CN103424464A - Automatic measurement method for micron and submicron-grade particle sample in-situ isotope element composition - Google Patents
Automatic measurement method for micron and submicron-grade particle sample in-situ isotope element composition Download PDFInfo
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- CN103424464A CN103424464A CN2013103018322A CN201310301832A CN103424464A CN 103424464 A CN103424464 A CN 103424464A CN 2013103018322 A CN2013103018322 A CN 2013103018322A CN 201310301832 A CN201310301832 A CN 201310301832A CN 103424464 A CN103424464 A CN 103424464A
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Abstract
The invention discloses an automatic measurement method for micron and a submicron-grade particle sample in-situ isotope element composition. The automatic measurement method comprises the following steps: particle samples are uniformly distributed on the surface of a flat conductive carrier; a stepping motor bearing the samples is moved to enable the samples to move to a target area, in which coordinates are arranged in advance; the target area is scanned line by line though primary ion beams, so that a secondary ion image in the target area is obtained; the secondary ion image is input into a secondary ion image processing unit to recognize the information of quantity, positions, outlines and intensity of the particle samples; scanning position, scanning region size and scanning integral time of each particle are obtained through particle sequence analyzing equipment; scanning bombard is performed on each particle, so that a sample secondary ion is obtained; a secondary ion is obtained through a mass spectrum system and a receiving device, and the isotope ratio or element ratio of each particle are finally calculated through a computer.
Description
Technical field
The present invention relates to a kind of micro to submicro particles sample in-situ isotopic element and form method for automatic measurement.
Background technology
The measurement of micro to submicro particles sample in-situ isotopic element, be that the isotopic element that particle to being of a size of several microns or submicron order carries out original position is measured, and it is widely used in the middle of geoscience and environmental science.As the isotope analysis of front solar system particle and the analysis of aerosol particle sulfur isotope etc.It is little that these analyze the size that main characteristics are particulate samples, and the particulate samples number is many.Existing measuring method is that at first the experimenter determines analyzed area substantially by optical camera, and then the moved by hand sample arrives the position of corresponding particle, more directly carries out the measurement of isotopic element ratio.Analyzing like this subject matter is the necessary often manual repeatable operation process of experimenter, and analysis efficiency is low.In addition, because these sample sizes are small, existing analytical approach tends to mistake and analyzes other non-target particles, and its experimental result is inaccurate.
Summary of the invention
In order to solve above technical matters, provide a kind of micro to submicro particles sample in-situ isotopic element to form method for automatic measurement.
Steps of the method are:
The first step: particulate samples is evenly distributed in smooth conductive carrier surface;
Second step: the target area coordinate sequence that provides the required particle scanned;
The 3rd step: the stepper motor that carries sample by movement makes sample move to the target area that has set coordinate in advance.Ion gun produces primary ions and reach sample surfaces after high pressure accelerates, and the voltage deflecting plate deflected ion beam bombardment particulate samples of lining by line scan, obtain the sample secondary ion;
The 4th step: secondary ion is drawn acceleration by high pressure, through after mass spectrometer system, according to the difference between mass number, is separated, and is then received by different receiving traps respectively, thereby obtains the secondary ion image;
The 5th step: the secondary ion image that obtains is input to the secondary ion image processing apparatus, identifies quantity, position, profile and the strength information of particulate samples.These information are stored in calculator memory with sequence form, are called the particle sequence information;
The 6th step: the particle sequence information that previous step obtains is transferred to particle sequential analysis device, and particle sequential analysis device is exported scanning position, the Scanning size of corresponding each particle in the particle sequence and scanned integral time.Successively each particle in the particle sequence is carried out to following operation: deflection primary ions bundle, to scanning position, scans bombardment in scanning area, obtains the sample secondary ion and passes through mass spectrometer system again.Isolate element or the isotope secondary ion of different quality number, received by different receivers, send Computer to and calculate isotopic ratio or element ratios;
The 7th step: the 3rd step to the six steps are repeated in the target area in all target areas coordinate sequence in second step.
