CN103424464B - A kind of micro to submicro particles sample in-situ isotopic element composition method for automatic measurement - Google Patents
A kind of micro to submicro particles sample in-situ isotopic element composition method for automatic measurement Download PDFInfo
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- CN103424464B CN103424464B CN201310301832.2A CN201310301832A CN103424464B CN 103424464 B CN103424464 B CN 103424464B CN 201310301832 A CN201310301832 A CN 201310301832A CN 103424464 B CN103424464 B CN 103424464B
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Abstract
The invention discloses a kind of micro to submicro particles sample in-situ isotopic element composition method for automatic measurement, the steps include: that particulate samples is evenly distributed in planar conductive carrier surface; Sample is made to move to the target area having set coordinate in advance by the stepper motor of mobile carrying sample.Adopt primary ions bundle to line by line scan target area, obtain the secondary ion image of target area.The secondary ion image that obtains is input to secondary ion image processing apparatus, identifies the quantity of particulate samples, position, profile and strength information.Obtain scanning position, the Scanning size of each particle through particle sequence analytical equipment again and scan integral time.In the enterprising line scanning bombardment of each particle, obtain sample secondary ion.Secondary ion is through mass spectrometer system, and receiving trap, is finally calculated isotopic ratio or the element ratios of each particle by computing machine.
Description
Technical field
The present invention relates to a kind of micro to submicro particles sample in-situ isotopic element composition method for automatic measurement.
Background technology
The measurement of micro to submicro particles sample in-situ isotopic element, be the isotopic element measurement particle being of a size of several microns or submicron order being carried out to original position, 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.These analyze main feature is that the size of particulate samples is little, and particulate samples number is many.Existing measuring method be experimenter first by optical camera determination general analysis region, then moved by hand sample is to the position of corresponding particle, more directly carries out the measurement of isotopic element ratio.Such analysis subject matter is experimenter's constantly manual repeatable operation process, and analysis efficiency is low.In addition, because these sample sizes are small, existing analytical approach often analyzes other non-targeted particles by mistake, 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 composition method for automatic measurement.
Steps of the method are:
The first step: particulate samples is evenly distributed in planar conductive carrier surface;
Second step: the target area coordinates sequence of carrying out the particle scanned required for providing;
3rd step: make sample move to the target area having set coordinate in advance by the stepper motor of mobile carrying sample.Ion gun produces primary ions and reach sample surfaces after high pressure accelerates, and voltage deflection plate deflected ion beam is lined by line scan bombardment particulate samples, obtains sample secondary ion;
4th step: secondary ion is drawn by high pressure and accelerated, and is separated, is then received by different receiving trap respectively after mass spectrometer system according to the difference between mass number, thus obtains secondary ion image;
5th step: the secondary ion image that obtains is input to secondary ion image processing apparatus, identifies the quantity of particulate samples, position, profile and strength information.These information are stored in calculator memory with sequence form, are called particle sequence information;
6th step: the particle sequence information transmission that previous step obtains is to particle sequence analytical equipment, and particle sequence analytical equipment exports scanning position, the Scanning size of each particle corresponding in particle sequence and scans integral time.Successively following operation is carried out to particle each in particle sequence: deflection primary ions bundle, to scanning position, carries out scanning bombardment in scanning area, obtains sample secondary ion and passes through mass spectrometer system again.Isolate element or the isotope secondary ion of different quality number, received by different receiver, send Computer to and calculate isotopic ratio or element ratios;
7th step: the 3rd step is repeated to the 6th step to the target area in target area coordinates sequences all in second step.
Technique effect of the present invention is: this method for automatic measurement can measure the elemental isotope of micron-submicron grade particles by automatic in-situ, go out particle according to the secondary ion image recognition of particle and then carry out elemental isotope analysis again and effectively avoid the experimental result inaccuracy brought owing to analyzing other non-targeted particles by mistake, and automatical analysis flow process improves analysis efficiency greatly, reduces experimenter's working strength.
Accompanying drawing explanation
Fig. 1: micro to submicro particles sample in-situ isotopic element composition method for automatic measurement schematic flow sheet;
Fig. 2: secondary ion image processing apparatus schematic diagram;
Fig. 3: particle sequence analytical equipment schematic diagram;
Fig. 4: silicon-carbide particle sample element silicon secondary ion image;
Fig. 5: silicon-carbide particle sample element silicon secondary ion imaged particles identification.
Embodiment
In order to solve the problem, the invention discloses micro to submicro particles sample in-situ isotopic element composition method for automatic measurement, detailed process is as follows:
(1) particulate samples is evenly distributed in planar conductive carrier surface, need particulate samples to be placed in inertia spreading agent and be prepared into suspending liquid, draw suspending liquid and drop in conductive carrier surface, conductive carrier surface can be through smooth high-purity goldleaf surface of cleaning or the single crystal silicon surface through cleaning, natural air drying or baking afterwards.
(2) provide required for carry out the target area coordinates sequence of the particle scanned.
