CN1255669C - Scanning electronic microscope standard substance and its making method - Google Patents
Scanning electronic microscope standard substance and its making method Download PDFInfo
- Publication number
- CN1255669C CN1255669C CN 03116182 CN03116182A CN1255669C CN 1255669 C CN1255669 C CN 1255669C CN 03116182 CN03116182 CN 03116182 CN 03116182 A CN03116182 A CN 03116182A CN 1255669 C CN1255669 C CN 1255669C
- Authority
- CN
- China
- Prior art keywords
- electron microscope
- substrate
- scanning electron
- disperse phase
- polystyrene standard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to the technical field of metering test standard quantity value transmission, particularly to a standard substance for calibrating the magnifications of a scanning electron microscope and a preparing method thereof. A base plate is coated with a measuring film which is coated with a conducting layer, and the measuring film is a hexagonal densely-arranged array of monodisperse polystyrene standard particles. The preparing method comprises: firstly, selecting a monodisperse polystyrene standard particle aqueous solution and the base plate; secondly, cleaning the base plate; thirdly, dripping and spraying the monodisperse polystyrene standard particle aqueous solution on the base plate; fourthly, putting the base plate forming an angle of 0 degree to 5 degrees with the horizontal plane in a decontamination chamber for natural drying. The standard substance of the present invention enlarges the calibrating range (1000 times to 200000 times) of a scanning electron microscope, and is capable of giving source tracing values within the calibrating range and additional uncertainty of given confidence intervals, and making the scanning electron microscope which is used within the calibrating range meet the demands of the ISO9000 quality certification system.
Description
Technical field
The present invention relates to metrology and measurement standard transmission of quantity value technical field, especially relate to a kind of standard substance (standard model) that is used for calibration scan electron microscope enlargement ratio and preparation method thereof.
Background technology
Enter today of 21 century at human society, along with the develop rapidly of worldwide nanosecond science and technology, nanosecond science and technology have been widely used in the data acquisition and the quality Control during Production of laboratory basic scientific research, product development exploitation.And present many quality certification systems, but the data that obtain as requirements such as ISO9000 series should have the value of the traceability of value.Simultaneously, the resolution of scanning electron microscope of observing important means as nanostructured is more and more higher, and this just need also will have the value that can trace to the source in the view data under the more and more higher enlargement ratio.But only limit to below 20,000 times from the obtainable standard substance calibration range that is used for scanning electron microscope of commerce at present.The certified reference material SRM484g of USA National Institute of Standard and Technology (NIST) (the regulation usable range is 1000 times～20000 times in the calibration file) for example; The grid grating standard substance of the 2160 lines/mm of Britain Agar scientific company, this standard substance is by physics Institute of Britain country (NPL) demarcation of tracing to the source.For the grid grating certified reference material of the 2160 lines/mm of Britain Agar scientific company, the calibration value of physics Institute of Britain country is that the uncertainty of per 10 lattice is ± 0.05 μ m that promptly the uncertainty of the spacing of 4.6 μ m is ± 0.05 μ m on the standard substance.When enlargement factor surpasses 20000 times, 4.6 the spacing of the final imaging of the spacing of μ m is greater than 9cm, the breadth (being sweep limit) that has surpassed the final imaging photo of general scanning electron microscope, the image of this multiplying power can't be calibrated, thereby the more and more higher requirement of current scanline electron microscope resolving power can't be adapted to.As the resolution of field ejecting gun electron microscope be about 1.0～1.5nm.For the development of the nanosecond science and technology that adapt to current sciemtifec and technical sphere, bring into play the effect of high resolution scanning electron microscope effectively, use 10～200,000 times enlargement ratio to come the photographic images photo will become more and more ordinary laboratory work.(1nm is 0.2mm on the photo of 200,000 times of amplifications, and the point resolution of human eye is 0.2mm) in order to adapt to the needs of the high magnification calibration of scanning electron microscope, the present invention has developed and can be used for calibrating 1000 times～200000 times standard substance (standard model).
