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[Masahiko Shimizu](https://orcid.org/0009-0009-3107-6829), [Katsuaki Nakazawa](https://orcid.org/0000-0002-6056-5615), Hisashi Shima, Hajime Matsumoto, Takahiko Takewaki, [Kazutaka Mitsuishi](https://orcid.org/0000-0002-9361-4057), [Ayako Hashimoto](https://orcid.org/0000-0002-1985-7667)

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[Atomic-scale insights into the Cu ion distribution in zeolites used for ammonia selective catalytic reduction during early hydrothermal degradation](https://mdr.nims.go.jp/datasets/2469d739-c407-4719-99a2-b2160ca124de)

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Atomic-scale insights into the Cu ion distribution in zeolites used for ammonia selective catalytic reduction during early hydrothermal degradation ChemCommChemical Communicationsrsc.li/chemcomm COMMUNICATION  Masahiko Shimizu, Kazutaka Mitsuishi, Ayako Hashimoto  et al .  Atomic-scale insights into the Cu ion distribution in zeolites used for ammonia selective catalytic reduction during early hydrothermal degradation ISSN 1359-7345Volume 62Number 105 February 2026Pages 3063–33923260 |  Chem. Commun., 2026, 62, 3260–3264 This journal is © The Royal Society of Chemistry 2026Cite this: Chem. Commun., 2026,62, 3260Atomic-scale insights into the Cu ion distributionin zeolites used for ammonia selective catalyticreduction during early hydrothermal degradationMasahiko Shimizu, *abc Katsuaki Nakazawa, d Hisashi Shima,aHajime Matsumoto,ab Takahiko Takewaki,a Kazutaka Mitsuishi *d andAyako Hashimoto *bcEarly hydrothermal degradation of Cu-SSZ-13 and Cu-SSZ-39 zeo-lites with similar Cu content was investigated. Electron ptychogra-phy revealed the Cu occupancy at the eight-membered ring sites ofCu-SSZ-39 is lower than that of Cu-SSZ-13, clearly demonstratingthat the former is more stable than the latter under hydrothermalaging conditions.Ammonia selective catalytic reduction (NH3-SCR) is a keyexhaust purification technology for diesel vehicles that uses acommercial catalyst, Cu-SSZ-13 zeolite with the CHA topo-logy.1–3 The catalyst performance declines considerably afterhydrothermal aging (HTA) above 800 1C. This problem remainsunresolved despite extensive research.4–10 However, Cu-SSZ-39with the AEI topology has high hydrothermal stability and isregarded as a promising alternative.11,12 Generally, the stabilityof Cu-exchange zeolites is influenced by several factors, such asthe zeolite framework, Si/Al ratio, and Cu loading.5,7,9,13 Thehydrothermal stability of Cu-exchange zeolites is greater for theAEI topology than the CHA topology and increases as the Si/Alratio and Cu loading decrease.5,7,11 Mechanistically, degrada-tion is thought to involve dealumination and the redistributionof Cu ions, leading to the formation of CuOx clusters andcollapse of the zeolite framework.6–9 Although these processesoriginate at the atomic scale, previous analyses have relied onspatially averaged data obtained using techniques such as X-raydiffraction (XRD) and spectroscopy.14,15 Thus, the atomic-levelmechanisms remain poorly understood.Transmission electron microscopy (TEM) enables directobservation at the atomic scale.16,17 However, zeolites arevery easily damaged by an electron beam.18,19 This sensitivityis particularly pronounced in Al-rich catalytic zeolites, necessi-tating a drastic reduction in the electron dose applied.20Consequently, it remains difficult to observe the degradedstructure of NH3-SCR catalysts at the atomic level, often limit-ing observation to nanometer-scale Cu aggregates.5 Electronptychography21–23 has emerged as a promising low-dose tech-nique to overcome this limitation. This technique has beenapplied to various beam-sensitive materials, includingzeolite.24–32 We previously used this technique to visualize Cuions in Cu-SSZ-13.33,34 Building on this foundation, our primarygoal in this study was to uncover the