公开(公告)号：EP2626886B1

公开(公告)日：2017-04-05

申请号：EP13154508.9

申请日：2013-02-08

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Schampers, Ruud ,  Piet, Trompenaars

IPC分类号： H01J37/28 ,  G01N1/42

CPC分类号： H01J37/28 ,  G01N1/42 ,  H01J2237/006 ,  H01J2237/31745

公开(公告)号：EP2824445B1

公开(公告)日：2016-03-02

申请号：EP13180398.3

申请日：2013-08-14

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Kuipers, Laurens

IPC分类号： G01N21/65 ,  H01J37/22 ,  H01J37/28

CPC分类号： H01J37/261 ,  G01N21/65 ,  H01J37/226 ,  H01J37/28 ,  H01J2237/31745

摘要： A method of examining a sample using a combined charged-particle microscope (4) and Raman spectroscope (6) , whereby: - Said microscope irradiates a sample (S) with a beam of charged particles so as to image a region of the sample; - Said spectroscope employs a light spot of width D to radiatively stimulate and spectroscopically analyze a portion of the sample, which method comprises the following steps: - Using the charged-particle microscope to identify a feature of interest in said region; - Choosing said portion that is analyzed by the Raman spectroscope to comprise this feature, wherein: - Said feature has at least one lateral dimension smaller than D; - Prior to analysis of said feature using the Raman spectroscope, an in situ surface modification technique is used to cause positive discrimination of an expected Raman signal from said feature relative to an expected Raman signal from said portion other than said feature.

公开(公告)号：EP2824445A1

公开(公告)日：2015-01-14

申请号：EP13180398.3

申请日：2013-08-14

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Kuipers, Laurens

IPC分类号： G01N21/65 ,  H01J37/22 ,  H01J37/28

CPC分类号： H01J37/261 ,  G01N21/65 ,  H01J37/226 ,  H01J37/28 ,  H01J2237/31745

摘要： A method of examining a sample using a combined charged-particle microscope (4) and Raman spectroscope (6) , whereby:
- Said microscope irradiates a sample (S) with a beam of charged particles so as to image a region of the sample;
- Said spectroscope employs a light spot of width D to radiatively stimulate and spectroscopically analyze a portion of the sample,

which method comprises the following steps:
- Using the charged-particle microscope to identify a feature of interest in said region;
- Choosing said portion that is analyzed by the Raman spectroscope to comprise this feature,

wherein:
- Said feature has at least one lateral dimension smaller than D;
- Prior to analysis of said feature using the Raman spectroscope, an in situ surface modification technique is used to cause positive discrimination of an expected Raman signal from said feature relative to an expected Raman signal from said portion other than said feature.

摘要翻译： 使用组合的带电粒子显微镜（4）和拉曼光谱仪（6）检查样品的方法，其中： - 所述显微镜用带电粒子束照射样品（S），以对样品的区域进行成像; - 所述分光镜采用宽度为D的光斑来辐射刺激并光谱分析样品的一部分，该方法包括以下步骤： - 使用带电粒子显微镜鉴定所述区域中的感兴趣特征; - 选择由拉曼光谱仪分析的所述部分以构成该特征，其中： - 所述特征具有至少一个小于D的横向尺寸; - 在使用拉曼光谱仪分析所述特征之前，使用原位表面修饰技术来从所述特征相对于来自除所述特征之外的所述部分的预期拉曼信号引起来自所述特征的预期拉曼信号的正面鉴别。

公开(公告)号：EP2626886A2

公开(公告)日：2013-08-14

申请号：EP13154508.9

申请日：2013-02-08

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Schampers, Ruud ,  Piet, Trompenaars

IPC分类号： H01J37/28 ,  G01N1/42

CPC分类号： H01J37/28 ,  G01N1/42 ,  H01J2237/006 ,  H01J2237/31745

摘要： The invention relates to a method of forming a vitrified sample on a sample holder (112) for inspection in an electron microscope (100, 106). It is known to spray a solution on a grid and then immerse the grid in a cryogenic liquid, such as ethane or liquid nitrogen. The invention proposes to spray (via 118) small droplets of the liquid on a cryogenic surface (112), such as a grid or a sample holder in vacuum. The liquid forms vitrified sample material (200, 202) when hitting the surface due to the low temperature of the grid or sample holder.
A lamella may be excavated from the thus formed sample material, to be studied in a TEM, or the vitrified sample material may be directly observed in a SEM. In an embodiment the material may be sprayed on a cryogenic liquid, to be scooped from the liquid and placed on a grid.

