CN1245606C - Process for measuring substance length by means of electron microscope - Google Patents
Process for measuring substance length by means of electron microscope Download PDFInfo
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- CN1245606C CN1245606C CN 03150837 CN03150837A CN1245606C CN 1245606 C CN1245606 C CN 1245606C CN 03150837 CN03150837 CN 03150837 CN 03150837 A CN03150837 A CN 03150837A CN 1245606 C CN1245606 C CN 1245606C
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000126 substance Substances 0.000 title abstract description 6
- 239000012925 reference material Substances 0.000 claims abstract description 57
- 238000011156 evaluation Methods 0.000 claims abstract description 13
- 238000005259 measurement Methods 0.000 claims description 79
- 238000001000 micrograph Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 abstract description 15
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 2
- 230000000877 morphologic effect Effects 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 5
- 238000006467 substitution reaction Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 201000009310 astigmatism Diseases 0.000 description 2
- 239000010421 standard material Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
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Abstract
The present invention relates to technical fields of material morphological analysis and measuring test, particularly to a method for measuring substance length by an electron microscope. The method has traceability values and uncertainty evaluation. The method comprises the following steps: the electron microscope is calibrated; images of measured materials are shot by the electron microscope; the images of the measured materials are measured; the length values L of the measured materials are calculated. The present invention realizes the evaluation method, the electron microscope measures the length of the materials, certified reference materials are used for calibrating, a microscopic scaleplate on output images of the electron microscope, which is uniquely relevant to the magnification of ultimate images, calibrates the electron microscope in a traceability manner, the calibrated electron microscope shoots images of the materials, the length of the shot materials are measured and calculated, and then, the uncertainty of the length of the materials are given. The measuring values of the measured materials have the traceability and have uncertainty evaluation values by the method, and the present invention changes the state that the measuring values of the existing electron microscopes do not have traceability and uncertainty evaluation at present.
Description
Technical field:
The present invention relates to physical form analysis and metrological testing technology field, especially relate to a kind of have the value of tracing to the source and have uncertainty evaluation, according to the method for certified reference material calibrated electronic microscope measurement of species length.
Background technology:
The internationalization guide was ratified in the 16th meeting at last since the ISO organizational standard material council (REMCO) in 1992, ISO Guide 30:1992 has had clear and definite definition to certified reference material: with the standard substance of certificate, it is a kind of or the multifrequency nature value is definite with the program of having set up traceability, make it to be traceable to the measurement unit that is used to represent this characteristic value of accurate reproduction, and each standard value all has the uncertainty of given confidence level.Drop into a large amount of manpower and financial resources both at home and abroad and carrying out nanotechnology research and industrialization exploration.Comprise the nano-particles size size, chemical analysis, the research of the physicochemical characteristics that phase structure and macroscopical aggregate showed.At present, the method that has the value of tracing to the source and have the electron microscope measurement of species length of uncertainty evaluation still belongs to blank, and this situation has restricted the research of field of nanometer material technology and the development of industrialization greatly.Along with quality certification systems such as ISO9000 series are people's approvals more and more widely, the quality of the products ﹠ services of oneself generally improves in constituent parts enterprise with quality certification system both at home and abroad, and above-mentioned correlated quality guarantee system requires the product specification technical data of authentic unit and other measurement data that the metering traceability will be arranged.
