Where To Draw Linecut In Gisaxs

Abstract

The majority morphology of the active layer of organic solar cells (OSCs) is known to be crucial to the device performance. The thin film device construction breaks the symmetry into the in-plane direction and out-of-plane direction with respect to the substrate, leading to an intrinsic anisotropy in the bulk morphology. However, the characterization of out-of-plane nanomorphology within the active layer remains a thousand challenge. Here, we utilized an Ten-ray scattering technique, Grazing-incident Transmission Small-angle X-ray Handful (GTSAXS), to uncover this new morphology dimension. This technique was implemented on the model systems based on fullerene derivative (P3HT:PC₇₁BM) and non-fullerene systems (PBDBT:ITIC, PM6:Y6), which demonstrated the successful extraction of the quantitative out-of-airplane acceptor domain size of OSC systems. The detected in-plane and out-of-plane domain sizes show strong correlations with the device performance, particularly in terms of exciton dissociation and charge transfer. With the help of GTSAXS, one could obtain a more fundamental perception nearly the three-dimensional nanomorphology and new angles for morphology control strategies towards highly efficient photovoltaic devices.

Introduction

Organic photovoltaics (OPVs) have gained much attending owing to their potential to offering low-toll, high-operation, and flexible devicesⁱ. To cope with the intrinsic strong exciton-binding free energy and short carrier diffusion length, OPVs usually utilize the bulk heterojunction (BHJ) device structure. Organic p-type (donor) and n-type (acceptor) semiconducting materials are mixed in the active layer to create rich donor/acceptor (D/A) interfaces for exciton dissociation. Concomitantly, circuitous majority morphology, in terms of molecular packing and phase separation, is generated, critically influencing exciton dissociation, charge transfer, and ship behaviors, and thus the overall device performance. The importance of majority morphology for the OPV device performance has been well recognized and intensively researched^{2,3,4,v,six,7} along with the progressing of the recording device ability conversion efficiency (PCE) over 18%⁸.

In general, the bulk morphology of an OPV active layer contains both the molecular level and nanoscale structural information. Grazing incidence wide-angle X-ray scattering (GIWAXS) is often implemented to investigate molecular-level structural data in terms of crystallinity, lattice constants, and crystalline domain orientations^nine. To learn the nanoscale structural information, grazing incidence small-scale-angle Ten-ray scattering (GISAXS)¹⁰ and resonant soft X-ray scattering (RSoXS)^eleven,12 are ofttimes employed. In 2022, Liao et al.¹³ carried out GISAXS measurements to study the consequence of additive ane,8-diiodooctane (DIO) on the phase separation of blend PCPDTBT:PC₇₁BM films and a fractal-like network model was used to fit the GISAXS horizontal profiles^xiii. Our group utilized the combination of GIWAXS and GISAXS to understand the morphology compatibility rule of a series of ternary BHJ systems^v,vi. In 2022, the miscibility and domain purity of PTB7:PC₇₁BM thin films with DIO was first revealed using RSoXS by Ade's group¹¹. The aforementioned group recently correlated the total scattering intensity with the Flory–Huggins interaction parameter (χ) of various OPV systems, which helped predict the attainable fill-factor^seven. However, the quantitative nanostructure exploited by GISAXS and RSoXS is and so far along the in-plane (IP) direction with respect to the thin film surface. Although GISAXS pattern contains the out-of-aeroplane (OOP) nanomorphology information, the scattering features are disturbed past the so-called Yoneda peak owing to reflection and refraction effects^fourteen. Annotation here, the IP and OOP directions are referring to the lateral and normal directions with respect to the sparse movie surface, respectively. More than complicated distorted-wave Born approximation (DWBA) needs to be accounted for information plumbing fixtures¹⁰, especially challenging when the feature of interest is in the vicinity of Yoneda height. On the other hand, in that location is a powerful technique–X-ray reflectivity (XRR), that tin can probe thin-film structural information along the surface normal directions¹⁵, such as moving-picture show thickness, interfacial roughness, and material distribution, however, it is still not straightforward to excerpt the OOP nanomorphology within the films by XRR.

Even so, the importance of the OOP nanomorphology has been noticed for years. In 2002, Huck et al.¹⁶ improved the quantum efficiency of the device by controlling the vertical stage separation in the organic BHJ agile layer of PFB:P8BT. Moreover, Campoy-Quiles et al.¹⁷ identified a generic stage separation order, whereby the polymer crystallized first and was followed past the diffusion of PC₆₁BM, forming lateral and vertical domains. In 2009, Yang et al.¹⁸ confirmed the existence of vertical phase separation using a P3HT:PC₇₁BM blend movie, in which P3HT appeared at the air-organic interface and PC₇₁BM appeared at the substrate-organic interface. They proposed to use an inverted device structure to solve this inhomogeneity upshot. Since then, diverse studies accept employed inverted structures for efficient charge collection. Given the critical event of OOP morphology, several studies have employed various methods to control information technology, for instance, by adding nanowires to the active layer¹⁹ or by using unlike interfaces²⁰. Thus, the control of OOP nanomorphology plays an important role in the optimization of the device performance, however, still at an empirical level, lack of viable quantitative label methods.

