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Polyamines are aliphatic hydrocarbons with terminal amino groups and are essential for biological activities. It has been reported that polyamines have health-promoting effects in animals, such as the extension of lifespan by polyamine intake. The identification of a high polyamine-producing bacterium from foods could lead to the development of a novel probiotic candidate. We aimed to identify high polyamine-producing bacteria from food, and isolated and collected bacteria from vegetables and fermented foods produced in Japan. We successfully acquired

Force measurement using zero-compliance mechanism is proposed and studied experimentally. A zero-compliance mechanism is composed of two suspensions connected in series; one of them is operated to ...

In the next generation SAOP (Self-aligned Octuplet patterning) process, the line width and LWR (Line Width Roughness) measurement of lines with sub-10 nm is required. We have already proposed a novel method of line width and LWR measurement with sub-nanometer uncertainty by using FIB (Focused Ion Beam) processing, and TEM (Transmission Electron Microscope) images as reference metrology. In the previous report, we applied the method to SAQP features. A specimen of the SAQP FinFET line and space device is coated with carbon and cut horizontally into a thin planar sample by the FIB sampling system. The thin sample is observed by using planar-TEM. The average PSD of LWR of SAQP FinFET sample at the upper and lower positions calculated from planar-TEM images. In this article, we apply the methodology to line width and roughness measurement of advanced features by SAOP process. The features are vertically or horizontally sliced as a thin specimen by FIB micro sampling system. LWR is calculated from the edges positions, and PSD (Power Spectrum Density) is analyzed for the reference metrology.

We have previously demonstrated our method to obtain unbias dense line’s LER (Line Edge Roughness) processed by EUV (Extreme Ultra-Violet) lithography. No special edge-detection, simulation modeling, beam-scan, nor image processing is required, except optimization of beam-dose parameters. For instance, threshold method that is a conventional edge-detection is used on SEM (Scanning Electron Microscopy) image taken by a conventional beam-scanning with a conventionally used beam-conditions. However, especially for EUV-lithographed features we must determine carefully landing voltage and beam-dose that cause artificial reduction of LER and LWR (Line Width Roughness) due to shrink of photo resist materials. Note that we made edge-detection interval at every 5 nm, that is as small as probe-beam diameter. For instance, we set the vertical magnification, the pixel-density, and the sum-line-per-point parameter at 52.7k, 1024, and 2, respectively. Although we can make the interval as small as sub-nanometer, it is not reliable to measure the sub-nanometer object that is only one-tenth of the probe-beam diameter. Then, we verified accuracy of our unbiased LWR by using two independent experimental methods: TEM and FIB-SEM. We obtained spectra of PSD (Power Spectrum Density) from the TEM, the FIB-SEM and our unbiassing CDSEM-method. We found the three PSDs agreed very well to each others. This result strongly implies that three independent methods measured an identical PSD, of true LWR. By our unbiassing CDSEM-method we can measure the true LWR which is calculated from the true PSD. In this work, by using the similar experimental-methods we verify accuracy of our wiggling measurement. Wiggling is a hot issue in production yield of post dry-etch process. Especially about 20 nm or less in the line-width, wiggling starts appearing due to decreased elastic-stiffness of the line feature. A reason why we study the accuracy of LER, LWR, and wiggling is inline monitor of stochastic failures. As they increase significantly in EUV lithography process, production yield may not be promising. Bisshop et al. [1] investigated pitch and/or space-width correlate to incidence of stochastic-failures, such as breaking-line and bridging-line, down to ppm (parts per million). However, the incidence of the stochastic failures should be reduced less to ppb (parts per billion) or ppt (parts per trillion) which is as small as tolerable particle contamination on a wafer. This implies significance of accurate LWR and/or wiggling monitor because in narrow line or space a-few-nanometer-LWR narrows locally them the more and causes the more stochastic failures. In this work, in order to control ppb-stochastic failures we figure out a correlation between LWR and the failures’ incidence. We need to measure billions of features, that requires too long measurement time for practical process-monitor. To shorten the measurement time we test an effective method to estimate such very few number of failures. Reference [1] Stochastic effects in EUV lithography: random, local CD variability, and printing failures, Peter De Bisschop, J. of Micro/Nanolithography, MEMS, and MOEMS, 16(4), 041013 (2017).

