CN105548333A - Method for analyzing content and distribution of Cr in Cr-doped zinc sulfide crystalline material - Google Patents
Method for analyzing content and distribution of Cr in Cr-doped zinc sulfide crystalline material Download PDFInfo
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- CN105548333A CN105548333A CN201610049491.8A CN201610049491A CN105548333A CN 105548333 A CN105548333 A CN 105548333A CN 201610049491 A CN201610049491 A CN 201610049491A CN 105548333 A CN105548333 A CN 105548333A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
- G01N27/628—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas and a beam of energy, e.g. laser enhanced ionisation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
The invention relates to a method for analyzing the content and distribution of Cr in a Cr-doped zinc sulfide crystalline material. According to the method, laser denudation inductively coupled plasma massspectrometry is utilized for analyzing the content and distribution of Cr in the Cr-doped zinc sulfide crystalline material. The method comprises the step that 1, the surface of a ZnS matrix material is plated with a Cr film to prepare a plurality of Cr:ZnS solid standard substances with different Cr contents, wherein Cr is evenly distributed in the Cr:ZnS solid standard substances; 2, the contents of Cr in the solid standard substances are obtained through inductively coupled plasma atomic emission spectrometry or the inductively coupled plasma massspectrometry, the response signal strength of Cr in the solid standard substances is measured through the laser denudation inductively coupled plasma massspectrometry, and a Cr standard work curve is drawn; 3, laser denudation inductively coupled plasma mass spectrometric detection is carried out on a Cr-doped zinc sulfide crystalline material sample to be detected, and the content and distribution of Cr in the sample to be detected are obtained.
Description
Technical field
The invention belongs to analytical chemistry field, relate to laser ablation-inductivity coupled plasma mass spectrometry analytical approach that Cr content and distribution in Cr zinc sulphide (Cr:ZnS) crystalline material are mixed in a kind of solid sampling analysis.
Background technology
As tunable middle infrared solid laser material at normal temperatures, Cr:ZnS crystalline material has a wide range of applications in fields such as environmental monitoring, atmospheric remote sensing, medical treatment, laser communications.The content of doped chemical Cr and homogeneity thereof evaluate the important indicator of crystal property.Doped chemical in material preparation process uneven/gradient distribution is the major issue prepared of puzzlement material always, therefore Accurate Determining Cr Content and distribution situation to crystal preparation and performance evaluation significant.At present, Cr doping content measures main employing inductively coupled plasma atomic absorption spectrum (ICP-AES) method and near-infrared absorption spectrum method.The average content of what these two kinds of methods measured is all Cr in sample, because of cannot the homogeneity of characterizing sample, therefore affects the accuracy of measurement result.And ICP-AES method needs pre-service solid sample to be cleared up into solution just can measure.
Laser ablation inductive coupling plasma mass spectrometry (LA-ICP-MS) technology has been one of most process useful of Elemental Composition cloth and isotope analysis in modern solid material.Method adopts Direct solid sampling analysis, there is no loaded down with trivial details sample pretreatment and complicated data handling procedure, and sample is almost harmless, can be used for holistic approach and the micro-zone in situ analysis of sample, obtain the element constitution and distribution information of a certain ad-hoc location.What the physical chemical differences due to sample affected laser degrades behavior, and Correction Problems is the difficult point of LA-ICP-MS method accurate quantitative analysis always.Solid etalon physical development is relatively slow, is difficult to find the standard substance mated with solid sample matrix phase completely.The solid etalon material of self-control Matrix Match, reduces matrix effect and the impact of element fractionation effect, becomes the important method realizing LA-ICP-MS quantitative test.
Summary of the invention
For overcoming the loaded down with trivial details pollution consuming time, easy of Chemical Pretreatment process, the shortcomings such as Elemental redistribution information cannot being provided, the invention provides the laser ablation-inductivity coupled plasma mass spectrometry analytical approach of the quantitative and distribution of doped chemical Cr in a kind of practicable Cr:ZnS crystalline material.
At this, the invention provides and a kind ofly mix the content of Cr and the analytical approach of distribution in Cr zinc sulfide crystal material, described method utilizes the analysis of laser ablation inductively coupled plasma-mass spectrometry method to mix content and the distribution of Cr in Cr zinc sulfide crystal material, and described method comprises:
1) plate Cr film to prepare the different Cr:ZnS solid etalon material of some Cr content at ZnS host surface, wherein, Cr is uniformly distributed in Cr:ZnS solid etalon material;
2) content of Cr in described solid etalon material is obtained by ICP-AES or inductively coupled plasma mass spectrometry, adopt laser ablation inductively coupled plasma-mass spectrometry method to measure the response signal intensity of Cr in described solid etalon material, draw Cr standard working curve;
3) laser ablation inductively coupled plasma-mass spectrometry mensuration is carried out to the Cr of mixing zinc sulfide crystal material sample to be measured, according to standard working curve, obtain content and distribution of mixing Cr in Cr zinc sulfide crystal material sample to be measured.
