DOI: 10.1180/0026461036730119. Preparation of TEM samples by focused ion beam (FIB) techniques: applications to the study of clays and phyllosilicates in meteorites

Preparation of TEM samples by focused ion beam (FIB) techniques: applications to the study of clays and phyllosilicates in meteorites

10.1180/0026461036730119

Crossref journal-article

Mineralogical Society

Mineralogical Magazine (7149)

Abstract

AbstractTransmission electron microscope samples were prepared of ALH 78045 and ALH 88045, two clay-and phyllosilicate-bearing Antarctic meteorites, using argon ion milling and focused ion beam (FIB) techniques. ALH 78045 contains clay- and phyllosilicate-filled veins that have formed by terrestrial weathering of olivine, orthopyroxene and metal. Very narrow (∼10 nm) intragranular clay-filled veins could be observed in the TEM samples prepared by argon ion milling, whereas differential thinning and lack of precision in the location of the electron-transparent areas hindered the study of wider (5 — 15 μm) phyllosilicate-filled intergranular veins. Using the FIB instrument, electron-transparent slices were cut from specific parts of the wider veins and lifted out for TEM study. Results show that these veins are occluded by cronstedtite, a mixed-valence Fe-rich phyllosilicate. This discovery shows that silicates can be both dissolved and precipitated during terrestrial weathering within the Antarctic ice. ALH 88045 is one of a small number of known CM1 carbonaceous chondrites. This meteorite is largely composed of flattened ellipsoidal aggregates of serpentine-group phyllosilicates. To determine the mineralogy and texture of phyllosilicates within specific aggregates, TEM samples were prepared by trenching into the cut edge of a sample using the FIB instrument. Results show that Mg-rich aggregates are composed of lath-shaped serpentine crystals with a ∼0.73 nm basal spacing, which is typical of the products of low temperature aqueous alteration within asteroidal parent bodies. Results of this work demonstrate that the FIB has enormous potential in a number of areas of Earth and planetary science.

Bibliography

Lee, M. R., Bland, P. A., & Graham, G. (2003). Preparation of TEM samples by focused ion beam (FIB) techniques: applications to the study of clays and phyllosilicates in meteorites. Mineralogical Magazine, 67(3), 581â592.

