CN110345889A - A method of utilizing energy spectrum analysis non-destructive testing sample film thickness - Google Patents
A method of utilizing energy spectrum analysis non-destructive testing sample film thickness Download PDFInfo
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- CN110345889A CN110345889A CN201910816128.8A CN201910816128A CN110345889A CN 110345889 A CN110345889 A CN 110345889A CN 201910816128 A CN201910816128 A CN 201910816128A CN 110345889 A CN110345889 A CN 110345889A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
- G01B15/02—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons for measuring thickness
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- Length-Measuring Devices Using Wave Or Particle Radiation (AREA)
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Abstract
The invention discloses a kind of methods using energy spectrum analysis non-destructive testing sample film thickness, using the film layer of heterogeneity in the case where accelerating electron bombardment, the principle of different characteristic X-ray can be excited, acceleration electron bombardment is carried out to mark block, the corresponding relationship standard curve between film layer characteristic element and film thickness is made, the intensity and frequency for carrying out the X-ray obtained after acceleration electron bombardment to sample to be tested is then analyzed, obtains the content of element, contrast standard curve, calculates thicknesses of layers.The present invention is only with common scanning electron microscope and energy disperse spectroscopy, it is put into without the additional special ancillary equipment of detection and accessory, it is at low cost and easy to operate, suitable in nanometer and micron range, inorganic non-metallic, macromolecule and all kinds of film layers of metal, the film thickness for being suitable for single layer, bilayer and sandwich diaphragm layer simultaneously detects, applied widely, and will not damage to sample.
Description
Technical field
The present invention relates to film thickness detection technique fields more particularly to a kind of using energy spectrum analysis non-destructive testing sample film thickness
Method.
Background technique
Currently, in actual production and life, to guarantee product is stable, long-term effective use, it usually needs to material into
Row surface covering treatment, such as anodic oxidation, spray painting, plating/chemical plating, PVD/CVD.The common function of these surface cover layers
Can have appearance beautification, improve Wear Resistance, improve product resistance to corrosion, change product electromagnetic performance etc..
For the normal realization for guaranteeing film layer function, it need to guarantee that film layer has certain thickness.Common film thickness detection method
There are microtomy, coulomb method, method of magnetic, x-ray method, β ray method etc..Wherein, microtomy and coulomb are owned by France in destructiveness detection, right
Test sample has damage, and method of magnetic is only applicable to the detection of magnetic material thicknesses of layers, and x-ray method is only used for metal and part is moulded
The detection of metal composition of layer in gum base materials, β ray method be similar to x-ray method, but radiate it is relatively large, it is used at present increasingly
It is few.The above detection method is typically necessary additional special detection ancillary equipment, and application range is small.
Summary of the invention
The object of the present invention is to provide a kind of methods using energy spectrum analysis non-destructive testing sample film thickness, can be used in nanometer
And in micro-scaled range, inorganic non-metallic, macromolecule and all kinds of film layers of metal, the film of single layer, bilayer or sandwich diaphragm layer
Thickness detection, it is easy to operate without additional detection ancillary equipment, and to sample nondestructive, it is applied widely.
The technical solution adopted by the present invention are as follows: a method of using energy spectrum analysis non-destructive testing sample film thickness, including such as
Lower step:
A. prepare mark block, scanning electron microscope and the energy of several different film thickness and film thickness all in nanoscale to micro-scaled range
Spectrometer, the mark block and sample to be tested are substance of the same race；
B. using specifying the acceleration electronics of running parameter to bombard all mark blocks respectively in scanning electron microscope, power spectrum letter is generated
Number, i.e., characteristic X-ray, the detector of energy disperse spectroscopy receive its signal and analyze the content of each component of film layer on bid block；
C. according to the content of the obtained different components of the mark block of different film thickness, containing for a main feature element is chosen
Amount, obtains the corresponding relationship between film thickness and film layer main feature constituent content, makes standard curve, and by corresponding relationship and mark
Directrix curve is recorded in database；
D. acceleration electron bombardment specimen surface identical with above-mentioned running parameter is used, energy spectrum signal, the detection of energy disperse spectroscopy are generated
Device receives its signal and analyzes the content of each component；
E. according to the content of each component measured, element identical with above-mentioned main feature element is chosen, by its content pair
Sighting target directrix curve obtains the film thickness of sample.
Preferably, in the step a, mark block with a thickness of 1nm-5 μm.
Preferably, in the step a, mark block is no less than 3.
