WO2014069156A1 - シリコンウェーハの評価方法及びそのエッチング液 - Google Patents

シリコンウェーハの評価方法及びそのエッチング液 Download PDF

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WO2014069156A1
WO2014069156A1 PCT/JP2013/077069 JP2013077069W WO2014069156A1 WO 2014069156 A1 WO2014069156 A1 WO 2014069156A1 JP 2013077069 W JP2013077069 W JP 2013077069W WO 2014069156 A1 WO2014069156 A1 WO 2014069156A1
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Prior art keywords
silicon wafer
lep
etching solution
etching
wafer
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PCT/JP2013/077069
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English (en)
French (fr)
Japanese (ja)
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善範 矢ヶ崎
典雄 大高
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信越半導体株式会社
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • 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
    • H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
    • H01L22/24—Optical enhancement of defects or not directly visible states, e.g. selective electrolytic deposition, bubbles in liquids, light emission, colour change
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32—Polishing; Etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • 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

Definitions

  • the present invention relates to a silicon wafer evaluation method and an etching solution thereof, and more specifically, an evaluation method for detecting crystal defects that degrade the electrical characteristics of a semiconductor device by selectively etching the surface of the silicon wafer, and It relates to the etching solution.
  • Patent Document 1 contains potassium dichromate at the stage where the surface of a wafer cut out from a silicon single crystal ingot is mirror-etched with a mixed solution of hydrofluoric acid and nitric acid (this stage wafer is called a mirror-etched wafer).
  • Patent Document 1 contains potassium dichromate at the stage where the surface of a wafer cut out from a silicon single crystal ingot is mirror-etched with a mixed solution of hydrofluoric acid and nitric acid (this stage wafer is called a mirror-etched wafer).
  • a method of selectively etching a crystal defect portion by dipping in a SECCO solution is disclosed. According to this method, a defective portion on the surface of the wafer appears as a ripple pattern (flow pattern), and the wafer can be easily evaluated without producing a polished wafer (at the stage of a mirror-etched wafer).
  • Patent Document 2 discloses that FPD observation shows a capability equivalent to that of secco solution, and selectively etches a mirror-etched wafer using a chromium-less etching solution that does not use potassium dichromate, which is a harmful substance. A method for detecting the above has been proposed.
  • LEP is visually observed by an operator through an optical microscope and counted. For this reason, LEP has a very low density, and it is not easy to find LEP by paying attention only to the shape of an ellipse.
  • the chromeless etching solution disclosed in Patent Document 2 is effective for FPD observation but has low sensitivity with respect to LEP. That is, since LEP is a micro-dislocation defect, even when selective etching is performed with a conventional chromeless etchant, the size of the elliptical shape is as small as several ⁇ m and observation is not easy.
  • an object of the present invention is to provide a silicon wafer evaluation method and an etching solution thereof that can easily observe LEP.
  • the silicon wafer evaluation method of the present invention is such that the volume ratio of hydrofluoric acid, nitric acid, acetic acid and water in the etching solution is (400) :( 5-10) :( 10-50):
  • the silicon wafer is immersed in an etching solution of (80 to 120) and containing iodine or iodide to selectively etch crystal defect portions and detect LEP.
  • an etching solution having a volume ratio of hydrofluoric acid, nitric acid, acetic acid and water of (400) :( 5-10) :( 10-50) :( 80-120) and containing iodine or iodide is prepared. Therefore, the LEP of a silicon wafer made of a single crystal grown at a low speed can be evaluated without using a Secco solution containing a harmful substance (chromium) that has a strong influence on the global environment and human body.
  • LEP which is observed only as an elliptical shape in the conventional etching solution, has an elliptical pattern having a ripple pattern (flow pattern) in the same manner as FPD in the majority of all LEPs.
  • flow pattern ripple pattern
  • the size of the elliptical shape (LEP) can be made larger than when a conventional etching solution is used (diameter of about 10 ⁇ m).
  • the FPD does not form a clear flow pattern, and only the LEP is easily observed.
  • the volume ratio of nitric acid is 5-10.
  • the volume ratio of nitric acid is less than 5, the shape of the flow pattern may not be clear.
  • the sharpness improves as the volume ratio of nitric acid increases, but when the volume ratio of nitric acid exceeds 10, surface roughness of the wafer surface may occur very strongly.
  • the etching rate is faster than when the etching solution of Patent Document 2 is used, so the size of the LEP (elliptical shape) can be increased and the shape of the flow pattern is also compared. Observed clearly and vividly. Therefore, by the evaluation method of the present invention, a flow pattern having a good shape can be clearly formed in the crystal defect portion of the surface layer of the silicon wafer, and LEP can be detected with high sensitivity.
