Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELs

Fixed targets are a popular form of sample-delivery system used in serial crystallography at synchrotron and X-ray free-electron laser sources. They offer a wide range of sample-preparation options and are generally easy to use. The supports are typically made from silicon, quartz or polymer. Of the...

Full description

Bibliographic Details
Main Authors: Melissa Carrillo, Thomas J. Mason, Agnieszka Karpik, Isabelle Martiel, Michal W. Kepa, Katherine E. McAuley, John H. Beale, Celestino Padeste
Format: Article
Language:English
Published: International Union of Crystallography 2023-11-01
Series:IUCrJ
Subjects:
Online Access:http://scripts.iucr.org/cgi-bin/paper?S2052252523007595
_version_ 1797641379500785664
author Melissa Carrillo
Thomas J. Mason
Agnieszka Karpik
Isabelle Martiel
Michal W. Kepa
Katherine E. McAuley
John H. Beale
Celestino Padeste
author_facet Melissa Carrillo
Thomas J. Mason
Agnieszka Karpik
Isabelle Martiel
Michal W. Kepa
Katherine E. McAuley
John H. Beale
Celestino Padeste
author_sort Melissa Carrillo
collection DOAJ
description Fixed targets are a popular form of sample-delivery system used in serial crystallography at synchrotron and X-ray free-electron laser sources. They offer a wide range of sample-preparation options and are generally easy to use. The supports are typically made from silicon, quartz or polymer. Of these, currently, only silicon offers the ability to perform an aperture-aligned data collection where crystals are loaded into cavities in precise locations and sequentially rastered through, in step with the X-ray pulses. The polymer-based fixed targets have lacked the precision fabrication to enable this data-collection strategy and have been limited to directed-raster scans with crystals randomly distributed across the polymer surface. Here, the fabrication and first results from a new polymer-based fixed target, the micro-structured polymer fixed targets (MISP chips), are presented. MISP chips, like those made from silicon, have a precise array of cavities and fiducial markers. They consist of a structured polymer membrane and a stabilization frame. Crystals can be loaded into the cavities and the excess crystallization solution removed through apertures at their base. The fiducial markers allow for a rapid calculation of the aperture locations. The chips have a low X-ray background and, since they are optically transparent, also allow for an a priori analysis of crystal locations. This location mapping could, ultimately, optimize hit rates towards 100%. A black version of the MISP chip was produced to reduce light contamination for optical-pump/X-ray probe experiments. A study of the loading properties of the chips reveals that these types of fixed targets are best optimized for crystals of the order of 25 µm, but quality data can be collected from crystals as small as 5 µm. With the development of these chips, it has been proved that polymer-based fixed targets can be made with the precision required for aperture-alignment-based data-collection strategies. Further work can now be directed towards more cost-effective mass fabrication to make their use more sustainable for serial crystallography facilities and users.
first_indexed 2024-03-11T13:44:48Z
format Article
id doaj.art-f31843acb84745068e23828005e2d59c
institution Directory Open Access Journal
issn 2052-2525
language English
last_indexed 2024-03-11T13:44:48Z
publishDate 2023-11-01
publisher International Union of Crystallography
record_format Article
series IUCrJ
spelling doaj.art-f31843acb84745068e23828005e2d59c2023-11-02T10:54:51ZengInternational Union of CrystallographyIUCrJ2052-25252023-11-0110667869310.1107/S2052252523007595zf5021Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELsMelissa Carrillo0Thomas J. Mason1Agnieszka Karpik2Isabelle Martiel3Michal W. Kepa4Katherine E. McAuley5John H. Beale6Celestino Padeste7Paul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandPaul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandPaul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandPaul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandPaul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandPaul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandPaul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandPaul Scherrer Institut, Forschungsstrasse 111, 5232 Villigen, SwitzerlandFixed targets are a popular form of sample-delivery system used in serial crystallography at synchrotron and X-ray free-electron laser sources. They offer a wide range of sample-preparation options and are generally easy to use. The supports are typically made from silicon, quartz or polymer. Of these, currently, only silicon offers the ability to perform an aperture-aligned data collection where crystals are loaded into cavities in precise locations and sequentially rastered through, in step with the X-ray pulses. The polymer-based fixed targets have lacked the precision fabrication to enable this data-collection strategy and have been limited to directed-raster scans with crystals randomly distributed across the polymer surface. Here, the fabrication and first results from a new polymer-based fixed target, the micro-structured polymer fixed targets (MISP chips), are presented. MISP chips, like those made from silicon, have a precise array of cavities and fiducial markers. They consist of a structured polymer membrane and a stabilization frame. Crystals can be loaded into the cavities and the excess crystallization solution removed through apertures at their base. The fiducial markers allow for a rapid calculation of the aperture locations. The chips have a low X-ray background and, since they are optically transparent, also allow for an a priori analysis of crystal locations. This location mapping could, ultimately, optimize hit rates towards 100%. A black version of the MISP chip was produced to reduce light contamination for optical-pump/X-ray probe experiments. A study of the loading properties of the chips reveals that these types of fixed targets are best optimized for crystals of the order of 25 µm, but quality data can be collected from crystals as small as 5 µm. With the development of these chips, it has been proved that polymer-based fixed targets can be made with the precision required for aperture-alignment-based data-collection strategies. Further work can now be directed towards more cost-effective mass fabrication to make their use more sustainable for serial crystallography facilities and users.http://scripts.iucr.org/cgi-bin/paper?S2052252523007595fixed targetsserial crystallographyfree-electron lasersmicro-structured polymer chipsaperturestime-resolved studiessample delivery
spellingShingle Melissa Carrillo
Thomas J. Mason
Agnieszka Karpik
Isabelle Martiel
Michal W. Kepa
Katherine E. McAuley
John H. Beale
Celestino Padeste
Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELs
IUCrJ
fixed targets
serial crystallography
free-electron lasers
micro-structured polymer chips
apertures
time-resolved studies
sample delivery
title Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELs
title_full Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELs
title_fullStr Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELs
title_full_unstemmed Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELs
title_short Micro-structured polymer fixed targets for serial crystallography at synchrotrons and XFELs
title_sort micro structured polymer fixed targets for serial crystallography at synchrotrons and xfels
topic fixed targets
serial crystallography
free-electron lasers
micro-structured polymer chips
apertures
time-resolved studies
sample delivery
url http://scripts.iucr.org/cgi-bin/paper?S2052252523007595
work_keys_str_mv AT melissacarrillo microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels
AT thomasjmason microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels
AT agnieszkakarpik microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels
AT isabellemartiel microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels
AT michalwkepa microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels
AT katherineemcauley microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels
AT johnhbeale microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels
AT celestinopadeste microstructuredpolymerfixedtargetsforserialcrystallographyatsynchrotronsandxfels