Primary funding for the work was provided by the Electron Microscopy of Soft Matter Program from the Office of Science, Office of Basic Energy Sciences, Materials Sciences and Engineering Division of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231. The battery assembly portion of the project was supported by the BATT program from the Vehicle Technologies program, through the Office of Energy Efficiency and Renewable Energy under U.S. DOE Contract DE-AC02-05CH11231. Hard X-ray microtomography experiments were performed at the Advanced Light Source which is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231. Katherine J. Harry was supported by a National Science Foundation Graduate Research Fellowship.

1. 전해질 준비 <ol><li> 260kg / 몰 폴리 (스티렌) - - 블록 - 폴리 (에틸렌 옥사이드) 공중 합체 (SEO) 음이온 중합을 사용하여 240kg / 몰을 합성. <ol><li> &lt;5 ppm의 물과 산소 레벨이 제어되는 아르곤 글로브 박스에 모든 추가 샘플 준비를 수행하고 남아있다. </li><li> 건조 리튬 비스 (트리 플루오로 메탄) 술폰이 미드 (LiTFSI를) 염과 무수 N 메틸 -2- 피 롤리 돈 (NMP)의 중합체 0.3 g을 용해. 13.13의 질량비를 검색 엔진 최적화 SEO 대량 0.275의 비율 NMP에 LiTFSI를 소금을 사용합니다. 참고 : 고분자의이 양이 약 20 샘플을 만들 수있을만큼 큰 멤브레인을 얻을 것입니다. </li><li> 닥터 블레이드를 사용하여 15cm 이상 15cm 정도에 니켈 박의 사각형 조각으로 제조 단계 중합체 및 염 혼합물의 모든 캐스트. 60 ° CO / N에서의 결과 필름을 건조시킵니다. </li><li> 건조 후, 니켈 박으로부터 막을 박리 9에서 진공하에 더 건조 시키0 ° C. </li><li> 나중에 사용하기 위해 글로브 박스에서 기밀 박스 내에 니켈 박과 상점에서 얻어진 프리 스탠딩 필름을 포장. </li></ol></li></ol> 2. 리튬 - 리튬 대칭 셀 준비 <ol><li> 직경의 7/16이 둥근 금속 펀치가 99.9 % 순수, 배터리 수준의 리튬 금속 호일의 롤에서 두 개의 리튬 금속 전극을 잘라하는 데 사용합니다. </li><li> 고분자 전해질 막의 일부를 잘라 직경 금속 펀치에 1/2를 사용한다. 주 : 리튬 금속이 부드럽고 고분자 전해질보다 펀치 쉽다. </li><li> 두 개의 리튬 금속 전극 사이에 고분자 전해질 막을 사이에두고 상기 전극 상에 니켈의 탭을 누른다. </li><li> 진공은 폴리 프로필렌, 나일론 안감 알루미늄 기밀 파우치 샘플을 밀봉. 주 : 하나는 전체 배터리를 연구하기를 원하는 경우, 리튬 전극 중 하나는 양극으로 쉽게 교환된다. </li></ol> 3. 대칭 셀 시클<html> G <ol><li> 전기 자전거 장비를 사용하여 90 ° C와 사이클에서 개최 오븐에 진공 밀봉 된 샘플을 놓습니다. 전해질 막을 통해 적당한 이온 전도성을 달성하기 위하여 순환하는 동안 샘플을 가열한다. 안전을 위해, 샘플을 180 ° C에서의 리튬 금속의 융점에 접근하지 않는 것을 보장한다. </li><li> 4 시간 동안 샘플을 통해 0.175 mA / cm 2의 전류 밀도를 전달하고 나머지 45 분에 따른다. 이어서, 4 시간 동안 샘플을 통해 -0.175 mA / cm 2의 전류 밀도를 전달하고 나머지 45 분에 따른다. 원하는만큼 여러 번이 자전거 루틴을 반복합니다. </li><li> 전지가 단락 회로를 표시함으로써 실패 때문. 30 μm의 두께 SEO 전해질을 통과하고,도 1에 도시 된 것과 비교할이 전류 밀도에 대한 전압 응답을 관찰 셀 전압 응답이 0.00 V로 떨어질 때 사이클링 루틴을 중지 리튬 덴 드라이트의 성장. </li></ol>&#39;타이틀 &quot;&gt; 4. 싱크로 하드 X 선 Microtomography 영상 <ol><li> 대칭 셀을 순환 한 후, 글러브 박스로 다시 데려와 그 주머니에서 제거합니다. </li><li> 봉지 재료에 셀의 중앙부를 밀봉 및 싱크로트론 시설로 운​​송 글로브 박스에서 제거 cell.Vacuum의 중앙부를 잘라 1/8 인치 금속 펀치를 사용한다. 