Preferably, in the step b, assigned work parameter includes electron accelerating voltage 5KV-30KV, operating distance
5mm-30mm, 30 times -30 ten thousand times of image magnification and energy-spectrum scanning time 5s-150s.
The beneficial effects of the present invention are: the present invention utilizes the film layer of heterogeneity in the case where accelerating electron bombardment, can excite not
With the principle of characteristic X-ray, acceleration electron bombardment is carried out to mark block, makes the corresponding pass between film layer characteristic element and film thickness
It is standard curve, then analyzes the intensity and frequency for carrying out the X-ray obtained after acceleration electron bombardment to sample to be tested, obtain member
The content of element, contrast standard curve calculate thicknesses of layers.This method is suitable in nanometer and micron range, inorganic non-metallic,
Macromolecule and all kinds of film layers of metal, while the film thickness for being suitable for single layer, bilayer and sandwich diaphragm layer detects, and is swept using common
Electron microscope and energy disperse spectroscopy are retouched, is put into without additional accessory, it is easy to operate and bad to sample nondestructive, it is applied widely.
Detailed description of the invention
Fig. 1 is flow chart of the invention；
Fig. 2 is that sample characteristics X-ray of the present invention generates process schematic；
Fig. 3 is fine aluminium specimen surface anodic oxidation film thickness testing standard curve synoptic diagram of the present invention；
Fig. 4 is epoxy resin coating thickness testing standard curve synoptic diagram in low-Carbon steel specimen surface of the present invention；
Fig. 5 is pure copper samples surface gold-plating thickness degree testing standard curve synoptic diagram of the present invention；
Fig. 6 is pure copper samples plating nickel on surface plated thickness testing standard curve synoptic diagram of the present invention.
In figure: accelerating electronics 1, sample 2, characteristic X-ray 3, detector 4.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.Based on the embodiments of the present invention, those of ordinary skill in the art institute without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
As shown in Figure 1, the present invention includes the following steps:
A. prepare mark block, scanning electron microscope and the energy of several different film thickness and film thickness all in nanoscale to micro-scaled range
Spectrometer, the mark block and sample to be tested are substance of the same race, i.e. the film layer of mark block and the film layer of sample to be tested is substance of the same race, area
It is not only that the thickness of film layer is different, film thickness can be confirmed by microtomy, when choosing mark block, the thickness of the mark block of selection
For 1nm-5 μm and no less than three；
B. using specifying the acceleration electronics 1 of running parameter to bombard all mark blocks respectively in scanning electron microscope, power spectrum letter is generated
Number, i.e. characteristic X-ray 3, the detector 4 of energy disperse spectroscopy receives its signal and analyzes containing for each component of film layer on bid block
Amount, use process is as shown in Fig. 2, the running parameter used are as follows: electron accelerating voltage 5KV-30KV, generally selection 15KV, work
Make distance 5mm-30mm, generally selection 15mm, 30 times -30 ten thousand times of image magnification, in practical operation, selected multiple is answered
Comprising nominative testing region, energy-spectrum scanning time 5s-150s, the sweep time of selection, which requires to obtain enough characteristic X-rays 3, to be obtained
Rate is taken, to ensure the precision detected；
C. according to the content of the obtained different components of the mark block of different film thickness, containing for a main feature element is chosen
Amount, obtains the corresponding relationship between film thickness and film layer main feature constituent content, makes standard curve, mark block is more, resulting
Standard curve is more accurate, specifically, using the content of the main feature element of selection as abscissa, using film thickness as ordinate,
Standard curve is made, and corresponding relationship and standard curve are recorded in database；
D. it uses acceleration electronics 1 identical with above-mentioned running parameter to bombard 2 surface of sample, generates energy spectrum signal, the inspection of energy disperse spectroscopy
Device 4 is surveyed to receive its signal and analyze the content of each component；
E. according to the content of each component measured, element identical with above-mentioned main feature element is chosen, by its content pair
Sighting target directrix curve obtains the film thickness of sample, can be obtained by manually computing corresponding relationship, also can be automatic by being preprogramed template
It is calculated.
In the step b, film layer is one of inorganic non-metallic, macromolecule and metallic diaphragm or a variety of compound.
In the step b, film layer is single layer, bilayer or sandwich diaphragm layer, but it includes different for requiring each tunic layer
Main feature element, these elements can generate respective characteristic X-ray 3.
