TW201913129A - Silicon wafer evaluation method and silicon wafer manufacturing method - Google Patents
Silicon wafer evaluation method and silicon wafer manufacturing method Download PDFInfo
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- H—ELECTRICITY
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- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
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- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B2203/00—Details of cleaning machines or methods involving the use or presence of liquid or steam
- B08B2203/005—Details of cleaning machines or methods involving the use or presence of liquid or steam the liquid being ozonated
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
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Abstract
Description
本發明係關於一種矽晶圓的評價方法及矽晶圓的製造方法。The present invention relates to a method for evaluating a tantalum wafer and a method for manufacturing a tantalum wafer.
研磨後的晶圓品質日益改善，在確認研磨洗淨後的晶圓品質的同時，將所確認的異常區分為源自研磨、源自洗淨或源自結晶則正變得困難。The quality of the wafer after polishing is improving, and it is becoming difficult to distinguish the confirmed abnormality from polishing, from washing, or from crystallization, while confirming the quality of the wafer after polishing.
目前，為了評估研磨狀態的品質，僅有研磨大量的晶圓而追蹤品質的傾向，而由於品質的差異將隨各樣的外在要素改變因而難以評價。又過往僅單次測定研磨後的晶圓，在製造數量龐大的晶圓的過程中即使如過往進行抽樣檢查，亦十分難以檢測出研磨品質的異常。又到了能夠顯著判別異常值的階段時通常已經為時已晚。At present, in order to evaluate the quality of the polishing state, only a large number of wafers are polished and the quality tends to be traced, and since the difference in quality is changed with various external elements, it is difficult to evaluate. In the past, only the polished wafer was measured in a single pass. Even in the process of manufacturing a large number of wafers, it is extremely difficult to detect the abnormality of the polishing quality even if the sample inspection is performed in the past. It is usually too late to reach a stage where the abnormal value can be discerned significantly.
雖作作為表面品質評價的方法過往有SC1-RT法，但此係用以進行源自矽結晶的缺陷或金屬汙染的評價的方法，並非用以評價源自研磨等加工的缺陷(加工缺陷)的方法(專利文獻1)。Although the SC1-RT method has been used as a method for evaluating surface quality, this method for evaluating defects or metal contamination derived from ruthenium crystal is not used to evaluate defects derived from processing such as grinding (machining defects). Method (Patent Document 1).
又，由於SC1-RT為使用鹼性水溶液，在原理上將會在Si、SiO2 進行蝕刻，因此晶圓表面粗糙的惡化十分顯著。Further, since SC1-RT uses an alkaline aqueous solution, Si and SiO 2 are etched in principle, so that the deterioration of the surface roughness of the wafer is remarkable.
又，過往的藉由臭氧水及HF處理的晶圓的品質評價方法，包含將自然氧化膜全部除去(剝離)的步驟(專利文獻2)，若是如此進行氧化膜的完全除去，則會引起源自結晶的缺陷的顯現存在化，而無法評價研磨等的加工缺陷。In addition, the method for evaluating the quality of wafers treated with ozone water and HF in the past includes a step of removing (peeling) all of the natural oxide film (Patent Document 2). If the oxide film is completely removed, the source is caused. The appearance of defects due to crystallization is present, and processing defects such as polishing cannot be evaluated.
〔先前技術文獻〕 ［專利文獻］ 專利文獻1：日本特開2002-353281號公報 專利文獻2：日本特開2013-004760號公報[PRIOR ART DOCUMENT] Patent Document 1: JP-A-2002-353281 (Patent Document 2)
〔發明欲解決的問題〕 本發明有鑑於上述問題，目的在於提供一種矽晶圓的評價方法，能夠將源自結晶的缺陷及因洗淨等而產生的顆粒等予以除外，僅將源自研磨等的加工的缺陷予以評價。 〔解決問題的技術手段〕[Problem to be Solved by the Invention] The present invention has been made in view of the above problems, and an object of the invention is to provide a method for evaluating a germanium wafer, which can exclude defects derived from crystals and particles generated by washing or the like, and only originate from polishing. The defects of processing such as are evaluated. [Technical means to solve the problem]
為了解決上述問題，本發明提供一種矽晶圓的評價方法，包含：一前表面缺陷測定步驟，對一矽晶圓預先進行表面缺陷測定；一洗淨步驟，對該矽晶圓交互地重複氧化處理及氧化膜除去處理，該氧化處理係藉由臭氧水以進行，該氧化膜除去處理係在不完全除去形成於該矽晶圓表面的氧化膜的條件下以氫氟酸進行；以及一增加缺陷測定步驟，對該洗淨步驟後的該矽晶圓進行表面缺陷測定，以將相對於該前表面缺陷測定步驟所測定的缺陷而增加的增加缺陷予以測定，其中，交互地重複該洗淨步驟及該增加缺陷測定步驟複數次，基於各次洗淨步驟後的該增加缺陷的測定結果以評價該矽晶圓。In order to solve the above problems, the present invention provides a method for evaluating a germanium wafer, comprising: a front surface defect measuring step of pre-measuring surface defects on a germanium wafer; and a cleaning step of alternately repeating oxidation of the germanium wafer Treatment and oxide film removal treatment by ozone water, which is carried out with hydrofluoric acid under conditions that do not completely remove the oxide film formed on the surface of the tantalum wafer; a defect measuring step of performing surface defect measurement on the germanium wafer after the cleaning step to measure an increased defect increased with respect to the defect measured in the front surface defect measuring step, wherein the cleaning is alternately repeated The step and the step of increasing the defect measurement are performed plural times, and the measurement result of the increased defect after each cleaning step is used to evaluate the silicon wafer.