  • the content of iodine or iodide in the etching solution is 0.03 g or more per liter of the total amount of the etching solution.
  • iodine or iodide is added to the etching solution in this way is that it is effective in preventing the occurrence of stains (stain film) adhering to the wafer surface. By preventing the occurrence of a stain film, the flow pattern can be confirmed clearly and stably, leading to a reduction in reaction start time and a uniform etching allowance, thereby improving evaluation accuracy.
  • the iodide include potassium iodide, and may be added as an aqueous solution.
  • the amount of iodine or iodide added is desirably 0.03 g or more with respect to 1 liter of the total amount of the etching solution.
  • the silicon wafer is preferably a wafer after chemical mirror polishing obtained by slicing from a silicon single crystal ingot.
  • the etching solution used in the present invention can form an elliptical etching pattern having a good shape even at the stage of a wafer after chemical mirror polishing, that is, a mirror etched wafer.
  • a subsequent mechanical and chemical polishing process which saves time and money for the preparation of the sample for evaluation.
  • Good it can be evaluated by omitting the cylindrical polishing process of the grown silicon single crystal ingot and slicing it, omitting the etching to remove polishing distortion, and performing mirror etching, so an evaluation sample can be obtained in a very short process.
  • the silicon wafer can be evaluated.
  • the etch-off amount of the silicon wafer by the etching is preferably 3 to 50 ⁇ m on both sides.
  • LEP is uniformly generated in a silicon single crystal when the silicon single crystal is grown, and exists uniformly in the depth direction with respect to the wafer surface.
  • the surface portion of the wafer is removed by etching, and LEP distributed in the depth direction is detected as it is removed, and the number of LEPs accumulates on the etched wafer surface. become.
  • LEP can be accurately evaluated by setting the etch-off amount, that is, the thickness of the silicon wafer removed by etching to 3 to 50 ⁇ m. If the etch-off amount is less than 3 ⁇ m, the density of LEP is too low to perform accurate evaluation. On the other hand, if the etch-off amount exceeds 50 ⁇ m, the LEP shape at the initial stage of etching may be lost, and the LEP density may be too high to perform accurate evaluation.
  • the etching it is preferable to perform the etching at an immersion start temperature of 10 to 30 ° C.
  • the immersion start temperature 10 to 30 ° C.
  • the immersion start temperature is less than 10 ° C.
  • the progress of etching is slow and the detection sensitivity is lowered.
  • the immersion start temperature exceeds 30 ° C.
  • the etching rate is high, and the liquid temperature rises accordingly, the etching progresses remarkably fast, the shape of the etching pattern collapses and the density becomes too high to be detected. Sometimes it becomes.
  • the etching solution of the present invention is an etching solution used for detecting LEP of a silicon wafer, and the etching solution contains hydrofluoric acid, nitric acid, acetic acid and water (400): (5 to 10): (10 to 50): (80 to 120), and iodine or iodide is contained in an amount of 0.03 g or more per liter of the total amount of the etching solution. . Thereby, the same effect as the evaluation method of the silicon wafer can be obtained.
  • FIG. 7A It is the figure which illustrated the elliptical pattern observed on the silicon wafer surface. It is a histogram of the long width X of LEP in an Example and Comparative Examples 1 and 2. FIG. It is a histogram of the short width Y of LEP in an Example and Comparative Examples 1 and 2. FIG. It is a histogram of the area of LEP in an Example and the comparative examples 1 and 2. FIG. It is an image of the sample of an Example. It is an enlarged image of the A section of Drawing 5A. It is an enlarged image of the B section of Drawing 5B. It is an image of the sample of an Example with high LEP density. It is an image of the sample of the comparative example 1. It is an enlarged image of the C section of Drawing 7A.
  • a known silicon single crystal substrate manufacturing method may be used as a silicon wafer manufacturing method.
  • a silicon wafer sliced from a silicon single crystal ingot pulled up by the Czochralski method can be used.
  • the crystal growth rate (pulling rate) of the silicon single crystal ingot is low, LEP is likely to be formed, and the necessity for evaluating the LEP increases. Therefore, here, particularly from the silicon single crystal ingot having a relatively low crystal growth rate.
  • a sliced silicon wafer can be used.
  • the surface of the sliced silicon wafer and a few ⁇ m in the depth direction from the surface need to be in a state in which processing distortion due to slicing or the like does not remain, so a chemical polishing liquid such as hydrofluoric acid and nitric acid By etching with a mixed acid having a ratio of about 1: 3, it is possible to prepare a mirror-etched wafer having a chemically mirror-finished surface while removing processing distortion on the surface of the silicon wafer.
  • a polished wafer may be prepared as an evaluation sample instead of the mirror-etched wafer.
  • a general manufacturing method of a polished wafer will be described.
  • a silicon wafer is cut out from a silicon single crystal ingot grown by the Czochralski method (slicing process) and cut out (sliced).
  • Chamfering is performed to remove the corners of the periphery of the silicon wafer (beveling process).
