangement orientation of the internal atomic structure of the material in solid state physics.
可選的,上述步驟2中,沉積速率控制在10~20A/s,直至金屬化合物薄膜的厚度達到製程需要的厚度。金屬化合物薄膜的厚度一般控制在200nm~1300nm。Optionally, in the above step 2, the deposition rate is controlled at 10-20A/s until the thickness of the metal compound film reaches the thickness required by the process. The thickness of the metal compound film is generally controlled at 200nm~1300nm.
在執行完成上述步驟3之後,停止對基座施加射頻偏壓功率,停止氣體通入,降低製程溫度,將腔室抽至高真空。基座從製程位降至傳片位,將沉積完成的晶圓移出製程腔室,完成金屬化合物薄膜的製備。After the
本發明實施例提供的金屬化合物薄膜的製備方法,在步驟2中,在利用由第一混合氣體形成的等離子體轟擊金屬靶材,同時對基座施加射頻偏壓功率,該射頻偏差功率會在基座上形成負偏壓,該偏壓可以優化等離子體中的離子的運動方向,以在晶圓上形成金屬化合物薄膜時調節金屬化合物薄膜的應力,使應力由張應力向壓應力轉變,促進薄膜向(002)生成晶向集中,解決了薄膜受力彎曲,甚至脫落的問題,進而提升了器件的可靠性。進一步地,通過向反應腔室通入第二惰性氣體,對基座施加射頻偏壓功率,該第二惰性氣體產生的等離子體可以對金屬化合物薄膜的表面進行蝕刻,可以進一步使應力由張應力向壓應力轉變,以進一步調節金屬化合物薄膜的應力。In the preparation method of the metal compound thin film provided by the embodiment of the present invention, in step 2, the metal target is bombarded with the plasma formed by the first mixed gas, and at the same time, the RF bias power is applied to the susceptor, and the RF bias power will be A negative bias voltage is formed on the base, which can optimize the direction of movement of ions in the plasma to adjust the stress of the metal compound film when the metal compound film is formed on the wafer, so that the stress changes from tensile stress to compressive stress, promoting The film is concentrated toward the (002) crystal direction, which solves the problem of bending or even falling off of the film under force, thereby improving the reliability of the device. Further, by introducing a second inert gas into the reaction chamber and applying radio frequency bias power to the base, the plasma generated by the second inert gas can etch the surface of the metal compound film, and the stress can be further changed from tensile stress to Shift to compressive stress to further tune the stress of metal compound films.
圖5示出了根據本發明兩個不同的實施例製備的氮化鋁薄膜的應力對比圖。橫坐標為施加的射頻偏壓功率(RF Bias),縱坐標為氮化鋁薄膜的應力(Stress),其中,正數為張應力,負數為壓應力。圖5中的實線表示在採用上述第一實施例中的方法沉積形成氮化鋁薄膜時,對基座施加射頻偏壓功率(Bias Process),施加的射頻偏壓功率的大小對氮化鋁薄膜應力的影響;圖5中的虛線表示在採用上述第二實施例中的方法沉積形成氮化鋁薄膜時,對基座施加射頻偏壓功率,在形成氮化鋁薄膜後,繼續對基座施加射頻偏壓功率(Bias Process+Bias Etch),對氮化鋁薄膜應力的影響。對比實線和虛線可知,相比於採用第一實施例中的方法,採用上述第二實施例中的方法可以進一步使應力由張應力向壓應力轉變。Fig. 5 shows a stress contrast diagram of aluminum nitride films prepared according to two different embodiments of the present invention. The abscissa is the applied radio frequency bias power (RF Bias), and the ordinate is the stress (Stress) of the aluminum nitride film, where the positive number is the tensile stress and the negative number is the compressive stress. The solid line in Fig. 5 indicates that when the aluminum nitride film is deposited and formed by the method in the above-mentioned first embodiment, the RF bias power (Bias Process) is applied to the base, and the magnitude of the applied RF bias power has a great influence on the aluminum nitride film The influence of film stress; the dotted line in Fig. 5 shows that when adopting the method in the above-mentioned second embodiment to deposit and form aluminum nitride film, apply radio frequency bias power to base, after forming aluminum nitride film, continue to base The effect of RF bias power (Bias Process+Bias Etch) on the stress of aluminum nitride film. Comparing the solid line and the dotted line, it can be seen that compared with the method in the first embodiment, the stress in the second embodiment above can further transform the stress from the tensile stress to the compressive stress.