Summary of the invention
It is 1000 times～200000 times that technical matters to be solved by this invention provides a kind of calibration magnification that is used for, and can in calibrating multiplying power scope, it provide the value of tracing to the source, and, make the high power view data that is calibrated have scanning electron microscope standard substance (standard model) that can the value of tracing to the source and preparation method thereof with the uncertainty of given fiducial interval.The technical scheme that the present invention solves its technical matters employing is: a kind of scanning electron microscope standard substance, be coated with the measurement film on its substrate, measure on the film and be coated with conductive layer, measuring film is the compact arranged single disperse phase polystyrene standard PArray of hexagonal, this standard particle array is formed by dried single disperse phase polystyrene standard particle aqueous solution, is equipped with substrate on the specimen holder.A kind of method for making of scanning electron microscope standard substance, it comprises the steps: that a. chooses single disperse phase polystyrene standard particle aqueous solution, chooses substrate; B. cleaning base plate; C. the water-soluble drop of single disperse phase polystyrene standard particle is sprinkled upon on the substrate; D. substrate is put into decontamination chamber's air dry horizontal by 0 °～5 °; E. substrate embeds specimen holder; F. dried single disperse phase polystyrene standard particle aqueous solution plates conductive layer on the substrate to being adsorbed on ion sputtering instrument, and described conductive layer is the gold layer, and the purity of gold layer is at least 99%, and the thickness of gold layer is 5nm～20nm.。Single disperse phase polystyrene standard particle aqueous solution is selected the product of U.S. Duke scientific company for use.Task proposed by the invention also can further be realized by following technical solution: be equipped with substrate on the specimen holder; It is that 1mm～1.5mm, diameter are the glass plate of 5mm～10mm less than 20nm, thickness that described substrate is selected surfaceness for use; The physical and chemical parameter of described single disperse phase polystyrene standard particle aqueous solution is solids content (content of polystyrene standard particle in aqueous solution) 0.2%～2%, density 1.05g/cm
3, refractive index 1.59@589nm/23 ℃, single disperse phase polystyrene standard particle diameter is the relative standard deviation 0.5%～2% of 0.2 μ m～10 μ m, single disperse phase polystyrene standard particle diameter, the use amount V of single disperse phase polystyrene standard particle aqueous solution is determined by following formula: V=CSd/p, surface area, the d that C is 0.3～1.0 in the formula, S is substrate are that diameter, the p of standard particle in single disperse phase polystyrene standard particle aqueous solution is the solids content of single disperse phase polystyrene standard particle aqueous solution; Described cleaning is that substrate is immersed in 100% the ethanol, and cleans 5～15 fens kinds with supersonic wave cleaning machine; The room temperature of described decontamination chamber is 18 ℃～22 ℃; Humidity is 60% ± 5%; Substrate embeds specimen holder; Dried single disperse phase polystyrene standard particle aqueous solution plates conductive layer on the substrate to being adsorbed on; Described conductive layer is the gold layer, and the purity of gold layer is at least 99%, and the thickness of gold layer is 5nm～20nm, and is gold-plated on dried single disperse phase polystyrene standard particle aqueous solution with ion sputtering instrument.The present invention is owing to adopt technique scheme, enlarged the calibration range (1000 times～200000 times) of scanning electron microscope, and can in its calibration range, provide the value of tracing to the source, and, make scanning electron microscope meet the requirement of ISO9000 quality certification system in being calibrated scope, using with the uncertainty of given fiducial interval.
Description of drawings
Below in conjunction with accompanying drawing and specific embodiments of the invention the present invention is described in further detail:
Fig. 1 is a structural representation of the present invention.
Fig. 2 is the A portion enlarged drawing (the array figure of dried single disperse phase polystyrene standard particle) of Fig. 1.
Fig. 3 is that 0.3 μ m standard particle amplifies 200,000 times diagrammatic sketch.
Fig. 4 is that 1.0 μ m standard particles amplify 2,000 times diagrammatic sketch.
With reference to Fig. 1, Fig. 2.The present invention includes to be coated with on conductive layer 1, the specimen holder 3 on substrate 2, measurement film 4, the measurement film 4 and be equipped with substrate 2.
Embodiment
Embodiment 1: with reference to Fig. 1, Fig. 2.Plating is measured film (dried single disperse phase polystyrene standard particle aqueous solution) on substrate of the present invention, and then gold-plated on the measurement film, can carry out magnification calibration.
Embodiment 2: with reference to Fig. 1, Fig. 2.Be convenient calibration, plating measured film and gold-plated substrate is inserted on the specimen holder, also can reach the technique effect identical with embodiment 1.
