CN104697916A - Method for recognizing and analyzing single particle of solid fuel particles - Google Patents
Method for recognizing and analyzing single particle of solid fuel particles Download PDFInfo
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- CN104697916A CN104697916A CN201510020202.7A CN201510020202A CN104697916A CN 104697916 A CN104697916 A CN 104697916A CN 201510020202 A CN201510020202 A CN 201510020202A CN 104697916 A CN104697916 A CN 104697916A
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Abstract
The invention discloses a method for recognizing and analyzing a single particle of solid fuel particles. The method comprises the following steps: analyzing an ash sample collected after the combustion of solid fuels by utilizing a CCSEM (computer control scanning electron microscope) technique, converting the geometric particle size of each ash particle determined via the CCESM technique by a particle size conversion formula into aerodynamic diameter, thus recognizing particulate matters at each particle size section in flying ash, such as PM0.5-10, PM0.5-2.5 and PM2.5-10 at the particle diameter size section of 0.5-10microns of the representative aerodynamic diameter; and analyzing the particle size of ash particles and the mineral composition information, thereby obtaining the mineral composition of PM0.5-2.5 and PM2.5-10 respectively, the enrichment situation of typical minerals in ash in PM0.5-2 and PM2.5-10 as well as the occurrence mode of typical ash formation elements in particulate matter at each particle size section. According to the method, the single particle of the particulate matter is counted and recognized by utilizing the advantages of the CCSEM technique in statistics via the particle size conversion method, and the theoretical and technical guidance can be provided for the establishment and analysis of important parameters of solid fuel particles, such as the source, the element occurrence mode.
Description
Technical field
The invention belongs to clean combustion and pollutant emission control technology field, be specifically related to a kind of ash particle to solid fuel ignition generation and carry out single particle analysis, to identify particle and to analyze the method for its individual particle physico-chemical property, be particularly useful for ash content containing Fe amount lower than 5% bituminous coal, stone coal and other volatile content lower than 30% solid fuel.
Background technology
Pellet (PM in air
10, the general name of the particle of equivalent aerodynamic diameter≤10 μm), especially fine particle (PM
2.5, aerodynamic diameter≤2.5 μm) high-load be considered to the arch-criminal causing China's city haze.The solid-fuelled burning such as steam coal is one of important source of China's Particulate Pollution, to coal be representative solid fuel ignition after the deep development of particle Treatment process be the major issue being related to national economy.
Analysis particle being carried out to the physico-chemical properties such as individual particle particle diameter, elemental composition effectively identifies its source, air borne feature, element occurrence patterns and pathogenic etc. important prerequisite, but the single particle analysis realizing particle also exists larger difficulty.By the PM of advanced person
10analytical technology means, as low pressure ram (Low Pressure Impactor, LPI), can obtain the physico-chemical property such as quality, elemental composition that each particle diameter section particle is total, can to PM by the scanning electron microscope (SEM-EDS) of being furnished with power spectrum
10carry out individual particle chemical composition analysis.But the physico-chemical property obtaining a large amount of particle could realize the sign of individual particle physico-chemical property on statistical significance.Traditional SEM-EDS technology is due to inferior positions such as manual operation, naked eyes identification particles, and efficiency is very low.And computing machine controls scanning electron-microscopy (Computer-Controlled Scanned Electron Microscope, CCSEM) single particle analysis can be carried out to a same sample 2000-3000 particle within a short period of time, therefore have the ability to realize PM
10efficiently, the single particle analysis on statistical significance.
Summary of the invention
The present invention is directed to the deficiency of current particle single particle analysis technology, a kind of method to solid fuel particle thing individual particle identification and analysis is provided, realizes PM
10the analysis of the feature such as mineral composition, mineral distribution, element occurrence patterns, the method can greatly deepen to coal be representative solid fuel ignition after the understanding of particle physico-chemical property.
