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Masahiro Ohkuma, [Ryo Matsumoto](https://orcid.org/0000-0001-6294-5403), Shintaro Adachi, Shinobu Onoda, Takao Watanabe, Kenji Ohta, [Yoshihiko Takano](https://orcid.org/0000-0002-1541-6928), Keigo Arai

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[Probing the Meissner effect in single crystals of Bi2Sr2Ca2Cu3O10+δ via wide-field quantum microscopy under high pressure](https://mdr.nims.go.jp/datasets/5cda0f35-03f4-4b5b-a397-997c90492757)

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Probing the Meissner effect in single crystals of $\mathbf{Bi_2Sr_2Ca_2Cu_3O_{10+\delta}}$ via wide-field quantum microscopy under high pressureProbing the Meissner effect in single crystals of Bi2Sr2Ca2Cu3O10+δ via wide-fieldquantum microscopy under high pressureMasahiro Ohkuma1,∗ Ryo Matsumoto2, Shintaro Adachi3, Shinobu Onoda4,Takao Watanabe5, Kenji Ohta6, Yoshihiko Takano2, and Keigo Arai11School of Engineering, Institute of Science Tokyo, Yokohama 226-8501, Kanagawa, Japan2Research Center for Materials Nanoarchitectonics (MANA),National Institute for Materials Science, Tsukuba 305-0047, Ibaraki, Japan3Department of Mechanical and Electrical Systems Engineering,Kyoto University of Advanced Science (KUAS), Kyoto 615-8577, Kyoto, Japan4National Institutes for Quantum Science and Technology (QST), Takasaki 370-1292, Gunma, Japan5Graduate School of Science and Technology, Hirosaki University, Hirosaki 036-8561, Aomori, Japan and6Department of Earth and Planetary Sciences, Institute of Science Tokyo, Meguro 152-8551, Tokyo, Japan(Dated: March 17, 2026)We investigated the pressure dependence of the superconducting transition temperature (Tc) inoptimally doped Bi2Sr2Ca2Cu3O10+δ (Bi-2223) single crystals using different pressure-transmittingmedia. Previous high-pressure studies have reported conflicting behaviors, ranging from a resurgenceof Tc of optimally doped Bi-2223 in fluid media to an insulating-like transition in solid media.However, a direct comparison of the effects of different pressure-transmitting media is lacking.Here, we employed wide-field quantum microscopy based on nitrogen-vacancy centers to probe themagnetic response under high pressure, utilizing cBN and KBr as media. We observed that adiamagnetic response near 70 K, indicative of the superconducting transition, persisted up to 23GPa in KBr, whereas it disappeared above 11 GPa and 70 K in cBN. These results demonstrate thehigh sensitivity of Bi-2223 to the pressure environment and highlight the critical role of hydrostaticpressure in cuprate superconductors.High-pressure techniques are powerful tools for directlymodulating material structures, enabling the explorationof emergent physical properties and the discovery of novelmaterials [1–3]. In characterizing physical properties un-der these extreme high-pressure conditions, on the orderof several tens of GPa or above, achieving isotropic com-pression is as crucial as the pressure magnitude. For in-stance, in superconducting phases that were recently dis-covered in nickel oxides under high pressure, maintain-ing isotropic pressure is known to be advantageous forstabilizing superconducting phases [4–8]. In the case ofBi-based cuprates, the pressure dependence of the super-conducting transition temperature (Tc) initially exhibitsa dome-shaped behavior [9–15]. In Bi2Sr2Ca2Cu3O10+δ(Bi-2223), however, while Tc exhibits an upturn at higherpressures when a fluid pressure-transmitting medium isused, the use of a solid medium leads to an insulating-liketransition and the subsequent disappearance of the zero-resistance state [10, 11]. Although high-pressure struc-tural analyses suggest that these discrepancies stem fromthe pressure-transmitting media dependence of structuralmodifications [16], there have been no direct compar-ative studies evaluating the superconducting propertiesusing different pressure-transmitting media in the high-pressure region.Tc under high pressure is mainly evaluated usingelectrical transport and magnetic measurements. Intransport measurements, the need for electrical con-tacts and wiring makes experiments using fluid-pressure-∗ okuma.m.36c3@m.isct.ac.jptransmitting media difficult. In conventional magneticmeasurements, the signal amplitude scales directly