公开(公告)号：EP2838109A1

公开(公告)日：2015-02-18

申请号：EP14180462.5

申请日：2014-08-11

Applicant: FEI Company

Inventor： Tiemeijer, Peter ,  Konings, Stan ,  Henstra, Alexander

IPC: H01J37/26

CPC classification number: H01J37/261 ,  H01J37/147 ,  H01J37/22 ,  H01J37/26 ,  H01J37/263 ,  H01J2237/006 ,  H01J2237/2605 ,  H01J2237/262

Abstract: An Environmental Transmission Electron Microscope suffers from gas-induced resolution deterioration. It is found that this deterioration was not a function of the current density on the sample, but of the total current of the beam of electrons. Inventors conclude that the deterioration is due to ionization of gas in the sample chamber of the ETEM, and propose to use an electric field in the sample chamber to remove the ionized gas, thereby diminishing the gas-induced resolution deterioration. The electric field need not be a strong field, and can be caused by, for example, biasing the sample 114 with respect to the sample chamber 138. A bias voltage of 100 V applied via voltage source 144 is sufficient for a marked improvement the gas-induced resolution deterioration. Polarization is not important. Alternatively an electric field perpendicular to the optical axis 104 can be used, for example by placing an electrically biased wire or gauze 154 off-axis in the sample chamber.

Abstract translation: 环境透射电子显微镜遭受气体引起的分辨率恶化。 发现这种劣化不是样品上电流密度的函数，而是电子束总电流的函数。 发明人得出结论：劣化是由于ETEM的样品室中的气体电离造成的，并且建议使用样品室中的电场来去除电离的气体，由此减少气体引起的分辨率劣化。 电场不需要是强场，并且可以由例如相对于样品室138偏置样品114引起。通过电压源144施加的100V偏压足以显着改善气体 导致分辨率恶化。 极化并不重要。 或者，可以使用垂直于光轴104的电场，例如通过在样品室中离轴地放置电偏置电线或纱布154。

公开(公告)号：EP2555221A1

公开(公告)日：2013-02-06

申请号：EP11176445.2

申请日：2011-08-03

Applicant: FEI COMPANY

Inventor： Konings, Stan ,  Kujawa, Stephan ,  Trompenaars, Piet

IPC: H01J37/26

CPC classification number: G01Q30/12 ,  B82Y35/00 ,  H01J37/20 ,  H01J37/26 ,  H01J2237/2001 ,  H01J2237/2002 ,  H01J2237/2003 ,  H01J2237/28

Abstract: The invention relates to a method of studying a sample in the active atmosphere in an Environmental Transmission Electron Microscope (ETEM). Such a study is used to study a reaction (chemical or physical) of a sample with a gas. Of special interest is the chemical reactions of a gas and a catalyst, as well as the physical change (phase change) of, for example, the growth of a whisker from the gas phase growing on a solid. Prior art studies involve introducing the sample on a side-entry sample holder in the sample chamber of an ETEM, heating the sample to a required temperature, wait for the sample to settle to a drift-free position and then expose the sample to a pressure of, for example, 10 mbar of heated, reactive gas. Because the temperature distribution of the sample holder is a function of the temperature and pressure of gas, the temperature distribution over the sample holder will slightly change when exposing the sample holder to the gas, as a result of which the sample will drift. To avoid, or at least minimize, the drift, the invention involves the exposure to inert gas at a desired temperature before exchanging the inert gas to the active gas. The invention is also of applicable to optical, X-ray or scanning probe microscopy.

Abstract translation: 本发明涉及在环境透射电子显微镜（ETEM）中在活性气氛中研究样品的方法。 这样的研究用于研究样品与气体的反应（化学或物理）。 特别感兴趣的是气体和催化剂的化学反应，以及例如生长在固体上的气相生长晶须的物理变化（相变）。 现有技术研究涉及将样品引入ETEM的样品室中的侧入样品架上，将样品加热至所需温度，等待样品沉降至无漂移位置，然后将样品暴露于压力 例如10毫巴的加热的反应气体。 因为样品架的温度分布是气体温度和压力的函数，所以当将样品架暴露于气体时，样品架上的温度分布会稍微改变，结果是样品会漂移。 为了避免或至少最小化漂移，本发明涉及在将惰性气体交换到活性气体之前在期望的温度下暴露于惰性气体。 本发明也适用于光学，X射线或扫描探针显微镜。