atomic-scale origins ofhydrothermal stability in Cu-exchanged zeolites.To achieve this goal, we investigated two strategically chosenzeolites with comparable Cu loadings (4.2–4.7 wt%): Cu-SSZ-39(AEI; Si/Al = 5.2, Cu/Al = 0.29) and Cu-SSZ-13 (CHA; Si/Al = 12.6,Cu/Al = 0.57). Compared with the Cu-SSZ-13 zeolite, the Cu-SSZ-39 zeolite was expected to be more stable owing to its topo-logy and lower Si/Al ratio. The compositions of the two zeoliteswere optimized to balance NOx conversion rate, hydrothermalstability, and selectivity.7,35,36 We employed a multiscale approachto evaluate the impact of HTA on both the catalytic activity andstructure of the zeolites. We used conventional structural char-acterization techniques (XRD and TEM) to obtain macroscopicinformation about the zeolites. We employed electron ptychogra-phy specifically to visualize changes in the zeolite at the atomiclevel. We combined these multiscale findings to elucidate thehydrothermal degradation mechanism.The topologies of the two investigated zeolites are shown inFig. 1a (CHA for SSZ-13) and Fig. 1b (AEI for SSZ-39). Thesestructures differ in the linkage of the double six-membered ring(d6r) units, which are arranged in parallel in CHA and areconnected via a mirror plane in AEI. Fig. 1c shows the two Cusites in Cu-SSZ-13 at room temperature under ambient condi-tions, as has been reported on the basis of Rietveld refinementof XRD data.37 The Cu ion at the d6r site (Fig. 1c, A site) ishydrothermally more stable than the eight-membered ring(8mr) site (Fig. 1c, B site), which is considered unstable.7,8,38a Science & Innovation Center, Mitsubishi Chemical Corporation,1000 Kamoshida-cho, Aoba-ku, Yokohama, Kanagawa, Japanb Research Center for Energy and Environmental Materials, National Institute forMaterials Science, 1-2-1 Sengen, Tsukuba, Ibaraki, Japanc Graduate School of Science and Technology, University of Tsukuba, 1-2-1 Sengen,Tsukuba, Ibaraki, Japand Center for Basic Research on Materials, National Institute for Materials Science, 1-2-1 Sengen, Tsukuba, Ibaraki, Japan. E-mail: mitsuishi.kazutaka@nims.go.jpReceived 4th November 2025,Accepted 2nd January 2026DOI: 10.1039/d5cc06274hrsc.li/chemcommChemCommCOMMUNICATIONOpen Access Article. Published on 08 January 2026. Downloaded on 3/24/2026 10:13:40 AM.  This article is licensed under a Creative Commons Attribution-NonCommercial 3.0 Unported Licence.View Article OnlineView Journal  | View Issuehttps://orcid.org/0009-0009-3107-6829https://orcid.org/0000-0002-6056-5615https://orcid.org/0000-0002-9361-4057https://orcid.org/0000-0002-1985-7667http://crossmark.crossref.org/dialog/?doi=10.1039/d5cc06274h&domain=pdf&date_stamp=2026-01-09https://rsc.li/chemcommhttp://creativecommons.org/licenses/by-nc/3.0/http://creativecommons.org/licenses/by-nc/3.0/https://doi.org/10.1039/d5cc06274hhttps://pubs.rsc.org/en/journals/journal/CChttps://pubs.rsc.org/en/journals/journal/CC?issueid=CC062010This journal is © The Royal Society of Chemistry 2026 Chem. Commun., 2026, 62, 3260–3264 |  3261Similarly, Cu-SSZ-39 is reported to possess two distinct Cu sitesanalogous to those in Cu-SSZ-13.5,39The hydrothermal stability of Cu-SSZ-13 and Cu-SSZ-39 wasevaluated via standard NH3-SCR activity tests. As shown inFig. S1 (gas hourly space velocity = 2.0 � 105 h�1), aging inthe 150–500 1C temperature range decreased the averageactivity by 9.8% for Cu-SSZ-13 but by only 3.1% for Cu-SSZ-39.Thus, it was confirmed that both zeolites exhibited reducedactivity due to aging, where the decrease in activity was smallerfor Cu-SSZ-39 than for Cu-SSZ-13.To clarify the structural changes induced by HTA, we firstinvestigated the samples before and after aging using severalconventional characterization techniques involving spatialaveraging, including XRD, scanning electron microscopy-energy dispersion X-ray spectroscopy (SEM-EDS), and TEM.The XRD patterns of Cu-SSZ-13 and Cu-SSZ-39 (Fig. S2) con-tained