Technique effect of the present invention is: this method for automatic measurement can automatic in-situ be measured the element isotope of micron-submicron grade particles, go out particle and then carry out again the element isotope analysis and effectively avoided because mistake is analyzed the experimental result inaccuracy that other non-target particles bring according to the secondary ion image recognition of particle, and the automatical analysis flow process has improved greatly analysis efficiency, reduced experimenter's working strength.
The accompanying drawing explanation
Fig. 1: micro to submicro particles sample in-situ isotopic element forms the method for automatic measurement schematic flow sheet;
Fig. 2: secondary ion image processing apparatus schematic diagram;
Fig. 3: particle sequential analysis device schematic diagram;
Fig. 4: silicon-carbide particle sample element silicon secondary ion image;
Fig. 5: silicon-carbide particle sample element silicon secondary ion image particle recognition.
Embodiment
In order to address the above problem, the invention discloses micro to submicro particles sample in-situ isotopic element and form method for automatic measurement, detailed process is as follows:
(1) particulate samples is evenly distributed in smooth conductive carrier surface, particulate samples need to be placed in to the inertia spreading agent and be prepared into suspending liquid, draw the suspending liquid fluid drips on the conductive carrier surface, the conductive carrier surface can be smooth high-purity goldleaf surface or the single crystal silicon surface through cleaning through cleaning, natural air drying or baking afterwards.
(2) provide the target area coordinate sequence of the required particle scanned.
(3) carry the stepper motor of sample to the scanning area that sets in advance coordinate by movement, ion gun ionizes out primary ions and accelerates bombardment at sample surfaces through high pressure, ion gun can be that Ces Ium Ion Sources can be also the oxonium ion source, voltage deflecting plate deflection primary ions bundle is scanned at sample surfaces line by line, obtains the sample secondary ion.The size of its scanning integral time and scanning area is setting value.
The secondary ion produced in (4) the 3rd steps, after accelerating, high pressure is separated according to the difference between mass number by mass spectrometer system, the ion of the different quality number of separating is received by different receiving traps respectively, and receiving trap can be that electron-multiplier can be also Faraday cup.The signal of receiving trap collection is converted to picture signal to computing machine, produces the secondary ion image, and the secondary ion image of generation stores hard disc of computer into.The strong and weak power that means secondary ion of its picture signal.
(5) the secondary ion image extracted is transferred to the secondary ion image processing apparatus and is processed.Image processing apparatus identifies particle by recognizer, output amounts of particles information, particle position information, and particle outline information and granule strength information, these information are referred to as the particle sequence information, and the particle sequence information file stores in calculator memory.The secondary ion image processing apparatus adopts the method for Threshold segmentation to carry out the identification of particulate samples, the input of secondary ion image processing apparatus comprises: need to carry out the secondary ion image of particle recognition, certain element of threshold decision foundation or isotope (usually getting certain element or isotope that signal value is higher) and artificial setting threshold.At first image processing apparatus judged whether to carry out artificial setting threshold before carrying out the image processing.If carry out artificial setting threshold, image processing apparatus is cut apart according to the artificial threshold value of setting, and extracts the sequence information of particle.If do not carry out artificial setting threshold, to adopt the adaptive thresholding algorithm to carry out threshold calculations be that the threshold value of each pixel is determined by the neighborhood centered by self to image processing apparatus, using average as threshold value, then cut apart, extracted the sequence information of particle.
(6) the particle sequence information passes through export scanning position, the Scanning size of particle sequence and scan integral time after particle sequential analysis device.Successively each particle in the particle sequence is carried out to following operation: deflection primary ions bundle, to scanning position, scans bombardment in scanning area, obtains the sample secondary ion and passes through mass spectrometer system again.Isolate element or the isotope secondary ion of different quality number, received by different receivers, send Computer to and calculate isotopic ratio or element ratios.
(7) the 3rd step to the six steps are repeated in the target area in all target areas coordinate sequence in step (2).