In this piece of work, to reveal the OOP nanomorphology of organic BHJ active layers, an 10-ray scattering technique called grazing-incident transmission small-angle X-ray scattering (GTSAXS) was employed²¹. This technique allows the detection of scattering under the surface horizon of the film which, different GISAXS, could exist modeled readily using modified simple Born approximation¹⁰. Nosotros first demonstrate the application of the GTSAXS method on a prototypical OPV arrangement, P3HT:PC₇₁BM^18,22, past comparing the results side-past-side with those of GISAXS. It is evident that GTSAXS could extract the IP structural data every bit GISAXS does, whereas meantime providing the OOP structural information. As a result, the statistical three-dimensional (3D) nanomorphology of the OPV BHJ sparse film was detected quantitatively past GTSAXS for the first time. Then, we generalize the applicability of this method to ii typical not-fullerene (NF) acceptor-based systems, PBDB-T:ITIC^23,24 and PM6:Y6²⁵ fabricated with different processing atmospheric condition. The correlation betwixt the 3D nanomorphology and device performance is discussed and established. It is suggested that the nanomorphology in the OOP direction should be i of the vital factors determining the device performance. This piece of work opens a new dimension of OPV BHJ morphology—the OOP nanomorphology, providing insights into the future authentic morphology command towards highly efficient devices. Furthermore, the proposed analysis scheme can be likewise readily migrated to written report the inner 3D nanostructure of other functional thin film systems beyond OPV, such equally polymer materials, nanofiltration membranes, quantum dot, and perovskite thin films.

Results

Direct comparison of GISAXS and GTSAXS

The experimental geometries of GTSAXS, GISAXS, and RSoXS are illustrated in Fig. 1a to highlight their cardinal differences in sparse-film structure probing. First, GTSAXS and GISAXS both utilize a grazing-incident axle^10,21, whereas RSoXS is typically performed in the normal incidence¹². Second, GISAXS collects the reflected outgoing beam, whereas RSoXS and GTSAXS both collect the transmitted outgoing axle. Specifically, RSoXS collects the point transmitted through the backside of the sparse picture show sample, but GTSAXS collects the signal exited from the front edge by aligning the cleaved front edge of the sparse film sample at the center of the goniometer stage (Supplementary Fig. 1, details in method department). To eliminate potential edge effects, 1 needs to carefully carve the sample at the middle region, in the same way as in cantankerous-exclusive scanning electron microscopy (SEM), to form a clean edge, as illustrated in Supplementary Fig. 2a, b. In principle, the orientation of the structure ordering probed is adamant by the direction of the scattering wave vector ${{{{{\bf{q}}}}}}={{{{{{\bf{k}}}}}}}_{f}-{{{{{{\bf{k}}}}}}}_{i}$. The q vector of GTSAXS and GISAXS have both parallel and vertical components with respect to the surface, thus capable of providing both the IP and OOP nanomorphology. In dissimilarity, RSoXS only offers IP nanomorphology since the q vector mainly falls in the IP direction. Therefore, in the following, we focus on comparing the scattering results of GTSAXS and GISAXS side-by-side.

**Fig. ane: Comparison of GTSAXS, GISAXS, and RSoXS.**

To demonstrate the capability of GTSAXS in extracting both the IP and OOP nanomorphology of the OPV active layer, we choose a model organization of P3HT:PC₇₁BM, whose IP nanomorphology was extensively studied by GISAXS and RSoXS previously^{xiv,26,27,28,29,thirty,31}. In principle, by impinging the grazing-incident low-cal at the front end edge of the sparse film sample, both GISAXS and GTSAXS signals could appear in the same two-dimensional (2D) scattering pattern, which is separated by the surface horizon²¹. Effigy 2a shows a 2D-scattering design of a P3HT:PC₇₁BM film measured with front border X-ray impinging at an incidence angle of 0.fifteen^o. The horizontal cyan dashed line at q _z ≈ 0.016 Å⁻¹ indicates the position of the surface horizon. The GISAXS signal appears higher up the surface horizon while the GTSAXS point appears below.

**Fig. 2: GISAXS and GTSAXS of fullerene-based BHJ.**

First, we performed the horizontal linecuts above and below the surface horizon to extract the GISAXS and GTSAXS intensity profiles respectively, both of which should offer the IP nanomorphology information of the P3HT:PC₇₁BM film, every bit shown in Fig. 2b. To enhance the overall intensity of the handful profiles, the GISAXS IP profile is oft obtained at the Yoneda peak position^ten, which is observed at the handful angle ${\alpha }_{f}={\alpha }_{i}+{\blastoff }_{{{{{{\rm{ct}}}}}}}$, where ${{{{{{\rm{\alpha }}}}}}}_{i}$ is the incident angle and ${{{{{{\rm{\alpha }}}}}}}_{{{{{{\rm{ct}}}}}}}$ is the critical angle of the sample. The critical angle of the P3HT:PC₇₁BM film is calculated to be 0.11° at 12 keV. In contrast, the GTSAXS IP profile is extracted at q _z = −0.008 Å^−one near the minimum achievable q _z, determined past the size of the beamstop. As manifested in Fig. 2b, GISAXS and GTSAXS IP profiles highly resemble each other, except for a relatively higher intensity of the GISAXS signal owing to the surface enhancement issue. Such a resemblance demonstrates that GTSAXS is comparably capable of revealing the IP nanomorphology as GISAXS does.