withthe sample volume, which often limits the pressurerange [17]. Consequently, existing approaches have dif-ficulty performing systematic studies across pressure-transmitting media ranging from solids to fluids and evengases. Recently, the negatively charged nitrogen-vacancy(NV) center in diamond has emerged as a highly sen-sitive nanoscale probe for sensing, including under ex-treme conditions [18–31]. The NV center has an elec-tronic spin of S = 1, whose spin state can be initializedand read out optically and coherently manipulated usingresonant microwave fields (Fig. 1a) [32, 33]. This tech-nique is known as optically detected magnetic resonance(ODMR). By integrating a thin layer of NV centers into adiamond anvil cell (DAC), it is possible to perform high-spatial-resolution imaging of physical quantities, such asmagnetic fields and stress, directly at the sample inter-face [26, 27]. In contrast to conventional magnetometry,which typically involves signals from the entire pressurecell, this quantum sensing platform enables the direct ob-servation of local magnetic fields. This spatially resolvedapproach offers a distinct advantage for the direct detec-tion of the Meissner effect in micrometer-sized samples,even above 100 GPa [30, 34, 35].In this study, we conducted wide-field quantum mi-croscopy to investigate the superconducting propertiesof Bi-2223 single crystals under high pressure using dif-ferent pressure-transmitting media KBr and cBN. BothKBr and cBN are solids; however, hydrostaticity can dif-fer due to different of the mechanical properties. We spa-tially resolved the diamagnetic signal via the NV centerarXiv:2603.15102v1  [cond-mat.supr-con]  16 Mar 2026mailto:okuma.m.36c3@m.isct.ac.jphttps://arxiv.org/abs/2603.15102v12and observed a pronounced dependence on the pressure-transmitting medium: a clear diamagnetic response per-sisted up to 23 GPa in KBr near 70 K, whereas it wassuppressed above 11 GPa in cBN. These results highlightthe critical role of hydrostatic pressure in cuprate super-conductors.Ground stateExcited stateSinglet state~2.87 GHza2.9 3.0 3.1 3.2 3.30.960.970.980.991.00 Out of sample On sampleIntensityFrequency (GHz)e23 GPa76±3 K|0>|±1>BKBrc dcBNPt foilPt foil Intensity4780014000RecBN+epoxycBN or KBrPt foil Bi2223bCryostatFIG. 1. (a) Energy diagram of the NV center. (b) Overviewof the experimental setup. (c) and (d) Wide-field photolumi-nescence image of the NV centers inside DAC using (c) KBrand (d) cBN. The red circles indicate the position of Bi-2223.Each scale bar represent 20 µm. (e) ODMR spectra of NVcenters above and outside the superconducting region.Pressure was applied using a DAC made of CuBe. Anoverview of the experimental setup is shown in Fig. 1b.We used a type Ib diamond anvil with a culet diame-ter of 300 µm and a {111}-oriented culet surface (SYN-TEK Co., Ltd.). To create NV centers, 12C+ ionswere implanted at an energy of 30 keV with a dose of5× 1012 cm−2, and the diamond anvil was subsequentlyannealed in vacuum at 1000 ◦C for 2 h. A rhenium gasketwas pre-indented to a thickness of 50 µm, and a hole witha diameter of 250 µm was drilled. To prevent electricalcontact between the microwave waveguide and the rhe-nium gasket, the hole was filled with a cBN–epoxy mix-ture, pre-indented, and then the sample chamber with adiameter of 100 µm was drilled. A Pt foil with thick-ness of 5 µm and Bi-2223 were placed on the diamondanvil. The sample chamber was filled with cBN or KBrpowder as the pressure-transmitting medium. Wide-fieldphotoluminescence images are shown in Figs. 1c and d.Pressure was estimated from the diamond Raman shiftmeasured at room temperature using a spectrometer (in-Via, Renishaw) [36]. The results of Raman spectroscopymeasurements are shown in supplemental material. TheBi-2223 single crystal was grown by the traveling-solventfloating-zone method, and as-grown Bi-2223 single crys-tals were annealed at 500 ◦C under a flowing 100% oxygengas (oxygen partial pressure of 1 atm) to obtain optimallydoped samples with Tc ∼ 110 K [37–40].Low-temperature wide-field ODMR measurementswere performed using a home-built optical setup inte-grated with a custom-built Gifford–McMahon refrigera-tor. The temperature was measured using a Cernox ther-mometer mounted on a stage in thermal contact