Embodiment 3: with reference to Fig. 1, Fig. 2.The physical and chemical parameter of at first selecting for use U.S.'s Duke scientific company to provide is solids content 1%, density 1.05g/cm
3, refractive index 1.59@589nm/23 ℃ particle diameter be the single disperse phase polystyrene standard particle aqueous solution (relative standard deviation 1.4% of single disperse phase polystyrene standard particle diameter) of 0.3 μ m, surfaceness (Ra) is that 1mm, diameter are that the glass plate of 10mm is as substrate less than 20nm, thickness; Then substrate is immersed in 100% the ethanol, with supersonic wave cleaning machine substrate is cleaned 8 fens kinds again; Then the water-soluble drop of single disperse phase polystyrene standard particle is sprinkled upon that (the use amount V of single disperse phase polystyrene standard particle aqueous solution should satisfy following formula: V=0.6Sd/p), make it form individual layer and the spherical array of the compact arranged standard particle of hexagonal on the substrate.The arrangement principle of the spherical array of standard particle is: along with the volatilization of moisture content, when moisture content is fewer and feweri, gradually the capillary force of Zeng Daing make single disperse phase polystyrene standard particle aqueous solution particle aggregation together, individual layer particle originally in blocks is last, and to form the compact arranged row of piece old.It is old that wherein the macroparticle of minute quantity is extruded row, makes the statistical standard deviation that forms the old particle of row will be better than original solution.Subsequently substrate and level being 0 °～5 °, to put into room temperature be that 18 ℃～22 ℃, humidity are the air dry of 60% ± 5% decontamination chamber, after the drying substrate is embedded specimen holder, (because the proper alignment of micro-meter scale particle, the formed film of at this moment single disperse phase polystyrene standard particle can observe with the naked eye the same branch luminous effect of similar diffraction grating under daylight.) use ion sputtering instrument Gold plated Layer on dried single disperse phase polystyrene standard particle at last, the thickness of gold layer is 8nm.
The present invention adopts that U.S.'s Duke scientific company provides has card standard spheroidal particle to be developed into to comprise 0.2 μ m; 0.3 μ m; 0.5 μ m; The arrangement spheroidal particle standard substance of 1 μ m is used for the calibration scan electron microscope at 1000 times～200000 times enlargement ratio.Single disperse phase polystyrene standard particle aqueous solution is an aqueous suspension, and the mean value of its grain size can be traceable to the length metering standard of Unite States Standard (USS) Institute for Research and Technology.Its density is 1.05g/cm
3, refractive index is 1.59@589nm (23 ℃), its other technical parameter such as table 1 (attached).
The present invention has made the compact arranged standard substance of large-area individual layer hexagonal with above-mentioned four kinds of standard particles.Because there is certain gray scale on the border of discrete particles, can't determine well that this will bring bigger error to measurement.In addition, if after discrete particles was wrapped up by Gold plated Layer, its real border more was difficult for being determined.So the present invention adopts standard particle closely to arrange, rather than standard particle is disperseed uniform method for making.Photo 1, photo 2 are that the 300nm standard particle made of the present invention amplifies 200,000 times diagrammatic sketch and 1.0 μ m standard particles and amplifies 2,000 times diagrammatic sketch.The present invention can see from photo 1, and when the enlargement ratio of scanning electron microscope reached 200,000 times, 0.3 μ m standard particle was 6cm, still can calibrate this multiple effectively.For the calibration of different enlargement ratios, the present invention advises adopting the standard particle of different-grain diameter: 0.2 μ m (20,000 times～300,000 times); 0.3 μ m (10,000 times～200,000 times); 0.5 μ m (5,000 times～50,000 times); 1.0 μ m (1,000 times～10,000 times).
The present invention needs to calibrate the present invention before the transmission of measurement standard value, and calibration steps example of the present invention is as follows: the XL/ESEM30 scanning electron microscope that the present invention adopts Dutch Philips company the condition contrast test such as carries out to the certified reference material (calibration value of physics Institute of Britain country is 4.6 μ m ± 0.05 μ m/10 lattice) of the 2160 lines/mm of Britain Agar scientific company and close-up row particle standard substance of the present invention.The scanning electron microscope condition of work that the present invention selects is: the 15kV/ accelerating potential; 2.4/ bundle spot size; 20,000 times/enlargement ratio; Secondary electron/detector; 10.0/ operating distance.5 different parts to Britain Agar standard specimen under this condition of work have been taken photo, and in the horizontal direction every photo has been carried out upper, middle and lower and measured for three times, the data that read see Table 2 (attached), under same condition, close-up row particle samples of the present invention is taken pictures again, 9 different samples have been chosen, each sample is all selected 6 arranged blocks, and 3 10 rows' measurement is carried out in each arrangement, and reading of data sees Table 3 (attached).