A 1,4-addition strategy using an enone and a copper reagent was studied for the synthesis of (-)-piperitylmagnolol. A MOM-protected biphenol copper reagent was added to BF3·OEt2-activated 4-isopropylcyclohexenone, whereas 1,4-addition of protected monophenol reagents possessing an allyl group was found to be unsuccessful. The allyl group was later attached to the p-,p'-diiodo-biphenol ring by Pd-catalyzed coupling with allylborate. The aforementioned iodide was synthesized using a new method for ortho-selective deiodination of o-,p-diiodophenols.

LER (Line Edge Roughness) and LWR (Line Width Roughness) of the semiconductor device are an important evaluation scale of the performance of the device. Conventionally, LER and LWR is evaluated from CD-SEM (Critical Dimension Scanning Electron Microscope) images. However, CD-SEM measurement has a problem that high frequency random noise is large, and resolution is not sufficiently high. For random noise of CD-SEM measurement, some techniques are proposed. In these methods, it is necessary to set parameters for model and processing, and it is necessary to verify the correctness of these parameters using reference metrology. We have already proposed a novel reference metrology using FIB (Focused Ion Beam) process and planar-TEM (Transmission Electron Microscope) method. In this study, we applied the proposed method to three new samples such as SAQP (Self-Aligned Quadruple Patterning) FinFET device, EUV (Extreme Ultraviolet Lithography) conventional resist, and EUV new material resist. LWR and PSD (Power Spectral Density) of LWR are calculated from the edge positions on planar-TEM images. We confirmed that LWR and PSD of LWR can be measured with high accuracy and evaluated the difference by the proposed method. Furthermore, from comparisons with PSD of the same sample by CD-SEM, the validity of measurement of PSD and LWR by CD-SEM can be verified.

A new metrology method of quantitatively measuring wiggling patterns in a Self-Aligned Double Patterning (SADP) process for 2D NAND technology has been developed with a CD-SEM metrology program on images from a Review-SEM system. The metrology program provided accurate modeling of various wiggling patterns. The Review-SEM system provided a-few-micrometer-wide Field of View (FOV), which exceeds precision-guaranteed FOV of a conventional CD-SEM. The result has been effectively verified by visual inspection on vertically compressed images compared with Wiggling Index from this new method. A best-known method (BKM) system has been developed with connected HW and SW to automatically measure wiggling patterns.

Measurement of line edge roughness (LER) is discussed from four aspects: edge detection, PSD prediction, sampling strategy, and noise mitigation, and general guidelines and practical solutions for LER measurement today are introduced. Advanced edge detection algorithms such as wave-matching method are shown effective for robustly detecting edges from low SNR images, while conventional algorithm with weak filtering is still effective in suppressing SEM noise and aliasing. Advanced PSD prediction method such as multi-taper method is effective in suppressing sampling noise within a line edge to analyze, while number of lines is still required for suppressing line to line variation. Two types of SEM noise mitigation methods, "apparent noise floor" subtraction method and LER-noise decomposition using regression analysis are verified to successfully mitigate SEM noise from PSD curves. These results are extended to LCDU measurement to clarify the impact of SEM noise and sampling noise on LCDU.

For EUV lithography features we want to decrease the dose and/or energy of CD-SEM’s probe beam because LER decreases with severe resist-material’s shrink. Under such conditions, however, measured LER increases from true LER, due to LER bias that is fake LER caused by random noise in SEM image. A gap error occurs between the right and the left LERs. In this work we propose new procedures to obtain true LER by excluding the LER bias from the measured LER. To verify it we propose a LER’s reference-metrology using TEM.

The addition of MeLi to boron enolates produced by the 1,4-addition of Ar2Cu(CN)Li2 to BF3·OEt2-activated enones was followed by the reaction with ClP(O)(OEt)2 to afford the corresponding enol phosphates in moderate to good yields. The scope of this method was examined with sterically hindered or electronically biased enones and/or reagents. This activation of boron enolates was successfully applied to the synthesis of the methyl ether of Δ(9)-tetrahydrocannabinol.