依據如此的矽晶圓的評價方法，能夠不使於洗淨步驟中源自結晶的缺陷顯著化而僅使加工缺陷顯著化，藉由於各次洗淨步驟後觀察所測定的增加缺陷的增加傾向，而將就源自結晶的缺陷或洗淨等所產生的顆粒等予以除外的加工缺陷予以評價一事變得可能，而能夠評價研磨等的加工品質。According to the evaluation method of the ruthenium wafer, it is possible to significantly reduce the processing defects without causing the defects derived from the crystallization in the cleaning step to be remarkable, and the increase tendency of the observed increased defects after the respective cleaning steps can be observed. In addition, it is possible to evaluate the processing defects which are excluded from the defects such as crystals or the particles generated by the cleaning, and the like, and it is possible to evaluate the processing quality such as polishing.
又於此狀況中，以在不完全除去該氧化膜的條件下以氫氟酸進行的該氧化膜除去處理，係以氫氟酸的濃度為0.1至1.0%，處理時間為2秒至20秒以進行為佳。In this case, the oxide film removal treatment with hydrofluoric acid under the condition that the oxide film is not completely removed is such that the concentration of hydrofluoric acid is 0.1 to 1.0%, and the treatment time is 2 seconds to 20 seconds. It is better to proceed.
依據如此的藉由氫氟酸的氧化膜除去處理，由於能夠控制自然氧化膜厚度，能夠更加確實地不完全除去氧化膜而除去氧化膜。According to such an oxide film removal treatment by hydrofluoric acid, since the thickness of the natural oxide film can be controlled, the oxide film can be removed more reliably and the oxide film can be removed.
又於此狀況中，以該洗淨步驟係交互地重複以臭氧水進行的該氧化處理及以氫氟酸進行的該氧化膜除去處理5次以上以進行為佳。In this case, it is preferable to repeat the oxidation treatment by ozone water and the oxide film removal treatment by hydrofluoric acid five times or more in this washing step.
如此，藉由交互地重複以臭氧水進行的氧化處理及以氫氟酸進行的氧化膜除去處理5次以上，能夠確實地使加工缺陷顯著化，因此能夠更加正確地評價加工品質。In this way, by repeating the oxidation treatment by ozone water and the oxide film removal treatment by hydrofluoric acid five times or more, the processing defects can be remarkably made remarkable, and the processing quality can be more accurately evaluated.
又於此狀況中，以作為該矽晶圓，使用經鏡面研磨後之物為佳。In this case, it is preferable to use the mirror-polished material as the tantalum wafer.
本發明的矽晶圓的評價方法中，藉由使用鏡面研磨後的矽晶圓，而能夠進行研磨品質的評價。In the evaluation method of the tantalum wafer of the present invention, the polishing quality can be evaluated by using the mirror-polished germanium wafer.
又於本發明的矽晶圓的評價方法中，能夠根據各次該洗淨步驟後的該增加缺陷的測定結果，評價該矽晶圓的起因於加工的缺陷。Further, in the evaluation method of the tantalum wafer of the present invention, it is possible to evaluate the defect caused by the processing of the tantalum wafer based on the measurement result of the increased defect after each of the cleaning steps.
本發明的矽晶圓的評價方法中，能夠使僅於洗淨步驟中研磨等的加工缺陷顯著化，又藉由觀察各次洗淨步驟後所測定的增加缺陷的增加傾向，而能夠僅將源自加工的缺陷予以評價，故使加工品質的評價變為可能。In the evaluation method of the tantalum wafer of the present invention, it is possible to make the processing defects such as polishing in the cleaning step remarkable, and to observe the increase tendency of the increased defects measured after each cleaning step, and it is possible to The defects originating from the processing are evaluated, so that the evaluation of the processing quality is made possible.
又本發明提供一種矽晶圓的製造方法，係對鏡面研磨前的矽晶圓進行鏡面研磨以製造一成為製品的矽晶圓，該矽晶圓的製造方法包含：一準備步驟，係準備鏡面研磨前的一實驗用矽晶圓；一鏡面研磨步驟，係對鏡面研磨前的該實驗用矽晶圓，以預定的鏡面研磨條件進行鏡面研磨；一前表面缺陷測定步驟，對該實驗用矽晶圓預先進行表面缺陷測定；一洗淨步驟，對該實驗用矽晶圓交互地重複氧化處理及氧化膜除去處理，該氧化處理係藉由臭氧水以進行，該氧化膜除去處理係在不完全除去形成於該實驗用矽晶圓表面的氧化膜的條件下以氫氟酸進行；以及一增加缺陷測定步驟，對該洗淨步驟後的該實驗用矽晶圓進行表面缺陷測定，以將相對於該前表面缺陷測定步驟所測定的缺陷而增加的增加缺陷予以測定，其中，交互地重複該洗淨步驟及該增加缺陷測定步驟複數次，基於個洗淨步驟後的該增加缺陷的測定結果以評價該矽晶圓，根據該實驗用矽晶圓的評價，將對於鏡面研磨前的該矽晶圓進行鏡面研磨後的研磨品質成為所期望的研磨品質的鏡面研磨條件予以篩選，並以該篩選出的鏡面研磨條件，製造對鏡面研磨前的該矽晶圓進行鏡面研磨而製造該成為製品的矽晶圓。The present invention provides a method for manufacturing a tantalum wafer by performing mirror polishing on a tantalum wafer before mirror polishing to produce a tantalum wafer as a product. The method for manufacturing the tantalum wafer includes: a preparation step, preparing a mirror surface An experimental wafer for polishing before polishing; a mirror polishing step for mirror polishing of the experimental wafer for pre-mirror polishing with predetermined mirror polishing conditions; a front surface defect determination step for the experiment The wafer is subjected to surface defect measurement in advance; a cleaning step is performed in which the oxidation treatment and the oxide film removal treatment are alternately repeated for the experiment, and the oxidation treatment is performed by ozone water, and the oxide film removal treatment is not performed. Performing surface defect detection on the test wafer after the cleaning step by completely removing the oxide film formed on the surface of the test wafer by hydrofluoric acid; and adding a defect measuring step An increased defect that is increased relative to the defect determined by the front surface defect determination step is determined, wherein the cleaning step and the additional defect determination are alternately repeated The number of times of the measurement of the increased defect after the cleaning step is evaluated several times, and the ruthenium wafer before the mirror polishing is mirror-polished by the evaluation of the ruthenium wafer for the experiment. The mirror polishing conditions in which the quality is desired to be polished are screened, and the tantalum wafer before the mirror polishing is mirror-polished by the mirror-grinding conditions selected to produce the tantalum wafer as the product.