In contrast, the OOP intensity profiles in the GISAXS and GTSAXS regions are noticeably different. As illustrated in Fig. 2a, the vertical linecuts are performed at the minimum achievable q _r position (q _r = 0.006 Å⁻¹), which is also limited by the beamstop. The surface horizon separates the purlieus of GISAXS and GTSAXS OOP profiles. The GISAXS OOP profile exhibits a pronounced Yoneda peak at q _z ~ 0.03 Å⁻¹. Attributable to the strong intensity of Yoneda pinnacle, the scattering features from the sample in the q _z range between ~ 0.01 and ~ 0.06 Å^−ane are totally shadowed. Even the powerful DWBA tin barely draw meaningful structural data in that region. Remarkably, the GTSAXS OOP profile, apparently free of Yoneda peak, presents feature intensity variation versus q, a common scattering feature of nanoscale PCBM clusters³¹. The IP and OOP GTSAXS/GISAXS profiles for bare Si substrate are presented in Supplementary Fig 3, which show typical q-dependent intensity decay profiles of diffuse scattering, which is obviously different from those profiles of thin-film samples, further confirming that GTSAXS is mainly detecting the structural features from the thin films.

Extraction of quantitative 3D nanomorphology information

To ready a standard experimental protocol to extract quantitative 3D nanomorphology information, we first examine the incident angle dependence of the IP and OOP intensity profiles, as plotted in Fig. 3. The 2d-scattering patterns acquired at 0.fifteen°, 0.xxx°, 0.45°, and 0.60° are shown in Supplementary Fig. 4. The IP profiles of GISAXS are extracted by the horizontal linecuts at the Yoneda peak positions of each incident bending, whereas the IP profiles of GTSAXS are all performed at q _z = −0.008 Å^−ane. The OOP profiles of GISAXS and GTSAXS are obtained by the vertical linecuts at q _r = 0.006 Å⁻ⁱ. Figure 3a, c compare the IP profiles of GISAXS and GTSAXS measured at different incident angles. Obviously, the intensity of GISAXS IP profile is significantly weakened and gradually loses its characteristic variation feature when the incident angle is lifted away from the critical angle. In contrast, the IP profile in the GTSAXS regime exhibits clear structural-related intensity variations, regardless of the incident angle used.

**Fig. 3: Formalism of GTSAXS measurements.**

For the OOP profiles, both the GISAXS and GTSAXS prove an incident angle dependence mainly due to the upshot of reflection acquired past the grazing incidence geometry (so-chosen "geometric distortion")²¹. Figure 3b, d presents the OOP profiles of GISAXS and GTSAXS measured at dissimilar incident angles after the geometric distortion correction²¹. The GISAXS OOP profiles manifest the shift of Yoneda summit with the incident angle, as expected. In contrast, the GTSAXS OOP profiles gradually collapse together when the incident angle increases, indicating that the geometric baloney effect tin be ignored at high incident angles (Supplementary Fig. five). Therefore, it is suggested to perform GTSAXS measurements at a high incident bending, i.due east. 0.sixty^o, where both the IP and the OOP nanomorphology tin can exist extracted without considering the geometric distortion.

To decide the nanophase separation length calibration, simple Born approximation models are readily adjusted to fit the scattering intensity profiles. For the P3HT:PC₇₁BM system, the hard-sphere model is usually employed^fourteen,31. The intensity of the scattering tin can be expressed with the formula:

$$I\left({{{{{\bf{q}}}}}}\right)\propto \left\langle {P}_{s}\left({{{{{\bf{q}}}}}},R\correct)\correct\rangle {S}_{{{{{{\rm{hs}}}}}}}\left({{{{{\bf{q}}}}}},R\correct)$$

(1)

where $\left\langle {P}_{s}\left({{{{{\bf{q}}}}}},R\right)\right\rangle$ is the form gene of spherical particles with the mean radius R under the Schulz distribution^32,33,34, ${South}_{{{{{{\rm{hs}}}}}}}\left({{{{{\bf{q}}}}}},R\right)$ is the construction factor with the hard-sphere interparticle interaction calculated under the Percus–Yevick Approximation³⁵. Thus, the PC₇₁BM domain sizes (2R _g) in the IP direction estimated from the GISAXS and GTSAXS IP profiles are 22 nm and 21 nm (solid lines in Fig. 3a, c) respectively, similar to previously reported values^14,31. It further confirms the capability of GTSAXS in extracting the IP domain sizes as GISAXS does. Here, information technology is known that multiple scattering features can maybe be observed in GISAXS horizontal linecut contour at the Yoneda peak for P3HT: PCBM blend films, which represent to the multiple characteristic structures within the sparse film, such as the sizes of PCBM aggregates and distances between those aggregates. Information technology is worth noting that practically adamant characteristic sizes for nanostructure of P3HT:PCBM organisation is highly dependent on the specific processing conditions of thin films and can vary within a sure range^36,37,38.