Data processing of the present invention and uncertainty evaluation:
A) to be used for the certified reference material (SRM) of relative Calibration be the standard substance of the 2160 lines/mm of Agar scientific company in the present invention, it adds laser interferometer by Britain's used scanning electron microscope of country's physical study calibrates, and its calibration value is: 4.6 μ m ± 0.05 μ m/10 lattice.Its relative uncertainty Da=0.05/4.6=1.1%.
B) scanning electron microscope is owing to the difference of operating distance, and its same enlargement ratio nominal value and actual value will have small variation.The degree of regulation of Philips XL/ESEM30 scanning electron microscope operating distance is 0.1mm, is 9.950～10.049 when 10mm.Enlargement ratio sees Table 4 (attached) with the data that operating distance changes.
Operating distance is made as X, and the mean value that the certified reference material of same enlargement ratio is measured with gap length is Y, carries out seemingly the closing of least square method of linear regression curve with the data of table 4.
Y=mX+b formula 1
Wherein: m=0.0136; B=4.596
ΔY＝0.0136ΔX
0.1 generation Δ X is got Δ Y=0.00136
ΔY/Y＝0.00136/4.737≈0.0003＝0.03％
Average value measured when wherein Y=4.737 is operating distance 10mm.
So the maximum functional distance is when 10mm, the uncertainty Db of the enlargement ratio that the 0.1mm uncertainty produces is approximately 0.03%.
C) the incomplete level of slotted line can be owing to the not quite identical uncertainty that produces of horizontal enlargement ratio of scanning electron microscope and vertical enlargement ratio.Calibration is amplifying 20 with the horizontal enlargement ratio of XL/ESEM30 scanning electron microscope with vertical enlargement ratio, the method for measuring of the error in the time of 000 times is as follows: at first the standard substance at Agar amplifies 20, in 000 times the same visual field, respectively get the mean value of measuring for three times and ask its ratio in vertical and horizontal direction.The ratio P of vertical here enlargement ratio and horizontal enlargement ratio is calculated by formula 2.
P=(3.81+3.82+3.82)/(3.81+3.79+3.80)=1.004 formula 2
For with the measurement state consistency of comparison certified reference material, the present invention adopts sample stage to rotate to make standard particle to measure the maintenance level.But from measuring on the photo, the incomplete level of slotted line, their angle maximum deviation are less than 2 °, so the uncertainty of the level inclination of image is 2 °.The uncertainty Dc that the incomplete level of image measurement line produces is expressed by formula 3.
Dc=1-[P
2* sin
2α+cos
2α]
1/2Formula 3
Wherein: P is the ratio of vertical enlargement ratio and horizontal enlargement ratio.
α is the maximum angle of slotted line and image level line.
With P=1.004, α=2 ° substitution formula 3
Dc＝|1-[1.004
2×sin
2(2°)+cos
2(2°)]
1/2|≈0.000014＝0.0014％
Therefore because the horizontal enlargement ratio of scanning electron microscope is not quite identical with vertical enlargement ratio, the incomplete level of slotted line and the uncertainty that produces is compared with the uncertainty of other reason generation can be ignored.
D) calibration is 0.01 μ m with the uncertainty of measured value in the time of 20,000 times of XL/ESEM30 scanning electron microscope computer picture software, so for 10 one group measurement, the uncertainty of every standard particle is Dd=1nm (0.33%).