Authors 3

M. R. Lee (first)
P. A. Bland (additional)
G. Graham (additional)

References 25 Referenced 89

{'key': 'S0026461X00008033_ref8', 'first-page': '162', 'article-title': 'Electron microscopy sample preparation for the biological and physical sciences using focused ion beams.', 'volume': '4', 'author': 'Giannuzzi', 'year': '1999', 'journal-title': 'Journal of Process Analytical Chemistry,'} / Journal of Process Analytical Chemistry, / Electron microscopy sample preparation for the biological and physical sciences using focused ion beams. by Giannuzzi (1999)
10.1111/j.1945-5100.1990.tb01004.x
{'key': 'S0026461X00008033_ref10', 'first-page': '56', 'article-title': 'In situ sectioning and analysis of cosmic dust using Focused Ion Beam microscopy', 'volume': '37', 'author': 'Graham', 'year': '2002', 'journal-title': 'Meteoritics and Planetary Science,'} / Meteoritics and Planetary Science, / In situ sectioning and analysis of cosmic dust using Focused Ion Beam microscopy by Graham (2002)
10.1016/0016-7037(93)90298-B
10.1016/S0016-7037(98)00199-9
{'key': 'S0026461X00008033_ref18', 'article-title': 'Novel scheme for the preparation of transmission electron microscopy specimens with the focused ion beam.', 'volume': '11', 'author': 'Overwijk', 'year': '1993', 'journal-title': 'Journal of Vacuum Science Technology,'} / Journal of Vacuum Science Technology, / Novel scheme for the preparation of transmission electron microscopy specimens with the focused ion beam. by Overwijk (1993)
{'key': 'S0026461X00008033_ref21', 'first-page': 'A137', 'article-title': 'Transmission electron microscopy of a presolar corundum.', 'volume': '37', 'author': 'Stroud', 'year': '2002', 'journal-title': 'Meteoritics and Planetary Sciences Supplement,,'} / Meteoritics and Planetary Sciences Supplement,, / Transmission electron microscopy of a presolar corundum. by Stroud (2002)
10.1016/S0016-7037(97)00357-8
10.1180/minmag.1981.044.335.19
{'key': 'S0026461X00008033_ref7', 'first-page': '249', 'article-title': 'Advances in the FIB lift-out technique for TEM specimen preparation: HRTEM lattice imaging.', 'volume': '26', 'author': 'Giannuzzi', 'year': '1998', 'journal-title': 'Microstructural Science,'} / Microstructural Science, / Advances in the FIB lift-out technique for TEM specimen preparation: HRTEM lattice imaging. by Giannuzzi (1998)
10.1016/S0016-7037(03)00486-1
10.1016/0016-7037(91)90400-Y
{'key': 'S0026461X00008033_ref4', 'first-page': '5', 'article-title': 'Development of ion-beam milling as a major tool for electron microscopy.', 'volume': '36', 'author': 'Barber', 'year': '1999', 'journal-title': 'Microscopy and Analysis,'} / Microscopy and Analysis, / Development of ion-beam milling as a major tool for electron microscopy. by Barber (1999)
{'key': 'S0026461X00008033_ref12', 'first-page': '529', 'article-title': 'Random structures of layer minerals as illustrated by cronstedtite. Possible iron content of kaolin.', 'volume': '24', 'author': 'Hendricks', 'year': '1939', 'journal-title': 'American Mineralogist,'} / American Mineralogist, / Random structures of layer minerals as illustrated by cronstedtite. Possible iron content of kaolin. by Hendricks (1939)
10.1007/BF01089843
10.1016/0012-821X(89)90029-0
10.2138/am-2001-8-917
10.1126/science.242.4877.417
{'key': 'S0026461X00008033_ref20', 'first-page': '153', 'article-title': 'A precise new method of microsampling chondritic material for transmission electron microscope analysis: preliminary application to calcium- aluminium-rich inclusions and associated matrix material in the Vigarano CV3 meteorite', 'volume': '35', 'author': 'Stroud', 'year': '2000', 'journal-title': 'Meteoritics and Planetary Sciences Supplement,'} / Meteoritics and Planetary Sciences Supplement, / A precise new method of microsampling chondritic material for transmission electron microscope analysis: preliminary application to calcium- aluminium-rich inclusions and associated matrix material in the Vigarano CV3 meteorite by Stroud (2000)
10.1007/PL00020250
10.1016/0016-7037(81)90120-4
{'key': 'S0026461X00008033_ref19', 'first-page': '336', 'volume-title': 'Advanced techniques in TEM specimen preparation', 'author': 'Roberts', 'year': '2001'} / Advanced techniques in TEM specimen preparation by Roberts (2001)
10.1016/0016-7037(86)90076-1
{'key': 'S0026461X00008033_ref16', 'first-page': '1', 'volume-title': 'Chemistry of Clays and Clay Minerals', 'volume': '6', 'author': 'Newman', 'year': '1987'} / Chemistry of Clays and Clay Minerals by Newman (1987)
10.1111/j.1945-5100.2000.tb01523.x

Dates

Type	When
Created	22 years, 2 months ago (June 19, 2003, 1:29 p.m.)
Deposited	4 years, 6 months ago (Feb. 3, 2021, 9:37 p.m.)
Indexed	5 months ago (April 1, 2025, 11:41 a.m.)
Issued	22 years, 3 months ago (June 1, 2003)
Published	22 years, 3 months ago (June 1, 2003)
Published Online	7 years, 1 month ago (July 5, 2018)
Published Print	22 years, 3 months ago (June 1, 2003)

Funders 0

None

BibTeX

@article{Lee_2003, title={Preparation of TEM samples by focused ion beam (FIB) techniques: applications to the study of clays and phyllosilicates in meteorites}, volume={67}, ISSN={1471-8022}, url={http://dx.doi.org/10.1180/0026461036730119}, DOI={10.1180/0026461036730119}, number={3}, journal={Mineralogical Magazine}, publisher={Mineralogical Society}, author={Lee, M. R. and Bland, P. A. and Graham, G.}, year={2003}, month=jun, pages={581–592} }