Method of the present invention is by the Cr:ZnS solid etalon material of self-control Matrix Match, laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) the overall homogeneity to solid etalon material is adopted to characterize, inductively coupled plasma spectrometry method (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS) measure Cr in solid etalon substance solution, in conjunction with the Cr element response signal intensity of LA-ICP-MS and the Cr content of mensuration, draw Cr standard working curve, direct solid analysis is to be measured mixes Cr content and distribution thereof in Cr zinc sulfide crystal material.Method of the present invention adopts direct solid sample introduction analysis, without the need to decomposing sample, effectively prevent loaded down with trivial details sample pretreatment process and the contamination that may exist or loss.By making the Cr:ZnS solid etalon material of Matrix Match by oneself, realize accurate quantitative analysis.In conjunction with high sensitivity and the laser ablation micrometer resolution of inductivity coupled plasma mass spectrometry, this method can be used for the micro-zone in situ analysis of the quantitative and distribution of trace doped element in laser material ZnS crystal, and the controllable growth for doped crystal provides effective means of numerical analysis.
In the present invention, prepare described solid etalon material and comprise: obtain ZnS host material by CVD (Chemical Vapor Deposition) method growth; Even, the fine and close Cr film of thickness is plated at ZnS host surface by Magnetic filter ion plating method; At vacuum seal (<10
-1pa) spread plating the ZnS host material after Cr film more than 14 days at 950 DEG C in quartz ampoule, diffusion terminates rear sanding and polishing, obtains described solid etalon material.
Preferably, described solid etalon material is at least 3, and Cr is evenly distributed in Cr:ZnS solid etalon material.
Preferably, step 2) comprising: obtain solution with solid etalon material described in aqua regia dissolution, measure Cr concentration in described solution by ICP-AES or inductively coupled plasma mass spectrometry, calculate the content of Cr in solid etalon material.The solid etalon substance weight that can take about (0.01g ~ 0.1g), adds 3ml chloroazotic acid, and it is for subsequent use that rear constant volume is dissolved in low-temperature heat on electric hot plate (60 DEG C) completely.
Preferably, step 2) in, laser ablation inductively coupled plasma-mass spectrometry measures the response signal intensity of Cr on Cr:ZnS solid etalon material diverse location, the time of each laser ablation of degrading on position is more than 50 seconds, preferably at least degrade at 3 diverse locations, thus the homogeneity of better characterizing sample.The relative deviation RSD value obtaining Cr response signal intensity in described solid etalon material is less than 10%.
Preferably, in described Cr standard working curve, the linear relationship between Cr content and response signal intensity is more than 0.99, can reach 0.999.
Preferably, described laser ablation adopts optical maser wavelength 213 nanometer, laser energy 30% ~ 80%, laser frequency 10 ~ 20Hz, laser beam spot 100 ~ 200 microns, the micro-meter per second of sweep speed 20 ~ 50, helium gas flow 0.6 ~ 0.8L/ minute.
Preferably, described laser ablation adopts line to degrade and/or mode is degraded in face.
Preferably, described inductivity coupled plasma mass spectrometry adopts argon gas to be carrier gas, argon flow amount 0.6 ~ 0.8L/ minute.
Accompanying drawing explanation
Fig. 1 is laser ablation response signal and the graph of a relation of time of the zones of different of different Cr content Cr:ZnS solid etalon material;
Fig. 2 is the standard working curve of laser ablation-inductively coupled plasma mass spectrometry when analyzing Cr:ZnS quantitative crystal;
Fig. 3 is Cr:ZnS crystal prototype pictorial diagram to be measured, and a, c, e are respectively sample 1 before polishing, after polishing and diametrically the pictorial diagram in cross section, and b, d, f are respectively sample 2 before polishing, after polishing and diametrically the pictorial diagram in cross section;
The imaging distribution plan of Cr in Fig. 4 Cr:ZnS crystal prototype, a and b is respectively sample 1 and sample 2.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that following embodiment is only for illustration of the present invention, and unrestricted the present invention.