圖6示出了根據本發明實施例和現有技術製備的氮化鋁薄膜的XRD測試結果對比圖。圖6的橫坐標為角度Angle((002)晶向),縱坐標為氮化鋁的強度Intensity。圖6中的虛線表示在現有技術採用的氮化鋁薄膜的製備方法沉積形成氮化鋁薄膜時,沒有對基座施加射頻偏壓功率;圖6中的實線表示在本發明實施例採用的氮化鋁薄膜的製備方法沉積形成氮化鋁薄膜時,對基座施加了射頻偏壓功率。對比實線和虛線可知,對基座施加射頻偏壓功率後,氮化鋁薄膜更多的向(002)晶向方向生長,作為本領域技術人員的公知常識形成氮化鋁薄膜時,在向(002)晶向方向生長的同時,也有部分向(102)晶向方向生長,為了提高薄膜品質,期望氮化鋁薄膜向(002)晶向方向生長。FIG. 6 shows a comparison chart of XRD test results of aluminum nitride thin films prepared according to the embodiment of the present invention and the prior art. The abscissa of Figure 6 is the angle Angle ((002) crystal orientation), and the ordinate is the intensity of aluminum nitride. The dotted line in Fig. 6 indicates that when the aluminum nitride thin film is deposited and formed by the preparation method of the aluminum nitride thin film adopted in the prior art, no radio frequency bias power is applied to the susceptor; the solid line in Fig. Preparation method of aluminum nitride film When depositing and forming the aluminum nitride film, a radio frequency bias power is applied to the base. Comparing the solid line and the dotted line, it can be seen that after the RF bias power is applied to the base, the aluminum nitride film grows more towards the (002) crystal direction. While growing in the direction of (002) crystal orientation, some of them also grow in the direction of (102) crystal orientation. In order to improve the quality of the film, it is expected that the aluminum nitride film grows in the direction of (002) crystal orientation.
以上描述以形成氮化鋁薄膜為例,應該理解本發明的方法還可以製備其他金屬化合物薄膜,如用於製備鈦、鉿或鉭的金屬化合物薄膜。The above description takes the formation of aluminum nitride thin film as an example, it should be understood that the method of the present invention can also prepare other metal compound thin films, such as metal compound thin films for preparing titanium, hafnium or tantalum.
前述內容概括數項實施例之特徵,使得熟習此項技術者可更佳地理解本揭露之態樣。熟習此項技術者應瞭解,其等可容易地使用本揭露作為用於設計或修改用於實行本文仲介紹之實施例之相同目的及/或達成相同優點之其他製程及結構之一基礎。熟習此項技術者亦應瞭解,此等等效構造不背離本揭露之精神及範疇,且其等可在不背離本揭露之精神及範疇之情況下在本文中作出各種改變、置換及更改。The foregoing content summarizes the features of several embodiments, so that those skilled in the art can better understand aspects of the present disclosure. Those skilled in the art should appreciate that they can readily use the present disclosure as a basis for designing or modifying other processes and structures for carrying out the same purposes and/or achieving the same advantages of the embodiments described herein. Those skilled in the art should also understand that such equivalent constructions do not depart from the spirit and scope of the present disclosure, and that they can make various changes, substitutions and alterations herein without departing from the spirit and scope of the present disclosure.