依據如此的矽晶圓的製造方法，能夠對實驗用矽晶圓在不使於洗淨步驟中源自結晶的缺陷顯著化而僅使加工缺陷顯著化，而藉由於各次洗淨步驟後觀察所測定的增加缺陷的增加傾向，能夠僅就源自結晶的缺陷或洗淨所產生的顆粒等予以除外的加工缺陷予以評價。藉由此實驗，對於鏡面研磨前的矽晶圓，能夠篩選出應以何種鏡面研磨條件進行鏡面研磨以能得到期望的研磨品質。藉由以如此所篩選的鏡面研磨條件製造矽晶圓，能夠製造具有期望的研磨品質的鏡面研磨矽晶圓。 〔對照先前技術之功效〕According to such a method of manufacturing a tantalum wafer, it is possible to significantly reduce the defects of the crystals of the experimental wafer without causing the crystals to be removed in the washing step, and to observe the processing defects only by the respective washing steps. The increased tendency to increase the defects measured can be evaluated only for processing defects excluding the defects caused by the crystals or the particles generated by the washing. By this experiment, it is possible to screen for the mirror polishing of the silicon wafer before the mirror polishing to obtain the desired polishing quality. By fabricating a tantalum wafer under the mirror polishing conditions thus screened, it is possible to manufacture a mirror-polished germanium wafer having a desired polishing quality. [Compared with the efficacy of prior art]
本發明的矽晶圓的評價方法， 能夠不使於洗淨步驟中源自結晶的缺陷顯著化而僅使加工缺陷顯著化，又藉由於各次洗淨步驟後觀察所測定的增加缺陷的增加傾向，能夠僅就源自結晶的缺陷或洗淨所產生的顆粒等予以除外的加工缺陷予以評價。又本發明能夠不使晶圓的表面粗糙惡化而進行洗淨，而使以微小粒徑的測定成為可能。又本發明的矽晶圓的製造方法中，藉由基於僅評價加工缺陷的實驗用矽晶圓的評價而篩選鏡面研磨條件，能夠製造具有期望的研磨品質的鏡面研磨矽晶圓。According to the method for evaluating a tantalum wafer of the present invention, it is possible to significantly reduce the processing defects without causing significant defects in crystals in the washing step, and to increase the increase in defects measured by observation after each washing step. There is a tendency to evaluate only the processing defects excluding the defects caused by the crystallization or the particles generated by the cleaning. Further, according to the present invention, it is possible to perform cleaning by reducing the surface roughness of the wafer, and it is possible to measure the fine particle diameter. Further, in the method for producing a tantalum wafer of the present invention, it is possible to produce a mirror-polished silicon wafer having a desired polishing quality by screening the mirror polishing conditions based on the evaluation of the experimental silicon wafer for evaluating only the processing defects.
如同上述，習知的矽晶圓的評價方法，具有源自結晶的缺陷的顯著化會發生，而無法評價研磨等的加工缺陷的問題。As described above, the conventional evaluation method of the tantalum wafer has a problem that the occurrence of defects due to crystallization occurs, and the problem of processing defects such as polishing cannot be evaluated.
而本案發明人們為了解決上述問題反覆精心研討的結果，發現將交互地重複進行藉由臭氧水的氧化處理及在不完全除去形成於矽晶圓表面的氧化膜的條件下藉由氫氟酸進行的氧化膜除去處理的洗淨步驟，以及對該洗淨步驟後的該矽晶圓進行表面缺陷測定，並將相對於該表面缺陷測定步驟所測定的缺陷的增加缺陷予以測定的增加缺陷測定步驟予以交互地重複進行，而基於各次洗淨步驟後的增加缺陷的測定結果以評價矽晶圓，則能夠不使洗淨步驟中源自結晶的缺陷顯著化而僅使源自加工的缺陷顯著化，能夠僅評價源自研磨等的加工的缺陷，而達成本發明。The inventors of the present invention have repeatedly studied the above problems in order to solve the above problems, and found that the oxidation treatment by ozone water and the incomplete removal of the oxide film formed on the surface of the germanium wafer are performed alternately by hydrofluoric acid. a cleaning step of the oxide film removing process, and a surface defect measurement of the germanium wafer after the cleaning step, and an increased defect measuring step for measuring an increase defect of the defect measured by the surface defect measuring step By repeating the interaction, and based on the measurement result of the increased defect after each cleaning step, the defect of the crystal is not significantly made, and the defect originating from the processing can be made remarkable. The present invention can be achieved by evaluating only defects resulting from processing such as polishing.
即本發明係提供一種矽晶圓的評價方法，包含：一前表面缺陷測定步驟，對一矽晶圓預先進行表面缺陷測定；一洗淨步驟，對該矽晶圓交互地重複氧化處理及氧化膜除去處理，該氧化處理係藉由臭氧水以進行，該氧化膜除去處理係在不完全除去形成於該矽晶圓表面的氧化膜的條件下以氫氟酸進行；以及一增加缺陷測定步驟，對該洗淨步驟後的該矽晶圓進行表面缺陷測定，以將相對於該前表面缺陷測定步驟所測定的缺陷而增加的增加缺陷予以測定，其中，交互地重複該洗淨步驟及該增加缺陷測定步驟複數次，基於各次洗淨步驟後的該增加缺陷的測定結果以評價該矽晶圓。That is, the present invention provides a method for evaluating a germanium wafer, comprising: a front surface defect measuring step of pre-measuring a surface defect on a wafer; and a cleaning step of alternately repeating oxidation treatment and oxidation of the germanium wafer Membrane removal treatment by ozone water, which is performed with hydrofluoric acid under conditions that do not completely remove the oxide film formed on the surface of the crucible wafer; and an increase defect determination step Performing a surface defect measurement on the germanium wafer after the cleaning step to measure an increased defect that is increased with respect to the defect measured in the front surface defect measuring step, wherein the cleaning step and the step are alternately repeated The defect measurement step is increased a plurality of times, and the measurement result of the increased defect after each cleaning step is used to evaluate the silicon wafer.