The object of the present invention is to provide and a kind ofly mix the content of Cr and the analytical approach of distribution in Cr zinc sulfide crystal material, by plating Cr film at ZnS host surface to prepare the different Cr:ZnS solid etalon material of some Cr content, LA-ICP-MS is utilized to characterize the homogeneity of mark solid etalon material, ICP-AES or ICP-MS measures the content of Cr in solid etalon material, in conjunction with the Cr element response signal intensity of LA-ICP-MS and the Cr content of mensuration, draw Cr standard working curve, line is adopted to degrade to the region to be measured of target sample or mode is degraded in face, obtain constituent content and some position information, thus Cr content and distribution thereof in Cr zinc sulfide crystal material is mixed in analysis.Method of the present invention can direct solid sample introduction, and sample only needs simple surperficial mechanical buffing, without the need to other pre-service any, can directly carry out quantitatively and Elemental redistribution imaging analysis.
About the preparation of solid etalon material, ZnS host material can be obtained by CVD (Chemical Vapor Deposition) method growth, even, the fine and close Cr film of thickness is plated at ZnS host surface by Magnetic filter ion plating method, spread plating the ZnS host material after Cr film more than 14 days at 950 DEG C in the quartz ampoule of vacuum seal (<10-1Pa), diffusion terminates rear sanding and polishing and obtains.Concrete, above-mentioned preparation method is with reference to FangZhenyietal (FangZhenyi, ChaiYichao, HaoYongliang, YangYaoyuan, DongYanping, YanZewu, TianHongchang, XiaoHongtao, WangHeming.JournalofCrystalGrowth, 2002, 237 – 239:1707 – 1710), A.F.Shchurovetal (A.F.Shchurov, E.M.Gavrishchuk, V.B.Ikonnikov, E.V.Yashina, A.N.Sysoev, D.N.Shevarenkov.InorganicMaterials, 2004, 40 (4): 336 – 339), wish native rich etal (Zhu Tufu, Shen Liru, Xu Guidong, Jin Fanya. Chinese Surface Engineering, 2008, 4 (21): 27-35) method such as.In described solid etalon material, between Cr doping content, coating film thickness and ZnS stromal thickness, there is following relation: film thickness (nm)=6.004 × 10
-18× ZnS stromal thickness (mm) × Cr doping content (atomcm
-3).
Cr standard working curve is drawn according to Cr element response signal intensity in the different solid etalon material of some (at least 3) Cr content and Cr content and is obtained.In solid etalon material, Cr content can be analyzed by ICP-AES or ICP-MS method.Cr content can be calculated as follows: Cr content (%)=solution concentration (gml
-1) × liquor capacity (ml) ÷ sample weighting amount (g) × 100.Concrete, as an example, such as solid etalon material accurately takes appropriate (such as 0.05g) after crushed in clean beaker, add appropriate (such as 3ml) chloroazotic acid, suitable can be placed in low-temperature heat on electric hot plate, and after sample dissolves completely, solution constant volume carries out ICP-AES concentration analysis to 100ml.
In solid etalon material, Cr element response signal intensity can be measured by LA-ICP-MS, and laser ablation mode can adopt line sweep mode of degrading to carry out degrading at the diverse location of solid etalon material and characterize its homogeneity.Preferably more than the 50 seconds time of laser ablation, in described solid etalon material, the RSD of the response signal intensity of Cr preferably remains on and is less than 10%.
The present invention utilizes homemade solid etalon material, and laser ablation inductively coupled plasma-mass spectrometry method carries out the quantitative of element Cr and distributional analysis to Cr:ZnS crystal prototype.Cr zinc sulfide crystal material sample is mixed to target, adopts direct solid sample introduction, only need simple surperficial mechanical buffing, without the need to other pre-service any, directly can carry out quantitatively and element distribution analysis, realize the distribution imaging analysis of doped chemical in crystal.In target sample, Cr constituent content obtains by standard working curve.By adopting line to degrade to the region to be measured of target sample or mode is degraded in face, content and the distribution characteristics information of the Cr of plane of crystal impact point position and/or target area can be obtained.
Feature of the present invention is:
(1) present method avoids the shortcomings such as conventional chemical/instrumental analysis preprocessing process is loaded down with trivial details, consuming time, pollution, environmental protection, simple and easy to do;
(2) in conjunction with high sensitivity and the laser ablation micrometer resolution of inductivity coupled plasma mass spectrometry, method of the present invention can be used for the micro-zone in situ analysis of the quantitative and distribution of trace doped element in laser material ZnS crystal;
(3) element of direct solid sample introduction of the present invention quantitatively and distributional analysis method model be applicable to other different types of middle infrared solid laser material (the II-VI group compound of doped transition metal ions) too) doped chemical quantitatively and be scattered in picture, thus provide analytical technology means, for assessment crystal property provides theories integration for the design of laser crystal material, exploitation and preparation.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The technological parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Instrument:
(1) the Nd:YAG laser ablation system of laser ablation system: Cetac213nm
(2) inductively coupled plasma spectrometry/mass spectrum (ICP-OES/MS): TheromfisherXSeries-II ICP-MS, AgilentTechnologies700SeriesICP-OES.