with theDAC and monitored with a temperature controller (LakeShore, Model 335). A green excitation laser (MLL-S-532B, CNI laser) was focused onto the sample throughan objective lens (M-PLAN APO 7.5X, Mitsutoyo), andthe red fluorescence was collected by the same objective.The photoluminescence was filtered by a long-pass filterand imaged onto an EMCCD camera (Andor, iXon Ultra897). Microwaves were generated using a signal generator(SynthHD, Windfreak) and amplified using a power am-plifier (ZHL-16W-43+, Mini-circuits). To minimize me-chanical vibrations, the cold head was deactivated dur-ing data acquisition so that the temperature increasedduring the measurement. The temperature was definedas the mean of the temperatures measured immediatelybefore and after each acquisition, while the temperatureuncertainty was taken as the full range between these twovalues. Each ODMR spectrum was acquired within upto 15 min. A magnetic field was applied along the ⟨111⟩direction using a coil wound around the DAC.The spin sublevels of the NV center undergo Zeemansplitting when a magnetic field is applied. When a su-perconductor is placed on top of the NV layer, the lo-cal magnetic field sensed by the NV centers is reducedbelow Tc owing to magnetic flux expulsion (the Meiss-ner effect). Consequently, the ODMR splitting measuredabove the superconducting region becomes smaller thanthat measured outside the superconducting region. Fig-ure 1e shows representative ODMR spectra obtained be-low Tc. After cooling the sample to below 20 K, weperformed zero-field cooling (ZFC) and acquired ODMRspectra during the subsequent warming process. A mag-netic field of approximately 4 mT was applied. Thepressure was 23 GPa, the temperature was 76 ± 3 K,and KBr was used as the pressure-transmitting medium(the corresponding wide-field image is shown in Fig. 2c).The spectrum exhibits three resolved resonance peaks:the two outer resonances are attributed to NV centers,whose axes are nearly aligned with the applied field,whereas the central feature originates from NV centerswith other crystallographic orientations. The fourth res-onance expected from these non-aligned orientations wasnot separately resolved because it overlapped with thehigh-frequency ⟨111⟩ resonance within the linewidth. Be-low Tc, the splitting associated with the field-aligned NVcenters is reduced above the superconducting region, in-dicating that Meissner screening persists even at 23 GPa.In the following section, we present the wide-field ODMRresults. In each measurement, the pressure was increasedat room temperature, and ODMR spectra were acquiredduring the warming process after ZFC.Figure 2 shows the results obtained using KBr as thepressure-transmitting medium. Data points for whichthe half-width of the 95% confidence interval of the fit-ted resonance frequencies of the two outer peaks exceeded5 MHz were excluded from the analysis. ODMR signals3were clearly observable only in the vicinity of the Pt foil.In regions where the ODMR features became barely dis-cernible, the fitted peak positions exhibited large uncer-tainties and were therefore excluded. We attribute thereduced ODMR visibility mainly to weaker microwavedriving and an insufficient signal-to-noise ratio owing tolimited averaging. In Figs. 2a–c, a clear diamagneticsignal was observed below 80 K. In contrast, the dia-magnetic signal disappeared well above Tc, as shown inFig. 2d. A comparison of Figs. 2b and c reveals that thediamagnetic signal is smaller in Fig. 2c, suggesting thatTc decreases with increasing pressure.Splitting (MHz)1502409 GPa70 ± 3 K17 GPa76 ± 3 K23 GPa76 ± 3 K23 GPa124 ± 3 KacbdFIG. 2. Map of the ODMR splitting using KBr as thepressure-transmitting medium. (a)–(c) Results below Tc withdifferent pressures. (d) Result above Tc at 23 GPa. Eachscale bar represents 20 µm.Next, we performed experiments using cBN as thepressure-transmitting medium. Figures 3a–c show im-ages acquired at temperatures of approximately 70 K. At0 GPa, a diamagnetic signal was observed over the entiresample area. However, analyzable ODMR spectra wereobtained only in the vicinity of the Pt foil upon pres-surization. A diamagnetic signal was detected directlybeneath the Pt foil at 6 GPa, whereas no clear diamag-netic signal was observed at 11 GPa above 70 