Last calibration value is:
The mean value of standard particle: Mp=0.3015 μ m (seeing Table 3)
Category-A uncertainty: Δ A=(10)
1/2* S (Overall Standard Deviation)=(10)
1/2*
0.0016＝0.0051μm(1.68％)
Wherein: S=[∑ (u
i-ū)
2/ (n-1)]
1/2(u
i: measured value/10 each time; N=161)
Category-B uncertainty: Δ B=(Da
2+ Db
2+ Dd
2)
1/2≈ 1.14% (3.4nm)
Wherein: Da, Db, Dd linear independence.The standard deviation S of the mean value of each sample measurement value
Sample=0.9nm (seeing Table 3)
From the data processing of standard particle sample and the result of uncertainty evaluation, the data that the mean value of standard particle and original Duke scientific company provide relatively, it be greatly 1.5nm (0.5%).This is mainly derived from particle in alignment processes, exists the slit that is difficult for discovering between each particle, and (behind gold (Au) layer in the sputter, it will more be difficult for discovering.) and the existence of the foreign body that in the particle polymerization process, carries over.The main source of category-B uncertainty be present in as the certified reference material of the Agar scientific company of calibration usefulness with the uncertainty and of tracing to the source as the image resolution ratio of Philips XL/ESEM30 of calibration usefulness, the resolution of measuring computer software and display screen is high not enough.The also bigger standard deviation that draws with TEM with the Duke scientific company of category-A uncertainty.It is considered herein that wherein main cause is that also the error of measured value is bigger, and arrange particle the function of removing king-sized and especially little particle is arranged, because these particles are unwell to arrangement, its result will be better than the monodispersity of original particle.If use image resolution ratio higher field ejecting gun scanning electron microscope and the higher computer software of screen resolution to calibrate, the result will be more satisfactory.From the homogeneity data (the standard deviation S sample of the mean value of each sample measurement value) of sample, it is considered herein that the data between each sample are quite consistent.In addition, when using this sample to come the calibration scan electron microscope, the present invention's suggestion is chosen to the arrangement particle of piece as far as possible and measures, in order to avoid introduce extra uncertainty.Above-mentioned calibration procedure only is the example that the present invention obtains the value of tracing to the source, and calibrates as adopting laser interferometer to add scanning electron microscope, will obtain better effect.
The comparison of the technical parameter of the certified reference material SRM484g of the scanning electron microscope of the present invention and USA National Institute of Standard and Technology (NIST) sees Table 5 (attached).This certified reference material is to be embedded in 0.5 μ m with thin gold (Au) layer, 1 μ m, 3 μ m, the standard substance of making after the section polishing of the metallic nickel of 5 μ m (Ni) layer.From the data of form 2, it is using " 3 → 4 ", and when " 4 → 5 ", its uncertainty is 1%～1.5%.When amplifying 20,000 times, use " 0 → 1 ", " 1 → 2 ", its calibration uncertainty will very fast change big (7.8%～3.8%) when " 2 → 3 ", so its regulation usable range in calibration file is 1,000 times-20,000 times.It is that the method that adopts laser interferance method to add scanning electron microscope is demarcated, and this is a kind of absolute method of measurement.In addition, the certified reference material of Britain Agar scientific company is the grid standard substance of traditional 2,160 lines/mm.The method that it adopts laser interferance method to add scanning electron microscope by Britain's National Physical Laboratory (NPL) is equally demarcated.Its uncertainty is 4.6 μ m+0.05 μ m/10 lattice (1.1%), and when its use is less than 10 lattice calibration scan electron microscopes, with the nothing value of tracing to the source, it also will limit it and use under high magnification like this.
Single disperse phase polystyrene standard particle aqueous solution stoste among the present invention derives from the certified reference material of Duke scientific company.Comprehensive itself definite value uncertainty, its synthetic overall uncertainty is bigger.For the particle of 3 μ m, be approximately 3.4nm (1.14%), standard deviation is 5.1nm (1.68%), standard deviation can be diminished by the mean value of measuring a plurality of particles (n) and is Δ A/ (n when measuring
1/2).The invention has the advantages that to have under the condition of the value of tracing to the source, calibrate big enlargement ratio (20,000 times～200,000 times) and the uncertainty of calibration is altered a great deal, and from the surface of standard substance, the summit of particle and the difference of height of junction are 1/2 of particle diameter, and (diameter is that the particle of 0.3 μ m is 0.15 μ m.) greater than other commercial scanning electron microscope standard substance, this has the better pictures contrast for the user when using sem observation, thereby brings great convenience.