Remarkably, the same model could fit well with the GTSAXS OOP profile, giving the PC₇₁BM domain size of 5 nm in the OOP management (Fig. 3d). Here, the excellent feasibility of the simple Born approximation scattering model to fit the OOP profiles of GTSAXS further indicates that the construction probed past GTSAXS should exist the vertical domain sizes of phase separation. The relatively smaller acceptor domain size in the OOP management compared with the domain size in the IP direction is probable attributable to the physical confinement imposed in the OOP direction by the thin film structure, which is also observed in NFA-based BHJ films studied below.

3D nanomorphology of NF BHJ systems

Having demonstrated the capability of GTSAXS in the prototypical fullerene-based organisation, we at present extend this method to NF systems and investigate the influence of OOP nanomorphology on the device performance. We cull a typical NF acceptor-based system, PBDB-T:ITIC^23,24 (Fig. 4a), and deliberately create a fix of diverse morphologies in the active layer past adding additives and thermal annealing. The additive we employ hither is DIO, which has been widely applied to optimize the morphology of OPV devices^39,40,41. It has been reported that DIO could change the relative solubility and solvent evaporation speed and mediate the degree of stage separation⁴⁰.

**Fig. 4: Three-dimensional nanomorphology of non-fullerene-based BHJ.**

Effigy 4b, c shows the IP and OOP-scattering profiles of PBDB-T:ITIC blend films, command, with DIO, with DIO, and thermal annealing, respectively. The corresponding 2nd-scattering patterns are shown in Supplementary Fig. 6. The line shape and handling-dependent variation of IP and OOP profiles are plainly distinct. All the IP profiles exhibit a consequent decay in the q region of 0.02–0.05 Å^−one, corresponding to averaged domain sizes of several tens of nm. In contrast, the OOP profiles of the films without or with DIO resemble each other by a handful shoulder in the q region of ~ 0.ane Å⁻¹, suggesting the existence of a much smaller averaged domain size of several nm. Moreover, thermal annealing imposes more than prominent changes to the OOP nanomorphology than to the IP nanomorphology. The scattering shoulder of annealed picture shifts to a much smaller q region (q ~ 0.03 Å⁻¹), corresponding to a substantial growth of averaged domain size in the OOP direction.

For NF-based system, a theoretical fit of the scattering contour with the fractal-like network model^6,13,42 as the structure factor in Eq. (1) is capable of estimating pure phase domain sizes, whereas the Debye-Anderson-Brumberger model⁴³ is often employed to model the handful from the amorphous intermixing and diffuse scattering. The fitted IP and OOP domain sizes are summarized in Table 1. Since the handful of pure PBDB-T film is much weaker than that of pure ITIC film (Supplementary Fig. 7), the fitted pure phase domain sizes are assigned to ITIC. For the pristine PBDB-T:ITIC thin picture, the ITIC domain size is found to exist 41 nm in the IP direction, similar to previously reported values of such organisation⁴¹. In contrast, the OOP domain size is fitted to be 4 nm, near an order of magnitude smaller than that in the IP direction. The addition of 0.5% DIO gives rise to an ITIC domain shrinking in both IP and OOP direction to 22 nm and 3 nm, respectively. Then, afterwards thermal annealing, the domain size in both directions expanded substantially, to 43 nm in the IP direction and 16 nm in the OOP direction. Figure 4d shows a schematic representation of the ITIC domain inside the active layer, depicted as ellipsoids distributed randomly. All the films present an anisotropic nanomorphology with meaning elongation in the IP directions, possibly related to the chemic construction and molecular packing motif of ITIC as well as the anisotropic sparse film structure.

Table i A summary of fitted domain sizes and device characteristics of PBDB-T:ITIC and PM6:Y6 systems.

Total size table

To understand the influence of 3D nanomorphology, particularly the newly obtained OOP domain sizes, on the photovoltaic device performance, solar cells fabricated with PBDB-T:ITIC blend films, control, with DIO, with DIO and thermal annealing, are fabricated. Device parameters are summarized in Tabular array i along with the extracted IP and OOP domain sizes for detailed comparison. The J–5 curves and external quantum efficiency (EQE) are presented in Fig. 5a and Supplementary Fig. 8, respectively. The open-circuit voltage (5 _OC) changes from 0.882 5 to 0.891 V past adding DIO, then to 0.838 V with further annealing. The corresponding Five _OC loss ($={East}_{g}-q{V}_{{OC}}$) is calculated to be 0.777 eV, 0.761 eV, and 0.812 eV, with the ring gap determined from the derivative EQE curve (Fig. 5b). Thus, it is suggested that the DIO & annealing device experiences the most astringent recombination, whereas the DIO device has the least. To determine the type of dominant recombination^44,45, the ideality gene (due north) is and then obtained from the slope of the log-linear plot of 5 _OC versus light intensity (Fig. 5c). It is institute that due north _{DIO&annealing} = 1.seventy >n _command = 1.56 >north _DIO = 1.19. This is consistent with the development of 3D nanomorphology. The DIO film has the smallest IP and OOP domain sizes. Consequently, the dominant recombination in the DIO device is bimolecular, owning to the most efficient exciton dissociation. In dissimilarity, the DIO&annealing device has the largest domain size in both IP and OOP directions. Especially, in the OOP management, the domain size is about five times of the control and DIO samples, which could suppress the exciton dissociation, cause severe monomolecular recombination.