公开(公告)号：EP2838108A1

公开(公告)日：2015-02-18

申请号：EP13180022.9

申请日：2013-08-12

Applicant: FEI COMPANY

Inventor： Tiemeijer, Peter ,  Henstra, Alexander ,  Konings, Stan

IPC: H01J37/26

CPC classification number: H01J37/261 ,  H01J37/147 ,  H01J37/22 ,  H01J37/26 ,  H01J37/263 ,  H01J2237/006 ,  H01J2237/2605 ,  H01J2237/262

Abstract: An Environmental Transmission Electron Microscope suffers from gas-induced resolution deterioration. It is found that this deterioration was not a function of the current density on the sample, but of the total current of the beam of electrons. Inventors conclude that the deterioration is due to ionization of gas in the sample chamber of the ETEM, and propose to use an electric field in the sample chamber to remove the ionized gas, thereby diminishing the gas-induced resolution deterioration. The electric field need not be a strong field, and can be caused by, for example, biasing the sample 114 with respect to the sample chamber 138. A bias voltage of 100 V applied via voltage source 144 is sufficient for a marked improvement the gas-induced resolution deterioration. Polarization is not important. Alternatively an electric field perpendicular to the optical axis 104 can be used, for example by placing an electrically biased wire or gauze 154 off-axis in the sample chamber.

Abstract translation: 环境透射电子显微镜遭受气体分解降解。 发现这种劣化不是样品上的电流密度，而是电子束的总电流的函数。 发明人得出结论，劣化是由于ETEM的样品室中的气体的离子化，并且建议在样品室中使用电场来去除电离气体，从而减少气体诱导的分辨率劣化。 电场不需要是强场，并且可以由例如相对于样品室138偏置样品114引起。经由电压源144施加的100V的偏置电压足以显着改善气体 引起分辨率恶化。 极化并不重要。 或者，可以使用垂直于光轴104的电场，例如通过将偏置电线或纱布154离轴放置在样品室中。

公开(公告)号：EP2555221B1

公开(公告)日：2013-07-24

申请号：EP11176445.2

申请日：2011-08-03

Applicant: FEI COMPANY

Inventor： Konings, Stan ,  Kujawa, Stephan ,  Trompenaars, Piet

IPC: H01J37/20 ,  H01J37/26

CPC classification number: G01Q30/12 ,  B82Y35/00 ,  H01J37/20 ,  H01J37/26 ,  H01J2237/2001 ,  H01J2237/2002 ,  H01J2237/2003 ,  H01J2237/28

Abstract: The invention relates to a method of studying a sample in the active atmosphere in an Environmental Transmission Electron Microscope (ETEM). Such a study is used to study a reaction (chemical or physical) of a sample with a gas. Of special interest is the chemical reactions of a gas and a catalyst, as well as the physical change (phase change) of, for example, the growth of a whisker from the gas phase growing on a solid. Prior art studies involve introducing the sample on a side-entry sample holder in the sample chamber of an ETEM, heating the sample to a required temperature, wait for the sample to settle to a drift-free position and then expose the sample to a pressure of, for example, 10 mbar of heated, reactive gas. Because the temperature distribution of the sample holder is a function of the temperature and pressure of gas, the temperature distribution over the sample holder will slightly change when exposing the sample holder to the gas, as a result of which the sample will drift. To avoid, or at least minimize, the drift, the invention involves the exposure to inert gas at a desired temperature before exchanging the inert gas to the active gas. The invention is also of applicable to optical, X-ray or scanning probe microscopy.

Abstract translation: 本发明涉及在环境透射电子显微镜（ETEM）中研究活性气氛中的样品的方法。 这种研究用于研究样品与气体的反应（化学或物理）。 特别感兴趣的是气体和催化剂的化学反应，以及例如生长在固体上的气相的晶须的生长的物理变化（相变）。 现有技术的研究包括将样品引入ETEM的样品室中的侧入口样品架上，将样品加热至所需温度，等待样品沉降到无漂移位置，然后将样品暴露于压力 例如为10毫巴的加热的反应性气体。 由于样品保持器的温度分布是气体的温度和压力的函数，当将样品保持器暴露于气体时，样品架上的温度分布将略有变化，结果样品将漂移。 为了避免或至少最小化漂移，本发明涉及在将惰性气体交换到活性气体之前，在所需温度下暴露于惰性气体。 本发明也适用于光学，X射线或扫描探针显微镜。