A novel method of sub-nanometer uncertainty for the 3D-profile measurement and LWR (Line Width Roughness) measurement by using FIB (Focused Ion Beam) processing, and TEM (Transmission Electron Microscope) and CD-SEM (Critical Dimension Scanning Electron Microscope) images measurement is proposed to standardize 3D-profile measurement through reference metrology. In this article, we apply the methodology to line profile measurements and roughness measurement of advanced FinFET (Fin-shaped Field-Effect Transistor) features. The FinFET features are horizontally sliced as a thin specimen by FIB micro sampling system. Horizontally images of the specimens are obtained then by a planar TEM. LWR is calculated from the edges positions on TEM images. Moreover, we already have demonstrated the novel on-wafer 3D-profile metrology as "FIB-to-CDSEM method" with FIB slope cut and CD-SEM measuring. Using the method, a few micrometers wide on a wafer is coated and cut by 45-degree slope using FIB tool. Then, the wafer is transferred to CD-SEM to measure the cross section image by top down CD-SEM measurement. We applied FIB-to-CDSEM method to a CMOS image sensor feature. The 45-degree slope cut surface is observed using AFM. The surface profile of slope cut surface and line profiles are analyzed for improving the accuracy of FIB-to-CDSEM method.

A method of sub-nanometer uncertainty for the 3D-profile measurement using TEM (Transmission Electron Microscope) images is proposed to standardize 3D-profile measurement through reference metrology. The proposed method has been validated for profiles of Si lines, photoresist features and advanced-FinFET (Fin-shaped Field-Effect Transistor) features in our previous investigations. However, efficiency of 3D-profile measurement using TEM is limited by measurement time including processing of the sample. In this article, we demonstrate a novel on-wafer 3D-profile metrology as "FIB-to-CDSEM method" with FIB (Focused Ion Beam) slope cut and CD-SEM (Critical Dimension Secondary Electron Microscope) measuring. Using the method, a few micrometer wide on a wafer is coated and cut by 45 degree slope using FIB tool. Then, the wafer is transferred to CD-SEM to measure the cross section image by top down CD-SEM measurement. We apply FIB-to-CDSEM method to CMOS sensor device. 3D-profile and 3D-profile parameters such as top line width and side wall angles of CMOS sensor device are evaluated. The 3D-profile parameters also are measured by TEM images as reference metrology. We compare the 3D-profile parameters by TEM method and FIB-to-CDSEM method. The average values and correlations on the wafer are agreed well between TEM and FIB-to- CDSEM methods.

For yield improvement of 3D-device manufacturing, metrology for the variability of individual device-features is on hot issue. Transmission Electron Microscope (TEM) can be used for monitoring the individual cross-section. However, efficiency of process monitoring is limited by the speed of measurement including preparation of lamella sample. In this work we demonstrate speedy 3D-profile measurement of individual line-features without the lamella sampling. For instance, we make a-few-micrometer-wide and 45-degree-descending slope in dense line-features by using Focused Ion Beam (FIB) tool capable of 300mm-wafer. On the descending slope, obliquely cut cross-section of the line features appears. Then, we transfer the wafer to Critical-Dimension Secondary Electron Microscope (CDSEM) to measure the oblique cross-section in normal top-down view. As the descending angle is 45 degrees, the oblique cross-section looks like a cross-section normal to the wafer surface. For every single line-features the 3D dimensions are measured. To the reference metrology of the Scanning TEM (STEM), nanometric linearity and precision are confirmed for the height and the width under the hard mask of the line features. Without cleaving wafer the 60 cells on the wafer can be measured in 3 hours, which allows us of near-line process monitor of in-wafer uniformity.

The addition of MeLi to boron enolates produced by the 1,4-addition of Ar2Cu(CN)Li2 to BF3·OEt2-activated enones was followed by the reaction with ClP(O)(OEt)2 to afford the corresponding enol phosphates in moderate to good yields. The scope of this method was examined with sterically hindered or electronically biased enones and/or reagents. This activation of boron enolates was successfully applied to the synthesis of the methyl ether of Δ9-tetrahydrocannabinol.