the characteristic diffraction peaks for the respectiveframeworks. Comparison of the full widths at half maximum ofselected peaks in the patterns obtained before and after HTA(Table S1) revealed no important differences for either zeolite,indicating that crystallinity of the framework was preservedupon aging. Similarly, no important changes were observed inthe Cu distribution in the zeolites: SEM-EDS mapping showedthat the Cu ions remained highly dispersed throughout thezeolite particles, regardless of hydrothermal treatment (Fig. S3).The TEM observations of the particle morphology (Fig. S4 andS5) revealed numerous faceted particles with single crystallinedomains in both zeolites before and after HTA. Additionally,the aged samples did not appear to contain CuOx clusters,5,40which have been reported to form as a result of considerablehydrothermal degradation. Considering the results of theseconventional characterization methods together shows thatHTA produced no important changes in the framework crystal-linity, interparticle elemental distribution, or particle morphol-ogy of either Cu-SSZ-13 or Cu-SSZ-39. This result suggests thatthe initial loss in catalytic activity was caused by more subtlestructural alterations that were not discernible by the tech-niques used.We subsequently employed electron ptychography to per-form a detailed, atomic-scale structural analysis of five sam-ples: fresh and hydrothermally aged Cu-SSZ-13 and Cu-SSZ-39as well as Cu-free H-SSZ-13 as a reference for the visualizationof Cu ions. The observation orientations were selected as the[100] directions in CHA and AEI, as shown in Fig. 1a and b(Fig. S6). Using this orientation made the d6r units alignparallel to the electron beam, directly revealing the structuraldifferences originating from the distinct linkage patterns ofthese units. Fig. S7–S11 show the ptychographic imagesacquired for the five samples over a field of view of approxi-mately 10 nm square. It has been reported that large defocus inptychographic images can cause internal pore artifacts.33,34Consequently, we carefully managed the defocus conditionsto ensure that the ptychographic observations were reliable. Wehave previously demonstrated that under this observation con-dition, artifacts are negligible for defocus below 5 nm, allowingatomic columns containing Cu to be clearly distinguished fromthose without Cu.33 Accordingly, we confirmed that the defocusfor each reconstructed image was maintained below 5 nm (seethe captions of Fig. S7–S11). To enhance the signal-to-noiseratio, a moving-average procedure was used to align andaverage approximately 20 equivalent sites for each sample.41The averaged images are presented in Fig. 2. The CHA frame-work (Fig. 1a) is clearly resolved in the image of the referenceH-SSZ-13 (Fig. 2a). The image of the fresh Cu-SSZ-13 sample(Fig. 2b) contains distinct bright spots in the 8mr region (asindicated by the white arrow). These spots are assigned to Cuions. This assignment is supported by the reconstructed defo-cus value of �1.4 nm (Fig. S12). By contrast, no such brightspots appear in the image of the sample subjected to HTA(Fig. 2c). A similar trend was observed for Cu-SSZ-39. The AEIframework is clearly resolved in the images of both the fresh(Fig. 2d) and aged (Fig. 2e) samples and is consistent with themodel presented in Fig. 1b. The image of the fresh sample alsocontains bright spots in the 8mr region, which are assignable toCu ions (reconstructed defocus: +1.4 nm; Fig. S13). However,these spots are absent in the image of the aged sample. Directvisualization of Cu ions at the d6r sites proved inconclusive,primarily because of strong overlap between the Cu ions and Si(Al) atomic columns in the chosen projection (Fig. S14). Thischallenge was particularly pronounced for the AEI structure,which lacks an alternative zone axis that can enable clear d6robservation. The averaged and original nonaveraged