| Sample number | Particle diameter | The calibration mean grain size | Standard deviation and relative standard deviation | Solids content |
| 3200A | 200nm | 199nm±6nm | 3.4nm(1.7％) | 1％ |
| 3300A | 300nm | 300nm±5nm | 4.3nm(1.4％) | 1％ |
| 3500A | 500nm | 499nm±5nm | 6.5nm(1.3％) | 1％ |
| 4009A | 1000nm | 993nm±21nm | 10nm(1.0％) | 1％ |
Table 1
| Agar scientific company certified reference material measurement data (2160 lines/mm grid grating) Acc.:15.0; Spot:2.4; Magn:20000x; Det:SE; WD:10.0 | ||||
| | | | | |
| Photo | ||||
| 1 | 4.74 | 4.74 | 4.74 | 4.740 |
| | 4.74 | 4.74 | 4.74 | 4.740 |
| | 4.74 | 4.74 | 4.74 | 4.740 |
| Photo 4 | 4.74 | 4.74 | 4.74 | 4.740 |
| Photo 5 | 4.74 | 4.74 | 4.74 | 4.740 |
| Photo 6 | 4.74 | 4.75 | 4.74 | 4.743 |
| Overall measurement mean value | 4.741 | |||
| The magnification factor: overall measurement mean value/4.6= | 1.031 | |||
Table 2
| Close-up row standard particle standard substance measurement data ACC.:15.0kV; Spot:2.4; Magn:20000x; Det:SE; WD:10.0 | |||||||||
| Sample number | Photo number | Arrange number | Measure 1 | | | Measure average | Particle size | Sample average | |
| 1 | 1 | 1 | 3.11 | 3.10 | 3.08 | 3.097 | 0.3097 | ||
| 1 | 1 | 2 | 3.10 | 3.11 | 3.10 | 3.103 | 0.3103 | ||
| 1 | 2 | 3 | 3.10 | 3.11 | 3.10 | 3.103 | 0.3103 | ||
| 1 | 3 | 4 | 3.11 | 3.13 | 3.10 | 3.113 | 0.3113 | ||
| 1 | 4 | 5 | 3.12 | 3.13 | 3.11 | 3.120 | 0.3120 | ||
| 1 | 4 | 6 | 3.09 | 3.10 | 3.11 | 3.100 | 0.3100 | 0.3106 | |
| 2 | 5 | 7 | 3.11 | 3.12 | 3.10 | 3.110 | 0.3110 | ||
| 2 | 5 | 8 | 3.11 | 3.12 | 3.13 | 3.120 | 0.3120 | ||
| 2 | 6 | 9 | 3.11 | 3.10 | 3.11 | 3.107 | 0.3107 | ||
| 2 | 7 | 10 | 3.10 | 3.11 | 3.12 | 3.110 | 0.3110 | ||
| 2 | 7 | 11 | 3.08 | 3.08 | 3.07 | 3.077 | 0.3077 | ||
| 2 | 8 | 12 | 3.12 | 3.11 | 3.09 | 3.107 | 0.3107 | 0.3105 | |
| 3 | 10 | 13 | 3.13 | 3.12 | 3.12 | 3.123 | 0.3123 | ||
| 3 | 10 | 14 | 3.12 | 3.12 | 3.13 | 3.123 | 0.3123 | ||
| 3 | 11 | 15 | 3.13 | 3.11 | 3.11 | 3.117 | 0.3117 | ||
| 3 | 11 | 16 | 3.11 | 3.08 | 3.12 | 3.103 | 0.3103 | ||
| 3 | 12 | 17 | 3.12 | 3.13 | 3.12 | 3.123 | 0.3123 | ||
| 3 | 12 | 18 | 3.11 | 3.13 | 3.13 | 3.123 | 0.3123 | 0.3119 | |
| 4 | 14 | 19 | 3.13 | 3.13 | 3.09 | 3.117 | 0.3117 | ||
| 4 | 14 | 20 | 3.11 | 3.12 | 3.10 | 3.110 | 0.3110 | ||
| 4 | 15 | 21 | 3.13 | 3.14 | 3.13 | 3.133 | 0.3133 | ||
| 4 | 15 | 22 | 3.13 | 3.11 | 3.09 | 3.110 | 0.3110 | ||
| 4 | 16 | 23 | 3.13 | 3.12 | 3.13 | 3.127 | 0.3127 | ||
| 4 | 16 | 24 | 3.10 | 3.12 | 3.13 | 3.117 | 0.3117 | 0.3119 | |
| 5 | 17 | 25 | 3.08 | 3.08 | 3.08 | 3.080 | 0.3080 | ||
| 5 | 17 | 26 | 3.08 | 3.11 | 3.09 | 3.093 | 0.3093 | ||
| 5 | 18 | 27 | 3.10 | 3.11 | 3.10 | 3.103 | 0.3103 | ||
| 5 | 19 | 28 | 3.11 | 3.07 | 3.08 | 3.087 | 0.3087 | ||
| 5 | 19 | 29 | 3.12 | 3.10 | 3.13 | 3.117 | 0.3117 | ||
| 5 | 20 | 30 | 3.07 | 3.06 | 3.06 | 3.063 | 0.3063 | 0.3091 | |
| 6 | 21 | 31 | 3.08 | 3.09 | 3.10 | 3.090 | 0.3090 | ||
After continuous
</entry></row></tbody></tgroup></table></tables>
Table 3
| Enlargement ratio changes experimental data Acc.:15.0kV with operating distance; Spot:2.4; Magn:20000x; Det:SE | ||||
| Operating distance (mm) | Measure 1 | | | Mean value |
| 6.0mm | 4.67 | 4.67 | 4.68 | 4.673 |