To achieve these goals, a kind of method to solid fuel particle thing individual particle identification and analysis provided by the invention, comprises the following steps:
(1) collect the ash sample after solid fuel ignition, profit is computerizedd control the geometry particle diameter of each ash particle of scanning electron microscope analysis, elemental composition, mineral species and content;
(2) adopt the reduction formula of geometry particle diameter and aerodynamic diameter, the geometry particle diameter of each ash particle step (1) obtained is scaled aerodynamic diameter;
(3) ash particle of aerodynamic diameter in each particle diameter section is identified;
(4) ash particle of the corresponding particle diameter section that ash particle and the low pressure ram based on aerodynamic principle of each particle diameter section step (3) identified are collected does the contrast of mass size distribution, or adopt the number ratio of grey born of the same parents' particle in the corresponding particle diameter section of scanning electron microscope analysis, whether checking particle diameter conversion method is effective, enters (5) step for effective solid-fuel sample;
(5) utilize the individual particle of the statistics of step (3) to each particle diameter section to carry out physico-chemical property analysis, comprise the mineral composition and content of analyzing each particle diameter section particle; Analyze the tax of specific mineralogical composition in each particle diameter section particle and deposit situation; Analyze the tax of main Ash forming elements in particle each particle diameter section, each mineralogical composition and deposit situation.
The present invention is directed to ash content containing Fe amount lower than 5% high-order coal or other volatile content lower than 30% solid fuel, collect burning after ash sample; By particle diameter reduction formula, geometry particle diameter CCSEM being analyzed gained ash sample is scaled aerodynamic diameter, realizes the identification of particle, namely identifies the particle of multiple particle diameter section, as the PM of representative aerodynamic diameter 0.5-10 μm particle diameter section
0.5-10, and PM
0.5-2.5and PM
2.5-10deng; To PM
0.5-10carry out single particle analysis, realize the mineral composition to each particle diameter section particle, certain minerals composition is composed and is deposited situation in each particle diameter section particle, and main Ash forming elements is the analysis such as occurrence patterns in particle each particle diameter section, each mineralogical composition.
In a word, the present invention, by particle after CCSEM technology identification solid fuel ignition and its physico-chemical property of analysis, carries out single particle analysis to the flying dust that burning generates, realizes PM
0.5-10the identification of individual particle and the analysis of physicochemical characteristic, abundant understanding solid fuel ignition generates the physical chemical characteristics on particle statistical significance, for the Establishment and analysis of the important parameter such as source, element occurrence patterns of solid fuel particle thing provides Theory and technology to instruct.
Accompanying drawing explanation
Fig. 1 is that CCSEM identifies the PM collected with LPI
0.5-10mass size distribution schematic diagram;
Fig. 2 is PM
0.5-2.5, PM
2.5-10the mineral composition schematic diagram respective with full ash;
Fig. 3 is PM
0.5-10and typical mineral composition each particle diameter section mass distribution schematic diagram in 10 μm;
Fig. 4 is the mass distribution schematic diagram of Fe element in ash (particle) each mineralogical composition.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is described in detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, but the present invention is not by the restriction of this embodiment.
A kind of method to particle individual particle identification and analysis after solid fuel ignition provided by the invention, its step comprises:
(1) collect the ash sample after solid fuel ignition, profit is computerizedd control the geometry particle diameter of each ash particle of scanning electron microscope (CCSEM) technical Analysis, elemental composition, mineral species and content;
By after flying dust and Brazil wax Homogeneous phase mixing through melting, cooling, grinding, polishing, the sample that obtained dispersion degree is good, obtains the backscatter images of sample in environmental scanning electronic microscope; Choose the data that enough picture number obtain 2000-3000 ash particle, to meet the analysis of statistical significance; The geometry particle diameter obtaining each ash particle and inorganic elements composition is analyzed in power spectrum " Particles " function; Each ash particle is divided to concrete grey mineral species by element composition, the quality of all particles of this kind and be the content of this mineralogical composition in ash.
(2) utilize the analysis result of step (1), adopt the geometry particle diameter of the just each ash particle of reduction formula of geometry particle diameter and aerodynamic diameter to be scaled aerodynamic diameter; Geometry particle diameter d and aerodynamic diameter d
aerreduction formula be
ash particle density p get step (1) define density value corresponding to mineral species.