The charge transfer backdrop of the films are further characterized past time-resolved photoluminescence (TRPL) measurement excited at 515 nm (Fig. 5d). The DIO&annealing sample shows the longest lifetime (0.42 ns), whereas the control sample and the DIO sample disuse faster with a lifetime of 0.24 ns. The shorter disuse time in the command and DIO samples is related to higher electron transfer efficiency from the donor to the acceptor, direct associated with the observed much smaller OOP domain sizes, which increment the D/A interfaces. Note hither, although the control and DIO samples have distinct IP domain sizes, it is not very sensitive to the decay fourth dimension. It is likely due to the reason that the OOP domain size is significantly smaller than the IP domain size, thus becomes the critical cistron here. Therefore, it is confirmed that the newly detected OOP domain size is strongly correlated with the device performance, particularly relevant with the exciton dissociation and accuse transfer process. Without the knowledge of OOP domain sizes, it becomes difficult to explicate the V _OC difference between the control and DIO&annealing devices of PBDB-T:ITIC arrangement, every bit they exhibit very similar IP domain sizes. Too, the college FF of DIO & annealing devices can exist attributed to the college crystallinity (Supplementary Fig. 9) and the larger OOP domain size formed connected electron ship pathways.

In order to further demonstrate the generality of the influence of the OOP domain size on the device operation, we also performed GTSAXS measurements on another benchmark system PM6:Y6²⁵ (Fig. 6a). The GTSAXS patterns and the corresponding IP and OOP intensity profiles are presented in Fig. 6b, d and Supplementary Fig. ten. The fitted IP and OOP domain sizes and device characteristics are summarized in Table i and Supplementary Fig. xi. The atomic strength microscopy (AFM) images are shown in Supplementary Fig. 12, presenting similar surface roughness of ~ane nm, consistent with the previous reports²⁵. The vertical linecuts at q _r = 0 Å^−ane below horizon present periodic oscillations, which is very similar to the previously reported results in GISAXS above horizon region⁴⁶. From the periodicity of the fringes (Supplementary Fig. 10a), we accept extracted the corresponding characteristic lengths of 79, 80, and 86 nm for the PM6:Y6 thin films, control, with CN, with CN&annealing, respectively. These should most likely originate from the correlation length of thin-film thickness, much larger than the vertical length scale extracted from GTSAXS, suggesting that GTSAXS measures inner domain sizes of stage separation along the surface normal management. As well, the vertical intensity profile does non change essentially in the minor q _r region, as indicated by the linecuts performed at q _r = 0.006 Å⁻¹ and q _r = 0.008 Å⁻¹, equally shown in Supplementary Fig. 10b, c. This means that the vertical domain size averaged over a big IP length tin can approximately present the overall averaged vertical domain sizes of the film.

**Fig. 6: GTSAXS of loftier-efficiency BHJ system.**

The fitted IP and OOP domain sizes of the pure phase are shown in Table one. The values are similar to the stage separation length scales (20 ~ thirty nm) indicated in the cross-sectional electron energy loss spectroscopy (EELS) maps of PM6:Y6 (CN&annealing) thin film (Supplementary Fig. 13a), in which the North-rich region refers to the acceptor Y6 stage, whereas the S-rich region refers to the donor enrichment phase. The cantankerous-sectional images testify that the domain-similar model should also be suitable to excerpt the quantitative OOP phase structural information for NFA systems, like to the previously reported PCBM based BHJ sparse films^47,48. In addition, the uniform handful length density distributions through the whole moving picture thickness extracted from XRR measurements (Supplementary Fig. fourteen) dominion out the possible handful contribution from enrichment or wetting layer on surface or interface. The domain size changes in response to the additive and thermal annealing are similar for both PBDB-T:ITIC and PM6:Y6 systems: the incorporation of the solvent condiment tends to slightly shrink the IP and OOP domain sizes while thermal annealing tends to enlarge them. This correlates with the changing trend of V _OC, which increases slightly first then decreases largely, similar to the trend observed in the PBDB-T:ITIC arrangement. Here, to further eliminate the concern of edge scattering, nosotros have measured the same PM6: Y6 sparse motion-picture show at diverse broken edges, shown in Supplementary Fig. 15. It is evident that both the IP- and OOP-scattering profiles of different edges are like, and the extracted domain sizes are consistent with each other in a statistical manner. GIWAXS patterns of PM6:Y6 films command, with CN, with CN&annealing (Supplementary Fig. 16) demonstrated that the molecular packing motifs are very similar, whereas the control film has relatively lower crystallinity. Therefore, although the brusque-circuit current (J _SC) and fill-factor (FF) increase betwixt control and CN added devices may be attributed to the crystallinity increase, the J _SC and FF increase between CN and CN&annealing devices, which has similar crystallinity, is more than probable due to the significant enlargement of vertical domain size, which provides more interconnected charge transport pathways for efficient charge collection. In addition, estimated by the Scherrer equation from the full-width at half-maximum of the—superlative position of the PM6:Y6 system (Supplementary Table 1), the size of nano-crystallites within the thin film is ~ two nm, much smaller than the length scale (15 ~ 30 nm) extracted from the OOP profile of GTSAXS. Thus, the scattering features on the OOP profile of GTSAXS should non represent the size of the nano-crystallites inside domains, but the whole boilerplate domain size. Information technology is worth noting that the attribute ratio of IP and OOP domain sizes are much larger than 1 for the PBDB-T:ITIC system and close to 1 for the PM6:Y6 system. This is probable attributable to the distinct chemic structure and in turn the packing motif of ITIC and Y6, which is worth further exploring in future work. Furthermore, the IP domain size of the PM6:Y6 system is more often than not smaller than that of PBDB-T:ITIC, whereas the OOP domain size of PM6:Y6 is larger than that of PBDB-T:ITIC, instead, which is in correspondence with the overall better FF of PM6:Y6, further confirming that the newly revealed OOP domain size of BHJ thin film is closely related to the charge send efficiency along the vertical direction. Thus, an additional avenue for time to come device optimization and new photovoltaic material evolution is allowed with the determination of OOP phase construction for agile layer thin flick by GTSAXS.

