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MA-tek FTP

Liquid Sample Preparation Technology for TEM

2019/07/08

Products made by nano-technology have been widely used in our daily life. Recently, countries in US and Europe have started to make laws about labeling and investigation of products made by nano-technology. It is necessary to have complete physical and chemical properties analysis on end products.

 

Many academic institutes have put efforts in the development of liquid cell technology for new type electron microscope (EM). This technology can be used to monitor nano-particles, specifically their 1) species, 2) shape distribution, 3) diameter distribution, 4) aggregation and agglomeration of particles, and 5) particle concentration.

 

In the end, this technology can provide qualitative and quantitative analysis results about complete status of nano-particles based on ISO/TR13014, ISO 13322-1, and -2 regulations.

 

 

The figure is the sketch of liquid cell device (K-kit) for electron microscope (EM). The K-kit is convenient, simple, and comprehensive and can be adapted to all kinds of EMs. Sampling can be directly obtained from the liquid sample. Therefore, end-products can be investigated to fit the requirement of the labeling of nano-materials.

 

It can be applied to commodity/food/medicine/bio-specimen/cosmetic/chemistry mechanical (CMP) slurry containing nano-particles in industry research & development and quality control activities. Liquid sample can be filled into the limited space, and electron or ion beam can directly observe and investigate physical and chemical properties of living body nano-particles immersed in the liquid covered with thin film materials.

 

For such application, because of fixed volume and thickness of the samples, concentration of nano-particles and be directly converted from the density of 2D nano-particle distribution after calculations.

 


(a-1) Reality picture of observation of liquid sample by 200 KV TEM in a dark room

(a-2) TEM bright field image

(a-3) Dimension measurement of nano-particles

(b-1) Reality picture of in-situ observation by 30 KV DB-FIB

(b-2) STEM bright filed image obtained by DB-FIB

(b-3) STEM dark filed image

This figure exhibits the results of TEM and DB-FIB observation on non-dilute CMP slurry filled in a micro device. In this study, it clearly demonstrates that it’s doable to observe nano-particles in the carrier either by 200 KV EM or 30 KV DB-FIB.