以下說明本發明的矽晶圓的評價方法。圖1係顯示本發明的矽晶圓的評價方法的一實施樣貌的步驟流程圖。The evaluation method of the tantalum wafer of the present invention will be described below. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing the steps of an embodiment of the evaluation method of the tantalum wafer of the present invention.
作為評價對象的矽晶圓，雖無特別限定，但以鏡面研磨後的矽晶圓為佳。若使用鏡面研磨後的矽晶圓，則能夠評價PID(Polishing Induced Defect)等的源自研磨的缺陷，而能夠進行研磨品質的評價。The tantalum wafer to be evaluated is not particularly limited, but a tantalum wafer after mirror polishing is preferred. When the mirror-polished silicon wafer is used, it is possible to evaluate the polishing-derived defects such as PID (Polishing Induced Defect) and evaluate the polishing quality.
首先，對於欲評價的矽晶圓預先進行測定表面缺陷的前表面缺陷測定步驟(圖1的(a))。能夠使用例如KLA-Tencor公司製的Surfscan SP5以進行。由於加工缺陷幾乎沒有大於40nm的粒徑，測定粒徑以40nm以下便足夠。First, a front surface defect measuring step of measuring a surface defect is performed in advance on the silicon wafer to be evaluated (Fig. 1 (a)). For example, Surfscan SP5 manufactured by KLA-Tencor Co., Ltd. can be used. Since the processing defect hardly has a particle diameter larger than 40 nm, it is sufficient to measure the particle diameter to 40 nm or less.
接著，進行將藉由臭氧水的氧化處理及在不完全除去形成於該矽晶圓表面的氧化膜的條件下以氫氟酸進行的氧化膜除去處理予以交互地重複的洗淨步驟(圖1的(b))。此洗淨步驟，以單片式洗淨裝置以進行為佳。Next, a washing step of alternately repeating the oxide film removal treatment by hydrofluoric acid under the condition of not completely removing the oxide film formed on the surface of the germanium wafer by the oxidation treatment of ozone water (FIG. 1) (b)). This washing step is preferably carried out in a one-piece cleaning apparatus.
洗淨步驟(b)係使研磨等的加工缺陷顯著化的步驟。藉由進行不完全除去氧化膜的藉由氫氟酸的氧化膜除去，以及藉由臭氧水進行的晶圓表面的再度氧化，藉此能夠不使源自結晶的缺陷顯著化，而僅使研磨等的加工缺陷顯著化。The washing step (b) is a step of making processing defects such as polishing remarkable. By performing the removal of the oxide film of the hydrofluoric acid which does not completely remove the oxide film, and the reoxidation of the surface of the wafer by the ozone water, it is possible to make the defects derived from the crystal remarkable, and only the polishing Processing defects such as are significant.
藉由習知的SC1-RT法(例如日本特開2000-208578號公報)或習知的臭氧水及HF處理的晶圓的品質評價方法中，雖無法評價研磨等的加工缺陷，但本發明中不完全除去氧化膜，藉由反覆進行使用臭氧水及氫氟酸的洗淨，不使源自結晶的缺陷顯著化，而僅使源自加工的缺陷顯著化的評價成為可能。又能夠不使晶圓的表面粗糙惡化而進行洗淨，使以微小粒徑的測定成為可能。In the conventional SC1-RT method (for example, JP-A-2000-208578) or the conventional ozone water and HF-treated wafer quality evaluation method, the processing defects such as polishing cannot be evaluated, but the present invention In the case where the oxide film is not completely removed, washing with ozone water and hydrofluoric acid is repeated, and the defects derived from the crystal are not marked, and only the evaluation derived from the processing defects is made possible. Further, it is possible to perform cleaning without deteriorating the surface roughness of the wafer, and it is possible to measure the fine particle diameter.
如此僅使研磨等加工缺陷顯著化，而使僅評價加工缺陷成為可能。In this way, only processing defects such as polishing are made remarkable, and it is possible to evaluate only processing defects.
另外，本發明中以洗淨步驟(b)不使源自結晶的缺陷顯著化，而僅使研磨等的加工缺陷顯著化的理由如以下所述。加工缺陷，係為研磨等的加工時於晶圓產生歪曲而成為變質層。雖然晶圓的氧化膜藉由氫氟酸而被除去，但加工變質層的部分的氧化膜會成為與周圍的氧化膜相異的蝕刻率，藉由反覆交互進行以臭氧水進行的處理及以氫氟梭進行的處理而逐漸顯著化。這是由於藉由以氫氟酸進行殘留氧化膜的蝕刻處理，使加工變質層與周圍部分的氧化膜厚度產生差異(加工變質層的部分的氧化膜較厚)，藉由反覆進行以臭氧水使氧化膜再次形成(將氧化膜厚度回復至均一)，更加使差異逐漸顯著。完全除去氧化膜時，由於加工變質層的氧化膜部分亦被除去，故即使反覆進行臭氧水處理及氫氟酸處理，亦由於沒有氧化膜而氧化膜厚度不會產生差異而不會發生顯著化，源自加工的缺陷評價則變得不可能。Further, in the present invention, the reason why the defects derived from crystals are not marked out in the washing step (b), and only the processing defects such as polishing are remarkable are as follows. The processing defect is a deterioration of the wafer during processing such as polishing, and becomes a deteriorated layer. Although the oxide film of the wafer is removed by hydrofluoric acid, the oxide film of the portion where the altered layer is processed becomes an etching rate different from that of the surrounding oxide film, and the treatment with ozone water is performed by alternately interacting with The treatment by hydrofluorofusone is gradually becoming more prominent. This is because the etching process of the residual oxide film by hydrofluoric acid causes a difference in the thickness of the oxide film between the affected layer and the surrounding portion (the oxide film of the portion where the altered layer is processed is thick), and ozone water is repeatedly performed by the etching. The oxide film is formed again (reducing the thickness of the oxide film to uniformity), and the difference is made more remarkable. When the oxide film is completely removed, since the oxide film portion of the process-affected layer is also removed, even if the ozone water treatment and the hydrofluoric acid treatment are repeatedly performed, there is no oxide film and the thickness of the oxide film does not vary and does not become noticeable. The evaluation of defects originating from processing becomes impossible.