公开(公告)号：EP1890137A1

公开(公告)日：2008-02-20

申请号：EP07114356.4

申请日：2007-08-15

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Roussel, Laurent ,  Busing, Wilhelmus

IPC分类号： G01N23/225

CPC分类号： G01N23/225 ,  H01J2237/31745

摘要： The invention relates to a method for obtaining images from slices of a specimen, the method comprising:
repeatedly obtaining an image of the surface layer of the specimen (1) and
removing the surface layer of the specimen, thereby bringing the next slice to the surface; characterized in that after at least one of the removals of a surface layer the specimen is exposed to a staining agent.
This method is especially suited for use in a particle-optical instrument equipped with both a scanning electron microscope column ( 20 ) and a focused ion beam column ( 10 ).
The specimen can e.g. be stained in situ by admitting a gas, such as OsO 4 (osmiumtetroxide), to the specimen. This method also makes it possible to perform differential staining by first making an image of the specimen exposed to a first staining agent, and subsequently making an image of the specimen when it is additionally stained by a second staining agent.

摘要翻译： 本发明涉及一种从样本切片获取图像的方法，所述方法包括：重复获得样本（1）的表面层的图像并去除样本的表面层，从而使下一切片到达表面 ; 其特征在于，在将表面层的至少一个清除部分暴露于染色剂之后。 该方法特别适用于装有扫描电子显微镜柱（20）和聚焦离子束柱（10）的粒子光学仪器。 样品可以例如 通过将诸如OsO 4（四氧化锇）的气体引入样品而被原位染色。 该方法还可以通过首先使样品暴露于第一染色剂的图像进行差异染色，并且随后在被第二染色剂另外染色时进行样品的图像。

公开(公告)号：EP2626886A3

公开(公告)日：2016-03-30

申请号：EP13154508.9

申请日：2013-02-08

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Schampers, Ruud ,  Piet, Trompenaars

IPC分类号： H01J37/28 ,  G01N1/42

CPC分类号： H01J37/28 ,  G01N1/42 ,  H01J2237/006 ,  H01J2237/31745

摘要： The invention relates to a method of forming a vitrified sample on a sample holder (112) for inspection in an electron microscope (100, 106). It is known to spray a solution on a grid and then immerse the grid in a cryogenic liquid, such as ethane or liquid nitrogen. The invention proposes to spray (via 118) small droplets of the liquid on a cryogenic surface (112), such as a grid or a sample holder in vacuum. The liquid forms vitrified sample material (200, 202) when hitting the surface due to the low temperature of the grid or sample holder.
A lamella may be excavated from the thus formed sample material, to be studied in a TEM, or the vitrified sample material may be directly observed in a SEM. In an embodiment the material may be sprayed on a cryogenic liquid, to be scooped from the liquid and placed on a grid.

公开(公告)号：EP2239628A1

公开(公告)日：2010-10-13

申请号：EP09157161.2

申请日：2009-04-02

申请人： FEI COMPANY

发明人： Faber, Pybe ,  Mulders, Johannes ,  De Jong, Alan ,  Van Vilsteren, Carmen

IPC分类号： G03F7/00 ,  G03F7/20 ,  B29C67/00

CPC分类号： H01J37/3178 ,  B29C64/135 ,  B29C2035/0827 ,  B29C2035/0833 ,  B29C2035/0844 ,  B29C2035/0877 ,  B29K2105/0076 ,  B29K2105/165 ,  B29L2023/005 ,  B29L2031/756 ,  B33Y10/00 ,  B82Y10/00 ,  B82Y40/00 ,  H01J37/3056 ,  H01J37/3174 ,  H01J2237/31732 ,  H01J2237/31749

摘要： The invention relates to a method for forming microscopic 3D structures. In the method according to the invention a substrate (105) is placed in a Scanning Electron Microscope (SEM). The SEM is equipped with a Gas injection System (GIS) (110) for directing a jet of precursor fluid to the substrate. The substrate is cooled below the freezing point of the precursor gas so that a frozen layer of the precursor gas can be applied to the substrate.
By now repeatedly applying a frozen layer of the precursor to the substrate and irradiate the frozen layer with an electron beam (102), a stack of frozen layers (130) is build, each layer showing an irradiated part (131) in which the precursor is converted to another material. After applying the last layer the temperature is raised so that the unprocessed precursor (132) can evaporate.
As a result 3D structures with overhanging features can be build.

