阅读说明：本技术 利用扫描电镜和能谱仪对火法冶炼产品进行分析的方法 (Method for analyzing pyrometallurgical products by using scanning electron microscope and energy spectrometer ) 是由 张文平 于 2019-10-12 设计创作，主要内容包括：本发明是一种利用扫描电镜和能谱仪对火法冶炼产品进行分析的方法,步骤包括样品制备,检测条件设定,样品检测,采谱分相,建立冶金相态数据库,相态匹配与成分分析,检测结果处理。优点在于：能够快速、准确得到火法冶炼产品的相态组成及成分含量,适合处理火法铅冶炼产品,最终得出的数据准确、可靠。(The invention relates to a method for analyzing pyrometallurgical products by utilizing a scanning electron microscope and an energy spectrometer. Has the advantages that: the method can quickly and accurately obtain the phase composition and the component content of the pyrometallurgical product, is suitable for treating the pyrometallurgical lead smelting product, and finally obtains accurate and reliable data.)

1. A method for analyzing pyrometallurgical products by utilizing a scanning electron microscope and an energy spectrometer is characterized by comprising the following steps of:

1) and preparing a sample: solidifying, grinding and carbon spraying are carried out on the ore sample to obtain a sample grinding sheet;

2) and setting detection conditions: placing the sample abrasive disc prepared in the step 1) on an electron microscope sample table, and setting electron microscope parameters, wherein the background threshold value is set to be 40;

3) and detecting a sample: starting safety scanning, and detecting a sample by adopting a full-particle measurement mode;

4) and spectrum collection and phase splitting: dividing each phase according to the gray level difference in the detection result, determining the element content of each phase component by adopting an energy spectrum, and assigning component content value to each phase;

5) establishing a metallurgical phase state database: inputting various phase types into a matching library, collecting component spectral lines corresponding to each phase type, and establishing a sample phase database;

6) phase matching and component analysis: matching the detection samples by adopting a phase database, determining the content of phase components in the samples, and obtaining the content of various elements in the samples;

7) and processing a detection result: and obtaining data including the content, phase composition and relative content of various elements in the sample according to the generated detection result.

2. The method for analyzing pyrometallurgical products using scanning electron microscopy and energy spectroscopy as claimed in claim 1 wherein the particle size of the pyrometallurgical sample in step 1) is controlled to within 5 mm.

3. The method for analyzing pyrometallurgical products with a scanning electron microscope and an energy spectrometer as claimed in claim 1, wherein the setting of the parameters of the electron microscope in step 2) further comprises evacuating to vacuumThe hollowness is less than 4.0 multiplied by 10^-3Pa, the maximum output of the energy spectrum is adjusted to 200kcps, and the maximum energy range is 20 kV.

4. The method for analyzing pyrometallurgical products with a scanning electron microscope and an energy spectrometer as claimed in claim 1, characterized in that the number of groups of each phase collected in step 5) is not less than 10.

5. The method for analyzing pyrometallurgical products with a scanning electron microscope and an energy spectrometer as claimed in claim 1, characterized in that the match failure rate in step 6) is controlled to within 3%.

Technical Field

The invention belongs to the field of detection technology and experimental research application of pyrometallurgical products, and particularly relates to a method for researching components of pyrometallurgical lead smelting products by using a scanning electron microscope and an energy spectrometer.

Background

At present, the phase composition and component detection technology of the pyrometallurgical lead smelting product mostly stays at a qualitative detection level, the component detection is generally carried out by adopting an inductively coupled plasma atomic emission spectrometry, the fluctuation of a detection result is large, the detection of the phase composition cannot be effectively and quantitatively analyzed, the detection result is disconnected from experimental research or first-line production, the obtained results are mutually contradictory, and a reference basis cannot be provided for the experimental research and the optimized production.

Disclosure of Invention

The invention aims to solve the technical problem of providing a method for analyzing a pyrometallurgical product by using a scanning electron microscope and an energy spectrometer, solving the problem that the phase composition and the component detection technology of the pyrometallurgical lead metallurgical product are disconnected from experimental research and first-line production, and ensuring that the detection and research provide accurate and practical reference basis for first-line production through data analysis.

The technical scheme of the invention is as follows:

a method for analyzing pyrometallurgical products by utilizing a scanning electron microscope and an energy spectrometer is characterized by comprising the following steps of:

1) and preparing a sample: solidifying, grinding and carbon spraying are carried out on the ore sample to obtain a sample grinding sheet;

2) and setting detection conditions: placing the sample abrasive disc prepared in the step 1) on an electron microscope sample table, and setting electron microscope parameters, wherein the background threshold value is set to be 40;

3) and detecting a sample: starting safety scanning, and detecting a sample by adopting a full-particle measurement mode;

4) and spectrum collection and phase splitting: dividing each phase according to the gray level difference in the detection result, determining the element content of each phase component by adopting an energy spectrum, and assigning component content value to each phase;

5) establishing a metallurgical phase state database: inputting various phase types into a matching library, collecting component spectral lines corresponding to each phase type, and establishing a sample phase database;

6) phase matching and component analysis: matching the detection samples by adopting a phase database, determining the content of phase components in the samples, and obtaining the content of various elements in the samples;

7) and processing a detection result: and obtaining data including the content, phase composition and relative content of various elements in the sample according to the generated detection result.

