CN103389236A - Preparation method of standard sample for resolution measurement of EDS (Energy Disperse Spectroscopy) - Google Patents
Preparation method of standard sample for resolution measurement of EDS (Energy Disperse Spectroscopy) Download PDFInfo
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- CN103389236A CN103389236A CN2013103240712A CN201310324071A CN103389236A CN 103389236 A CN103389236 A CN 103389236A CN 2013103240712 A CN2013103240712 A CN 2013103240712A CN 201310324071 A CN201310324071 A CN 201310324071A CN 103389236 A CN103389236 A CN 103389236A
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Abstract
The invention discloses a preparation method of a standard sample for resolution measurement of an EDS (Energy Disperse Spectroscopy). The preparation method comprises the following steps of: preparing a mixed solution of collodion and isoamyl acetate; dropwise adding the mixed solution to water so as to form a collodion liquid film; gently putting an electron microscope copper wire mesh or nickel wire mesh on the collodion liquid film, pressing the electron microscope copper wire mesh or nickel wire mesh on the water by using a glass sheet which is put in obliquely, and then immediately taking out the glass sheet; blowing or exhaling air to the side, which is provided with the collodion film, of the taken out glass sheet so as to form micropores; carrying out carbon praying treatment so as to obtain a micro aperture plate with sprayed carbon, and putting the micro aperture plate with sprayed carbon on filter paper, wherein the side with sprayed carbon is at the upside; dropwise adding ultrasonically dispersed Mn powder turbid liquid on the micro aperture plate, thus finally obtaining the standard sample for resolution measurement of the EDS. The prepared Mn standard sample can achieve accurate results and is convenient to use; Mn particles are directly attached to the surface of the micro aperture plate with sprayed carbon and are not wrapped with the collodion film, the image resolution ratio and the energy spectral resolution ratio are higher; the preparation process is capable of realizing batch production and multiple standard samples can be prepared once.
Description
Technical field
The present invention relates to the measuring method of energy spectrometer resolution, refer to particularly a kind of preparation method of the standard model for the energy spectrometer resolution measurement.
Background technology
Energy spectrometer is the annex of often joining on the electro-optical devices such as transmission electron microscope, scanning electron microscope, electron probe, its principle is according to producing the characteristic X-ray of different-energy after high-power electron beam and sample effect, determine in sample to contain which kind of element according to the energy value of ray, determine the relative content of this element according to the intensity at ray peak.Occurring in nature, the peak position of a lot of elements is more close, even overlapping,, in order to differentiate the close element of peak position, needs energy spectrometer to have higher resolution.Energy spectrometer when Installation and Debugging, is at first measured its resolution.
The measurement of energy spectrometer resolution, general method are to adopt the sample that contains the Mn element, gather the characteristic X-ray energy spectrogram of sample, measure the halfwidth at Mn element Ka linear system peak, as the resolution of this energy spectrometer.For scanning electron microscope, electron probe, sample can be reguline metal, and the Mn standard model becomes more readily available; And for transmission electron microscope, the requirement of sample is stricter, and the sample that can observe under transmission electron microscope only has metallic film and the sample take standard copper (nickel) net as carrier, does not have suitable Mn standard model to be used for measuring the resolution of energy spectrometer.
Summary of the invention
Purpose of the present invention will overcome the existing deficiency of prior art exactly, and a kind of preparation method of the standard model for the energy spectrometer resolution measurement is provided.