Claims (7)
1. a micro to submicro particles sample in-situ isotopic element forms method for automatic measurement, it is characterized in that, the step of this measuring method is:
The first step: particulate samples is evenly distributed in smooth conductive carrier surface;
Second step: the target area coordinate sequence that provides the required particle scanned;
The 3rd step: the stepper motor that carries sample by movement makes sample move to the target area that has set coordinate in advance, ion gun produces primary ions and reach sample surfaces after high pressure accelerates, the voltage deflecting plate deflected ion beam bombardment particulate samples of lining by line scan, obtain the sample secondary ion;
The 4th step: secondary ion is drawn acceleration by high pressure, through after mass spectrometer system, according to the difference between mass number, is separated, and is then received by different receiving traps respectively, thereby obtains the secondary ion image;
The 5th step: the secondary ion image that obtains is input to the secondary ion image processing apparatus, identifies quantity, position, profile and the strength information of particulate samples;
These information are stored in calculator memory with sequence form, are called the particle sequence information;
The 6th step: the particle sequence information that previous step obtains is transferred to particle sequential analysis device, and particle sequential analysis device is exported scanning position, the Scanning size of corresponding each particle in the particle sequence and scanned integral time;
Successively each particle in the particle sequence is carried out to following operation: deflection primary ions bundle is to scanning position, scan bombardment in scanning area, obtain the sample secondary ion and pass through again mass spectrometer system, isolate element or the isotope secondary ion of different quality number, received by different receivers, send Computer to and calculate isotopic ratio or element ratios;
The 7th step: the 3rd step to the six steps are repeated in the target area in all target areas coordinate sequence in second step.
2. micro to submicro particles sample in-situ isotopic element according to claim 1 forms method for automatic measurement, it is characterized in that, the described first step: particulate samples is prepared into to suspending liquid, draws the suspending liquid fluid drips on the conductive carrier surface, natural air drying or baking afterwards.
3. micro to submicro particles sample in-situ isotopic element according to claim 1 forms method for automatic measurement, it is characterized in that, described the 3rd step comprises: need to carry the stepper motor of sample to the scanning area that sets in advance coordinate by movement, scan again bombardment, and the size of scanning integral time and scanning area is setting value.
4. micro to submicro particles sample in-situ isotopic element according to claim 1 forms method for automatic measurement, it is characterized in that, described the 4th step comprises: the secondary ion produced in the 3rd step, after accelerating, high pressure is separated according to the difference between mass number by mass spectrometer system, the ion of the different quality number of separating is received by different receiving traps respectively, be converted to picture signal to computing machine, produce the secondary ion image, the secondary ion image of generation stores hard disc of computer into.
5. micro to submicro particles sample in-situ isotopic element according to claim 1 forms method for automatic measurement, it is characterized in that, described the 5th step comprises: be transferred to the secondary ion image processing apparatus from the secondary ion image described in the 4th step and processed;
Image processing apparatus identifies particle by recognizer, output amounts of particles information, particle position information, and particle outline information and granule strength information, these information are referred to as the particle sequence information, and the particle sequence information file stores in calculator memory.
6. form method for automatic measurement according to the micro to submicro particles sample in-situ isotopic element described in claim 5, described secondary ion image processing apparatus adopts the method for Threshold segmentation to carry out the identification of particulate samples, the input of secondary ion image processing apparatus comprises: need to carry out the secondary ion image of particle recognition, certain element of threshold decision foundation or isotope and artificial setting threshold;
If carry out artificial setting threshold, image processing apparatus is cut apart according to the artificial threshold value of setting, and extracts the sequence information of particle;
If do not carry out artificial setting threshold, image processing apparatus adopts the adaptive thresholding algorithm to carry out calculated threshold to be cut apart, extract the sequence information of particle.
7. form method for automatic measurement according to the micro to submicro particles sample in-situ isotopic element described in claim 6, described particle sequence information is exported scanning position, the Scanning size of particle sequence and scans integral time by particle sequential analysis device.
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