| 7.0mm | 4.69 | 4.69 | 4.68 | 4.687 |
| 8.0mm | 4.71 | 4.70 | 4.72 | 4.710 |
| 9.0mm | 4.72 | 4.74 | 4.72 | 4.727 |
| 10.0mm | 4.73 | 4.74 | 4.74 | 4.737 |
| 11.0mm | 4.74 | 4.74 | 4.75 | 4.743 |
| 12.0mm | 4.76 | 4.77 | 4.75 | 4.760 |
| 13.0mm | 4.77 | 4.75 | 4.75 | 4.757 |
| 14.0mm | 4.78 | 4.79 | 4.79 | 4.787 |
| 15.0mm | 4.81 | 4.80 | 4.81 | 4.807 |
Table 4
| Line is right | Distance values (μ m) | Calibrated distance value (μ m) | Uncertainty (μ m) |
| 0→1 | 0.5 | ±0.034 | |
| 1→2 | 0.5 | ±0.039 | |
| 2→3 | 1 | ±0.038 | |
| 3→4 | 3 | ±0.044 | |
| 4→5 | 5 | ±0.051 | |
| 0→5 | (10) | (±0.059) |
Table 5
Claims (6)
1. scanning electron microscope standard substance is characterized in that: be coated with the measurement film on its substrate, measure on the film and be coated with conductive layer, measuring film is the compact arranged single disperse phase polystyrene standard PArray of hexagonal, is equipped with substrate on the specimen holder.
2. the method for making of a scanning electron microscope standard substance is characterized in that: it comprises the steps,
A. choose single disperse phase polystyrene standard particle aqueous solution, choose substrate;
B. cleaning base plate;
C. the water-soluble drop of single disperse phase polystyrene standard particle is sprinkled upon on the substrate;
D. substrate is put into decontamination chamber's air dry horizontal by 0 °～5 °;
E. substrate embeds specimen holder;
F. dried single disperse phase polystyrene standard particle aqueous solution plates conductive layer on the substrate to being adsorbed on ion sputtering instrument, and described conductive layer is the gold layer, and the purity of gold layer is at least 99%, and the thickness of gold layer is 5nm～20nm.
3. the method for making of a kind of scanning electron microscope standard substance according to claim 2 is characterized in that: it is that 1mm～1.5mm, diameter are the glass plate of 5mm～10mm less than 20nm, thickness that described substrate is selected surfaceness for use.
4. the method for making of a kind of scanning electron microscope standard substance according to claim 2 is characterized in that: the physical and chemical parameter of described single disperse phase polystyrene standard particle aqueous solution is solids content 0.2%～2%, density 1.05g/cm
3, refractive index 1.59@589nm/23 ℃, single disperse phase polystyrene standard particle diameter is the relative standard deviation 0.5%～2% of 0.2 μ m～10 μ m, single disperse phase polystyrene standard particle diameter, the use amount V of single disperse phase polystyrene standard particle aqueous solution is determined by following formula: V=CSd/p, surface area, the d that C is 0.3～1.0 in the formula, S is substrate are that diameter, the p of standard particle in single disperse phase polystyrene standard particle aqueous solution is the solids content of single disperse phase polystyrene standard particle aqueous solution.
5. the method for making of a kind of scanning electron microscope standard substance according to claim 2 is characterized in that: described cleaning is that substrate is immersed in 100% the ethanol, and cleans 5～15 fens kinds with supersonic wave cleaning machine.