(3) utilize step (2) identifiable design to go out the particle of each particle diameter section, as the particle of aerodynamic diameter 0.5-10 μm of particle diameter section, be designated as PM
0.5-10, and the particle of multiple typical particle diameter section, as PM
0.5-2.5, PM
2.5-10deng.
It should be noted that the technology acuracy by scanning electron microscope limit, the single particle analysis of superfine particulate matter within 0.5 μm cannot be realized at present.
(4) validity confirming particle diameter scaling results in two ways can be adopted: one is adopt the LPI based on aerodynamic principle to collect PM
10, the PM that itself and step (3) identify
0.5-10do the contrast of mass size distribution to verify the validity that CCSEM test converts with grain diameter; Two exist situation for what observe grey born of the same parents' particle in scanning electron microscope shape appearance figure, and the existence of grey born of the same parents can cause ash particle density and reduction formula input value to have difference.
Effective checking is thought when every grade particles thing data deviation is less than 20% in mass size distribution in " verification mode one "; " verification mode two " observes after shape appearance figure, grey born of the same parents' numbers of particles account for total ash particle ratio lower than 10% time, think effective checking.Multiple data test result shows, ash content measures the high-order coal such as bituminous coal, stone coal lower than 5% containing Fe, and volatile content is lower than producing less grey born of the same parents' particle after other solid fuel ignition of 30%, and particle diameter scaling results and LPI test result substantially identical, be therefore applicable to this reduction formula.Two kinds of verification modes can be chosen any one kind of them, and verify that rear invalid solid-fuel sample is then thought and are not suitable for the method.
(5) through step (4) checking after to PM
0.5-10individual particle physico-chemical property analyze.Identify aerodynamic diameter and mineral species, the content of each ash particle based on step (1)-(3), the mineral composition of each particle diameter section particle can be obtained after gathering, as PM
0.5-2.5and PM
2.5-10respective mineral species and content, and situation is deposited in the tax of certain specific mineralogical composition kind in each particle diameter section particle.The element composition of each ash particle is identified based on step (1), calculate the quality of certain element in this ash particle, after the aerodynamic diameter gathering each ash particle and mineralogical composition kind data, the tax of main Ash forming elements in particle each particle diameter section, each mineralogical composition can be analyzed and deposit situation.
Example:
The method to particle individual particle identification and analysis after solid fuel ignition disclosed in the present embodiment, concrete steps are as follows:
(1) fuel selected by the present embodiment is a kind of typical steam coal: Yangquan stone coal, collects coal dust 1300 DEG C, ash sample after air atmosphere burning in laboratory scale sedimentation furnace.
(2) utilize CCSEM technical Analysis ash sample, the concrete grammar of analysis is: in environmental scanning electronic microscope, obtain flying dust sample backscatter images clearly, obtains the geometry particle diameter of each ash particle; The inorganic elements composition that energy spectrum analysis obtains individual particle is carried out to ash particle; Enough picture number are chosen, to ensure that computing machine meets 2000-3000 ash particle of statistical calculations meaning to sample automatic analysis in power spectrum " Particles " function; Each ash particle is divided to concrete mineral species by respective element composition; The all ash particle quality being defined as mineral of the same race add and are the content of this grey mineralogical composition.
(3) utilize the analysis result of step (2), adopt geometry particle diameter d and aerodynamic diameter d
aerreduction formula
the geometry particle diameter of each ash particle is scaled aerodynamic diameter, ash particle density p get step (2) define the density value of mineral, identifiable design goes out PM thus
0.5-10.
(4) LPI is adopted to collect PM
10, the PM that itself and step (3) identify
0.5-10do the contrast of massfraction domain size distribution within the scope of same particle size, as shown in Figure 1, the PM that two kinds of methods are collected
0.5-2.5domain size distribution is closely similar, and the Particle distribution difference of 2.5-10 μm of scope is relatively larger, may be that part ash born of the same parents particle is on the impact of reduction formula accuracy; In general, the domain size distribution that under this example, two kinds of methods obtain coincide good.Scanning electron microscope shape appearance figure also shows in ash sample and there is grey born of the same parents' particle hardly, and each grey mineralogical composition density value impact adopted reduction formula is very little.