(3) by moving the stepper motor of carrying sample to the scanning area setting coordinate in advance, ion gun ionizes out primary ions and accelerates bombardment at sample surfaces through high pressure, ion gun can be Ces Ium Ion Sources also can be oxonium ion source, voltage deflection plate deflection primary ions bundle scans at sample surfaces line by line, obtains 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, be separated according to the difference between mass number by mass spectrometer system after high pressure accelerates, the ion of the different quality number separated is received by different receiving traps respectively, and receiving trap can be electron-multiplier also can be Faraday cup.The signal of receiving trap collection is converted to picture signal to computing machine, and produce secondary ion image, the secondary ion image of generation is stored into hard disc of computer.Its picture signal power represents the power of secondary ion.
(5) the secondary ion image extracted is transferred to secondary ion image processing apparatus and processes.Image processing apparatus identifies particle by recognizer, and export amounts of particles information, particle position information, particle outline information and granule strength information, these information are referred to as particle sequence information, and particle sequence message file is stored in calculator memory.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 the secondary ion image carrying out particle recognition, certain element of threshold decision foundation or isotope (usually getting certain higher element of signal value or isotope) and manually set threshold value.First image processing apparatus judged whether manually to set threshold value before carrying out image procossing.If manually set threshold value, then image processing apparatus is split according to the threshold value of artificial setting, extracts the sequence information of particle.If manually do not set threshold value, the threshold value that then image processing apparatus adopts adaptive thresholding algorithm to carry out threshold calculations and each pixel is determined by the neighborhood centered by self, using average as threshold value, then split, extract the sequence information of particle.
(6) particle sequence information is by exporting scanning position, the Scanning size of particle sequence and scanning integral time after particle sequence analytical equipment.Successively following operation is carried out to particle each in particle sequence: deflection primary ions bundle, to scanning position, carries out scanning bombardment in scanning area, obtains sample secondary ion and passes through mass spectrometer system again.Isolate element or the isotope secondary ion of different quality number, received by different receiver, send Computer to and calculate isotopic ratio or element ratios.
(7) the 3rd step is repeated to the 6th step to the target area in target area coordinates sequences all in step (2).
Claims (3)
1. a micro to submicro particles sample in-situ isotopic element composition method for automatic measurement, it is characterized in that, the step of this measuring method is:
The first step: particulate samples is placed in inertia spreading agent and is prepared into suspending liquid, draw suspending liquid and drop in conductive carrier surface, surperficial or through cleaning the single crystal silicon of smooth high-purity goldleaf that cleaning is passed through on conductive carrier surface is surperficial, natural air drying or baking afterwards;
Second step: the target area coordinates sequence of carrying out the particle scanned required for providing;
3rd step: make sample move to the target area having set coordinate in advance by the stepper motor of mobile carrying sample, ion gun produces primary ions and reach sample surfaces after high pressure accelerates, voltage deflection plate deflected ion beam is lined by line scan bombardment particulate samples, obtains sample secondary ion;
4th step: secondary ion is drawn by high pressure and accelerated, and is separated, is then received by different receiving trap respectively, be converted to picture signal to computing machine after mass spectrometer system according to the difference between mass number, produces secondary ion image;
5th step: the secondary ion image described in the 4th step is transferred to secondary ion image processing apparatus and processes;
Secondary ion image processing apparatus identifies particle by recognizer, export amounts of particles information, particle position information, particle outline information and granule strength information, these information are referred to as particle sequence information, and particle sequence message file is stored in calculator memory;
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 the secondary ion image carrying out particle recognition, certain element that the signal value of threshold decision foundation is higher or isotope and adopt the threshold value of artificial setting;
First image processing apparatus judged whether manually to set threshold value before carrying out image procossing;
If manually set threshold value, then image processing apparatus is split according to the threshold value of artificial setting, extracts the sequence information of particle;
If manually do not set threshold value, then image processing apparatus adopts adaptive thresholding algorithm to carry out calculated threshold to split, and namely the threshold value of each pixel is determined by the neighborhood centered by self, average is extracted the sequence information of particle as threshold value; These information are stored in calculator memory with sequence form, are called particle sequence information;
6th step: the particle sequence information transmission that previous step obtains is to particle sequence analytical equipment, and particle sequence analytical equipment exports scanning position, the Scanning size of each particle corresponding in particle sequence and scans integral time; Successively following operation is carried out to particle each in particle sequence: deflection primary ions bundle is to scanning position, scanning bombardment is carried out in scanning area, obtain sample secondary ion and pass through mass spectrometer system again, isolate element or the isotope secondary ion of different quality number, received by different receiver, send Computer to and calculate isotopic ratio or element ratios;
7th step: the 3rd step is repeated to the 6th step to the target area in target area coordinates sequences all in second step.
2. micro to submicro particles sample in-situ isotopic element composition method for automatic measurement according to claim 1, it is characterized in that, described 3rd step comprises: need to carry the stepper motor of sample to the scanning area setting coordinate in advance by movement, then carry out scanning bombardment; And the size scanning integral time and scanning area is setting value.
3. micro to submicro particles sample in-situ isotopic element composition method for automatic measurement according to claim 1, it is characterized in that, described 4th step comprises: the secondary ion produced in the 3rd step, be separated according to the difference between mass number by mass spectrometer system after high pressure accelerates, the ion of the different quality number separated is received by different receiving traps respectively, be converted to picture signal to computing machine, produce secondary ion image, the secondary ion image of generation is stored into hard disc of computer.
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