Technical solution of the present invention is further discussed in detail with reference to embodiments:
Embodiment 1
The thickness of fine aluminium specimen surface anode oxide film is tested, is the application of field of inorganic nonmetal, and is single layer film layer.It is grasped
It is as follows to make process:
A. prepare scanning electron microscope, energy disperse spectroscopy, several fine aluminium mark blocks with anode oxide film film layer, and these mark blocks
Thicknesses of layers is all in 1nm-5 μ m and film thickness is all different, mark block can pass through change anodic process parameter preparation, film
Thickness can confirm that the mark block of selection is no less than three by eddy-current method or ball-milling method；
B. the acceleration electronics 1 of running parameter is specified to bombard all mark blocks respectively using in scanning electron microscope, in characteristic X-ray
Excites scope in generate 3 signal of characteristic X-ray, the detector 4 of energy disperse spectroscopy receives its signal and simultaneously analyzes the strong of characteristic X-ray 3
Degree and frequency obtain the content of each component of film layer on mark block, and use process is as shown in Fig. 2, with thicknesses of layers
Increase, 3 intensity of characteristic X-ray of film layer corresponding element will increase, and be presented as that constituent content increases, the running parameter of use are as follows:
Electron accelerating voltage 15KV, operating distance 15mm, 150 times of image magnification, energy-spectrum scanning time 35s；
C. according to the content of the obtained different components of the mark block of different film thickness, containing for anode characteristic element O element is chosen
Amount, obtains the corresponding relationship between the film thickness of anode oxide film and O constituent content, makes standard curve, mark block is more, resulting
Standard curve is more accurate, specifically, using the content of the O element of selection as abscissa, using the film thickness of anode oxide film as vertical
Coordinate as shown in figure 3, making standard curve, and corresponding relationship and standard curve is recorded in database；
D. acceleration electronics 1 identical with above-mentioned running parameter is used to bombard the table of the fine aluminium sample with anode oxide film film layer
Face, generates energy spectrum signal, and the detector 4 of energy disperse spectroscopy receives its signal and analyzes the content of each component；
E. according to the content of each component measured, the content of selection O element and by its content reference standard curve, sun is obtained
The thickness of pole oxidation film can be obtained by manually computing corresponding relationship, can be also calculated automatically by being preprogramed template.
Embodiment 2
The epoxy resin coating thickness on low-Carbon steel specimen surface is tested, is the application of the field of polymers.Its operating procedure and above-mentioned step
Rapid essentially identical, specific difference is: the mark block of selection is the mild steel coated with epoxy resin coating, and mark block can pass through change
The preparation of lacquer spraying technique parameter, specific film thickness can be confirmed using benching tunnelling method；The scanning electron chosen when test mark block film layer content is aobvious
The running parameter of micro mirror is acceleration voltage 15KV, operating distance 15mm, 50 times of amplification factor, energy-spectrum scanning time 45s, test
Obtain mark block on film layer each component content, the content of selected characteristic Elements C element and make react its content with
The standard curve of film thickness corresponding relationship, as shown in figure 4, specimen surface is then bombarded using the acceleration electronics 1 of identical running parameter,
3 signal of characteristic X-ray is generated in the excites scope of characteristic X-ray, analyzes the intensity and frequency of characteristic X-ray 3, obtains C member
The content of element, comparative diagram 4 obtain the thickness of epoxy resin coating.
Embodiment 3
Pure copper samples plating nickel on surface plated thickness is tested, Au is superficial film, and Ni is bottom film layer, for answering for metal field
With, and film layer is the double-deck film layer.Its operating procedure and above-mentioned steps are essentially identical, and specific difference is: choosing have first
The fine copper mark block of the gold-plated film layer of nickel plating, mark block are no less than three, and mark block can be tested by Hull slot and be prepared, and specific film thickness can use
Microtomy confirmation；The running parameter for the scanning electron microscope chosen when test mark block film layer content are as follows: acceleration voltage 15KV, work
Make distance 15mm, 300 times of amplification factor, energy-spectrum scanning time 50s, according to 3 signal of characteristic X-ray that test obtains, analysis is special
The intensity and frequency for levying X-ray 3, obtain the content of Au, Ni element, and content and the film layer for then first making superficial film Au are thick
The corresponding relationship standard curve of degree, as shown in figure 5, then test Ni content and Ni thicknesses of layers relationship when, this experiment
It chooses the thicknesses of layers of Au respectively to be tested for 0.01 μm, 0.05 μm, 0.4 μm of three numerical value as three groups, every group of mark block
The thickness for being no less than three and Ni layers of plating is all different, and it is respectively 0.01 μm, 0.05 μ that similarly test, which obtains the thicknesses of layers of Au,
M, 0.4 μm when Ni content and Ni thickness degree corresponding relationship standard curve, as shown in Figure 6.Then identical running parameter is used
Acceleration electronics 1 bombard specimen surface, comparative diagram 5 and Fig. 6 obtain the thickness of nickel plating Gold plated Layer.