當結合附圖閱讀時,從以下詳細描述最佳理解本揭露之態樣。應注意,根據產業中之標準實踐,各種構件未按比例繪製。事實上,為了論述的清楚起見可任意增大或減小各種構件之尺寸。 圖1示出了本發明實施例採用的磁控濺射設備的結構圖; 圖2示出了本發明第一實施例提供的金屬化合物薄膜的製備方法的流程圖; 圖3示出了本發明第二實施例提供的金屬化合物薄膜的製備方法的流程圖; 圖4示出了本發明第三實施例提供的金屬化合物薄膜的製備方法的流程圖; 圖5示出了根據本發明兩個不同的實施例製備的金屬化合物薄膜的應力對比圖; 圖6示出了根據本發明實施例和現有技術製備的金屬化合物薄膜的薄膜XRD測試結果對比圖。 Aspects of the present disclosure are best understood from the following detailed description when read with the accompanying drawings. It should be noted that, in accordance with the standard practice in the industry, various components are not drawn to scale. In fact, the dimensions of the various components may be arbitrarily increased or decreased for clarity of discussion. Fig. 1 shows the structural diagram of the magnetron sputtering equipment that the embodiment of the present invention adopts; Fig. 2 shows the flowchart of the preparation method of the metal compound film provided by the first embodiment of the present invention; Fig. 3 shows the flowchart of the preparation method of the metal compound thin film provided by the second embodiment of the present invention; Fig. 4 shows the flowchart of the preparation method of the metal compound film provided by the third embodiment of the present invention; Fig. 5 shows the stress contrast figure of the metal compound film prepared according to two different embodiments of the present invention; FIG. 6 shows a comparison chart of thin film XRD test results of metal compound thin films prepared according to the embodiment of the present invention and the prior art.
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JP6030589B2 (en) * | 2014-02-13 | 2016-11-24 | 株式会社アルバック | Hard mask forming method and hard mask forming apparatus |
TWI564410B (en) * | 2014-04-25 | 2017-01-01 | 明志科技大學 | Physical vapor deposition of an aluminium nitride film |
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CN107267934B (en) * | 2017-05-13 | 2019-03-22 | 宁波工程学院 | A kind of screw in injection molding machine surface reinforcing method |
CN210727894U (en) * | 2018-11-30 | 2020-06-12 | 深圳先进技术研究院 | Super-hydrophobic medical instrument |
CN110218984B (en) * | 2019-07-17 | 2022-11-25 | 北京北方华创微电子装备有限公司 | Thin film deposition method |
US11492700B2 (en) * | 2019-10-18 | 2022-11-08 | Taiwan Semiconductor Manufacturing Co. | Shutter disk having lamp, power, and/or gas modules arranged at the first side of the shutter disk of thin film deposition chamber |
CN111058090B (en) * | 2020-01-03 | 2021-08-13 | 北京北方华创微电子装备有限公司 | Preparation method of metal nitride hard mask |
CN111286696B (en) * | 2020-03-24 | 2022-11-25 | 北京北方华创微电子装备有限公司 | Preparation method of semiconductor hard mask film |
CN111850469A (en) * | 2020-07-20 | 2020-10-30 | 中国科学院兰州化学物理研究所 | DLC resistive electrode in-situ preparation method for large-area microstructure gas detector |
CN112760602B (en) * | 2020-12-14 | 2022-08-16 | 北京北方华创微电子装备有限公司 | Method for depositing metal nitride film |
CN112708852B (en) * | 2020-12-22 | 2022-12-16 | 安徽工业大学 | Method for improving performance of AlCrN coating cutter through in-situ high-energy Ar + etching post-treatment |
CN113862622B (en) * | 2021-09-24 | 2023-10-13 | 北京北方华创微电子装备有限公司 | Preparation method of metal compound film |
-
2021
- 2021-09-24 CN CN202111123778.8A patent/CN113862622B/en active Active
-
2022
- 2022-09-16 TW TW111135164A patent/TWI810071B/en active
- 2022-09-16 WO PCT/CN2022/119220 patent/WO2023045835A1/en unknown
Also Published As
Publication number | Publication date |
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WO2023045835A1 (en) | 2023-03-30 |
CN113862622B (en) | 2023-10-13 |
CN113862622A (en) | 2021-12-31 |
TWI810071B (en) | 2023-07-21 |
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