Summary of the invention:
Technical matters to be solved by this invention provide a kind of have the value of tracing to the source and have uncertainty evaluation, according to the method for certified reference material calibrated electronic microscope measurement of species length.The technical scheme that the present invention solves its technical matters employing is: a kind of method according to certified reference material calibrated electronic microscope measurement of species length, and it comprises the steps: a. calibrated electronic microscope; B. take the measured matter image with electron microscope; C. measure the measured matter image; D. calculate the length value L of measured matter, the computing formula of the length value L of described calculating measured matter is L=M * L
X/ M
XX, L is the length value of measured matter in the formula; M is the micro scale calibration value; L
XLength measurements for measured matter; M
XXBe micro scale length measurements on the electron microscope image of measured matter.Task proposed by the invention also can further be realized by following technical solution: 1. described calibrated electronic microscope for putting into certified reference material the position of the placement sample that is calibrated electron microscope; 2. will be calibrated electron microscope and adjust to normal duty; 3. take the document image of certified reference material, and on being calibrated the output device of electron microscope the running parameter of electron microscope during the document image of the document image of the certified reference material that is taken of output and records photographing certified reference material; 4. be used in the length measurements of the certified reference material that is taken on the length metering instrument survey record image in the calibrating term of validity, and be recorded as D
X5. be used in the length measurements of the micro scale on the length metering instrument survey record image in the calibrating term of validity, and be recorded as M
X6. the displayed value with micro scale on the document image is recorded as M
07. calculate the micro scale calibration value M on the document image that is calibrated electron microscope, the computing formula of M is: M=D
0* M
X/ D
X, M is the micro scale calibration value in the formula; D
0Length value for certified reference material; D
XLength measurements for the certified reference material on the document image; M
XLength measurements for the micro scale on the document image; 8. calculate the uncertainty u (M) of the micro scale calibration value that is calibrated electron microscope, the computing formula of u (M) is: u (M)=[u
2(M)]
1/2=[(M
X/ D
X)
2u
2(D
0)+(D
0/ D
X)
2u
2(M
X)+(-D
0M
X/ D
X 2)
2u
2(D
X)]
1/2, u in the formula (M) is the uncertainty of micro scale calibration value; M
XBe the micro scale length measurements on the document image; D
XLength measurements for the certified reference material on the document image; U (D
0) be the uncertainty of certified reference material; D
0Length value for certified reference material; U (M
X) be the uncertainty of the micro scale length measurements on the document image; U (D
X) for the uncertainty of the certified reference material length measurements on the document image, describedly take the measured matter image with electron microscope and adjust to normal duty for the electron microscope that 1. will calibrate in the term of validity; 2. take the measured matter image, and electron microscope image, the described measurement measured matter image of output measured matter is the length measurements of measured matter on the electron microscope image of exporting on the output device of length metering instrument measurement by the electron microscope in the calibration term of validity that 1. is used in the calibrating term of validity on the output device of the electron microscope in the calibration term of validity, and be recorded as L
X2. the length metering instrument that is used in the calibrating term of validity is measured by the micro scale length measurements on the electron microscope image of the measured matter of exporting on the output device of calibrating the electron microscope in the term of validity, and is recorded as M
XXLength value L to measured matter is carried out uncertainty evaluation, and the computing formula of assessment uncertainty u (L) is: u (L)=[(L
X/ M
XX)
2u
2(M)+(M/M
XX)
2u
2(L
X)+(-M * L
X/ M
XX 2)
2u
2(M
XX)]
1/2, u in the formula (L) is the uncertainty of the length value of measured matter; L
XLength measurements for measured matter; M
XXMicro scale length measurements on the electron microscope image of the measured matter of exporting on the output device of the electron microscope in the calibration term of validity of serving as reasons; U (M) is the uncertainty of micro scale calibration value; M is the micro scale calibration value; U (L
X) be the uncertainty of the length measurements of measured matter; U (M