Give-and-take

In summary, the awarding of synchrotron-based GTSAXS in studying the 3D nanomorphology, peculiarly the OOP nanomorphology, of the thin moving-picture show agile layer of organic solar cells has been demonstrated for the first time. It signifies that GTSAXS could offer simultaneous and incident bending-insensitive detection of IP and OOP nanomorphology, while the conventional GISAXS could only provide IP nanomorphology due to the strong reflection and refraction furnishings. At a relatively higher incidence angle, the GTSAXS profiles can be fitted by simple Built-in approximation and quantitative domain sizes tin can be readily extracted. Nosotros showed that this technique is applicable to both fullerene systems and NF systems, while different structure models need to exist employed for the data analysis (details in Supplementary Information Tabular array ii).

From the device data, the OOP domain size is strongly correlated with the exciton dissociation and charge transfer process, and every bit a event, can account for the Five_OC loss. Nevertheless, one still needs to consider other morphological factors, such as crystallinity, crystalline orientation, domain purity and miscibility etc^{2,3,4,5,6,seven}, to obtain a comprehensive understanding of the morphology impact on the device operation.

Methods

X-ray scattering

GIWAXS and GISAXS measurements were carried out with a Xeuss ii.0 SAXS/WAXS laboratory beamline using a Cu X-ray source (8.05 keV, 1.54 Å) and a Pilatus3R 300 Yard detector. The incidence angle is 0.2^o. GTSAXS measurements were performed at beamline BL19U2 of the National Facility for Protein Science Shanghai (NFPS) at Shanghai Synchrotron Radiation Facility (SSRF). The wavelength, λ, of X-ray radiation was prepare as 1.02 Å for P3HT:PC₇₁BM samples, 0.918 Å for PBDB-T:ITIC samples, and 1.01 Å for PM6:Y6 samples, respectively. The beam size at sample stage, divergence, and sampling expanse of the grazing-incident 10-ray in this experiment were 400 × 60 μmⁱⁱ (W×H), 80 × 30 μrad (Westward×H), and ~ 1.15 mm². Scattered X-ray intensities were collected using a Pilatus 1 Yard detector (DECTRIS Ltd). The sample-to-detector distance was set such that the detecting range of momentum transfer [ q = 4πsinθ/λ, where 2θ is the scattering angle] of SAXS experiments was 0.006–0.47 Å⁻¹.

GTSAXS measurement

To set a thin-motion picture sample suitable for GTSAXS label, one has to cleave the sample from the center area to create a clean border (Supplementary Fig. 2) and place the front edge at the center of the goniometer phase to align with the rotational axis of the incidence angle (Supplementary Fig. one). The sampling region is illustrated in Supplementary Fig. 1b. The theoretical penetration depth of X-ray through silicon substrate versus incident bending at $\lambda =$ 1.014 Å is plotted in Supplementary Fig. 17. The estimated penetration depth is ~ 2.eight μm at an incident angle of 0.6°, which is much thicker than the sample film and thinner than the silicon substrate. Thus, most of the scattering signals should leave from the front edge. Like to the optical alignment for conventional GIWAXS/GISAXS measurements, we perform one meridian scan first, which will give a step-wise height profile of the sparse picture show sample, as illustrated in Supplementary Fig. 18a. And then nosotros align the beam to the median meridian position, followed by a rocking scan of the incident angle. Since the cleaved edge of the sample is at the eye of the goniometer stage, the incident angle profile is not symmetric with respect to 0 caste. The intensity decreases when the incident angle moves away from 0 caste on the negative side and remains constant on the positive side (Supplementary Fig. 18b). One can repeat these steps several times to increase the accuracy of the alignment. After the optical alignment, the sample stage is rotated to the desired incident angle for GTSAXS measurements, as shown in Supplementary Fig. 18c. The maximum exposure time for the measurement of the individual samples was set to be 40 s in this synchrotron-based GTSAXS measurement, which tin avoid the potential bug of beam damage and simultaneously ensure that enough statistical handful signals can be collected. Detailed information on model plumbing equipment is given in Supplementary Information (Supplementary Table 2).

