CN114354576A

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Info

Publication number: CN114354576A
Application number: CN202210004052.0A
Authority: CN
Inventors: 余兴; 王海舟; 李小佳; 孙丹丹; 朱一妃; 石慧; 侯艳霞; 沈学静
Original assignee: Ncs Testing Technology Co ltd
Current assignee: Ncs Testing Technology Co ltd
Priority date: 2022-01-05
Filing date: 2022-01-05
Publication date: 2022-04-15
Anticipated expiration: 2042-01-05
Also published as: CN114354576B

Abstract

The invention provides a small sample analysis method used in glow analysis, which comprises the following steps: s1, placing the surface to be analyzed of the small sample in the middle of the bottom of the sample inlaying machine, inlaying the small sample in conductive resin by a hot inlaying method, exposing the surface to be analyzed of the small sample outwards, and polishing the inlaid small sample to meet the requirements of glow analysis on the surface of the sample; s2, covering the conductive resin area around the polished small sample with micron-sized thick metal foil difficult to sputter high-purity metal; s3, placing the small sample processed in the step (S) into a glow analyzer for analysis, wherein when the small sample is placed, the center of the surface to be analyzed of the small sample is aligned with the center of the glow source anode cylinder, so that the small sample is in a glow analysis area; s4, setting corresponding glow discharge parameters, and analyzing according to the glow analysis program. The invention is used for glow discharge analysis of small samples with small area and thin sheet/film samples, and has the advantages of simple operation, low cost, rapidness, practicability and the like.

Description

Small sample analysis method for glow analysis

Technical Field

The invention relates to the technical field of material analysis and characterization, in particular to a small sample analysis method used in glow analysis.

Background

Glow discharge is a low pressure gas discharge that is used as an efficient source of atomization and excitation for elemental analysis of solid materials. The sample atoms are stripped layer by layer from the surface of the sample by cathode sputtering, and then enter glow discharge plasma to be excited and ionized, and a glow discharge sputtering pit can be formed on the surface of the sample. Glow analysis typically has both dc and rf power supplies, with dc requiring the sample to be either conductive or semi-conductive, and rf power allowing analysis of conductive, semi-conductive and non-conductive samples. Generally, the glow analysis is a block sample which has certain mechanical strength, the surface of the sample to be analyzed is flat and smooth, and the area of the surface to be analyzed of the sample needs to be large enough to cover at least an anode cylinder of a glow source or slightly larger than the anode cylinder, so as to ensure the stability of glow discharge and the analysis requirement.

The Chinese utility model patent 'a model is ELEMENT GD glow discharge mass spectrograph test sample platform for small-size sample' (authorization notice No.: CN 210923569U) discloses a model is ELEMENT GD glow discharge mass spectrograph test sample platform for small-size sample, including high-purity copper sample platform body, high-purity copper sample platform body on open flutedly, the recess in be equipped with soldering tin. The advantages are that: through seting up the recess at high-purity copper body, put into proper amount soldering tin in the recess, can make small-size sample fix on high-purity copper sample, soldering tin can not expose the lower surface of sample, soldering tin when having avoided the test is to the influence of sample. However, the sample table is specially used for ELEMENT GD glow discharge mass spectrometer testing small-size samples, is only suitable for samples with the diameter of 10mm-20mm, and does not have wide applicability.

The Chinese utility model patent "sheet clamp for glow discharge mass spectrometer" (authorization notice number: CN210403655U) discloses a sheet clamp for glow discharge mass spectrometer, which comprises a base, a chute, a sliding mechanism, an L-shaped rod, a connecting mechanism, a U-shaped plate, a clamping plate and a fixing mechanism. The clamp can freely stretch out and draw back inside and outside the mass spectrometer, so that an operator can conveniently limit and fix the thin sheet, and normal detection work is guaranteed. However, the slice clamp is used in a glow discharge mass spectrometer, is suitable for slice samples, and cannot normally detect samples with small surfaces or uneven surfaces.

At present, a special small sample clamp is needed for some small samples such as needle-shaped samples, and meanwhile, the situation of unstable signal drift exists in the analysis process; and some thin film samples have the defects of no certain mechanical strength, generally incapability of being directly analyzed and the like.

Disclosure of Invention

The invention aims to provide a small sample analysis method for glow analysis, which is used for conducting resin inlaying and grinding/polishing treatment on a small sample, and simultaneously covering an inlaid conducting resin area with a metal foil difficult to sputter, so as to realize glow discharge analysis on the small sample with a small area and a thin sheet/film small sample.