For achieving the above object, the present invention is used for the preparation method of the standard model of energy spectrometer resolution measurement, comprises the steps:
(1) preparation collodion+acetic acid isoamyl fat mixed solution: according to collodion and acetic acid isoamyl fat volume ratio, be 1:7 ~ 12, get respectively collodion and acetic acid isoamyl fat, mix, wherein, described collodion is the mixed solution of mass percent 10% guncotton and mass percent 90% ether;
(2) in filling the container of pure water, drip 2 ~ 4 above-mentioned mixed solutions that prepare on the water surface, wait for after 1～3 minute, form one deck collodion liquid film on the water surface;
(3) copper mesh of transmission electron microscope special use or nickel screen are put down gently on the collodion liquid film;
(4) copper mesh or nickel screen place complete after, glass sheet is pushed down Electronic Speculum copper mesh or nickel screen on the water surface, oblique being pressed in container and immediately taken out;
(5) glass sheet that takes out there are top blast gas or the expiration of collodion membrane, allow collodion membrane in the middle of Electronic Speculum copper mesh or nickel screen under the effect of air-flow, form a lot of tiny micropores;
(6) naturally placed 1 ~ 2 hour, after the moisture content on glass sheet evaporates fully, spray carbon and process, obtain spraying the little aperture plate after carbon;
(7) add metal M n powder in absolute ethyl alcohol, the suspension of gained was disperseed 8 ~ 10 minutes with ultrasound wave;
Little aperture plate that (8) will spray after carbon is positioned on filter paper, and spray carbon faces up, and the Mn powder suspension dripping on little aperture plate after 1 ~ 2 ultrasound wave disperses, after absolute ethanol volatilizes, can obtain the standard model for the energy spectrometer resolution measurement.
In step (7), while adding metal M n powder in absolute ethyl alcohol, first toothpick is soaked in absolute ethyl alcohol, with the position of soaking of toothpick, dip metal M n powder, dissolve in absolute ethyl alcohol, then suspension is disperseed with ultrasound wave.
In the present invention, described metal M n powder is nanoscale.Nano level powder particle more easily sticks on prepared little aperture plate, difficult drop-off, and sample is easily preserved; And energy spectrum analysis nanoscale fine particle more easily gather can spectrogram, prevent in the excessive gatherer process of particle that the dead time is bigger than normal.
Beneficial effect of the present invention is: with the mixed solution of collodion and isoamyl acetate, drop in the static water surface and form one deck collodion membrane, copper mesh or nickel screen are placed on collodion membrane and with glass sheet and pick up, copper mesh or nickel screen, collodion membrane successively above glass sheet, with the method for facing to collodion membrane, blowing or exhaling, make the collodion surface form micron-sized aperture, form little aperture plate after spray carbon, the sample of placing on little grid has higher resolution.The powder of metal M n is dispersed in the solution of absolute ethyl alcohol, use ultrasound wave that particle is uniformly dispersed, take the little aperture plate of spray after carbon as carrier, suspension after ultrasound wave is disperseed drops on little aperture plate, little aperture plate after absolute ethanol volatilizes can directly be observed in transmission electron microscope, little aperture plate contains the Mn particle in hole, can carry out the energy spectrum analysis under transmission electron microscope, gather the energy spectrogram of Mn element, and carry out the measurement of energy spectrometer resolution.
What the present invention prepared is a kind of sample for use in transmitted electron microscope of simple metal Mn particle, is convenient to the test of energy spectral resolution, and the preparation method is simple, and measurement result is accurate.When the present invention is applicable to transmission electron microscope installation energy spectrometer annex, the preparation of the standard model of energy spectrometer resolution measurement.Compare with conventional art, the present invention has following advantage:
(1) the energy spectrometer resolution of the method preparation is accurate, easy to use with Mn standard specimen testing result;
(2) the Mn particle is attached directly to spray carbon net surface, there is no the parcel of collodion membrane, and image resolution ratio and energy spectral resolution are higher;
(3) preparation process can the mass operation, once prepares a plurality of standard specimens;
(4) standard model of preparation can long preservation, and is easy to carry.
Description of drawings
Fig. 1 is the structural representation of the present invention's copper mesh that contains a plurality of mesh used.
Fig. 2 is the shape appearance figure of little grid hole and Mn particle in single mesh after sample preparation.
Fig. 3 is for adopting the energy spectrogram of Mn particle in the resulting standard model of the present invention.
Fig. 4 is that the Ka linear system of Mn element in standard model is measured halfwidth measurement result figure.
Embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments.