摘要翻译： 本发明涉及一种用于形成微观3D结构的方法。 在根据本发明的方法中，将衬底（105）放置在扫描电子显微镜（SEM）中。 SEM配备有用于将前体流体射流引导到基底的气体注入系统（GIS）（110）。 将衬底冷却到低于前体气体的凝固点，使得前体气体的冷冻层可以施加到衬底上。 现在，将反应前体的冷冻层重复地施加到基板上并用电子束（102）照射冷冻层，构成一堆冷冻层（130），每个层显示辐射部分（131），其中前体 被转换为另一种材料。 在施加最后一层之后，升高温度，使得未处理的前体（132）可以蒸发。 因此，可以构建具有突出特征的3D结构。

公开(公告)号：EP2151847A1

公开(公告)日：2010-02-10

申请号：EP09167310.3

申请日：2009-08-06

申请人： FEI COMPANY

发明人： Botman, Aurelién ,  Freitag, Bert ,  Mulders, Johannes

IPC分类号： H01J37/317 ,  G01N1/28 ,  H01L21/31 ,  H01L21/3205

CPC分类号： G01N1/286 ,  G01N1/32 ,  H01J37/317 ,  H01J37/3178 ,  H01J2237/31745

摘要： The invention relates to a method for producing high-quality samples for e.g. TEM inspection. When thinning samples with e.g. a Focused Ion Beam apparatus (FIB), the sample often oxidizes when taken from the FIB due to the exposure to air. This results in low-quality samples, that may be unfit for further analysis. By forming a passivation layer, preferably a hydrogen passivation layer, on the sample in situ , that is: before taking the sample from the FIB, high quality samples are obtained.

摘要翻译： 生产高质量样品的方法本发明涉及一种生产高质量样品的方法， TEM检查。 当用例如 聚焦离子束装置（FIB）中，由于暴露于空气中，从FIB中取样时样品经常会氧化。 这导致低质量的样品，这可能不适合进一步分析。 通过在样品上原位形成钝化层，优选氢钝化层，即：在从FIB取样品之前，获得高质量样品。

公开(公告)号：EP2787523B1

公开(公告)日：2016-02-10

申请号：EP13162084.1

申请日：2013-04-03

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Geurts, Remco ,  Trompenaars, Piet ,  Bosch, Eric

IPC分类号： H01J37/02 ,  H01J37/305 ,  H01J37/317

CPC分类号： C23C14/48 ,  G01N1/286 ,  G01N1/32 ,  H01J37/02 ,  H01J37/3053 ,  H01J37/3171 ,  H01J37/3178 ,  H01J2237/004 ,  H01J2237/006 ,  H01J2237/31732 ,  H01J2237/3174 ,  H01J2237/31742 ,  H01J2237/31745 ,  H01J2237/31749

公开(公告)号：EP2787523A1

公开(公告)日：2014-10-08

申请号：EP13162084.1

申请日：2013-04-03

申请人： FEI COMPANY

发明人： Mulders, Johannes ,  Geurts, Remco ,  Trompenaars, Piet ,  Bosch, Eric

IPC分类号： H01J37/02 ,  H01J37/305 ,  H01J37/317

CPC分类号： C23C14/48 ,  G01N1/286 ,  G01N1/32 ,  H01J37/02 ,  H01J37/3053 ,  H01J37/3171 ,  H01J37/3178 ,  H01J2237/004 ,  H01J2237/006 ,  H01J2237/31732 ,  H01J2237/3174 ,  H01J2237/31742 ,  H01J2237/31745 ,  H01J2237/31749

摘要： Samples such as semiconductor samples to be imaged in a Transmission Electron Microscope must, after excavating said sample from a wafer, be thinned to form a lamella with a thickness of, for example, 20 nm. This is commonly done by sputtering with ions in a charged particle apparatus equipped with a Scanning Electron Microscope (SEM) column and Focused Ion Beam (FIB) column, further equipped with one or more Gas Injection Systems (GISses). Likewise metallic samples (comprising for example steel and silicon) are inspected in the material science.
A problem when milling a lamella to such a thickness is that a large part of the lamella becomes amorphous due to the bombardment with ions, and that ions get implanted in the sample.
The invention provides a solution to said problem by applying a voltage difference between the capillary of the GIS (201) and the sample (200), and directing a beam of ions or electrons (206) to the jet of gas (207). The beam thereby ionizes gas that is accelerated to the sample, where (when using a low voltage between sample and GIS) low energy milling occurs, and thus little sample thickness becomes amorphous.

摘要翻译： 在透射电子显微镜中成像的半导体样品等样品必须在从晶片上挖掘所述样品之后变薄以形成例如厚度为20nm的薄片。 这通常通过在装备有扫描电子显微镜（SEM）柱和聚焦离子束（FIB）柱的带电粒子设备中使用离子进行溅射来进行，所述柱进一步配备有一个或多个气体注入系统（GISses）。 同样在材料科学中检测金属样品（包括例如钢和硅）。 将薄层研磨至这样厚度时的问题在于，由于用离子轰击，大部分薄层变为无定形，并且离子被植入样品中。 本发明通过在GIS（201）的毛细管和样本（200）之间施加电压差并且将离子束或电子（206）引导到气体射流（207）来提供对所述问题的解决方案。 由此，电子束使被加速到样品的气体电离，其中（当在样品和GIS之间使用低电压时）发生低能量研磨，因此很少样品厚度变为非晶态。