In order to achieve the purpose, the invention provides the following scheme:

a method for small sample analysis in glow analysis comprising the steps of:

s1, placing the surface to be analyzed of the small sample in the middle of the bottom of the sample inlaying machine, inlaying the small sample in conductive resin by a hot inlaying method, exposing the surface to be analyzed of the small sample outwards, and polishing the inlaid small sample to meet the requirements of glow analysis on the surface of the sample;

s2, covering the conductive resin area around the polished small sample with micron-sized thick metal foil difficult to sputter high-purity metal;

s3, placing the small sample processed in the step (S) into a glow analyzer for analysis, wherein when the small sample is placed, the center of the surface to be analyzed of the small sample is aligned with the center of the glow source anode cylinder, so that the small sample is in a glow analysis area;

s4, setting corresponding glow discharge parameters, and analyzing according to the glow analysis program.

Further, in step S2, the step of covering the micron-sized thick metal foil difficult to sputter in the conductive resin area around the polished small sample specifically includes:

when covering, the area of the conductive resin which can be sputtered by the glow source anode cylinder is not exposed, the covered high-purity metal foil is flat and smooth, and the covered high-purity metal foil which is difficult to sputter does not generate glow discharge sputtering. For a thin slice/film small sample with a large enough area, the anode cylinder sputtering area of the glow source can be covered, and high-purity metal foil covering on the conductive resin area can be omitted.

Further, the diameter or the side length of the small sample is smaller than the diameter of the anode cylinder of the glow source.

Further, the thickness of the difficult-to-sputter high-purity metal foil is several tens of μm.

Further, the high-purity metal foil is high-purity metal tantalum foil.

According to the specific embodiment provided by the invention, the invention discloses the following technical effects: the small sample analysis method for glow analysis provided by the invention realizes the fixation and glow analysis sputtering of the small sample by inlaying and grinding/polishing the conductive resin of the small sample, and covers the high-purity metal foil which is difficult to sputter in the conductive resin area sputtered by the glow analysis, thereby avoiding the unstable discharge influence caused by the sputtering of the conductive resin.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.

FIG. 1 is a schematic structural diagram of a small sample inlay and resin area overlay high purity metal foil front face of the present invention;

FIG. 2 is a schematic cross-sectional view of a small sample inlay and resin area overlay high purity metal foil in accordance with the present invention;

FIG. 3 is a diagram of a small sample inlay of the present invention with the resin areas not covered by high purity metal foil;

FIG. 4 is a diagram of a small sample inlay and resin area overlay high purity metal foil object of the present invention;

FIG. 5 is a diagram of a sample after glow analysis in which a small sample resin-embedded area is not covered with a high-purity metal foil;

FIG. 6 is a diagram of a small sample after being subjected to glow analysis with a high purity metal foil covering a resin-embedded area;

description of reference numerals: 1. a conductive resin; 2. a high-purity metal foil; 3. a small sample; 4. and (4) glow source anode cylinder.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.

As shown in fig. 1 and fig. 2, the method for analyzing a small sample in glow analysis provided by the present invention comprises the following steps:

s1, placing the surface to be analyzed of thesmall sample 3 in the middle of the bottom of the sample inlaying machine, inlaying the small sample in theconductive resin 1 by a hot inlaying method, exposing the surface to be analyzed of thesmall sample 3 outwards, and performing grinding and polishing treatment on the inlaid small sample to meet the requirement of glow analysis on the surface of the sample;

s2, covering theconductive resin 1 area around thesmall sample 3 after polishing treatment with micron-sizedthick metal foil 2 difficult to sputter;

s3, placing thesmall sample 3 processed in the step (S) into a glow analyzer for analysis, wherein when thesmall sample 3 is placed, the center of the surface to be analyzed of thesmall sample 3 is aligned with the center of the glowsource anode cylinder 4, so that thesmall sample 3 is in a glow analysis area;

In step S2, for theconductive resin region 1 around the polishedsmall sample 3, covering a micron-sizedthick metal foil 2 difficult to be sputtered with high purity, specifically including:

when covering, the area of theconductive resin 1 which can be sputtered by the glowsource anode cylinder 4 is not exposed, the covered high-purity metal foil 2 is flat and smooth, and the covered high-purity metal foil 2 which is difficult to sputter does not generate glow discharge sputtering.