(1) preparation collodion+acetic acid isoamyl fat mixed solution: get collodion 8ml with graduated cylinder respectively, acetic acid isoamyl fat 90ml, be added to collodion in acetic acid isoamyl fat, and concussion mixes, wherein, collodion is the mixed solution of mass percent 10% guncotton and mass percent 90% ether;
(2) get the 1000ml large beaker and fill pure water, with glue head dropper, drip 2 ~ 4 above-mentioned mixed solutions that prepare on the water surface; Wait for after 1～3 minute, form one deck collodion liquid film on the water surface, acetic acid isoamyl fat volatilizees;
(3) the special-purpose copper mesh of transmission electron microscope that will be is as shown in Figure 1 put down gently on the collodion liquid film with tweezers, once can place a plurality of nets, net with net between separate, can not be overlapping.
(4) copper mesh place complete after, the glass sheet of suitable dimension is pushed down copper mesh on the water surface, oblique being pressed in beaker, and taking out immediately; At this moment, what be close to glass sheet is copper mesh, is collodion above copper mesh;
(5) glass sheet that takes out is had the top blast gas of collodion membrane: air-flow needs moderate, lip magnifies deep breathing and gets final product, air-flow is too small can not form micropore, air-flow is excessive may cause whole collodion membrane to break, purpose is to allow collodion membrane in the middle of copper mesh under the effect of air-flow, form a lot of tiny micropores, place sample on micropore, improve image and energy spectral resolution;
(6) naturally placed 1 hour, after the moisture content on glass sheet evaporates fully, spray carbon and process, obtain spraying the little aperture plate after carbon;
(7) get a 10ml test tube, add the 3ml absolute ethyl alcohol, first toothpick is soaked in absolute ethyl alcohol, with the position of soaking of toothpick, dip nano level metal Mn powder, dissolve in absolute ethyl alcohol, then suspension was disperseed 8 minutes with ultrasound wave; When ultrasound wave disperses, get one, the beaker of 200ml, and the water of dress 80ml, test tube is inserted in beaker, beaker is put into ultrasonic container, can not allow beaker because buoyancy tilts;
Little aperture plate that (8) will spray after carbon is positioned on filter paper, and spray carbon faces up, and with bamboo let, dips in nanoscale Mn powder suspension after upper ultrasound wave disperses, drips 1 ~ 2 on little aperture plate, after absolute ethanol volatilizes, obtains the standard model for the energy spectrometer resolution measurement.
(1) preparation collodion+acetic acid isoamyl fat mixed solution: get collodion 12ml with graduated cylinder respectively, acetic acid isoamyl fat 90ml, be added to collodion in acetic acid isoamyl fat, and concussion mixes, wherein, collodion is the mixed solution of mass percent 10% guncotton and mass percent 90% ether;
(2) get the 1000ml large beaker and fill pure water, with glue head dropper, drip 2 ~ 4 above-mentioned mixed solutions that prepare on the water surface; Wait for after 2 minutes, form one deck collodion liquid film on the water surface, acetic acid isoamyl fat volatilizees;
(3) the special-purpose copper mesh of transmission electron microscope that will be is as shown in Figure 1 put down gently on the collodion liquid film with tweezers, once can place a plurality of nets, net with net between separate, can not be overlapping;
(4) copper mesh place complete after, the glass sheet of suitable dimension is pushed down copper mesh on the water surface, oblique being pressed in beaker, and taking out immediately; At this moment, what be close to glass sheet is copper mesh, is collodion above copper mesh;
(5) glass sheet that takes out is had the top blast gas of collodion membrane: air-flow needs moderate, lip magnifies deep breathing and gets final product, air-flow is too small can not form micropore, air-flow is excessive may cause whole collodion membrane to break, purpose is to allow collodion membrane in the middle of copper mesh under the effect of air-flow, form a lot of tiny micropores, place sample on micropore, improve image and energy spectral resolution;
(6) naturally placed 1 hour, after the moisture content on glass sheet evaporates fully, spray carbon and process, obtain spraying the little aperture plate after carbon;
(7) get a 10ml test tube, add the 5ml absolute ethyl alcohol, first toothpick is soaked in absolute ethyl alcohol, with the position of soaking of toothpick, dip nano level metal Mn powder, dissolve in absolute ethyl alcohol, then suspension was disperseed 10 minutes with ultrasound wave; When ultrasound wave disperses, get one, the beaker of 200ml, and the water of dress 80ml, test tube is inserted in beaker, beaker is put into ultrasonic container, can not allow beaker because buoyancy tilts;
Little aperture plate that (8) will spray after carbon is positioned on filter paper, and spray carbon faces up, and with bamboo let, dips in Mn powder suspension after upper ultrasound wave disperses, drips 1 ~ 2 on little aperture plate, after absolute ethanol volatilizes, obtains the standard model for the energy spectrometer resolution measurement.