Line edge roughness (LER) and linewidth roughness (LWR) of a semiconductor device are important measures for evaluating its performance. Conventionally, LER and LWR have been evaluated from critical dimension scanning electron microscope (CD-SEM) images. However, the problem with CD-SEM measurement is that the high-frequency image noise is large, and the resolution is not sufficiently high. In order to overcome the problem of image noise in CD-SEM measurement, some techniques have been proposed. In these methods, it is necessary to set the parameters for the model and processing, and it is required to verify the correctness of these parameters using reference metrology. We have already proposed a reference metrology using the focused ion beam process and planar transmission electron microscope (planar-TEM) method. In this study, we apply the proposed method to three new samples, namely self-aligned quadruple patterning fin-shaped field-effect transistor device, extreme ultraviolet lithography (EUV) conventional resist, and EUV new material resist. The LWR and the power spectral density (PSD) of LWR are calculated from the edge positions on planar-TEM images. We confirm that the LWR and the PSD of LWR can be measured with high accuracy and evaluate the difference between PSD by the proposed method and that by CD-SEM images. Furthermore, from comparisons with the PSD of the same sample obtained using CD-SEM, the validity of measurement of PSD and LWR by CD-SEM is verified.

Measurement of line edge roughness (LER) is discussed from four aspects: edge detection, power spectrum densities (PSD) prediction, sampling strategy, and noise mitigation. General guidelines and practical solutions for LER measurement today are introduced. Advanced edge detection algorithms such as the wave-matching method are shown to be effective for robustly detecting edges from low SNR images, whereas a conventional algorithm with weak filtering is still effective in suppressing SEM noise and aliasing. An advanced PSD prediction method such as the multitaper method is effective in suppressing sampling noise within a line edge to analyze, whereas a number of lines are still required for suppressing line-to-line variation. Two types of SEM noise mitigation methods, such as the “apparent noise floor” subtraction method and LER-noise decomposition using regression analysis, are verified to successfully mitigate SEM noise from PSD curves. These results are extended to local critical-dimension uniformity (LCDU) measurement to clarify the impact of SEM noise and sampling noise on LCDU.

A novel method of sub-nanometer uncertainty for the line profile measurement using TEM (Transmission Electron Microscope) images is proposed to calibrate CD-SEM (Critical Dimension Scanning Electron Microscope) line width measurement and to standardize line profile measurement through reference metrology. The proposed method has been validated for profile of Si line and photoresist features in our previous investigations. In this article, we apply the methodology to line profile measurements of advanced-FinFET (Fin-shaped Field-Effect Transistor) features. The FinFET features are sliced as thin specimens of 100 nm thickness by FIB (Focused Ion Beam) micro sampling system. Cross-sectional images of the specimens are obtained then by TEM. The profiles of fin, hardmask and dummy gate of FinFET features are evaluated using TEM images. The width of fin, the length of hardmask, and the length of dummy gate of FinFET features are measured and compared to CD-SEM measurement. The TEM results will be used to implement CD-SEM and CD-AFM reference metrology.

Change in the cross-sectional profile of a photoresist (PR) pattern due to shrinkage was evaluated to investigate the mechanism of electron beam-induced shrinkage. A scanning transmission electron microscope (STEM) was used to observe the cross-sectional profiles of PR lines after atomic-layer deposition of metal oxide and carbon deposition on the sample surface. A HfO2 thin layer enhanced the profile contrast in the STEM measurements without blurring the edge, which enabled the precise cross-sectional measurement of the PR patterns. We found interesting features associated with shrinkage from the detailed profile change obtained using this method, such as a rounding of the pattern top, a necking of the sidewall profile, a rounding of the foot in the pattern on the organic underlying layer, and voltage-independent sidewall shrinkage under a large electron beam dose. These behaviors along with the results from a Monte Carlo simulation are discussed. Consequently, these observations experimentally clarified that the elastic deformation effect and the impact of the secondary electrons emitted from the spaces around the pattern into the sidewall are important to interpret the change in the shape of the pattern induced by shrinkage.