images(Fig. S7–S11) yielded consistent key results for the 8mrsites—namely, the presence of Cu ions in the fresh samplesand the absence of these ions in the aged samples.To determine the relative quantity of Cu ions at the 8mr sitesof the two zeolites and how this quantity changes upon HTA, wecompared the contrast values of the five samples. In ptycho-graphy, the retrieved phase contrast increases with the pro-jected potential of the sample, provided that the phase shift ofelectron wave remains below 2p. Considering that no phaseinversion was observed for the Si (Al) columns, the relativequantity of Cu ions at the 8mr sites was determined bycomparing the contrast for the five samples. Fig. 3 shows theline profiles obtained from the averaged ptychographic imagesof the five samples shown in Fig. 2. The extracted regioncorresponds to the area between two O atomic columnsFig. 1 Framework models of (a) SSZ-13 (CHA) and (b) SSZ-39 (AEI) viewedalong the [100] direction. (c) Two Cu sites in Cu-SSZ-13 viewed perpendi-cular to the eight-membered ring (8mr) site:37 the double six-memberedring (d6r; A, large green atom) and 8mr (B, large pink atom). To guide theeye, the d6r and 8mr sites are indicated by green and pink lines connectingSi atoms for SSZ-13, respectively, and by red and light-blue lines for SSZ-39, respectively. Element colors: Si (Al) = blue, O = red.Communication ChemCommOpen Access Article. Published on 08 January 2026. Downloaded on 3/24/2026 10:13:40 AM.  This article is licensed under a Creative Commons Attribution-NonCommercial 3.0 Unported Licence.View Article Onlinehttp://creativecommons.org/licenses/by-nc/3.0/http://creativecommons.org/licenses/by-nc/3.0/https://doi.org/10.1039/d5cc06274h3262 |  Chem. Commun., 2026, 62, 3260–3264 This journal is © The Royal Society of Chemistry 2026(delineated by the red box) in the SSZ-13 (CHA) and SSZ-39(AEI) models viewed along the [100] direction, as illustrated inthe inset (left) of Fig. 3. In the line profile of H-SSZ-13, a weakpeak appears near the center between the O columns. Thispeak is presumed to mainly result from contributions fromadsorbed volatile organic compounds or a surface amorphouslayer produced by beam damage. In the line profile of thefresh Cu-SSZ-13 sample, the large peak near the centerbetween the two O columns can be interpreted as originatingfrom Cu ions, as mentioned above. Notably, the high peakintensity for the line profile of the fresh Cu-SSZ-13 sampledecreases in the line profile of the aged sample. The peakintensity for the aged sample profile is similar to that ofH-SSZ-13, indicating a substantial reduction of Cu ions inthe 8mr upon aging. Similar behavior is observed for Cu-SSZ-39: the 8mr center contrast for the fresh sample exceedsthat of H-SSZ-13, suggesting the presence of Cu ions; however,the 8mr center contrast for the aged sample is comparableto that of H-SSZ-13, again indicating Cu loss from the 8mr.The contrast for the 8mr region in the aged sample washigher for Cu-SSZ-13 than for Cu-SSZ-39. Both sampleswere prepared to have similar Cu contents. In previousstudies,5,38,42 Cu sites were reported to be either 8mr or d6r.Therefore, the Cu-SSZ-39 sample studied here has a lower Cuoccupancy at the 8mr site than Cu-SSZ-13. That is, Cu-SSZ-39can be considered to have a higher Cu occupancy at the d6rsite than Cu-SSZ-13.Fig. 3 Line profiles for the eight-membered ring (8mr) region obtained fromthe ptychographic images shown in Fig. 2. The line profiles were acquired forthe regions between the two O atomic columns indicated by the red boxes inthe inset (left). The values on the vertical axis were normalized using themaximum and minimum values for each line profile. The origin of thehorizontal axis is placed at one O column. The unnormalized profiles showingidentical relative trends for the samples are provided in Fig. S15.Fig. 2 Ptychographic images viewed along the [100] direction of (a) H-SSZ-13 (without Cu), (b) Cu-SSZ-13, (c) Cu-SSZ-13-HTA, (d) Cu-SSZ-39, and(e) Cu-SSZ-39-HTA. All the images were subjected to moving averaging by performing alignment and averaging over approximately 20 sites. The whitearrows indicate areas of bright spots in the eight-membered ring (8mr) region of both zeolites before hydrothermal aging (HTA). Scale bar: 0.5 nm.ChemComm CommunicationOpen Access Article. Published on 08 January 2026. Downloaded on 3/24/2026 10:13:40 AM.  