주 : 감소 된 직경을 갖는 샘플을 이미징함으로써, X 선 검출기의 시야 외부 물질의 양이 감소된다. 이것은 여분의 물질이 발생하는 노이즈를 감소시킴으로써 전체 이미지 품질을 향상시킨다. 또한, 높은 X 선 흡수 니켈 집 전체를 제거하여 맑은 X 선 영상을 획득하기 위해,이 특정 파우치 디자인 필요하다. </li><li> 일단 빔라인에서, 샘플 단계에 샘플을 부착하는 폴리이 미드 테이프를 사용합니다. 원한다면, 얼라인먼트 돕기 위해 샘플 위에 작은 금속 마커 테이프. 대략 SAMP의 중심에 금속을 배치 마커제작은 샘플을 한 번 정렬, 회전되는 주위에 위치를 표시합니다. </li><li> 시스템에 최적화 된 노출 시간으로 이미지 샘플을 20 keV로의 X 선을 사용한다. 스캔 시간 및 이미지 당 카운트의 수가 균형을 노출 시간을 최적화한다. 수집 된 이미지의 수에 의해 노출 시간을 곱하여 총 검사 시간을 추정한다. <ol><li> 여기에서, 5 내지 10 분의 주사 시간의 결과로, 300 밀리의 노출 시간을 사용한다. </li></ol></li><li> 모든 beamtime 시프트의 시작 부분에 광학 렌즈와 연관된 픽셀 크기를 측정한다. 참고 :도 2에 도시 된 이미지를 촬영하기 위해 사용 4X 렌즈를 들어, 픽셀 크기는 1.61 μm의 / 픽셀이었다. 높은 배율 렌즈 (10 배 및 20 배)도 사용할 수 있습니다. </li><li> 위치가 180도 회전을 통해으로보기의 검출기의 현장에서 유지되도록 검출 시스템에 대해 회전 스테이지에 샘플을 정렬. </li><li> 에 가까운 샘플의 위치를시료는 임의의 회전 각도 검출기에 충돌하지 않는 것을 보장하면서 가능한 한 검출기. 주 : 거리 증가 검출기 샘플로, 프레 넬 위상차가 재구성 된 이미지에서 더 두드러 질 것이다. 이 기능을 모호하게하고 가난한 해결 될 수 있습니다. 파우치 전지의 경우, 검출기의 거리에 샘플을 얻어 검출기로부터 3cm 정도이다. </li><li> 일단 0과 180 사이의 샘플 회전을 통해 수집 된 1,025 이미지로 구성된 검사를 수행 정렬됩니다. &quot;명 시야&quot;를 수집 시야에서 샘플을 이동시킴으로써 화상 (또한 &quot;플랫 필드&quot;또는 &quot;배경&quot;라고도 함). 또한, 빔이 꺼져있는 동안 이미지를 복용하여 &quot;어두운 필드&quot;이미지를 수집합니다. 불균일 한 조명, 신틸 레이터 응답, 및 CCD 카메라 응답에 대한 샘플 이미지를 정상화하려면 다음을 사용합니다. </li></ol> 5. 영상 재구성 <ol><li> Tomographically각 이미지는 다음의 절차를 사용하여 볼륨의 슬라이스를 나타내는 화상의 스택에 1,025 방사선의 세트를 재구성. <ol><li> 첫째, 방사선 이미지와 &quot;시야&quot;이미지 모두에서 &quot;어두운 필드&quot;이미지를 빼서 이미지를 정상화. 그 결과 &quot;시야&quot;이미지로 나눈 결과 방사선 이미지를 나눈다. </li><li> 다음에, 제조자의 프로토콜에 따라 정규화 된 방사선 화상에 대한 단층 촬영 재구성, 투영 각도의 일련 3D 이미지로 변환되는 과정을 수행한다. 주 : 재구성 소프트웨어는 일련의 이미지를 출력하는 누적 sample.When 통해 수평 슬라이스를 나타내는 각각의 재구성 된 이미지 세트는 샘플의 3 차원 X 선 흡수 맵을 형성한다. </li></ol></li><li> 샘플 내부의 모습을 볼 수있는 개별 조각 또는 3 차원의 샘플을 시각화.</li></ol> 6. 데이터 시각화 및 처리 <ol><li> 데이터 시각화 및 분석 할 수 상용 및 오픈 소스 이미지 처리 소프트웨어 패키지의 무리 중 하나를 사용합니다. (22), (23) </li><li> 원하는 소프트웨어를 재구성 된 이미지의 스택을 열면, XY, XZ 및 복원 데이터의 YZ 관점을 보여 orthoslices을 만들 수 있습니다. </li><li> 이러한 이미지를 통해 팬과 그림 2의 리튬 덴 드라이트 같은 관심의 기능을 검색합니다. </li><li> 다음의 3 차원에 대한 관심의 기능을 렌더링하기 위해 분할 (디지털 표시) 및 3D 렌더링 도구를 사용합니다. </li><li> 세그먼트 디지털 이미지, 레이블 필드를 만든 재료에 대응하는 샘플의 영역을 선택하도록 임계 화 도구를 사용. </li><li> 도 2b에 도시 된 것과 같은 화상을 재현하기 위해, 암 픽셀 리튬과 밝은 픽셀 전해질 라벨. 에 포함 된 리튬 레이블수지상 별도로 상하 전극으로부터 리튬. <ol><li> 오렌지에 수지상 리튬과 파란색 고분자 전해질을 렌더링합니다. 회색 상하 리튬 금속 전극을 렌더링 및 오렌지 수지상 리튬 공개 투명도 값을 조정한다. 많은 관점에서 구조를 보려면이 세 가지 차원의 재건을 돌립니다. </li></ol></li></ol>