XX) uncertainty of micro scale length measurements on the electron microscope image of the measured matter exported on the output device of the electron microscope of calibration in the term of validity of serving as reasons.Claim 2 of the present invention 1. in the definition of the certified reference material mentioned be the internationalization guide of the last approval of the 16th meeting of the ISO organizational standard material council (REMCO) in 1992, ISOGuide 30:1992 is to the definition of certified reference material: with the standard substance of certificate, it is a kind of or the multifrequency nature value is definite with the program of having set up traceability, make it to be traceable to the measurement unit that is used to represent this characteristic value of accurate reproduction, and each standard value all has the uncertainty of given confidence level.Claim 2 of the present invention 2. in will be calibrated electron microscope and adjust to normal duty and be meant: will be calibrated the electron microscope start; Adjust the running parameter of instrument, as: running parameters such as accelerating potential, enlargement ratio are to the duty that requires; Focus an image to correct; With the astigmatizer cancellation astigmatism that disappears.Claim 2 of the present invention 3. in be calibrated electron microscope output device refer to be calibrated incidental photographic means of electron microscope or all kinds of high resolution printers etc.; The electron microscope image of certified reference material refers to the image film of photographic means shooting or the digital picture of printer prints; The running parameter of electron microscope is meant accelerating potential, enlargement ratio of electron microscope etc.Claim 2 of the present invention 4. in the calibrating term of validity, refer to be measured assay approval and in the measurement verification term of validity of this length metering instrument; The length metering instrument can be tool microscope, vernier caliper, straight steel ruler (150mm) etc.5. the micro scale on the image of claim 2 of the present invention refers to the line segment of the bright length gauge value of a segment mark on the electron microscope document image.The uncertainty u (M) of the micro scale calibration value that 8. is calibrated electron microscope of claim 2 of the present invention is derived by following formula (uncertainty is propagated rule):
u
2(M)＝∑(f/X
i)
2u
2(X
i)
Wherein:
M＝f(D
0，M
X，D
X)＝D
0×M
X/D
X；
f/D
0＝M
X/D
X；
f/M
X＝D
0/D
X；
f/D
X＝-D
0M
X/D
X 2
Because each component is uncorrelated mutually, thereby synthetic variance u
2(M) be: u
2(M)=( f/ D
0)
2u
2(D
0)+( f/ M
X)
2u
2(M
X)+( f/ D
X)
2u
2(D
X)
=(M
X/ D
X)
2u
2(D
0)+(D
0/ D
X)
2u
2(M
X)+(-D
0M
X/ D
X 2)
2u
2(D
X) u (M)=[u
2(M)]
1/2=[(M
X/ D
X)
2u
2(D
0)+(D
0/ D
X)
2u
2(M
X)+(-D
0M
X/ D
X 2)
2u
2(D
X)]
1/2 Claim 3 of the present invention 1. in the electron microscope that will calibrate in the term of validity refer to that the enlargement ratio of this electron microscope is with the certified reference material calibration and in effective service life; Adjusting to normal duty refers to this electron microscope start; Adjust the running parameter of instrument, as: running parameters such as accelerating potential, enlargement ratio are to the duty that calibration value is arranged; Focus an image to correct; With the astigmatizer cancellation astigmatism that disappears.The computing formula of uncertainty u in the claim 6 of the present invention (L) is: u (L)=[u
2(L)]
1/2=[(L
X/ M
XX)
2u
2(M)+(M/M
XX)
2u
2(L
X)+(-M * L
X/ M
XX 2)
2u
2(M
XX)]
1/2Identical with the explanation 8. of claim 2 of the present invention.The present invention since adopt technique scheme realized with electron microscope measurement of species length, use certified reference material calibrate with the enlargement ratio of final image have on unique related electron microscope output image micro scale to electron microscope have the traceability calibration, and the be taken length of material of image, the measurements and calculations of using the electron microscope of calibrating to take material also can provide the uncertainty evaluation method of material length.This method makes the measured value of substances to be measured have traceability and has the uncertainty evaluation value that the measured value that has changed present electron microscope does not have the state of traceability and uncertainty evaluation.
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 the electron microscope image of output certified reference material on the output device that is calibrated scanning electron microscope in the embodiment of the invention.
Fig. 2 is the scanning electron microscope image of measured matter in the embodiment of the invention.
With reference to Fig. 1, Fig. 2: 1 is the length measurements D of certified reference material
X2 is the displayed value M of micro scale
0(its displayed value on document image is 2 μ m); 3 is the length measurements M of the micro scale on the document image
X4 is the length measurements L of measured matter
X5 is the micro scale length measurements M on the electron microscope image of measured matter
XX
Embodiment:
Embodiment: with reference to Fig. 1, Fig. 2.