(1) preparation collodion+acetic acid isoamyl fat mixed solution: get collodion 10ml with graduated cylinder respectively, acetic acid isoamyl fat 90ml, be added to collodion in acetic acid isoamyl fat, and concussion mixes, wherein, collodion is the mixed solution of mass percent 10% guncotton and mass percent 90% ether;
(2) get the 1000ml large beaker and fill pure water, with glue head dropper, drip 2 ~ 4 above-mentioned mixed solutions that prepare on the water surface; Wait for after 1 ~ 3 minute, form one deck collodion liquid film on the water surface, acetic acid isoamyl fat volatilizees;
(3) the special-purpose nickel screen of transmission electron microscope that will be is as shown in Figure 1 put down gently on the collodion liquid film with tweezers, once can place a plurality of nets, net with net between separate, can not be overlapping;
(4) nickel screen place complete after, the glass sheet of suitable dimension is pushed down nickel screen on the water surface, oblique being pressed in beaker, and taking out immediately; At this moment, what be close to glass sheet is nickel screen, is collodion above nickel screen;
(5) glass sheet that takes out is had the top blast gas of collodion membrane: air-flow needs moderate, lip magnifies deep breathing and gets final product, air-flow is too small can not form micropore, air-flow is excessive may cause whole collodion membrane to break, purpose is to allow collodion membrane in the middle of nickel screen under the effect of air-flow, form a lot of tiny micropores, place sample on micropore, improve image and energy spectral resolution;
(6) naturally placed 1 hour, after the moisture content on glass sheet evaporates fully, spray carbon and process, obtain spraying the little aperture plate after carbon;
(7) get a 10ml test tube, add the 4ml absolute ethyl alcohol, first toothpick is soaked in absolute ethyl alcohol, with the position of soaking of toothpick, dip nano level metal Mn powder, dissolve in absolute ethyl alcohol, then suspension was disperseed 9 minutes with ultrasound wave; When ultrasound wave disperses, get one, the beaker of 200ml, and the water of dress 80ml, test tube is inserted in beaker, beaker is put into ultrasonic container, can not allow beaker because buoyancy tilts;
(8) will spray the good little aperture plate of carbon and be positioned on filter paper, spray carbon faces up, and with bamboo let, dips in Mn powder suspension after upper ultrasound wave disperses, drips 1 ~ 2 on little aperture plate, after absolute ethanol volatilizes, obtains the standard model for the energy spectrometer resolution measurement.
After preparation of standard sample, as shown in Figure 2, white aperture is little grid of 0.3 ~ 1.0 micron for formation diameter after blowing to the shape appearance figure of the interior Mn particle of single mesh, and black particle is metal M n.
Fig. 3 be prepare Mn particle in the standard model of gained can the spectrogram result, the Ka linear system of Mn element is wherein measured halfwidth, measurement result is seen Fig. 4, the resolution of measured energy spectrometer is 132ev.
The present invention also all installs OXFORD company energy spectrometer on 2100F type transmission electron microscope, 2000FX type transmission electron microscope, the standard model that uses preparation method of the present invention to obtain has carried out the measurement of energy spectral resolution, and this sample uses simple, and measurement result is accurate.