JSON

{
  "indexed": {
    "date-parts": [
      [
        2025,
        4,
        1
      ]
    ],
    "date-time": "2025-04-01T15:41:56Z",
    "timestamp": 1743522116601
  },
  "reference-count": 25,
  "publisher": "Mineralogical Society",
  "issue": "3",
  "license": [
    {
      "start": {
        "date-parts": [
          [
            2018,
            7,
            5
          ]
        ],
        "date-time": "2018-07-05T00:00:00Z",
        "timestamp": 1530748800000
      },
      "content-version": "unspecified",
      "delay-in-days": 5513,
      "URL": "https://www.cambridge.org/core/terms"
    }
  ],
  "content-domain": {
    "domain": [],
    "crossmark-restriction": false
  },
  "published-print": {
    "date-parts": [
      [
        2003,
        6
      ]
    ]
  },
  "abstract": "<jats:title>Abstract</jats:title><jats:p>Transmission electron microscope samples were prepared of ALH 78045 and ALH 88045, two clay-and phyllosilicate-bearing Antarctic meteorites, using argon ion milling and focused ion beam (FIB) techniques. ALH 78045 contains clay- and phyllosilicate-filled veins that have formed by terrestrial weathering of olivine, orthopyroxene and metal. Very narrow (\u223c10 nm) intragranular clay-filled veins could be observed in the TEM samples prepared by argon ion milling, whereas differential thinning and lack of precision in the location of the electron-transparent areas hindered the study of wider (5 \u2014 15 \u03bcm) phyllosilicate-filled intergranular veins. Using the FIB instrument, electron-transparent slices were cut from specific parts of the wider veins and lifted out for TEM study. Results show that these veins are occluded by cronstedtite, a mixed-valence Fe-rich phyllosilicate. This discovery shows that silicates can be both dissolved and precipitated during terrestrial weathering within the Antarctic ice. ALH 88045 is one of a small number of known CM1 carbonaceous chondrites. This meteorite is largely composed of flattened ellipsoidal aggregates of serpentine-group phyllosilicates. To determine the mineralogy and texture of phyllosilicates within specific aggregates, TEM samples were prepared by trenching into the cut edge of a sample using the FIB instrument. Results show that Mg-rich aggregates are composed of lath-shaped serpentine crystals with a \u223c0.73 nm basal spacing, which is typical of the products of low temperature aqueous alteration within asteroidal parent bodies. Results of this work demonstrate that the FIB has enormous potential in a number of areas of Earth and planetary science.</jats:p>",
  "DOI": "10.1180/0026461036730119",
  "type": "journal-article",
  "created": {
    "date-parts": [
      [
        2003,
        6,
        19
      ]
    ],
    "date-time": "2003-06-19T17:29:15Z",
    "timestamp": 1056043755000
  },
  "page": "581-592",
  "source": "Crossref",
  "is-referenced-by-count": 89,
  "title": "Preparation of TEM samples by focused ion beam (FIB) techniques: applications to the study of clays and phyllosilicates in meteorites",
  "prefix": "10.1180",
  "volume": "67",
  "author": [
    {
      "given": "M. R.",
      "family": "Lee",
      "sequence": "first",
      "affiliation": []
    },
    {
      "given": "P. A.",
      "family": "Bland",
      "sequence": "additional",
      "affiliation": []
    },
    {
      "given": "G.",
      "family": "Graham",
      "sequence": "additional",
      "affiliation": []
    }
  ],
  "member": "7149",
  "published-online": {
    "date-parts": [
      [
        2018,
        7,
        5
      ]
    ]
  },
  "reference": [
    {
      "key": "S0026461X00008033_ref8",
      "first-page": "162",
      "article-title": "Electron microscopy sample preparation for the biological and physical sciences using focused ion beams.",
      "volume": "4",
      "author": "Giannuzzi",
      "year": "1999",
      "journal-title": "Journal of Process Analytical Chemistry,"
    },
    {
      "key": "S0026461X00008033_ref23",
      "doi-asserted-by": "publisher",
      "DOI": "10.1111/j.1945-5100.1990.tb01004.x"
    },
    {
      "key": "S0026461X00008033_ref10",
      "first-page": "56",
      "article-title": "In situ sectioning and analysis of cosmic dust using Focused Ion Beam microscopy",
      "volume": "37",
      "author": "Graham",
      "year": "2002",
      "journal-title": "Meteoritics and Planetary Science,"
    },
    {
      "key": "S0026461X00008033_ref24",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/0016-7037(93)90298-B"
    },
    {
      "key": "S0026461X00008033_ref5",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/S0016-7037(98)00199-9"
    },
    {
      "key": "S0026461X00008033_ref18",
      "article-title": "Novel scheme for the preparation of transmission electron microscopy specimens with the focused ion beam.",
      "volume": "11",
      "author": "Overwijk",
      "year": "1993",
      "journal-title": "Journal of Vacuum Science Technology,"
    },
    {
      "key": "S0026461X00008033_ref21",
      "first-page": "A137",