又如同本發明不完全使氧化膜除去，反覆進行臭氧水及氫氟酸處理，以隨時殘留有蝕刻量少的氧化膜，而不使氧沉澱物等結晶缺陷或金屬汙染所致的坑洞等的缺陷顯著化。Further, as in the present invention, the oxide film is not completely removed, and ozone water and hydrofluoric acid treatment are repeatedly performed to leave an oxide film having a small etching amount at any time, without causing crystal defects such as oxygen precipitates or pits due to metal contamination. The defects are significant.
另一方面，習知的SC1-RT法，藉由大量進行蝕刻所致的顯著化，而不僅使加工缺陷亦使氧沉澱物等的結晶缺陷顯著化。On the other hand, the conventional SC1-RT method is characterized by a large amount of etching, and not only the processing defects but also the crystal defects such as oxygen precipitates are marked.
又習知的以臭氧水及氫氟酸處理的晶圓的品質評價方法包含將自然氧化膜全部除去(剝離)的步驟，雖然能夠使用臭氧水及氫氟酸將氧化膜完全除去而不使表面粗糙惡化而評價，但以此方法，藉由氫氟酸除去自然氧化膜時結晶缺陷亦會顯著化。Further, a method for evaluating the quality of a wafer treated with ozone water and hydrofluoric acid includes a step of removing (peeling) all of the natural oxide film, and the oxide film can be completely removed without using ozone water and hydrofluoric acid. The roughness was deteriorated and evaluated, but in this way, crystal defects were also remarkable when the natural oxide film was removed by hydrofluoric acid.
本發明中臭氧水的臭氧濃度雖無特別限定，以5ppm至30ppm為佳。為了產生自然氧化膜以5ppm以上為佳，自實際上的實施濃度的觀點來看，以30ppm以下為佳。又一次的臭氧水的處理時間，為了形成自然氧化膜以10秒以上為佳。The ozone concentration of the ozone water in the present invention is not particularly limited, and is preferably 5 ppm to 30 ppm. In order to produce a natural oxide film, it is preferably 5 ppm or more, and it is preferably 30 ppm or less from the viewpoint of practical concentration. The treatment time of the ozone water again is preferably 10 seconds or more in order to form a natural oxide film.
氫氟酸的濃度雖無特別限定，但以0.1%至1.0%為佳。若為0.1%以上，由於能夠正確地控制濃度而佳。又為了控制自然氧化膜的膜厚度，以1.0%以下為佳。又一次的氫氟酸處理時間以約2秒至20秒為佳。若為2秒以上，供給至晶圓的氫氟酸能夠遍佈，若為20秒以下，則能夠確實地殘留氧化膜而進行氧化膜除去處理而佳。The concentration of hydrofluoric acid is not particularly limited, but is preferably 0.1% to 1.0%. If it is 0.1% or more, it is preferable because the concentration can be accurately controlled. Further, in order to control the film thickness of the natural oxide film, it is preferably 1.0% or less. The hydrofluoric acid treatment time is again about 2 seconds to 20 seconds. When it is 2 seconds or more, the hydrofluoric acid supplied to the wafer can be spread over, and if it is 20 seconds or less, it is preferable to carry out the oxide film removal process reliably and to carry out an oxide film removal process.
以臭氧水的氧化處理及以氫氟酸的氧化膜除去處理的重複次數，以約5次至50次為佳。若重複次數為5次以上，則能夠確實地使加工缺陷顯著化。又若為50次以下，則能夠壓低洗淨步驟時間，生產量提升而佳。進一步，若為50次以下，則由於能夠不使矽晶圓的表面粗糙惡化並評價而佳。又即使不重複超過50次，亦由於能夠把握晶圓的加工品質傾向而充分。The number of repetitions of the oxidation treatment of ozone water and the removal treatment by the oxide film of hydrofluoric acid is preferably about 5 to 50 times. When the number of repetitions is five or more, the processing defects can be surely made remarkable. Further, if it is 50 times or less, the washing step time can be lowered, and the throughput is improved. Further, when the thickness is 50 or less, it is preferable that the surface roughness of the tantalum wafer is not deteriorated and evaluated. Further, even if it is not repeated more than 50 times, it is sufficient to grasp the processing quality of the wafer.
接著，對洗淨步驟(b)後的矽晶圓進行表面缺陷測定，對以前表面缺陷測定步驟(a)所測定的缺陷，進行將已增加的缺陷予以測定的增加缺陷測定步驟(c)。Next, the surface defect measurement is performed on the germanium wafer after the cleaning step (b), and the increased defect measured step (c) is performed on the defect measured in the previous surface defect measuring step (a).
此增加缺陷測定步驟(c)中，僅將相對於經前表面缺陷測定步驟(a)中測定的缺陷所增加的缺陷予以測定。測定能夠使用例如與前表面缺陷測定步驟相同的KLA-Tencor公司製的Surfscan SP5，進行同點座標測定，而僅測定增加的缺陷的增加數。In the increased defect measuring step (c), only the defects added with respect to the defects measured in the pre-surface defect measuring step (a) are measured. For the measurement, for example, Surfs SP5 manufactured by KLA-Tencor Co., Ltd., which is the same as the front surface defect measurement step, can be used to perform the same-point coordinate measurement, and only the increase in the number of increased defects can be measured.