For a thin slice/film small sample with a large enough area, the sputtering area of the glowsource anode cylinder 4 can be covered, and the high-purity metal foil 2 covering of theconductive resin 1 area can be omitted.

The small sample size of the invention is in the range of 3mm-20mm in diameter/side length, depending on the diameter of the anode cylinder of the glow analyzer. Wherein the small sample size cannot cover the glow source anode cartridge.

For small samples of the flakes/films, from a few hundred μm to a few mm in thickness, there is no mechanical strength and the glow analysis cannot be carried out directly.

In a specific example, a stainless steel sheet sample was analyzed using a small sample analysis method used in glow analysis, the sample size being 5mm x 3mm, and the glow source anode cylinder diameter being 8 mm. The specific operation steps are as follows:

(1) placing a stainless steel sheet sample at the middle position of the bottom of the sample inlaying machine, filling conductive resin powder, and inlaying and fixing the stainless steel sheet sample by a hot inlaying method;

(2) and (3) sequentially carrying out corresponding grinding/polishing treatment on the embedded small samples according to the requirements of glow analysis on the surfaces of the samples, so that the surfaces of the small samples on the analysis surface are flat and flush with the embedded conductive resin areas, as shown in figure 3.

(3) The conductive resin area on the surface of the inlaid sample after grinding/polishing treatment is carefully covered by adopting a high-purity metal tantalum foil with the thickness of about 60 mu m, and meanwhile, the area of the conductive resin which can be sputtered by the glow source anode cylinder is not exposed after the high-purity metal tantalum foil is covered, and the covered high-purity metal tantalum foil is flat and smooth, as shown in figure 4.

(4) Placing the small stainless steel sheet sample processed in the step into a glow analyzer for analysis, wherein when the sample is placed, the center of the analysis surface of the small sample is required to be aligned to the center of a glow source anode cylinder, so that the small sample is in a glow analysis area; setting corresponding glow discharge parameters, and analyzing according to a glow analysis program.

For example, fig. 5 is a diagram of a sample after glow analysis of a small sample inlaid resin area not covered with a high-purity metal foil, sputtering occurs in the inlaid resin area connected with the small sample, and for example, in fig. 5, sputtering occurs in the inlaid conductive resin area (upper part of the sample) and the shape of a sputtering pit is not good, which directly affects normal glow discharge analysis, affects stability of an analysis process, and discharge parameters are unstable and fluctuate greatly in the glow discharge process;

FIG. 6 is a diagram of a sample after glow analysis of a small sample resin-embedded area covered with a high-purity metal foil, the covered high-purity metal foil is not sputtered, the surface of the small sample is subjected to normal glow analysis, the analysis process is stable, and the result is good.

The small sample analysis method for glow analysis provided by the invention can solve the problems that the small sample cannot cover a glow source anode cylinder so that glow analysis is difficult to perform, and the embedded conductive resin is sputtered to influence normal glow analysis due to small sample area after embedding, and is suitable for glow discharge spectrum and glow discharge mass spectrometry analysis, and sample preparation for material microstructure characterization by adopting glow discharge sputtering.

The invention realizes the fixation and glow analysis sputtering of the small sample by inlaying and grinding/polishing the conductive resin of the small sample, and covers the high-purity metal foil which is difficult to sputter in the conductive resin area sputtered by the glow analysis, thereby avoiding the unstable discharge influence caused by the conductive resin sputtering.

The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.

Claims

1. A method for analyzing a small sample for use in glow analysis, comprising the steps of:

2. The method for analyzing a small sample in glow analysis according to claim 1, wherein said step S2 of covering the conductive resin area around the polished small sample with a micron-sized thick metal foil hard to sputter comprises:

when covering, the area of the conductive resin which can be sputtered by the glow source anode cylinder is not exposed, the covered high-purity metal foil is flat and smooth, and the covered high-purity metal foil which is difficult to sputter does not generate glow discharge sputtering.

3. A method for small sample analysis in glow analysis according to claim 1 wherein the diameter or side length of said small sample is less than the diameter of the glow source anode cylinder.

4. The method for small sample analysis in glow analysis according to claim 1, wherein said high purity metal foil has a thickness of several tens of μm.

5. The method for analyzing a small sample in glow analysis according to claim 1, wherein said high purity metal foil is a high purity metal tantalum foil.