  • mechanical polishing is applied to eliminate unevenness on the silicon wafer surface, increase flatness, and minimize surface scratches (lapping process; sometimes referred to as a wrapped wafer at this stage).
  • the strained polishing layer formed on the surface layer of the silicon wafer is removed by mixed acid etching to obtain a silicon wafer having improved chemical flatness (chemical etching process; this is called a chemically etched wafer at this stage) is there).
  • polishing is performed while overlapping the mechanical action by the free abrasive grains and the etching action by the chemical substance on the surface of the chemically etched wafer.
  • the mechanochemical polishing method is employed, and this polishing method is usually composed of two or three steps. That is, it is called primary polishing, secondary polishing (in some cases, there is also tertiary polishing), and finish polishing in the order of the steps.
  • polishing cloth Polishing is performed while relaxing the polishing conditions such as decreasing the hardness and setting the conditions so that the flatness and surface roughness of the mirror surface polished at each stage become low values.
  • a polished wafer is manufactured through the above processes. In the following description, it is assumed that a mirror-etched wafer is prepared as an evaluation sample.
  • an etchant used to detect crystal defects (LEP) of the prepared mirror-etched wafer As the etchant, hydrofluoric acid, nitric acid, acetic acid and water in the etchant have a volume ratio of (400) :( 5-10) :( 10-50) :( 80-120), and iodine or An etching solution containing 0.03 to 0.15 g of iodide with respect to 1 liter of the total amount of the etching solution is prepared.
  • the etching solution a commercially available semiconductor grade chemical solution can be used.
  • hydrofluoric acid (50% by weight) is for semiconductors of Daikin Industries, Ltd.
  • nitric acid (61% by weight) is Kanto Chemical.
  • the EL grade of Co., Ltd. and acetic acid (99.7% by weight) can be prepared by mixing the special grade of Kanto Chemical Co., Ltd. as it is at the above volume ratio.
  • water it is preferable to use ultrapure water used in the semiconductor industry in consideration of adhesion of dust and dirt to the wafer during the etching process.
  • the mirror etched wafer obtained as described above is added to the etching solution of the present invention having a liquid temperature of 10 to 30 ° C., and the etching off time is 3 to 50 ⁇ m on both sides of the mirror etched wafer. Then, it is left to stand without stirring, and the crystal defect portion is selectively etched. As a result, an elliptical etching pattern can appear on the surface of the mirror-etched wafer. This elliptical etching pattern is a pattern resulting from LEP. Further, most of all elliptical shapes (LEPs) appearing on the mirror-etched wafer surface (about 80% as shown in the examples below) have a flow pattern similar to FPD.
  • LEPs elliptical shapes
  • the remaining 20% appears as a conventional elliptical single pattern.
  • the flow pattern can be easily confirmed by visual observation by placing the etched wafer under light collection.
  • the existence of an elliptical pattern (LEP) in the flow pattern can be easily confirmed by confirming the confirmed flow pattern in an enlarged form with an optical microscope or the like.
  • the LEP cannot be confirmed unless the entire surface of the wafer is scanned with an optical microscope or the like.
  • the number of elliptical patterns is measured as an LEP density by visual detection through an optical microscope or by an automatic detection device that automatically detects LEP (see Japanese Patent Application Laid-Open No. 2004-117147). Based on the above, the quality of the crystal quality of the silicon wafer is evaluated.
  • a silicon wafer for evaluation after being sliced from a silicon single crystal ingot having a diameter of 300 mm, a conductivity type of P type, and a resistivity of about 10 ⁇ ⁇ cm grown under various manufacturing conditions, a chemical mirror polishing (mirror etching) solution A wafer (mirror etched wafer) in a mirror state was prepared. These sample wafers were divided into four fan shapes. LEP was evaluated according to each condition of the following Example and comparative example with respect to the wafer.
  • a conventional chromeless etchant specifically, an etchant having a volume ratio of 400: 3: 33: 80 (hereinafter referred to as a conventional etchant) of 50 wt% hydrofluoric acid, 61 wt% nitric acid, 99.7 wt% acetic acid and water. 12 liters of chromeless solution) was prepared. This conventional chromeless solution was mixed with 132 ml of 61 wt% nitric acid and 480 ml of water. Further, 63.6 ml of 0.1 mol / liter potassium iodide aqueous solution was added to prepare the etching solution of the present invention.
  • the volume ratio of the prepared etching solution is hydrofluoric acid 400, nitric acid 5.3, acetic acid 33, and water 90.
  • the content of potassium iodide is about 0.08 g per liter of the total amount of the etching solution.
  • the etching solution was allowed to stand for 1 day, and then immersed in the etching solution with the above-described 30 samples standing vertically at an immersion start temperature of 24 ° C., without stirring. Left for a minute.
  • the etch-off amount at this time was about 28 ⁇ m on both sides.
  • the size of each elliptical pattern that appeared on the surface of each sample wafer was measured.