之後，進行再洗淨步驟(b)及增加缺陷測定步驟(c)。進行這些步驟複數次，基於各次洗淨步驟後的增加缺陷的測定結果，例如增加缺陷的增加傾向(趨勢)，或增加缺陷的增加量，而評價矽晶圓。Thereafter, the re-washing step (b) and the defect-removing step (c) are performed. These steps are performed plural times, and the ruthenium wafer is evaluated based on the measurement result of the increased defect after each cleaning step, for example, increasing the tendency (trend) of the increase in the defect, or increasing the amount of increase in the defect.
如此，交互地進行洗淨步驟(b)及增加缺陷測定步驟(c)複數次，基於增加缺陷的測定結果(增加缺陷的趨勢或增加缺陷數)而評價矽晶圓，以能夠將源自結晶的缺陷及洗淨等所產生的顆粒予以除外，僅評價研磨等的加工缺陷。Thus, the cleaning step (b) is alternately performed and the defect measuring step (c) is increased plural times, and the germanium wafer is evaluated based on the measurement result of increasing the defect (increasing the tendency of the defect or increasing the number of defects) so as to be able to be derived from the crystallizing Except for defects caused by defects and washing, etc., only processing defects such as polishing are evaluated.
在研磨等的加工條件良好之物中，由於不產生源自加工的缺陷(較少)，因此即使重複洗淨步驟(b)及增加缺陷測定步驟(c)，增加缺陷的增加趨勢小，而增加缺陷數少。另一方面，若研磨加工品質不良，則由於產生源自加工的缺陷，因此若是重複洗淨及表面缺陷測定則增加缺陷的增加趨勢變大而增加缺陷數變多。藉由基於此趨勢或增加缺陷數以評價研磨加工品質，而能夠確認於此時間點的加工狀態。In a case where the processing conditions such as polishing are good, since defects (less) originating from processing are not generated, even if the cleaning step (b) is repeated and the defect measuring step (c) is increased, the tendency of increasing the defect is small, and Increase the number of defects. On the other hand, if the quality of the polishing process is poor, defects due to processing are generated. Therefore, in the case of repeated cleaning and surface defect measurement, the tendency of increasing the number of defects increases, and the number of defects increases. The processing state at this time point can be confirmed by evaluating the polishing processing quality based on this tendency or increasing the number of defects.
亦即，在增加缺陷的線圖形狀相近時，越是趨勢為大者，或是增加缺陷數為大者，即為含有潛在的加工缺陷，加工品質會不良。That is, when the shape of the line graph in which the defect is added is similar, the trend is larger, or the number of defects is increased, that is, the processing defect is poor, and the processing quality is poor.
如同前述，本發明中，藉由使用臭氧水及氫氟酸而不完全除去氧化膜地重複進行洗淨一事，不僅能夠抑制晶圓的表面粗糙惡化及顆粒等的附著，亦能夠不使源自結晶的缺陷顯著化而僅使研磨等的加工缺陷顯著化。又，藉由觀察各次洗淨步驟後所測定的增加缺陷的增加傾向，能夠僅就源自結晶的缺陷及洗淨等所產生的顆粒等予以除外的源自研磨等加工的缺陷予以評價。又使至今未有的微小區域下的缺陷評價變得可能。As described above, in the present invention, by repeatedly using ozone water and hydrofluoric acid without completely removing the oxide film, it is possible to suppress not only deterioration of surface roughness of the wafer but also adhesion of particles or the like, and it is also possible to prevent The defects of crystallization are remarkable, and only processing defects such as polishing are remarkable. Moreover, by observing the tendency of the increase of the increase of the defect measured after each washing step, it is possible to evaluate only the defects derived from the processing such as polishing, which are excluded from the defects such as crystal defects and the particles generated by the cleaning or the like. It is also possible to evaluate defects in a small area that has not been available so far.
又上述的矽晶圓的評價方法，能夠應用於對鏡面研磨前的矽晶圓進行鏡面研磨而成為製品的製造矽晶圓的方法。此矽晶圓的製造方法中，在製造成為製品的矽晶圓之前，對實驗用矽晶圓進行依照上述矽晶圓的評價方法的實驗，預先篩選鏡面研磨的鏡面研磨條件，以經篩選的鏡面研磨條件進行鏡面研磨而進行成為製品的矽晶圓的製造。具體而言，如同下述而進行矽晶圓的製造。Further, the above-described method for evaluating a tantalum wafer can be applied to a method of mirror-polishing a tantalum wafer before mirror polishing to produce a tantalum wafer. In the method for manufacturing a tantalum wafer, before the tantalum wafer to be a product is produced, the experimental wafer is subjected to an experiment according to the evaluation method of the tantalum wafer, and the mirror polishing conditions of the mirror polishing are screened in advance to be screened. The mirror polishing conditions are mirror-polished to produce a tantalum wafer to be a product. Specifically, the fabrication of a germanium wafer is performed as follows.