At first, calibrated electronic microscope.Its step is as follows: 1. certified reference material is put into the placement sample position (on the sample stage) that is calibrated scanning electron microscope; 2. will be calibrated scanning electron microscope and adjust to normal duty; 3. take the image of certified reference material, and at the electron microscope image (Fig. 1) and the microscopical running parameter of recorded electronic that are calibrated output certified reference material on the output device of scanning electron microscope; 4. be used in the length measurements of the certified reference material on length metering instrument (straight steel ruler) the survey record image in the calibrating term of validity, and be recorded as D
X5. be used in the length measurements of the micro scale on the length metering instrument survey record image in the calibrating term of validity, and be recorded as M
X6. write down the displayed value of micro scale, and be recorded as M
0
The calibration value M of micro scale is calculated by following formula:
M＝D
0×M
X/D
X ············(1)
In the formula:
The calibration value of M----micro scale;
D
0The length value of----certified reference material (4.6 μ m: certified reference material manufacturer provides);
M
X----length measurements (supposing to be measured as 16mm) of micro scale on the document image with straight steel ruler;
D
XThe length measurements of----certified reference material (supposing to be measured as 39mm) with straight steel ruler.
Value substitution (1) formula is got: M=D
0* M
X/ D
X=1.89 μ m
The computing formula of uncertainty u (M) that is calibrated the micro scale calibration value of scanning electron microscope is: u (M)=[u
2(M)]
1/2=[(M
X/ D
X)
2u
2(D
0)+(D
0/ D
X)
2u
2(M
X)+(-D
0M
X/ D
X 2)
2u
2(D
X)]
1/2(2)
In the formula:
The uncertainty of u (M)----micro scale calibration value;
M
X----micro scale length measurements (16mm) on the document image;
D
XThe length measurements (39mm) of----certified reference material on the document image;
U (D
0) uncertainty (the 0.05 μ m: the data that the certified reference material certificate provides) of----certified reference material;
D
0The length value of----certified reference material (4.6 μ m: the data that the certified reference material certificate provides);
U (M
X) uncertainty of----micro scale length measurements on the document image;
U (D
X) uncertainty of----certified reference material length measurements on the document image.
Uncertainty u (the D of certified reference material measured value
X) come from two factors.One is the calibration uncertainty u of straight steel ruler
1(C
1) (the determined permission uncertainty of the national metrological verification regulations of straight steel ruler value is 0.1mm), the standard uncertainty u that introduces when another is measured for observing
1(C
2).The uncertainty of introducing when measuring for straight steel ruler is 0.5mm, observes Measurement Uncertainty here and can suppose that obeying rectangle (evenly) distributes, so its standard uncertainty u (C
2) be 0.5mm/3
1/2≈ 0.3mm.Uncertainty u (the D of certified reference material measured value
X) calculate by following formula:
u
2(D
X)＝u
2 1(C
1)+u
2 1(C
2) ·········(3)
Uncertainty u (the M of micro scale length measurements
X) introduce when observe measuring by straight steel ruler equally, can with the uncertainty u (D of certified reference material measured value
X) calculate with quadrat method:
u
2(M
X)＝u
2 2(C
1)+u
2 2(C
2) ·········(4)
U (D with (3) and (4) formula
X) and u (M
X) expression formula substitution (2) formula and value substitution u (M) expression formula of each variable got:
u(M)＝{(M
X/D
X)
2u
2(D
0)+(D
0/D
X)
2[u
2 2(C
1)+u
2 2(C
2)]
+(-D
0M
X/D
X 2)
2[u
2 1(C
1)+u
2 1(C
2)]}
1/2＝0.045μm
Wherein:
M
X＝16mm；D
X＝39mm；u(D
0)＝0.05μm；D
0＝4.6μm；
U
1(C
1)＝0.1mm；U
1(C
2)＝0.3mm；U
2(C
1)＝0.1mm；U
2(C
2)＝0.3mm。
Then, take the measured matter image, the steps include: 1. this scanning electron microscope to be adjusted to normal duty with the scanning electron microscope in the calibration term of validity; 2. take the measured matter image, and on the output device of this scanning electron microscope, export the electron microscope image (Fig. 2) of measured matter.