(5) step (1)-(3) are utilized to identify PM
0.5-10, and utilize step (4) to confirm the validity of this particle diameter conversion method; Subsequently to PM
0.5-10individual particle physical chemical characteristics make a concrete analysis of.
Fig. 2 analyzes the mineral composition of each particle diameter section particle, with PM
0.5-2.5, PM
2.5-10be example with full ash sample, result shows, PM
0.5-2.5main grey mineralogical composition is Fe silico-aluminate, mixing silico-aluminate and difficult identification composition, and PM
2.5-10primaries mineralogical composition be mullite and Fe silico-aluminate.
Fig. 3 analyzes the tax of certain minerals composition in each particle diameter section particle and deposits situation, with PM
0.5-10the comparison of distribution can find, Fe silico-aluminate is enriched in below 2.5 μm of particles more, and mullite phase constituent is the comparatively coarse particle particle diameter section being present in 2.5-10 μm then more.
Fig. 4 analyzes the tax of Ash forming elements in particle each particle diameter section, each mineralogical composition and deposits situation, and for Fe element, Fe is at PM
0.5-2.5in be present in Fe silico-aluminate more and difficult identify composition; PM
2.5-10in Fe be distributed in Fe silico-aluminate, mullite and difficult identify that the content in composition is all larger.
The invention is not restricted to the restriction of embodiment, be equally applicable to ash content containing Fe amount lower than 5% coal and volatile content lower than 30% solid fuel.The above, be only a kind of embodiment of the present invention, but the scope of protection of the invention is not limited thereto.Anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (4)
1., to a method for solid fuel particle thing individual particle identification and analysis, comprise the following steps:
(1) collect the ash sample after solid fuel ignition, profit is computerizedd control the geometry particle diameter of each ash particle of scanning electron microscope analysis, elemental composition, mineral species and content;
(2) adopt the reduction formula of geometry particle diameter and aerodynamic diameter, the geometry particle diameter of each ash particle step (1) obtained is scaled aerodynamic diameter;
(3) ash particle of aerodynamic diameter in each particle diameter section is identified;
(4) ash particle of the corresponding particle diameter section that ash particle and the low pressure ram based on aerodynamic principle of each particle diameter section step (3) identified are collected does the contrast of mass size distribution, or adopt the number ratio of grey born of the same parents' particle in the corresponding particle diameter section of scanning electron microscope analysis, whether checking particle diameter conversion method is effective, enters (5) step for effective solid-fuel sample;
(5) utilize the individual particle of the statistics of step (3) to each particle diameter section to carry out physico-chemical property analysis, comprise the mineral composition and content of analyzing each particle diameter section particle; Analyze the tax of specific mineralogical composition in each particle diameter section particle and deposit situation; Analyze the tax of main Ash forming elements in particle each particle diameter section, each mineralogical composition and deposit situation.
2. method according to claim 1, is characterized in that, the computerized control method of scanning electron microscope analysis ash particle of described profit is as follows: flying dust and Brazil wax Homogeneous phase mixing are obtained sample, obtains flying dust backscatter images in scanning electron microscope; Choose enough picture number to obtain 2000-3000 the ash particle meeting statistical analysis, then analyze geometry particle diameter and the element composition of each ash particle.
3. method according to claim 1, is characterized in that: for comprising PM
0.5-2.5, PM
2.5-10and PM
0.5-10carry out respectively adding up at interior particle that is arbitrary or several particle diameter section and analyze.
4. method according to claim 1, is characterized in that: be suitable for fuel be ash content contain Fe amount lower than 5% bituminous coal, stone coal and other volatile content lower than 30% solid fuel.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114814076A (en) * | 2022-04-12 | 2022-07-29 | 华中科技大学 | Calculation method and measurement method for contamination average interface energy of fly ash particles |
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2015
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