首先，準備鏡面研磨前的實驗用矽晶圓。接著對此鏡面研磨前的實驗用矽晶圓，以指定的鏡面研磨條件進行鏡面研磨。對於進行有如此的鏡面研磨的實驗用矽晶圓，與上述的矽晶圓的評價方法相同，進行前表面缺陷測定步驟、洗淨步驟及增加缺陷測定步驟(參照圖1的(a)至圖1的(c))。具體而言，進行如同以下的各步驟。首先，對於進行了鏡面研磨的實驗用矽晶圓，預先進行測定表面缺陷的前表面缺陷測定步驟。接著，對實驗用矽晶圓，進行洗淨步驟，交互地重複氧化處理及氧化膜除去處理，該氧化處理係藉由臭氧水以進行，該氧化膜除去處理係在不完全除去形成於該矽晶圓表面的氧化膜的條件下以氫氟酸進行。接著，進行增加缺陷測定步驟，對該洗淨步驟後的該矽晶圓進行表面缺陷測定，以將相對於該前表面缺陷測定步驟所測定的缺陷而增加的增加缺陷予以測定。First, prepare a test wafer for pre-mirror polishing. This experiment was performed on the wafer before the mirror polishing, and the mirror polishing was performed under the specified mirror polishing conditions. In the same manner as the evaluation method of the above-described tantalum wafer, the test wafer for such mirror polishing is subjected to the front surface defect measurement step, the cleaning step, and the increased defect measurement step (see (a) to FIG. 1). 1 (c)). Specifically, the following steps are performed. First, for the experimental wafer for mirror polishing, the front surface defect measurement step for measuring the surface defect is performed in advance. Next, the enamel wafer for the experiment is subjected to a cleaning step, and the oxidation treatment and the oxide film removal treatment are alternately repeated. The oxidation treatment is performed by ozone water, and the oxide film removal treatment is formed in the ruthenium after incomplete removal. The oxide film on the surface of the wafer is subjected to hydrofluoric acid under the conditions of an oxide film. Next, an increased defect measuring step is performed, and the surface defect after the cleaning step is subjected to surface defect measurement to measure an increased defect which is increased with respect to the defect measured in the front surface defect measuring step.
交互地重複上述洗淨步驟及增加缺陷測定步驟複數次，基於各次洗淨步驟後的增加缺陷的測定結果以評價實驗用矽晶圓。進一步，基於此實驗用矽晶圓的評價，將對鏡面研磨前的矽晶圓進行鏡面研磨後的研磨品質成為期望的研磨品質的鏡面研磨的鏡面研磨條件予以篩選。以此處所篩選的鏡面研磨條件，對鏡面研磨前的矽晶圓進行鏡面研磨而製造成為製品的矽晶圓。The above-described washing step and the step of increasing the defect measuring are repeated alternately, and the test wafer for evaluation is evaluated based on the measurement result of the increased defect after each washing step. Further, based on the evaluation of the tantalum wafer for this experiment, the mirror polishing conditions of the mirror polishing of the desired polishing quality after the mirror polishing of the tantalum wafer before the mirror polishing were performed were selected. The tantalum wafer before the mirror polishing was mirror-polished by the mirror polishing conditions screened here to produce a tantalum wafer as a product.
經以不產生(較少)鏡面研磨後的加工缺陷的研磨條件所研磨的鏡面研磨矽晶圓，即使重複洗淨步驟(b)及增加缺陷測定步驟(c)，增加缺陷的增加的趨勢亦小，增加缺陷數亦少。另一方面，若研磨加工品質不良，則將產生源自加工的缺陷，因此若重複洗淨及表面缺陷測定，增加缺陷的增加的趨勢變大而增加缺陷數變多。基於此趨勢或增加缺陷數評價實驗用矽晶圓的研磨加工品質，藉此能夠篩選出對於鏡面研磨前的矽晶圓應以何種的鏡面研磨條件進行鏡面研磨以能夠得到期望的研磨品質。The mirror-polished silicon wafer polished by the polishing conditions which do not produce (less) mirror-finished processing defects, even if the cleaning step (b) is repeated and the defect determination step (c) is increased, the tendency of increasing the defects is increased. Small, the number of defects increased is also small. On the other hand, if the quality of the polishing process is poor, defects originating from the processing will occur. Therefore, if the cleaning and surface defects are repeated, the tendency to increase the number of defects increases, and the number of defects increases. Based on this trend or increasing the number of defects, the polishing quality of the test wafer is evaluated, whereby it is possible to screen out the mirror polishing conditions of the germanium wafer before the mirror polishing to obtain the desired polishing quality.
更具體而言，能夠在增加缺陷的線圖形狀相近時，選擇沒有斜率或是斜率變小的鏡面研磨條件。例如，能夠設定鏡面研磨條件而使圖1所示的流程圖中重複氫氟酸→臭氧水的次數約為十次的增加缺陷數平均為十個以下、五個以下或一個以下。 〔實施例〕More specifically, it is possible to select mirror polishing conditions having no slope or a small slope when the shape of the line graph in which the defects are increased is similar. For example, the mirror polishing conditions can be set such that the number of increased defects in which the number of times of hydrofluoric acid → ozone water is repeated ten times in the flowchart shown in FIG. 1 is on average ten or less, five or less, or one or less. [Examples]
以下，雖表示實施例及比較例而更具體地說明本發明，但本發明並非限定於這些實施例。Hereinafter, the present invention will be more specifically described by showing examples and comparative examples, but the present invention is not limited to these examples.
(實施例) 使用以相異的研磨條件(研磨條件1至4)被最終研磨且結束洗淨後的矽晶圓，進行前表面缺陷測定(圖1的(a))。對於進行了前表面缺陷測定的晶圓，藉由交互重複進行以臭氧水的氧化處理及以氫氟酸的氧化膜除去處理以進行洗淨(圖1的(b))。(Example) The front surface defect measurement was performed using the tantalum wafer which was finally polished by the different polishing conditions (polishing conditions 1 to 4) and the cleaning was completed (Fig. 1 (a)). The wafer on which the front surface defect was measured was subjected to oxidation treatment with ozone water and oxide film removal treatment with hydrofluoric acid by interaction (Fig. 1 (b)).
洗淨條件，為臭氧水濃度為10ppm，每次的臭氧水處理時間為20秒，氫氟酸濃度為0.3%，每次的氫氟酸處理時間為5秒，以顯示於圖1的流程使氫氟酸→臭氧水的重複次數為五次而進行洗淨，之後將其乾燥。另外每一次氫氟酸處理皆進行了於晶圓表面殘留氧化膜的氧化膜除去。The washing condition is that the ozone water concentration is 10 ppm, the ozone water treatment time is 20 seconds, the hydrofluoric acid concentration is 0.3%, and the hydrofluoric acid treatment time is 5 seconds each time, which is shown in the flow of FIG. The hydrofluoric acid→ozone water was washed five times and then dried. In addition, each hydrofluoric acid treatment was performed by removing the oxide film remaining on the surface of the wafer.