K. Wefurther increased the pressure up to 19 GPa; however noclear diamagnetic signal was detected above 30 K withour current setup. After pressure release, a very weakdiamagnetic signal reappeared, as shown in Fig. 3d. A re-duction in the diamagnetic signal after pressurization hasalso been observed in magnetic measurements of cupratesuperconductors [41, 42].Figure 4 summarizes the temperature dependence ofthe ODMR splitting. The shift was calculated as the dif-ference between the mean values of the pixels on the sam-ple and those in the background, with error bars repre-senting the combined uncertainty derived from the stan-dard deviations of both pixel groups. In the measure-ments using KBr, the onset of the diamagnetic signalSplitting (MHz)1802100 GPa69± 3 K6 GPa68 ± 3 K11 GPa69 ± 3 K0 GPa35 ± 4 KacbdFIG. 3. Map of the ODMR splitting using cBN as thepressure-transmitting medium. (a) and (b) Results below Tcwith different pressures. (c) Result above Tc at 11 GPa. (d)Result after pressure releasing from 19 GPa. Each scale barrepresents 20 µm.a bKBr cBNFIG. 4. Temperature dependence of ODMR splitting. Re-sults using (a) KBr and (b) cBN as the pressure-transmittingmedia. The shift was calculated as the difference betweenthe mean values of pixels on the sample and those in thebackground, with error bars representing the combined un-certainty derived from the standard deviations of both pixelgroups. Bars represents the onset temperature where the dia-magnetic signals are observed.shifts toward lower temperatures with increasing pres-sure, suggesting a decrease in Tc. Conversely, in cBN,the non-hydrostatic pressure significantly suppresses su-perconductivity. At 11 GPa, the diamagnetic responsewas clearly visible; however, at 19 GPa, we could notresolve clear a diamagnetic signal down to 30 K in oursetup. This behavior is consistent with previous elec-trical measurements using cBN, which reported a muchlower zero-resistance temperature and insulating-like re-sistance behavior. Notably, after releasing the pressurefrom 19 GPa, a diamagnetic signal re-emerged below60 K. However, the diamagnetic signal was observed at alower temperature than in the initial state, and its mag-nitude did not fully recover. This irreversibility suggeststhat the Tc suppression in cBN is not solely driven by lat-tice compression; rather, extrinsic effects, such as latticedistortion or grain refinement, likely play a significant4role.Our results indicate that when cBN is used as apressure-transmitting medium, superconductivity can bestrongly suppressed and may evolve toward an insulating-like behavior. Similar tendencies have also been reportedfor Bi2Sr2CaCu2O8+δ (Bi-2212), suggesting that the be-havior of Bi-based cuprates under high pressure may de-pend sensitively on the pressure environment. For exam-ple, an insulating-like behavior has been reported whenusing cBN, whereas with silicone oil, Tc is reported toincrease again above approximately 40 GPa [12, 13]. Re-lated behavior has also been discussed for experimentsusing NaCl as a pressure-transmitting medium, where aninsulating-like change appears upon pressurization [14].Notably, in the report, no obvious cracks were observedafter pressurization, and zero resistance as well as metal-lic conductivity were recovered after pressure release, im-plying that the insulating-like behavior is not caused byextrinsic effects [14]. While structural analyses underhigh pressure emphasize the importance of hydrostatic-ity in cuprate superconductors, a unified understandingof why different pressure media can lead to qualitativelydifferent outcomes remains elusive [16].To resolve these discrepancies, a local and non-contactprobe that can operate under high-pressure environmentsis highly desirable. Wide-field quantum microscopy un-der high pressure is well suited to address this issue be-cause it enables contact-free, spatially resolved measure-ments of magnetic responses in micrometer-scale sam-ples. This capability opens a route to systematicallyvary the pressure-transmitting medium from solids togases and track how superconducting signatures evolveunder controlled pressure environments. In particular,the spatial information provided by NV-based magne-tometry may help disentangle contributions from hydro-staticity versus