Secondly, the step of measuring the measured matter image is as follows: the length metering instrument (straight steel ruler) that 1. is used in the calibrating term of validity is measured the length measurements of measured matter on the measured matter image, and is recorded as L
X2. be used in the micro scale length measurements on length metering instrument (straight steel ruler) the measurement measured matter image in the calibrating term of validity, and be recorded as M
XXOnce more, calculate the length value L of measured matter, its computing formula is:
L＝M×L
X/M
XX ··············(5)
In the formula:
The length value of L----measured matter;
The calibration value of M----micro scale (1.89 μ m);
L
XThe length measurements of----measured matter (10 particles of 1 measurement: 41mm);
M
XXMicro scale length measurements (16mm) on----measured matter image.
Value substitution (5) formula is got: L=M * L
X/ M
XX=4.84 μ m
The diameter of each particle=L/10=0.484 μ m
After obtaining to calculate the length value of measured matter, can also carry out uncertainty evaluation.The computing formula of uncertainty u (L) is: u (L)=[(L
X/ M
XX)
2u
2(M)+(M/M
XX)
2u
2(L
X)+(-M * L
X/ M
XX 2)
2u
2(M
XX)]
1/2(6)
In the formula:
The uncertainty of the length value of u (L)----measured matter;
L
XThe length measurements of----measured matter (10 particles of 1 measurement: 41mm);
M
XXMicro scale length measurements (16mm) on----measured matter image;
The uncertainty of the calibration value of u (M)----micro scale (0.045 μ m);
The calibration value of M----micro scale (1.89 μ m);
U (L
X)----measured matter length measurements uncertainty (with calibration example:
[(0.3)
2+(0.1)
2]
1/2≈0.31mm)；
U (M
XX) the uncertainty of micro scale length measurements on----measured matter image
(routine with calibration: [(0.3)
2+ (0.1)
2]
1/2≈ 0.31mm).
With the variable of value substitution (6) formula get measured matter length value (uncertainty of 10 particle diameter length overalls:
u(L)＝[(L
X/M
XX)
2u
2(M)+(M/M
XX)
2u
2(L
X)+(-M×L
X/M
XX 2)
2u
2(M
XX)]
1/2
＝0.15μm
Relative uncertainty=u (the L)/L=3.1% of 10 particle diameter length overalls.
Alleged electron microscope refers in particular to scanning electron microscope and transmission electron microscope among the present invention's " a kind of method according to certified reference material calibrated electronic microscope measurement of species length ".Because of scanning electron microscope and transmission electron microscope are all exported by image the material measurement of length, on the image of output, all there is micro scale to demarcate the enlargement ratio of this image, so come the microscopical enlargement ratio of calibrated electronic to be applicable to scanning electron microscope and transmission electron microscope simultaneously with the method for calibration micro scale.And the method that compares and measures with micro scale and measured matter length is applicable to scanning electron microscope and transmission electron microscope simultaneously.The alleged material of the present invention is with the measuring object of the electron microscope of prior art.Usable range of the present invention is with the electron microscope usable range of prior art.
Claims (5)
1. the method according to certified reference material calibrated electronic microscope measurement of species length is characterized in that it comprises the steps:
A. calibrated electronic microscope;
B. take the measured matter image with electron microscope;
C. measure the measured matter image;
D. calculate the length value L of measured matter, the computing formula of the length value L of described calculating measured matter is L=M * L
X/ M
XX, L is the length value of measured matter in the formula; M is the micro scale calibration value; L
XLength measurements for measured matter; M
XXBe micro scale length measurements on the electron microscope image of measured matter.
