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MSc, Eng

  LABORATORY OF SPECTRAL CHEMICAL ANALYSIS (L-6)

Scope of accreditation of research laboratory No AB 120
issued by Polish Centre for Accreditation Issue No. 12 of 7 July 2015.

 

Head of the laboratory

The experts

Prof. Wojciech Maziarz, PhD, D.Sc.
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Honorata Kazimierczak, PhD
Anna Wójcik, MSc, Eng


Address:

Institute of Metallurgy and Materials Science Polish Academy of Sciences

ul. Reymont 25, 30-059 Krakow

phone: (48) 12 295 28 98, fax: (48) 12 295 28 04

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The procedures within the scope of accreditation:

Quantitative and qualitative analysis of chemical composition in areas 4 mm in diameter and at depth up to 150 µm using the method of emission spectroscopy (P/19/IB-15 edition 4, modified at 17.01.2012)

Apparatus: Glow Discharge Spectrometer JY 10 000 RF

 

 


Description of the method:
The Glow Discharge Spectrometer JY 10 000 RF is basically used for global quantitative and qualitative chemical analysis of conductive and non-conductive materials. It is also possible to carry out depth profiling and to determine elemental concentration as a function of distance from the surface of metals, semiconductors and ceramics.
The operating scheme of Glow Discharge source is presented in Fig. 1. There are two electrodes in the discharge chamber. A tubular, ground copper anode (4 mm in diameter) faces the sample, which acts as the cathode, maintained at RF potential of 13.56 MHz. The lamp is filled with argon at low pressure. Accelerated ions of Ar assure uniform sputtering of the sample in front of the anode. Then, the atoms of the sample are excited, mainly by collisions with electrons. The resulting plasma produces a spectrum characteristic for the sample composition. This characteristic spectrum is separated on diffraction gratings and its intensities are analyzed in photomultipliers installed on the Roland circle (Fig. 2). The intensities of the characteristic spectrum of particular elements are stored on hard disc and can be compared with the intensity of standards.

 



Fig.1. Diagram of RF-lamp operation

One of the important functions of the apparatus is to provide the possibility of performing profile analysis. This method is used to investigate changes of chemical concentration within surface layers (down to over 150 mm) with typical depth resolution of 5 to 10 nm. It is of particular importance for the investigation of layers, surfaces exposed to wearing, functional gradient materials.



Fig. 2. Optical scheme of spectrometer


Present capabilities of the JY 10000 RF spectrometer

1. Bulk analysis
Quantitative analysis of the chemical composition of homogeneous bulk materials can be performed for 35 elements, accessible in the present configuration of the instrument (Ag, Al, As, B, Bi, C, Ca, Cd, Ce, Co, Cr, Cu, Fe, In, Li, Mg, Mn, Mo, N, Nb, Nd, Ni, O, P, Pn, S, Si, Sb, Sn, Ti, V, W, Y, Zn, Zr). Chemical composition data are obtained from the 4 mm wide area on the specimen surface (penetration depth: up to 150 mm). The detection of elements depends on their amount in particular materials, ranging from 0.01 up to over a dozen ppm. The following materials can be analyzed:

  • Aluminum base alloys
  • High strength aluminum base alloys
  • Zn-Al alloys,
  • Carbon steels
  • Alloyed steels
  • Stainless steels
  • Tool steel

2. Depth profiling
The instrument is capable of performing chemical analysis at the surface or at the depth of over 150 microns, with typical depth resolution of 5 to 10 nm. The analysis can be performed simultaneously for 35 elements set up on the polychromators, or additionally for one element set up on the monochromator.

The typical examples:



Depth profile of polyester layers on steel

 



Depth profile of many-layered arrangement on silicon




Sample preparation

A sample should be at least 25x25 mm for square shape or 25 mm in diameter for cylindrical samples. The thickness of samples conducting electrical current should not exceed 50 mm. A sample made of non-conductive materials should not be thicker than 5 mm.

The surface should be smooth and clean. While selecting the sample preparation method, the same rules should be followed as in the case of metallographic specimens.

Important requirement: the top and bottom surfaces of a sample should be parallel.

 


Persons interested in co-operation should contact:

The Head of the Laboratory L-6:

Wojciech Maziarz, PhD, Eng.

phone: +48 12 295 28 57

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