      "article-title": "Transmission electron microscopy of a presolar corundum.",
      "volume": "37",
      "author": "Stroud",
      "year": "2002",
      "journal-title": "Meteoritics and Planetary Sciences Supplement,,"
    },
    {
      "key": "S0026461X00008033_ref25",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/S0016-7037(97)00357-8"
    },
    {
      "key": "S0026461X00008033_ref2",
      "doi-asserted-by": "publisher",
      "DOI": "10.1180/minmag.1981.044.335.19"
    },
    {
      "key": "S0026461X00008033_ref7",
      "first-page": "249",
      "article-title": "Advances in the FIB lift-out technique for TEM specimen preparation: HRTEM lattice imaging.",
      "volume": "26",
      "author": "Giannuzzi",
      "year": "1998",
      "journal-title": "Microstructural Science,"
    },
    {
      "key": "S0026461X00008033_ref14",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/S0016-7037(03)00486-1"
    },
    {
      "key": "S0026461X00008033_ref22",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/0016-7037(91)90400-Y"
    },
    {
      "key": "S0026461X00008033_ref4",
      "first-page": "5",
      "article-title": "Development of ion-beam milling as a major tool for electron microscopy.",
      "volume": "36",
      "author": "Barber",
      "year": "1999",
      "journal-title": "Microscopy and Analysis,"
    },
    {
      "key": "S0026461X00008033_ref12",
      "first-page": "529",
      "article-title": "Random structures of layer minerals as illustrated by cronstedtite. Possible iron content of kaolin.",
      "volume": "24",
      "author": "Hendricks",
      "year": "1939",
      "journal-title": "American Mineralogist,"
    },
    {
      "key": "S0026461X00008033_ref15",
      "doi-asserted-by": "publisher",
      "DOI": "10.1007/BF01089843"
    },
    {
      "key": "S0026461X00008033_ref17",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/0012-821X(89)90029-0"
    },
    {
      "key": "S0026461X00008033_ref11",
      "doi-asserted-by": "publisher",
      "DOI": "10.2138/am-2001-8-917"
    },
    {
      "key": "S0026461X00008033_ref13",
      "doi-asserted-by": "publisher",
      "DOI": "10.1126/science.242.4877.417"
    },
    {
      "key": "S0026461X00008033_ref20",
      "first-page": "153",
      "article-title": "A precise new method of microsampling chondritic material for transmission electron microscope analysis: preliminary application to calcium- aluminium-rich inclusions and associated matrix material in the Vigarano CV3 meteorite",
      "volume": "35",
      "author": "Stroud",
      "year": "2000",
      "journal-title": "Meteoritics and Planetary Sciences Supplement,"
    },
    {
      "key": "S0026461X00008033_ref1",
      "doi-asserted-by": "publisher",
      "DOI": "10.1007/PL00020250"
    },
    {
      "key": "S0026461X00008033_ref3",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/0016-7037(81)90120-4"
    },
    {
      "key": "S0026461X00008033_ref19",
      "first-page": "336",
      "volume-title": "Advanced techniques in TEM specimen preparation",
      "author": "Roberts",
      "year": "2001"
    },
    {
      "key": "S0026461X00008033_ref9",
      "doi-asserted-by": "publisher",
      "DOI": "10.1016/0016-7037(86)90076-1"
    },
    {
      "key": "S0026461X00008033_ref16",
      "first-page": "1",
      "volume-title": "Chemistry of Clays and Clay Minerals",
      "volume": "6",
      "author": "Newman",
      "year": "1987"
    },
    {
      "key": "S0026461X00008033_ref6",
      "doi-asserted-by": "publisher",
      "DOI": "10.1111/j.1945-5100.2000.tb01523.x"
    }
  ],
  "container-title": "Mineralogical Magazine",
  "original-title": [],
  "language": "en",
  "link": [
    {
      "URL": "https://www.cambridge.org/core/services/aop-cambridge-core/content/view/S0026461X00008033",
      "content-type": "unspecified",
      "content-version": "vor",
      "intended-application": "similarity-checking"
    }
  ],
  "deposited": {
    "date-parts": [
      [
        2021,
        2,
        4
      ]
    ],
    "date-time": "2021-02-04T02:37:03Z",
    "timestamp": 1612406223000
  },
  "score": 1,
  "resource": {
    "primary": {
      "URL": "https://www.cambridge.org/core/product/identifier/S0026461X00008033/type/journal_article"
    },
    "secondary": [
      {
        "URL": "http://minmag.geoscienceworld.org/cgi/doi/10.1180/0026461036730119",
        "label": "geoscienceworld"
      }
    ]
  },
  "subtitle": [],
  "short-title": [],
  "issued": {
    "date-parts": [
      [
        2003,
        6
      ]
    ]
  },
  "references-count": 25,
  "journal-issue": {
    "issue": "3",
    "published-print": {
      "date-parts": [
        [
          2003,
          6
        ]
      ]
    }
  },
  "alternative-id": [
    "S0026461X00008033"
  ],
  "URL": "http://dx.doi.org/10.1180/0026461036730119",
  "relation": {},
  "ISSN": [
    "0026-461X",
    "1471-8022"
  ],
  "subject": [],
  "container-title-short": "Mineral. mag.",
  "published": {
    "date-parts": [
      [
        2003,
        6
      ]
    ]
  }
}