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M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Resolution+of+the+Modulus+versus+Adhesion+Dilemma+in+Solid+Polymer+Electrolytes+for+Rechargeable+Lithium+Metal+Batteries.">Resolution of the Modulus versus Adhesion Dilemma in Solid Polymer Electrolytes for Rechargeable Lithium Metal Batteries.</a> J Electrochem Soc. 159, A222-A227 (2012).</li><li>Panday, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+Molecular+Weight+and+Salt+Concentration+on+Conductivity+of+Block+Copolymer+Electrolytes.">Effect of Molecular Weight and Salt Concentration on Conductivity of Block Copolymer Electrolytes.</a> Macromolecules. 42, 4632-4637 (2009).</li><li>Schneider, C. A., Rasband, W. S., Eliceiri, K. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NIH+Image+to+ImageJ:+25+years+of+image+analysis.">NIH Image to ImageJ: 25 years of image analysis.</a> Nat methods. 9, 671-675 (2012).</li><li>Henke, B. L., Gullikson, E. M., Davis, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=X-Ray+Interactions+-+Photoabsorption,+Scattering,+Transmission+and+Reflection+at+E=50-30,000+Ev,+Z=1-92+(Vol+54,+Pg+181,+1993).">X-Ray Interactions - Photoabsorption, Scattering, Transmission and Reflection at E=50-30,000 Ev, Z=1-92 (Vol 54, Pg 181, 1993).</a> Atom Data Nucl Data. 55, 349-349 (1993).</li></ol>

The authors have nothing to disclose.