non-hydrostatic stress and local strain,which are difficult to separate in conventional bulk mag-netometry or transport measurements. Furthermore, ifadvanced quantum-metrology protocols, such as quan-tum noise spectroscopy, can be extended to high-pressureconditions, it is expected to provide deeper insights intothe pressure-driven transition [43, 44].Given that the superconductivity of cuprates can besensitive to the pressure environment, it is crucial todistinguish intrinsic pressure effects from those arisingfrom non-hydrostatic pressure. Previous studies on Hg-based cuprates under hydrostatic pressure using a cubicanvil cell (CAC) have successfully demonstrated zero re-sistance up to approximately 22 GPa [45, 46]. Further-more, comparative magnetic measurements using SQUIDhave revealed that Tc is maximally enhanced under hy-drostatic pressure compared to uniaxial strain conditions[42], underscoring the critical role of hydrostatic pres-sure in cuprate superconductors. However, achievinghigher pressures in CAC presents significant technicalchallenges. Although DAC can generate higher pressures,SQUID magnetometry becomes difficult under high pres-sures where the sample space is restricted owing to in-sufficient magnetic signals. In this context, NV-basedmagnetometry offers a distinct advantage: it provideshigh sensitivity even for micrometer-sized samples anddoes not require electrical contacts. This enables the useof fluid-pressure-transmitting media within the DAC, en-suring a hydrostatic environment even at ultra-high pres-sures. Consequently, this technique paves the way for ex-tending the pressure-Tc phase diagram and exploring thepotential secondary superconducting dome in the unex-plored high-pressure regime [47].More broadly, wide-field quantum microscopy un-der high pressure has emerged as a contact-free, spa-tially resolved tool for probing quantum phenomena inmicrometer-scale samples, where conventional magne-tometry and transport measurements often face funda-mental limitations. Because many quantum materials,such as van der Waals layered compounds and nick-elate superconductors, are fragile and/or highly sensi-tive to non-hydrostatic stress, the ability to operate ina DAC without electrical contacts and with improvedhydrostatic pressure environments is particularly valu-able. This approach provides a practical route to extendpressure–temperature phase diagrams to higher pressuresunder more hydrostatic conditions and to explore emer-gent quantum phenomena. In the future, combining NV-based magnetometry with fluid pressure-transmittingmedia and complementary in-situ diagnostics (e.g., stressmapping and low-temperature pressure calibration) willfurther strengthen the quantitative interpretation andenable systematic studies across a broad range of quan-tum materials.In conclusion, we demonstrated wide-field quantummicroscopy using the NV center of a Bi-2223 single crys-tal under high pressure. By directly imaging the localdiamagnetic response associated with the Meissner effect,we observed a pronounced dependence on the pressure-transmitting medium: a clear superconductivity-relateddiamagnetic signal persisted up to 23 GPa in KBr near70 K, whereas it was suppressed above 11 GPa and 70K in cBN. These results underscore the critical role ofhydrostatic pressure in establishing reliable pressure-Tcrelationships in Bi-based cuprate superconductors.DATA AVAILABILITYThe data that support the findings of this study areavailable from the corresponding author upon reasonablerequest.ACKNOWLEDGMENTSThis work was supported by JSPS KAKENHI Grantnumbers JP23K26528, JP23KK0267, JP24KJ1035,JP25K01508. This work was also supported by JSTASPIRE Grant number JPMJAP24C1. M.O. receives5funding from JSPS Grant-in-Aid for JSPS Fellows Grant number JP24KJ1035.[1] K. Shimizu, K. Amaya, and N. Suzuki, J. Phys. Soc.Jpn. 74, 1345 (2005).[2] S. Yamanaka, Dalton Trans. 39, 1901 (2010).[3] H.-K. Mao, X.-J. Chen, Y. Ding, B. Li, and L. Wang,Rev. Mod. Phys. 90, 015007 (2018).[4] H. Sun, M. Huo, X. Hu, J. Li, Z. Liu, Y. Han, L. Tang,Z. Mao, P. Yang, B. Wang, J. Cheng, D.-X. Yao, G.-M.Zhang, and M. Wang, Nature 621, 493 (2023).[5] H. Sakakibara, M. Ochi, H. Nagata, Y. Ueki, H. Saku-rai, R. Matsumoto, K. 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