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Title: Accessing crystal–crystal interaction forces with oriented nanocrystal atomic force microscopy probes

Abstract

Biominerals serve as crucial structures of living systems and play an important role for biochemical processes. Understanding their crystallization mechanisms is therefore central to many areas of biology, biogeoscience and biochemistry. Some biominerals, such as bone and dentin, are hierarchical nanocomposite structures constructed by sequentially added individual oriented nanocrystals. The driving forces that enable this oriented assembly are still poorly understood, with advances in understanding limited in part by the availability of techniques that can precisely measure the delicate interactions between nanocrystals, as a function of their separation distance and mutual orientation. Here we provide a novel and comprehensive protocol for i.) fabricating oriented single nanocrystal atomic force microscopy (AFM) probes using focus ion beam (FIB) milling - probes that are capable of accessing the nanoscale forces between oriented single-crystal faces, and ii.) performing oriented nanocrystal interaction force measurements using dynamic force spectroscopy (DFS) and environmental transmission electron microscopy (ETEM)-AFM techniquqes. These methods have recently led to seminal breakthroughs in force quantification for understanding oriented aggregation at the nanoscale. First, we detail two FIB milling based methods to fabricate AFM nanocrystal probes. One method requires careful pre-coating with a protective layer to avoid FIB damage to the face of interest,more » which is later chemically removed, and the other entails removal of the FIB damage layer with in situ polishing. We illustrate how to fabricate oriented nanocrystal force probes using commercial bulk crystals or nano/micro-crystals of calcite, zinc oxide, and rutile; the methods are fully transferrable to the apatites comprising bone minerals. The typical protocol for fabricating one AFM crystal probe takes 2-3 h. Finally, we describe how to measure interaction forces between nanocrystals in solution conditions of interest by performing AFM based DFS, or in the controlled environment of ETEM, using the resulting oriented nanocrystal probes. In addition, we illustrate how to quantify the direction-specific interaction forces for a given pair of interacting oriented nanocrystal faces, and how to relate this information generally to understanding crystallization by particle attachment.« less

Authors:
ORCiD logo; ; ; ; ; ; ; ;
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1476994
Report Number(s):
PNNL-SA-131668
Journal ID: ISSN 1754-2189
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Journal Name:
Nature Protocols
Additional Journal Information:
Journal Volume: 13; Journal Issue: 9; Journal ID: ISSN 1754-2189
Publisher:
Nature Publishing Group
Country of Publication:
United States
Language:
English

Citation Formats

Zhang, Xin, He, Yang, Liu, Jia, Bowden, Mark E., Kovarik, Libor, Mao, Scott X., Wang, Chongmin, De Yoreo, James J., and Rosso, Kevin M. Accessing crystal–crystal interaction forces with oriented nanocrystal atomic force microscopy probes. United States: N. p., 2018. Web. doi:10.1038/s41596-018-0027-4.
Zhang, Xin, He, Yang, Liu, Jia, Bowden, Mark E., Kovarik, Libor, Mao, Scott X., Wang, Chongmin, De Yoreo, James J., & Rosso, Kevin M. Accessing crystal–crystal interaction forces with oriented nanocrystal atomic force microscopy probes. United States. doi:10.1038/s41596-018-0027-4.
Zhang, Xin, He, Yang, Liu, Jia, Bowden, Mark E., Kovarik, Libor, Mao, Scott X., Wang, Chongmin, De Yoreo, James J., and Rosso, Kevin M. Sat . "Accessing crystal–crystal interaction forces with oriented nanocrystal atomic force microscopy probes". United States. doi:10.1038/s41596-018-0027-4.
@article{osti_1476994,
title = {Accessing crystal–crystal interaction forces with oriented nanocrystal atomic force microscopy probes},
author = {Zhang, Xin and He, Yang and Liu, Jia and Bowden, Mark E. and Kovarik, Libor and Mao, Scott X. and Wang, Chongmin and De Yoreo, James J. and Rosso, Kevin M.},
abstractNote = {Biominerals serve as crucial structures of living systems and play an important role for biochemical processes. Understanding their crystallization mechanisms is therefore central to many areas of biology, biogeoscience and biochemistry. Some biominerals, such as bone and dentin, are hierarchical nanocomposite structures constructed by sequentially added individual oriented nanocrystals. The driving forces that enable this oriented assembly are still poorly understood, with advances in understanding limited in part by the availability of techniques that can precisely measure the delicate interactions between nanocrystals, as a function of their separation distance and mutual orientation. Here we provide a novel and comprehensive protocol for i.) fabricating oriented single nanocrystal atomic force microscopy (AFM) probes using focus ion beam (FIB) milling - probes that are capable of accessing the nanoscale forces between oriented single-crystal faces, and ii.) performing oriented nanocrystal interaction force measurements using dynamic force spectroscopy (DFS) and environmental transmission electron microscopy (ETEM)-AFM techniquqes. These methods have recently led to seminal breakthroughs in force quantification for understanding oriented aggregation at the nanoscale. First, we detail two FIB milling based methods to fabricate AFM nanocrystal probes. One method requires careful pre-coating with a protective layer to avoid FIB damage to the face of interest, which is later chemically removed, and the other entails removal of the FIB damage layer with in situ polishing. We illustrate how to fabricate oriented nanocrystal force probes using commercial bulk crystals or nano/micro-crystals of calcite, zinc oxide, and rutile; the methods are fully transferrable to the apatites comprising bone minerals. The typical protocol for fabricating one AFM crystal probe takes 2-3 h. Finally, we describe how to measure interaction forces between nanocrystals in solution conditions of interest by performing AFM based DFS, or in the controlled environment of ETEM, using the resulting oriented nanocrystal probes. In addition, we illustrate how to quantify the direction-specific interaction forces for a given pair of interacting oriented nanocrystal faces, and how to relate this information generally to understanding crystallization by particle attachment.},
doi = {10.1038/s41596-018-0027-4},
journal = {Nature Protocols},
issn = {1754-2189},
number = 9,
volume = 13,
place = {United States},
year = {2018},
month = {9}
}

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