Claims (3)
1. a preparation method who is used for the standard model of energy spectrometer resolution measurement, comprise the steps:
(1) preparation collodion+acetic acid isoamyl fat mixed solution: according to collodion and acetic acid isoamyl fat volume ratio, be 1:7 ~ 12, get respectively collodion and acetic acid isoamyl fat, mix, wherein, described collodion is the mixed solution of mass percent 10% guncotton and mass percent 90% ether;
(2) in filling the container of pure water, drip 2 ~ 4 above-mentioned mixed solutions that prepare on the water surface, wait for after 1～3 minute, form one deck collodion liquid film on the water surface;
(3) copper mesh of transmission electron microscope special use or nickel screen are put down gently on the collodion liquid film;
(4) copper mesh or nickel screen place complete after, glass sheet is pushed down Electronic Speculum copper mesh or nickel screen on the water surface, oblique being pressed in container and immediately taken out;
(5) glass sheet that takes out there are top blast gas or the expiration of collodion membrane, allow collodion membrane in the middle of Electronic Speculum copper mesh or nickel screen under the effect of air-flow, form a lot of tiny micropores;
(6) naturally placed 1 ~ 2 hour, after the moisture content on glass sheet evaporates fully, spray carbon and process, obtain spraying the little aperture plate after carbon;
(7) add metal M n powder in absolute ethyl alcohol, the suspension of gained was disperseed 8 ~ 10 minutes with ultrasound wave;
Little aperture plate that (8) will spray after carbon is positioned on filter paper, and spray carbon faces up, and the Mn powder suspension dripping on little aperture plate after 1 ~ 2 ultrasound wave disperses, after absolute ethanol volatilizes, can obtain the standard model for the energy spectrometer resolution measurement.
2. the preparation method of the standard model for the energy spectrometer resolution measurement according to claim 1, it is characterized in that: in step (7), while adding metal M n powder in absolute ethyl alcohol, first toothpick is soaked in absolute ethyl alcohol, dip metal M n powder with the position of soaking of toothpick, dissolve in absolute ethyl alcohol, then suspension is disperseed with ultrasound wave.
3. the preparation method of the standard model for the energy spectrometer resolution measurement according to claim 1 and 2, it is characterized in that: described metal M n powder is nanoscale.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103868922A (en) * | 2014-03-13 | 2014-06-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Phase identification method for vanadium slag rich in various impurity elements |
| CN106706688A (en) * | 2016-11-23 | 2017-05-24 | 武汉钢铁股份有限公司 | Accurate analysis method for tissues of rust layer on steel plate surface |
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2013
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Patent Citations (4)
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|---|---|---|---|---|
| JPH08261897A (en) * | 1995-03-24 | 1996-10-11 | Matsushita Electric Ind Co Ltd | Preparation of sample of transmission electron microscope and its preparation device |
| JP2005114578A (en) * | 2003-10-08 | 2005-04-28 | Jeol Ltd | Sample preparation method device and sample observation device |
| CN102706709A (en) * | 2012-06-08 | 2012-10-03 | 武汉钢铁(集团)公司 | Method for preparing transmission electron microscope sample of rust layer powder test sample |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103868922A (en) * | 2014-03-13 | 2014-06-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Phase identification method for vanadium slag rich in various impurity elements |
| CN103868922B (en) * | 2014-03-13 | 2016-09-28 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of vanadium slag Discriminating materials method rich in Determination of Multi-Impurities |
| CN106706688A (en) * | 2016-11-23 | 2017-05-24 | 武汉钢铁股份有限公司 | Accurate analysis method for tissues of rust layer on steel plate surface |
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Effective date of registration: 20170726 Address after: 430083, Hubei Wuhan Qingshan District Factory No. 2 Gate joint stock company organs Patentee after: Wuhan iron and Steel Company Limited Address before: 15 Wuchang, Wuhan Friendship Avenue, No. 999, block A, layer (Wuhan Iron and steel science and technology innovation department), No. 430080, Patentee before: Wuhan Iron & Steel (Group) Corp. |
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