X 선은 대기에의 노출없이 샘플의 용이 한 촬영이 가능 보호용 파우치 물질을 관통 할 수 있기 때문에 하드 X 선 microtomography 많은 전기 화학적 활성 물질 등 공기에 민감한 샘플에 특히 적합하다. 아마도 이것은 영상 법의 가장 중요한 특징은 관통 X 선은 사용자가이를 파괴하지 않고 시료의 내부를 볼 수있게한다는 것이다. 주사 전자 현미경과 전통적인 광학 현미경, 전극 수있는 경우에만 이미지?...

Researchers are actively investigating battery chemistries with theoretical energy densities over an order of magnitude larger than traditional lithium-ion batteries.1,2 These high-energy-density batteries will make electric vehicles more competitive with their gasoline-powered counterparts.3 However, these new chemistries have several failure modes that preclude their use in commercial technologies. For example, these battery chemistries require a lithium metal anode to achieve large enhancements in energy density; unfortunately, lithium metal is prone to dendrite growth as lithium ions are reduced at the anode surface during charging.4-9 Additionally, breakage of active particles in the cathode and poor adhesion within the battery can cause cell failure.10
Many modes of battery failure occur on the micrometer scale. However, most battery materials are air sensitive making sample preparation for analysis by electron microscopy and traditional optical microscopy difficult. Synchrotron hard X-ray microtomography allows one to visualize the interior of a battery without disassembly.11-14 Furthermore, the technique produces a three-dimensional (3D) reconstruction of the assembled cell making it easy to find locations of failure.15 Finding robust techniques that enable researchers to develop the scientific understanding required to accurately predict the lifetime of a battery is critical for the design of next generation battery technologies. The procedure discussed herein will specifically demonstrate how one can prepare and image model batteries to study the growth of lithium metal dendrites through solid polymer electrolyte membranes.
Computed tomography (CT) scanning is not a new technique and has been used frequently for failure analysis in industry. Synchrotron-based X-ray microtomography is advantageous because the high brightness and flux of the source allow collection of images with high resolution and good signal to noise in a much shorter amount of time.16 Additionally, one can take advantage of the X-ray energy resolution to image at energies around a chemical species&#8217; absorption edge, causing the components containing that chemical species to be identified.17 It was found that the synchrotron source provides sufficient flux to achieve good contrast between lithium metal and solid polymer electrolyte membranes enabling one to image lithium metal dendrites.15
The study discussed herein uses a high modulus, block copolymer electrolyte membrane.18 These high modulus membranes suppress lithium dendrite growth, lengthening the lifetime of batteries.19,20 However, dendrites still eventually puncture the membrane causing the battery to fail by short-circuit. It is important to understand the nature of dendrite formation and growth in these high modulus electrolyte membranes in order to design strategies to prevent their growth.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Anhydrous N-methyl-2-pyrrolidone&#160;</td>
			<td>MILLIPORE</td>
			<td>MX1396-7</td>
			<td></td>
		</tr>
		<tr>
			<td>Lithium bis(trifluoromethane)sulfonamide</td>
			<td>MILLIPORE</td>
			<td>8438730010</td>
			<td></td>
		</tr>
		<tr>
			<td>Lithium metal</td>
			<td>FMC Lithium</td>
			<td>None</td>
			<td>Lectro Max 100</td>
		</tr>
		<tr>
			<td>Pouch material</td>
			<td>MTI Corporation</td>
			<td>EQ-alf-400-7.5M</td>
			<td></td>
		</tr>
		<tr>
			<td>Nickel tabs</td>
			<td>MTI Corporation</td>
			<td>EQ-PLiB-NTA3</td>
			<td></td>
		</tr>
	</tbody>
</table>

failure analysis of batteries using synchrotron-based hard x-ray microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

상술 대칭 리튬 리튬 전지가 90 ℃로 순환되는 경우, 전압 응답은도 1에 도시 된 것과 같이 보인다. 결국, ​​리튬 덴 드라이트가 전해질을 통해 성장하고, 세포가 단락에 의해 실패 할 것이다. 이 경우도 2에 도시 한 단락에 의해 실패한 샘플에서 나타나는 것처럼,인가 전류 전압 응답은 0.00 V. 수상 돌기 아래로 떨어질 것이다. 비전해질 스패닝 수지상은 샘플에서 발견된?...