GTSAXS sample fabrication

To fabricate P3HT:PC₇₁BM sparse films, P3HT, and PC₇₁BM were simultaneously dissolved in o-DCB to course a solution of concentration 50 mg/ml. The mass ratio of the 2 components is 1:1. The solution was heated to 55°C for an 60 minutes and stirred overnight. To fabricate thin-film samples for X-ray characterization, the solution was spin-coated onto a clean Si substrate. The samples were so annealed for 10 min. To fabricate PBDB-T: ITIC thin films, PBDB-T, and ITIC were dissolved in chlorobenzene. The solution was heated to 55°C for an hr and stirred overnight. For samples with DIO additive, earlier spin-coating, 0.5 vol% DIO was added and the solution was then stirred for 30 min. The sparse films were fabricated by spin-coating solutions on Si substrate. 1 of the samples was and then annealed at 160°C for 10 min. PM6:Y6 thin films were fabricated using solutions with a total concentration of 15.four mg/ml and D/A ratio of one:i.2, the spin-coating charge per unit was 3000 rpm. Various PM6:Y6 thin films were made under conditions of equally-cast, with 0.five vol% 1-chloronaphthalene, with 0.five vol% 1-chloronaphthalene, and thermal annealing at 90°C for ten min, respectively.

Information technology is worth noting that in the present work, we follow the convention to choose silicon wafer as the substrate for 10-ray scattering characterizations^49,fifty,51, because information technology will impose minimal groundwork scattering signals is compared with ITO substrates and real devices, as shown by the GISAXS linecuts in Supplementary Figs. 19–21. As shown in GIWAXS of thin films on Si substrates and in real devices (Supplementary Figs. 17–eighteen), in these two circumstances, both the IP lamellar peaks and OOP-stacking peaks are highly consistent with each other. Furthermore, the phase construction of sparse film on Si substrate is too very similar to that in a real device, as indicated in EELS maps of Supplementary Fig. 13. Thus, the crystalline construction and nanomorphology of NFA-based thin films were not obviously altered when using silicon substrates.

Device fabrication

The inverted structure was utilized for PBDB-T:ITIC blends as ITO/ZnO/PBDB-T:ITIC/MoO₃/Al. The ZnO layer was spin-coated then broiled at 200 °C in the air for 30 min. PBDB-T:ITIC solutions were prepared and spin-coated on the ZnO layer similarly to GTSAXS samples. After that, the MoO₃ layer (ca. 6 nm) was thermally evaporated as the hole transporting layer, and the Al (ca. 100 nm) was evaporated as the tiptop electrode.

The conventional construction was utilized for PM6:Y6 blends as ITO/PEDOT: PSS/PM6:Y6/PFN-Br/Ag. The PEDOT:PSS layer was spin-coated so broiled at 130 °C in the air for 20 min. PM6:Y6 solutions were prepared and spin-coated on the PEDOT:PSS layer similar to GTSAXS thin film samples. After that, the PFN-Br layer was spin-coated every bit the electron transporting layer and the Ag (ca. 100 nm) were thermally evaporated as the pinnacle electrode.

Device label

The solar jail cell performance was measured by a Keysight source meter unit nether an AM 1.five G (100 mW cm⁻ⁱⁱ) solar simulator using a solar simulator (SS-F5-3A, Enlitech, Taiwan, Cathay). External quantum efficiency data were taken by a solar‐cell spectral‐response measurement arrangement (QER, Enlitech, Taiwan, People's republic of china).

TRPL measurement

TRPL of blends was measured using a habitation-setup microfluorescence system. The excitation calorie-free (515 nm) was generated by femtosecond laser (Light Conversion Pharos, 1030 nm, <300 fs, 1 MHz). TRPL decay kinetics were collected using a TCSPC module (PicoHarp 300) and a SPAD detector (IDQ, id100).

Scanning electron microscopy

A cantankerous-sectional epitome of a thin-film sample on Si substrate was taken by high-resolution field emission scanning electron microscopy.

Diminutive strength microscopy

AFM measurements were obtained by using a Dimension Icon AFM (Bruker) in a taping mode.

X-ray reflectivity

The XRR measurements were conducted by a Rigaku Smartlab reflectometer with Cu Kα X-ray source (λ = 1.541 Å) at China Spallation Neutron Source.

Cantankerous-sectional sample fabrication

The cross-sectional sample was prepared by a DualBeam FIB-SEM organization (Thermo Scientific Scios 2), equipped with platinum (Pt) deposition cartridge and EasyLift nanomanipulator. To minimize the ion beam damage, the sample was protected by a ~ 100 nm carbon coating first past a Sharpie black marker. After that, a several micrometer thick platinum layer was deposited using the gallium ion beam. After crude milling past 30 kV ion axle, the ~ 2 μm thick plate was lifting out and attached on the edge of a copper finger, following thinning processes were using a 5 kV ion beam for minimizing the ion beam damage and the final lamella was <100 nm thick.