Preferably, the granularity of the pyrometallurgical sample in the step 1) is controlled within 5 mm.

Preferably, the step 2) of setting the electron microscope parameters further comprises vacuumizing until the vacuum degree is less than 4.0 × 10^-3Pa, the maximum output of the energy spectrum is adjusted to 200kcps, and the maximum energy range is 20 kV.

Preferably, the number of groups of each phase collected in step 5) is not less than 10.

Preferably, the matching failure rate in the step 6) is controlled within 3%.

The invention has the advantages that: the characteristics of high efficiency and accuracy of detection of a scanning electron microscope and an energy spectrometer are fully utilized, effective identification and quantitative analysis of different phases in a sample are realized in effective time according to the characteristic that components in a detected sample are different due to different gray levels, so that the unification of detection results and experiments and production is achieved, and the application value is improved.

Detailed Description

The invention is further illustrated by the following specific examples.

Taking the analysis and research of the lead smelting water quenching slag product as an example.

1. Sample preparation: solidifying, grinding, polishing and spraying carbon on a lead smelting water-quenched slag sample to obtain a sample abrasive disc; if the sample granularity exceeds 5mm, the sample granularity needs to be controlled within 5mm through crushing.

2. Setting detection conditions: placing the prepared sample abrasive disc on an electron microscope sample stage, vacuumizing the electron microscope to be less than 4.0 multiplied by 10^-3Pa, adjusting the saturation point, displacement and inclination of the filament, centering and astigmation of a lens cone, standardizing the gray scale and detecting the base number at 150Kcps, adjusting the brightness and contrast, focusing to obtain a clear image, setting the background threshold value to be 40 (the background value of the material for curing the sample is less than 40, and is set to be 40 in order to shield the curing material), outputting 200Kcps at the maximum energy of the energy spectrum, setting the maximum energy range to be 20kV and other parameters.

3. Sample detection: and starting the safety scanning, and then detecting the sample by adopting a full-particle measurement mode.

4. Spectrum collection and phase splitting: according to the gray level difference in the detection result, the phases in the sample are divided into five types, namely an iron silicate phase (containing zinc), an iron oxide phase, an iron silicate phase, an iron oxide phase (containing zinc) and a copper-lead-bismuth phase, element contents of the five phase components are determined by adopting an energy spectrum, and the actually measured contents of the five phase element components are shown in table 1.

TABLE 1 content of five phase element components

5. Establishing a metallurgical phase database: inputting the five phase types into a matching library, collecting component spectral lines corresponding to the five phase types, and establishing a sample phase database. Note: the component spectral lines of the sample are obtained by combining an electron microscope and an energy spectrum, the phase states with different gray scales are selected by the electron microscope, and then the component spectral lines can be obtained by the energy spectrometer.

6. Phase matching and component analysis: and (3) matching the detection samples by adopting a phase database, wherein the actually determined content of the phase components in the samples is shown in a table 2. And then calculating the content of various elements in the sample. The actual calculated contents of the various elements in the sample are shown in table 3.

The content of the elements is obtained by statistics after scanning by an energy spectrometer, the phase components are obtained by different gray values identified by an electron microscope, and the relative content of the phase is obtained by different gray values and the component content obtained by an energy spectrum.

For example, copper: as is clear from table 1, the copper content in the copper-lead-bismuth phase is 42.11%, and from table 2, the copper-lead-bismuth phase is 2.20%, so that the copper content in the samples shown in table 3 is: 42.11%. 2.20%. 100 ═ 0.93%.

TABLE 2 content of phase component in sample

Phase name	Main elements of	Content (%)
			Ferric silicate phase (containing zinc)	Fe、O、Si、Ca、Al、K、Mn、Mg、Na、S、Zn	54.46
Iron oxide phase	Fe、O	4.30
			Iron silicate phase	Fe、O、Si、Ca、Al、K、Mn、Mg、Na	33.14
Iron oxide phase (containing zinc)	Fe、O、Al、Zn、Mn、Cr、Mg	5.89
			Copper-lead-bismuth phase	Bi、Pb、O、Cu、Te、Ag、Fe、Al	2.20
Total up to		100.00

TABLE 3 content of various elements in the samples

Element(s)	Ag(g/t)	Pb	Cu	Bi	Fe	S	Zn
								Grade (%)	23.10	0.46	0.93	0.63	31.35	0.36	0.55
Element(s)	Al	Si	Mg	Ca	K	Na	Mn
								Grade (%)	3.85	12.73	1.76	9.96	2.14	1.83	2.03

7. And (3) processing a detection result: and obtaining data including the content, phase component condition and relative content of various elements in the sample according to the generated detection result, and forming a detection analysis report.