This article is licensed under a Creative Commons Attribution-NonCommercial 3.0 Unported Licence.View Article Onlinehttp://creativecommons.org/licenses/by-nc/3.0/http://creativecommons.org/licenses/by-nc/3.0/https://doi.org/10.1039/d5cc06274hThis journal is © The Royal Society of Chemistry 2026 Chem. Commun., 2026, 62, 3260–3264 |  3263Next, we present a mechanism for hydrothermal degrada-tion on the basis of our experimental results. Although theactivity tests indicated differing stabilities for the two zeolites,no structural changes reflecting different degradation levelswere detected using the conventional techniques. By contrast,atomic-scale electron ptychography clearly revealed a reductionin the Cu ion occupancy at the 8mr sites after aging. A keyfinding is that the less stable Cu-SSZ-13 contained a higherinitial quantity of Cu ions at these 8mr sites than the morestable Cu-SSZ-39. This observation supports previous reportsproposing that these mobile 8mr ions migrate to formframework-disrupting CuOx clusters.5,7,9 Therefore, the loss ofCu ions from the 8mr sites can be interpreted as the onset of astructural response to HTA.In this study, electron ptychography was used to visualizeearly hydrothermal degradation at the atomic level. Subtlechanges in the Cu ion occupancy at the 8mr sites were success-fully captured using this technique, whereas no structuralchanges were observed using XRD or conventional TEM. Thesefindings provide concrete, atomic-scale evidence for theproposed degradation mechanism, going beyond previousinferences from spatially-averaged data.14,15 Considering thatthe 8mr and d6r Cu sites are known to differ not only inhydrothermal stability but also in activity and selectivity,5,9 amultiscale approach including electron ptychography providesguidelines for the rational design of highly durable and high-performance zeolites based on control of the arrangement ofCu ions.M. S. led the investigation, data analysis, and writing of theoriginal manuscript. A. H. and K. M. supervised the project.M. S., T. T., and K. M. conceptualized the study. K. M. devel-oped the methodology and software, with support fromK. N. H. M. acquired funding. H. S. provided resources. Allauthors discussed the results and approved the final manuscript.We thank H. Mizukami (MCC) for performing the XRDmeasurements and Q. Han (MCC) for preparing samples. Thisstudy was a collaboration between MCC and NIMS. This studywas partially supported by the ‘‘Advanced Research Infrastruc-ture for Materials and Nanotechnology in Japan (ARIM)’’department of the Ministry of Education, Culture, Sports,Science, and Technology (MEXT) (Grant Number JPMXP1224NM5123) and by KAKENHI, Japan Society for the Promotion ofScience (Grant Number 24K15598, K.M.). We thank Edanz(https://jp.edanz.com/ac) for editing a draft of this manuscript.Conflicts of interestThere are no conflicts to declare.Data availabilityThe data supporting this article have been included as part ofthe supplementary information (SI). Supplementary information:sample preparation, activity test conditions, characterizationconditions, and figures/a table for material characterizations.See DOI: https://doi.org/10.1039/d5cc06274h.References1 A. M. Beale, F. Gao, I. Lezcano-Gonzalez, C. H. F. Peden andJ. Szanyi, Chem. Soc. Rev., 2015, 44, 7371–7405.2 J. H. Kwak, R. G. Tonkyn, D. H. Kim, J. Szanyi and C. H. F. Peden,J. 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