接著，對洗淨步驟後的矽晶圓進行表面缺陷測定，將相對於以前表面缺陷測定步驟(a)測定的缺陷所增加的增加缺陷予以測定(圖1的(c))。另外，前表面缺陷測定及增加缺陷測定，係使用KLA-Tencor公司製的Surfscan SP5，以粒徑19nm以上進行測定，藉由進行同點座標測定，而僅測定增加的增加缺陷。Next, surface defects were measured on the germanium wafer after the cleaning step, and the increased defects added to the defects measured in the previous surface defect measuring step (a) were measured ((c) of FIG. 1). In addition, the measurement of the front surface defect and the measurement of the increased defect were carried out by using Surfscan SP5 manufactured by KLA-Tencor Co., Ltd., and the measurement was performed at a particle diameter of 19 nm or more, and only the increased increase defect was measured by the same-point coordinate measurement.
洗淨步驟及增加缺陷測定步驟，重複進行了以臭氧水的處理→以氫氟酸的處理至合計重複次數為50次(即洗淨步驟及增加缺陷測定步驟的重複次數為10次)。The washing step and the step of increasing the defect were repeated, and the treatment with ozone water was repeated → the treatment with hydrofluoric acid was repeated until the total number of repetitions was 50 (that is, the number of repetitions of the washing step and the step of increasing the defect measuring step was 10).
各次洗淨步驟後，僅將相對於前表面缺陷測定的結果所增加的缺陷的個數作為增加缺陷數，將以臭氧水的處理→以氫氟酸的處理的合計重複次數及增加缺陷數統整而顯示於表1。又將以臭氧水的處理→以氫氟酸的處理的合計重複次數與增加缺陷數的關係製圖而顯示於圖2。基於表1及圖2，評價增加缺陷的增加的趨勢或缺陷的增加量。After each cleaning step, only the number of defects increased with respect to the result of the measurement of the front surface defect is taken as the number of defects to be increased, and the number of repetitions of the treatment with ozone water → the treatment with hydrofluoric acid and the number of defects increased The overall is shown in Table 1. Further, it is shown in Fig. 2 by plotting the relationship between the total number of repetitions of the treatment with ozone water and the treatment with hydrofluoric acid and the number of increased defects. Based on Table 1 and FIG. 2, the increase tendency of the increase defect or the increase amount of the defect was evaluated.
又當以SEM觀察洗淨後的晶圓表面，得知於晶圓表面結晶缺陷沒有顯著化，而僅有如圖3的(A)所示的加工缺陷顯著化，而得知能夠評價加工品質。Further, when the surface of the wafer after the cleaning was observed by SEM, it was found that the crystal defects on the surface of the wafer were not marked, and only the processing defects as shown in FIG. 3(A) were remarkable, and it was found that the processing quality can be evaluated.
如圖2所示，得知：研磨條件1至4，各研磨條件的增加缺陷的增加趨勢相異，由於研磨條件1幾乎沒有增加趨勢，因此不產生源自加工的缺陷，即為研磨品質良好。又得知：研磨條件2至4，增加的趨勢愈大，也就是依研磨條件4、研磨條件3及研磨條件2的順序，研磨品質為不良。As shown in Fig. 2, it was found that the polishing conditions 1 to 4, the increase tendency of the increase defects of the respective polishing conditions was different, and since the polishing condition 1 hardly increased, there was no defect originating from the processing, that is, the polishing quality was good. . Further, it was found that the polishing conditions were 2 to 4, and the increase tendency was larger, that is, the polishing quality was poor depending on the polishing conditions 4, the polishing conditions 3, and the polishing conditions 2.
【表1】
(比較例) 以日本特開2000-208578號所記載的藉由SC1-RT法的評價方法，進行矽晶圓的評價。具體而言，使用由氨、雙氧水及水所構成的處理液，於矽晶圓表面施加蝕刻處理而檢測出缺陷。但是，該處理所檢測出的，主要如圖3的(B)所示的顆粒及結晶缺陷。又，即使使用KLA-Tencor公司製的Surfscan SP5，由於粒徑19nm以上係表面粗糙惡化，而無法測定。(Comparative Example) The evaluation of the ruthenium wafer was carried out by the evaluation method of the SC1-RT method described in JP-A-2000-208578. Specifically, a treatment liquid composed of ammonia, hydrogen peroxide, and water is used, and an etching treatment is applied to the surface of the tantalum wafer to detect defects. However, the particles and crystal defects shown in Fig. 3(B) were mainly detected by this treatment. In addition, even if Surfscan SP5 manufactured by KLA-Tencor Co., Ltd. was used, the surface roughness of 19 nm or more was deteriorated, and measurement was impossible.
另外，本發明並不為前述實施例所限制。前述實施例為例示，具有與本發明的申請專利範圍所記載的技術思想為實質相同的構成，且達成同樣作用效果者，皆包含於本發明的技術範圍。Further, the present invention is not limited by the foregoing embodiments. The above-described embodiments are exemplified, and have substantially the same configuration as the technical idea described in the patent application scope of the present invention, and the same effects are achieved in the technical scope of the present invention.
圖1係顯示本發明的矽晶圓的評價方法的一實施樣貌的步驟流程圖。 圖2係顯示實施例中的藉由臭氧水的處理→藉由氫氟酸的處理的合計重複次數與增加缺陷數的關係的量表圖。 圖3的(A)係觀察實施例中洗淨後的晶圓表面的SEM圖，(B)係比較例所檢測出的缺陷的SEM圖。BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing the steps of an embodiment of the evaluation method of the tantalum wafer of the present invention. Fig. 2 is a graph showing the relationship between the total number of repetitions by the treatment of ozone water → the treatment by hydrofluoric acid and the number of increased defects in the examples. Fig. 3(A) is an SEM image of the surface of the wafer after washing in the example, and (B) is an SEM image of the defect detected in the comparative example.
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