Watch this Scientific Journal Video about Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography at JoVE.com

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

싱크로 기반 하드 X 선 Microtomography를 사용하여 배터리의 실패 분석

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

failure-analysis-batteries-using-synchrotron-based-hard-x-ray

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

8.8K 조회수.  University of California Berkeley. Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

비디오: Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

건설과 리튬 이온 배터리의 동전 전지의 테스트

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

연구

공학

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

제자리 중성자 분말 회절에서 사용자 정의 - 만든 리튬 이온 배터리를 사용하여

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Reservoir Condition Pore-scale Imaging of Multiple Fluid Phases Using X-ray Microtomography

X-ray microtomography was used to image, at a resolution of 6.6 &#181;m, the pore-scale arrangement of residual carbon dioxide ganglia in the pore-space of a carbonate rock at pressures and temperatures representative of typical formations used for CO2 storage. Chemical equilibrium between the CO2, brine and rock phases was maintained using a high pressure high temperature reactor, replicating conditions far away from the injection site. Fluid flow was controlled using high pressure high temperature syringe pumps. To maintain representative in-situ conditions within the micro-CT scanner a carbon fiber high pressure micro-CT coreholder was used. Diffusive CO2 exchange across the confining sleeve from the pore-space of the rock to the confining fluid was prevented by surrounding the core with a triple wrap of aluminum foil. Reconstructed brine contrast was modeled using a polychromatic x-ray source, and brine composition was chosen to maximize the three phase contrast between the two fluids and the rock. Flexible flow lines were used to reduce forces on the sample during image acquisition, potentially causing unwanted sample motion, a major shortcoming in previous techniques. An internal thermocouple, placed directly adjacent to the rock core, coupled with an external flexible heating wrap and a PID controller was used to maintain a constant temperature within the flow cell. Substantial amounts of CO2 were trapped, with a residual saturation of 0.203 &#177; 0.013, and the sizes of larger volume ganglia obey power law distributions, consistent with percolation theory.

We present a methodology for the imaging of multiple fluid phases at reservoir conditions by the use of x-ray microtomography. We show some representative results of capillary trapping in a carbonate rock sample.

여러 유체 페이즈 저수지 조건 기공 크기의 이미징 X 레이 Microtomography 사용

X-ray microtomography was used to image, at a resolution of 6.6 &#181;m, the pore-scale arrangement of residual carbon dioxide ganglia in the pore-space ...

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction.
Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of &gt; 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm.
Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed.

The use of energy dispersive X-ray tomography in the scanning transmission electron microscope to characterize elemental distributions within single nanoparticles in three dimensions is described.

개별 나노 입자의 3D 원소 매핑에 대한 에너지 분산 X 선 단층 촬영

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial ...

Measurement of X-ray Beam Coherence along Multiple Directions Using 2-D Checkerboard Phase Grating

A procedure for a technique to measure the transverse coherence of synchrotron radiation X-ray sources using a single phase grating interferometer is reported. The measurements were demonstrated at the 1-BM bending magnet beamline of the Advanced Photon Source (APS) at Argonne National Laboratory (ANL). By using a 2-D checkerboard &#960;/2 phase-shift grating, transverse coherence lengths were obtained along the vertical and horizontal directions as well as along the 45&#176; and 135&#176; directions to the horizontal direction. Following the technical details specified in this paper, interferograms were measured at different positions downstream of the phase grating along the beam propagation direction. Visibility values of each interferogram were extracted from analyzing harmonic peaks in its Fourier Transformed image. Consequently, the coherence length along each direction can be extracted from the evolution of visibility as a function of the grating-to-detector distance. The simultaneous measurement of coherence lengths in four directions helped identify the elliptical shape of the coherence area of the Gaussian-shaped X-ray source. The reported technique for multiple-direction coherence characterization is important for selecting the appropriate sample size and orientation as well as for correcting the partial coherence effects in coherence scattering experiments. This technique can also be applied for assessing coherence preserving capabilities of X-ray optics.

The measurement protocol and data analysis procedure are given for obtaining transverse coherence of a synchrotron radiation X-ray source along four directions simultaneously using a single 2-D checkerboard phase grating. This simple technique can be applied for complete transverse coherence characterization of X-ray sources and X-ray optics.