6. the method for making of a kind of scanning electron microscope standard substance according to claim 2 is characterized in that: the room temperature of described decontamination chamber is 18 ℃～22 ℃; Humidity is 60% ± 5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116182 CN1255669C (en) | 2003-04-04 | 2003-04-04 | Scanning electronic microscope standard substance and its making method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116182 CN1255669C (en) | 2003-04-04 | 2003-04-04 | Scanning electronic microscope standard substance and its making method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1536345A CN1536345A (en) | 2004-10-13 |
| CN1255669C true CN1255669C (en) | 2006-05-10 |
Family
ID=34320263
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03116182 Expired - Fee Related CN1255669C (en) | 2003-04-04 | 2003-04-04 | Scanning electronic microscope standard substance and its making method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1255669C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102207470A (en) * | 2011-03-16 | 2011-10-05 | 上海市计量测试技术研究院 | Standard substance for calibrating magnification of industrial computed tomography (CT) system |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108445027A (en) * | 2018-03-19 | 2018-08-24 | 广东省新材料研究所 | Fine EBSD characterizations sample of a kind of non-conductive painting/coating of nanometer and preparation method thereof |
| TWI676794B (en) * | 2018-07-10 | 2019-11-11 | 精準基因生物科技股份有限公司 | Sensing device |
| CN113720867B (en) * | 2021-10-11 | 2024-01-30 | 昆明理工大学 | Method for preparing antimony trioxide standard sample of scanning electron microscope |
-
2003
- 2003-04-04 CN CN 03116182 patent/CN1255669C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102207470A (en) * | 2011-03-16 | 2011-10-05 | 上海市计量测试技术研究院 | Standard substance for calibrating magnification of industrial computed tomography (CT) system |
| CN102207470B (en) * | 2011-03-16 | 2013-05-29 | 上海市计量测试技术研究院 | Standard substance for calibrating magnification of industrial computed tomography (CT) system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1536345A (en) | 2004-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| YuG et al. | Molecular resolution imaging of macromolecular crystals by atomic force microscopy | |
| Markiewicz et al. | Atomic force microscope tip deconvolution using calibration arrays | |
| JP2010027743A (en) | Glass substrate for imprint, resist pattern forming method, and method and apparatus for inspecting glass substrate for imprint | |
| CN1255669C (en) | Scanning electronic microscope standard substance and its making method | |
| CN110865058A (en) | Concentration gradient fluorescence calibration sheet of laser microarray chip scanner and calibration method | |
| Wang et al. | Thickness determination of biological samples with a zeta-calibrated scanning tunneling microscope. | |
| CN105277576A (en) | Tem sample mounting geometry | |
| Spieser et al. | Rheology of cellulose nanofibrils and silver nanowires for the development of screen-printed antibacterial surfaces | |
| CN1305100C (en) | Method of measuring performance of scanning electron microscope | |
| Giannazzo et al. | Experimental aspects and modeling for quantitative measurements in scanning capacitance microscopy | |
| CN108017048B (en) | Method for producing semiconductor layer | |
| Guckenberger et al. | Scanning tunnelling microscopy of biomacromolecules | |
| CN117269218A (en) | Characterization method of nanofiber morphology features, measurement device, electronic equipment and storage medium | |
| Kumagai et al. | Development of NMIJ CRM 5207-a tungsten dot-array for the image sharpness evaluation in scanning electron microscopy–structure evaluation and determination of dot-pitch | |
| CN113484545B (en) | Multi-sample carrying net of transmission electron microscope and matched sample preparation table, preparation and use method thereof | |
| CN1245606C (en) | Process for measuring substance length by means of electron microscope | |
| Hiesgen et al. | Problems of roughness measurements using STM | |
| Hiraga et al. | Nanometer scale marker for fluorescent microscopy | |
| DE112021000887T5 (en) | Fluid immersion control for inverted microscopy | |
| Barbet et al. | Scanning tunneling microscopy of colloidal gold beads | |
| CN105115866A (en) | Measurement system and measurement method for particle size of single nano particle | |
| CN104167376A (en) | Testing method of porosity of porous low k material | |
| CN1255850C (en) | Correcting method for astigmatism of scanning electronic microscope | |
| Spallek | Electron microscopy studies on structure-property relationships of nanoparticulate transparent electrodes for printed electronics | |
| US10732166B2 (en) | Method for in-line measurement of quality of microarray |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060510 Termination date: 20110404 |