Manual electron microscopy (TEM) and scanning TEM (Stem)

TEM and STEM of the cantankerous-exclusive samples were performed using JEOL JEM-2100F TEM/Stem (Tokyo, Nippon) operated at 200 kV. EELS mapping was carried out nether 200 kV accelerating voltage with a 13 mrad convergence angle for the optimal probe condition. Energy dispersion of 0.seven eV per channel and 21 mrad drove angle were set up for EELS. Loftier-bending annular nighttime-field STEM images were acquired with an 89 mrad inner angle simultaneously. The N and S intensity maps were extracted from the EELS mapping by integrating across the free energy windows of 401–409 (K edge) and 162–173 (L_2,iii edge) eV, respectively.

Reporting summary

Further information on inquiry design is bachelor in the Nature Research Reporting Summary linked to this article.

Data availability

The relevant data are available from the authors upon reasonable asking.

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Acknowledgements

We thank the Inquiry Grants Quango (RGC) of Hong Kong (Full general Research Fund No. 14303519, Articulation Laboratory Funding Scheme Project no. JLFS/P-102/18, and NSFC/RGC Joint Enquiry Scheme Grant No. N_CUHK418/17), and CUHK direct grant (no. 4442384). Nosotros also thank the beam fourth dimension and technical supports provided past 19U2 beamline at SSRF, Shanghai. Y.Z. thanks RGC of Hong Kong (General Research Fund No. 15305020) and the Hong Kong Polytechnic Academy grant (No. ZVRP). 10.Z. thanks NSFC (No. 51761165023). H.Z. acknowledges the National Key Research and Development Program of China (2017YFA0207700). X.L. and X.W. acknowledge back up from Guangdong-Hong Kong-Macao Joint Laboratory for Neutron Handful Scientific discipline and Applied science (Grant no. 2022B121205003). The authors appreciate the helpful discussions with professor Peter Müller-Buschbaum and Xinyu Jiang.

Writer data

Writer notes

These authors contributed equally: Xinxin Xia, Tsz-Ki Lau.

Affiliations

Department of Physics, The Chinese Academy of Hong Kong, New Territories, Hong Kong, 999077, Mainland china

Xinxin Xia, Tsz-Ki Lau, Yuhao Li, Minchao Qin, Yiqun Xiao, Pok Fung Chan, Heng Liu, Luhang Xu, Guilong Cai & Xinhui Lu
Department of Applied Physics, Research Plant for Smart Free energy, The Hong Kong Polytechnic Academy, Hung Hom, Hong Kong, China

Xuyun Guo & Ye Zhu
Department of Electronic and Information Engineering, Research Institute for Smart Energy (Ascension), The Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong, China

Kuan Liu & Gang Li
Center for Chemistry of High-Functioning & Novel Materials, Department of Chemistry, Zhejiang University, Hangzhou, 310027, Zhejiang, Red china

Zeng Chen & Haiming Zhu
Spallation Neutron Source Scientific discipline Heart, Dongguan, 523803, China

Xiaozhi Zhan
Constitute of High Energy Physics, Chinese Academy of Sciences, Beijing, 100049, People's republic of china

Xiaozhi Zhan
National Facility for Protein Science in Shanghai, Zhangjiang Laboratory, Shanghai Advanced Enquiry Institute, Chinese Academy of Science, No.333, Haike Route, Shanghai, 202204, People's Republic of Communist china

Na Li
Beijing National Laboratory for Condensed Matter Physics and Institute of Physics, Chinese University of Sciences, Beijing, 100190, Prc

Tao Zhu
School of Materials Science and Engineering, Peking University, Beijing, 100871, People's republic of china

Xiaowei Zhan
Department of Physics and Eye for Neutron Scattering, City Academy of Hong Kong, Kowloon, Hong Kong, People's republic of china

Xun-Li Wang

Contributions

Ten.L. supervised the piece of work. Ten.X. and T.50. contributed as to this piece of work. 10.X., T.50. conducted the GTSAXS measurements with the support of Northward.L., X.Ten., and T.Fifty. conducted the GIWAXS/GISAXS and EQE measurements. X.X. performed the fabrication and characterization of the devices. X.Chiliad. performed the cross-sectional TEM measurements under the supervision of Y.Z. 1000.Q. helped with data analysis. Z.C. carried out the TRPL measurements under the supervision of H.Z. XZ.Z. performed XRR measurements under the supervision of T.Z. K.L. conducted the AFM measurements nether the supervision of G.50. P.C., L.X., H.L. and G.C. helped with the supplementary GTSAXS measurements. Y.Fifty. carried out the SEM measurements. Y.X. helped with the sample grooming for GTSAXS. Ten.Ten., T.L. and Ten.Fifty. prepared the manuscript, XW.Z., N.L., H.Z., X.Westward provided revisions. All authors discussed the results and commented on the manuscript.

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Correspondence to Xinhui Lu.

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Xia, X., Lau, TK., Guo, X. et al. Uncovering the out-of-plane nanomorphology of organic photovoltaic majority heterojunction past GTSAXS. Nat Commun 12, 6226 (2021). https://doi.org/ten.1038/s41467-021-26510-vi

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Received: 13 Apr 2022
Accepted: 27 September 2022
Published: 28 October 2022
DOI : https://doi.org/x.1038/s41467-021-26510-vi

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