  • the size of the elliptical pattern is a longer width X of the elliptical pattern (corresponding to the length of the major axis of the ellipse) (hereinafter referred to as a long width), and shorter.
  • the width Y (corresponding to the length of the minor axis of the ellipse) (hereinafter referred to as the short width) and the area were measured.
  • the long width X and the short width Y were measured from an enlarged image of an elliptical pattern using image analysis software (software that can calculate the distance between pixels).
  • a value obtained by multiplying the long width X and the short width Y was defined as an area (X ⁇ Y) of the pattern (LEP).
  • FIG. 2 to 4 show LEP size histograms (frequency distribution) as measurement results of the LEP (elliptical pattern) size (long width X, short width Y, area).
  • FIG. 2 shows a histogram of the LEP long width X in Examples and Comparative Examples 1 and 2, in detail, the horizontal axis indicates the long width X, and the vertical axis indicates a plurality of samples ( Example 1 and Comparative Example 1 indicate 30% of the long width X obtained from 30 samples and Comparative Example 2 37 samples), that is, the frequency.
  • FIG. 3 shows a histogram of the short width Y of the LEP in Examples and Comparative Examples 1 and 2. Specifically, the horizontal axis indicates the short width Y, and the vertical axis indicates the short width Y obtained from each sample.
  • FIG. 4 shows a histogram of LEP areas in Examples and Comparative Examples 1 and 2. Specifically, the horizontal axis indicates the area, and the vertical axis indicates which area section is what percentage of the area obtained from each sample. The frequency of whether it belongs to is shown.
  • the average value of the sizes (long width X, short width Y, area) of the plurality of LEPs is calculated, and one long width X, short per sample is calculated. Width Y and area were obtained. Further, the long width X, the short width Y, and the area can be obtained by the number of samples (30 sheets in the case of Example and Comparative Example 1 and 37 sheets in the case of Comparative Example 2). Shows a histogram of the long width X, the short width Y, and the area of those 30 sheets and 37 sheets.
  • Table 1 below is a table of LEP size measurement results in Examples and Comparative Examples 1 and 2.
  • the first column in Table 1 indicates the number of samples N.
  • the second column shows the average value of the long width X obtained from each sample.
  • the third column shows the average value of the short width Y obtained from each sample.
  • the fourth column shows the average area obtained from each sample.
  • the etching solution of the present invention in the etching solution of the present invention, a LEP having a larger size (area) is more easily observed than the conventional etching solution (particularly, the conventional chromeless solution).
  • the average value of the long width X of the example is 14.9 ⁇ m
  • the average value of the short width Y is 10.4 ⁇ m
  • LEP which is a micro dislocation defect is observed in a large size having a diameter of 10 ⁇ m or more.
  • 5A to 5C show images obtained by appropriately selecting one of the 30 samples of the embodiment and imaging a part of the surface of the selected sample.
  • FIG. 5A shows an image with the same magnification
  • FIG. 5B shows an enlarged image of part A in FIG. 5A
  • FIG. 5C shows an enlarged image of part B in FIG. 5B. Note that the enlarged image in FIG. 5C is an image having a unit length of 10 ⁇ m.
  • FIG. 6 is an equal-magnification image of the sample of Example 1 different from the samples of FIGS. 5A to 5C, and shows an image of a sample having a higher LEP density than the samples of FIGS. 5A to 5C. .
  • the LEP flow pattern (white portion) can be easily observed visually. As described above, when the etching solution of the present invention is used, the LEP flow pattern is observed, so that the LEP can be easily found and observed.
  • FIG. 7A and FIG. 7B are images obtained by picking one of the 30 samples of Comparative Example 1 (conventional chromeless liquid) appropriately and capturing a part of the surface of the selected sample.
  • FIG. 7A shows the same-size image
  • FIG. 7B is an enlarged image (enlarged image of the elliptical pattern 4 (LEP)) in part C of FIG. 7A.
  • the enlarged image in FIG. 7B is an image having the same enlargement ratio as that in FIG.
  • FIGS. 7A and 7B when the etching solution of Comparative Example 1 was used, no LEP flow pattern was observed. It can also be seen that pattern 3 in FIG. 5C is larger than pattern 4 in FIG. 7B.
  • the incidence of LEP having a flow pattern was measured for the samples of Example and Comparative Example 1. Specifically, three samples A, B, and C are appropriately selected from the 30 samples in the embodiment, and the number of all LEPs N1, the flow pattern for each of the samples A, B, and C is selected. The number of LEPs having N2 and the occurrence rate of LEPs having a flow pattern (N2 / N1 ⁇ 100) were measured. Further, one sample D is appropriately selected from the 30 samples of Comparative Example 1, and the total number of LEPs N1, the number of LEPs having a flow pattern N2, and the flow pattern are associated with the sample D. The incidence of LEP (N2 / N1 ⁇ 100) was measured. Table 2 below shows the measurement results.
  • the electrical characteristics of the silicon wafer are deteriorated without using potassium dichromate which is a harmful substance to the global environment and the human body. LEP can be easily observed.