The present invention, in the case where accelerating electron bombardment, can excite the principle of different characteristic X-ray using the film layer of heterogeneity, right
Mark block carries out acceleration electron bombardment, and with the increase of thicknesses of layers, the characteristic X ray strength of film layer corresponding element will increase, i.e.,
It is presented as that constituent content increases, and then makes the corresponding relationship standard curve between film layer characteristic element and film thickness, then divide
Analysis carries out the intensity and frequency of the X-ray obtained after acceleration electron bombardment to sample to be tested, obtains the content of element, contrast standard
Curve calculates thicknesses of layers.The present invention is special without additional detection only with common scanning electron microscope and energy disperse spectroscopy
Ancillary equipment processed and accessory investment, it is at low cost and easy to operate, it is suitable in nanometer and micron range, inorganic non-metallic, high score
Son and all kinds of film layers of metal, while the film thickness for being suitable for single layer, bilayer and sandwich diaphragm layer detects, it is applied widely, and not
Sample can be damaged.
Claims (4)
1. a kind of method using energy spectrum analysis non-destructive testing sample film thickness, which comprises the steps of:
A. prepare several groups of difference film thickness and mark block, scanning electron microscope and energy of the film thickness all in nanoscale to micro-scaled range
Spectrometer, the mark block and sample to be tested are substance of the same race；
B. using specifying the acceleration electronics of running parameter to bombard all mark blocks respectively in scanning electron microscope, power spectrum letter is generated
Number, i.e., characteristic X-ray, the detector of energy disperse spectroscopy receive its signal and analyze the content of each component of film layer on bid block；
C. according to the content of the obtained different components of the mark block of different film thickness, containing for a main feature element is chosen
Amount, obtains the corresponding relationship between film thickness and film layer main feature constituent content, makes standard curve, and by corresponding relationship and mark
Directrix curve is recorded in database；
D. acceleration electron bombardment specimen surface identical with above-mentioned running parameter is used, energy spectrum signal, the detection of energy disperse spectroscopy are generated
Device receives its signal and analyzes the content of each component；
E. according to the content of each component measured, element identical with above-mentioned main feature element is chosen, by its content pair
Sighting target directrix curve obtains the film thickness of sample.
2. the method according to claim 1 using energy spectrum analysis non-destructive testing sample film thickness, it is characterised in that: described
In step a, mark block with a thickness of 1nm-5 μm.
3. the method according to claim 1 using energy spectrum analysis non-destructive testing sample film thickness, it is characterised in that: described
In step a, mark block is no less than 3 groups.
4. the method according to claim 1 using energy spectrum analysis non-destructive testing sample film thickness, it is characterised in that: described
In step b, assigned work parameter includes electron accelerating voltage 5KV-30KV, operating distance 5mm-30mm, image magnification 30
- 30 ten thousand times and energy-spectrum scanning time 5s-150s again.
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| CN110763716A (en) * | 2019-11-12 | 2020-02-07 | 长江存储科技有限责任公司 | Test method and device |
| CN113218344A (en) * | 2020-02-04 | 2021-08-06 | 本田技研工业株式会社 | Method for inspecting membrane electrode structure |
| CN115356365A (en) * | 2022-10-18 | 2022-11-18 | 胜科纳米(苏州)股份有限公司 | Method for determining acceleration voltage in X-ray energy spectrum analysis and energy spectrum analysis method |
| CN115466953A (en) * | 2022-10-11 | 2022-12-13 | 郑煤机智鼎液压有限公司 | Laser cladding layer thickness detection method |
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| CN109556541A (en) * | 2019-01-14 | 2019-04-02 | 汪诚 | A kind of metal surface alloying layer thickness non-destructive testing device and method based on X-ray |
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| CN101133300A (en) * | 2005-09-26 | 2008-02-27 | 杰富意钢铁株式会社 | Method for measuring surface layer oxide film thickness of galvanized steel plate |
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