2. a kind of method according to certified reference material calibrated electronic microscope measurement of species length according to claim 1 is characterized in that: 1. described calibrated electronic microscope for putting into certified reference material the position of the placement sample that is calibrated electron microscope; 2. will be calibrated electron microscope and adjust to normal duty; 3. take the document image of certified reference material, and on being calibrated the output device of electron microscope the running parameter of electron microscope during the document image of the document image of the certified reference material that is taken of output and records photographing certified reference material; 4. be used in the length measurements of the certified reference material that is taken on the length metering instrument survey record image in the calibrating term of validity, and be recorded as D
X5. be used in the length measurements of the micro scale on the length metering instrument survey record image in the calibrating term of validity, and be recorded as M
X6. the displayed value with micro scale on the document image is recorded as M
07. calculate the micro scale calibration value M on the document image that is calibrated electron microscope, the computing formula of M is: M=D
0* M
X/ D
X, M is the micro scale calibration value in the formula; D
0Length value for certified reference material; D
XLength measurements for the certified reference material on the document image; M
XLength measurements for the micro scale on the document image; 8. calculate the uncertainty u (M) of the micro scale calibration value that is calibrated electron microscope, the computing formula of u (M) is: u (M)=[u
2(M)]
1/2=[(M
X/ D
X)
2u
2(D
0)+(D
0/ D
X)
2u
2(M
X)+(-D
0M
X/ D
X 2)
2u
2(D
X)]
1/2, u in the formula (M) is the uncertainty of micro scale calibration value; M
XBe the micro scale length measurements on the document image; D
XLength measurements for the certified reference material on the document image; U (D
0) be the uncertainty of certified reference material; D
0Length value for certified reference material; U (M
X) be the uncertainty of the micro scale length measurements on the document image; U (D
X) be the uncertainty of the certified reference material length measurements on the document image.
3. a kind of method according to certified reference material calibrated electronic microscope measurement of species length according to claim 1 is characterized in that: described is that the electron microscope that 1. will calibrate in the term of validity is adjusted to normal duty with electron microscope shooting measured matter image; 2. take the measured matter image, and export the electron microscope image of measured matter on the output device of the electron microscope in the calibration term of validity.
4. a kind of method according to claim 1 according to certified reference material calibrated electronic microscope measurement of species length, it is characterized in that: described measurement measured matter image is examined and determine the length measurements of the interior length metering instrument measurement of the term of validity by measured matter on the electron microscope image of exporting on the output device of calibrating the electron microscope in the term of validity for 1. being used in, and is recorded as L
X2. the length metering instrument that is used in the calibrating term of validity is measured by the micro scale length measurements on the electron microscope image of the measured matter of exporting on the output device of calibrating the electron microscope in the term of validity, and is recorded as M
XX
5. a kind of method according to claim 1 according to certified reference material calibrated electronic microscope measurement of species length, it is characterized in that: the length value L to measured matter is carried out uncertainty evaluation, and the computing formula of assessment uncertainty u (L) is: u (L)=[(L
X/ M
XX)
2u
2(M)+(M/M
XX)
2u
2(L
X)+(-M * L
X/ M
XX 2)
2u
2(M
XX)]
1/2, u in the formula (L) is the uncertainty of the length value of measured matter; L
XLength measurements for measured matter; M
XXMicro scale length measurements on the electron microscope image of the measured matter of exporting on the output device of the electron microscope in the calibration term of validity of serving as reasons; U (M) is the uncertainty of micro scale calibration value; M is the micro scale calibration value; U (L
X) be the uncertainty of the length measurements of measured matter; U (M
XX) uncertainty of micro scale length measurements on the electron microscope image of the measured matter exported on the output device of the electron microscope of calibration in the term of validity of serving as reasons.
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|---|---|---|---|
| CN 03150837 CN1245606C (en) | 2003-09-08 | 2003-09-08 | Process for measuring substance length by means of electron microscope |
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|---|---|---|---|
| CN 03150837 CN1245606C (en) | 2003-09-08 | 2003-09-08 | Process for measuring substance length by means of electron microscope |
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| Publication Number | Publication Date |
|---|---|
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| CN1245606C true CN1245606C (en) | 2006-03-15 |
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2003
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101532942B (en) * | 2009-04-24 | 2010-12-01 | 航空工业总公司过滤与分离机械产品质量监督检测中心 | Calibration method of an online oil pollution degree detector |
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