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PCT/JP2013/077069 2012-11-05 2013-10-04 シリコンウェーハの評価方法及びそのエッチング液 WO2014069156A1 (ja)

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CN111662717A (zh) * 2020-07-14 2020-09-15 北京航空航天大学宁波创新研究院 一种硒化铋材料的金相腐蚀液以及金相显示方法

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JP6179530B2 (ja) 2015-01-23 2017-08-16 信越半導体株式会社 貼り合わせｓｏｉウェーハの製造方法

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JP3629694B2 (ja) * 1998-02-19 2005-03-16 信越半導体株式会社 シリコンウェーハの評価方法
JP3651440B2 (ja) * 2002-01-16 2005-05-25 信越半導体株式会社 シリコンウェーハの評価方法及びそのエッチング液

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JP3692812B2 (ja) * 1998-06-04 2005-09-07 信越半導体株式会社 窒素ドープした低欠陥シリコン単結晶ウエーハおよびその製造方法

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Publication number Priority date Publication date Assignee Title
JP3629694B2 (ja) * 1998-02-19 2005-03-16 信越半導体株式会社 シリコンウェーハの評価方法
JP3651440B2 (ja) * 2002-01-16 2005-05-25 信越半導体株式会社 シリコンウェーハの評価方法及びそのエッチング液

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111662717A (zh) * 2020-07-14 2020-09-15 北京航空航天大学宁波创新研究院 一种硒化铋材料的金相腐蚀液以及金相显示方法
CN111662717B (zh) * 2020-07-14 2021-08-31 北京航空航天大学宁波创新研究院 一种硒化铋材料的金相腐蚀液以及金相显示方法

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