2-D 바둑판 위상 격자를 사용하여 여러 길을 따라 X 선 빔 일관성의 측정

A procedure for a technique to measure the transverse coherence of synchrotron radiation X-ray sources using a single phase grating interferometer is ...

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data acquisition times with high spatial resolution. In the electronics industry there is serious interest in performing failure analysis on 3D microelectronic packages, many which contain multiple levels of high-density interconnections. Often in tomography there is a trade-off between image resolution and the volume of a sample that can be imaged. This inverse relationship limits the usefulness of conventional computed tomography (CT) systems since a microelectronic package is often large in cross sectional area 100-3,600 mm2, but has important features on the micron scale. The micro-tomography beamline at the Advanced Light Source (ALS), in Berkeley, CA USA, has a setup which is adaptable and can be tailored to a sample&#39;s properties, i.e., density, thickness, etc., with a maximum allowable cross-section of 36 x 36 mm. This setup also has the option of being either monochromatic in the energy range ~7-43 keV or operating with maximum flux in white light mode using a polychromatic beam. Presented here are details of the experimental steps taken to image an entire 16 x 16 mm system within a package, in order to obtain 3D images of the system with a spatial resolution of 8.7 &#181;m all within a scan time of less than 3 min. Also shown are results from packages scanned in different orientations and a sectioned package for higher resolution imaging. In contrast a conventional CT system would take hours to record data with potentially poorer resolution. Indeed, the ratio of field-of-view to throughput time is much higher when using the synchrotron radiation tomography setup. The description below of the experimental setup can be implemented and adapted for use with many other multi-materials.

For this study synchrotron radiation micro-tomography, a non-destructive three-dimensional imaging technique, is employed to investigate an entire microelectronic package with a cross-sectional area of 16 x 16 mm. Due to the synchrotron&#39;s high flux and brightness the sample was imaged in just 3 min&#160;with an 8.7 &#181;m spatial resolution.

멀티 스케일 3 차원 마이크로 전자 패키지를 조사하는 방사광 Microtomography 사용

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data ...

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

비 양성 자성 리튬 O의 전기 시험 프로토콜 및 특성<sub&gt; 2</sub&gt; 배터리

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve geologic seals and allow CO2 to escape. However, the dissolution processes at reservoir conditions are poorly understood. Thus, time-resolved experiments are needed to observe and predict the nature and rate of dissolution at the pore scale. Synchrotron fast tomography is a method of taking high-resolution time-resolved images of complex pore structures much more quickly than traditional &#181;-CT. The Diamond Lightsource Pink Beam was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 hours. The images were segmented and the porosity and permeability were measured using image analysis and network extraction. Porosity increased uniformly along the length of the sample; however, the rate of increase of both porosity and permeability slowed at later times.

Synchrotron fast tomography was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 h.

싱크로 빠른 단층 촬영을 사용하여 탄산염의 반응의 동적 기공 규모의 저수지 조건 이미징

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve ...

Applying X-ray Imaging Crystal Spectroscopy for Use as a High Temperature Plasma Diagnostic

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line intensity ratios. By using a Johann spectrometer viewing the plasma, it is possible to construct profiles of plasma parameters such as density, temperature, and velocity with good spatial and time resolution. However, benchmarking atomic code modeling of X-ray spectra obtained from well-diagnosed laboratory plasmas is important to justify use of such spectra to determine plasma parameters when other independent diagnostics are not available. This manuscript presents the operation of the High Resolution X-ray Crystal Imaging Spectrometer with Spatial Resolution (HIREXSR), a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma. In addition, this manuscript covers a laser blow-off system that can introduce such ions to the plasma with precise timing to allow for perturbative studies of transport in the plasma.

X-ray spectra provide a wealth of information on high temperature plasmas. This manuscript presents the operation of a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma.

하이 온도 플라즈마 진단으로 사용하기 위해 X 선 영상 크리스탈 분광학 적용

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

싱크로 기반 하드 X 선 Microtomography를 사용하여 배터리의 실패 분석

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