Embodiment 1
(1) preparation of Cr:ZnS solid etalon material
Thermal diffusion method is adopted to prepare solid etalon material.Preparation process comprises: first obtain ZnS host material by the growth of vapour deposition (CVD) method, then utilize Magnetic filter ion film plating (FAD) method to plate even, the fine and close Cr film of thickness in ZnS stromal surface.Then by material package (<10 in vitreosil pipe
-1pa), the crystalline material that more than 2 weeks time obtained uniform doping is spread under 950 DEG C of high temperature.Polishing is carried out after diffusion process terminates.
(2) LA-ICP-MS instrument parameter and combination analysis
The instrument parameter adopted after optimizing is: laser ablation adopts the Nd:YAG laser sampling system of Cetac213nm, optical maser wavelength 213nm, laser energy 50%, laser frequency 10Hz, laser beam spot 1000 μm, sweep speed 50 μm/s, helium gas flow 0.6L/min; ICP-MS is ThermoXseries II CCT type level Four bar, and argon gas is carrier gas, argon flow amount 0.7L/min.
Laser ablation mode adopts line sweep and/or Surface scan to degrade sampling.Degrade, the laggard line scan of blank counts 10s degrades at every turn, stops degrading rear continuation and purges a period of time.The signals collecting mode of ICP-MS is time resolution, i.e. the time dependent curve of signal intensity.
(3) sign of Cr:ZnS solid etalon material homogeneity
Under instrument parameter condition after optimization, the overall homogeneity of LA-ICP-MS method to Cr:ZnS solid etalon material characterizes.Respectively to the solid etalon material of Cr concentration different in (1), carry out line sweep in zones of different and degrade continuously, the corresponding relation (Fig. 1) of record Cr mass signal intensity and sweep time and scanning position.Experiment shows, concentration different geometric position in solid etalon material of doped chemical Cr is evenly distributed, different site of analysis relative standard deviation less (RSD<10%), meets as the basic demand of standard model to homogeneity.
Inductively coupled plasma atomic emission spectrum (ICP-AES) method measures Cr content in Cr:ZnS solid etalon material.Sample accurately takes 0.05g after crushed in the polytetrafluoroethylene beaker of cleaning, adds 3ml chloroazotic acid, is placed in low-temperature heat on electric hot plate.After sample dissolves completely, solution carries out ICP-AES concentration analysis.
In conjunction with the concentration that Cr element response signal intensity and the ICP-AES of LA-ICP-MS measure, draw
52cr standard working curve (Fig. 2).Experiment shows, its linear dependence reaches more than 0.99.The solid etalon material of homemade Cr:ZnS can be used for the quantitative test of Cr content.
(4) LA-ICP-MS quantitatively and distribution imaging analysis
The Cr:ZnS sample (sample 1 and sample 2, Fig. 3) of 2 different Cr content is carried out quantitatively and Elemental redistribution imaging analysis.Instrument parameter is with described in (2), and employing face is degraded mode and degraded sample in cross section.Cr constituent content is obtained by standard working curve.Adopt Surface scan to degrade mode, obtain the corresponding signal of sample in whole target area, and adopt Suffer8.0 software to process data, obtain imaging distribution plan (Fig. 4).Result shows, in sample 2, Cr constituent content is overall higher than sample 1.Cr element distributes similar in 2 samples, and all presents gradient distribution.
Claims (9)
1. mix the content of Cr and an analytical approach for distribution in Cr zinc sulfide crystal material, it is characterized in that, described method utilizes the analysis of laser ablation inductively coupled plasma-mass spectrometry method to mix content and the distribution of Cr in Cr zinc sulfide crystal material, and described method comprises:
1) plate Cr film to prepare the different Cr:ZnS solid etalon material of some Cr content at ZnS host surface, wherein, Cr is uniformly distributed in Cr:ZnS solid etalon material;
2) content of Cr in described solid etalon material is obtained by ICP-AES or inductively coupled plasma mass spectrometry, adopt laser ablation inductively coupled plasma-mass spectrometry method to measure the response signal intensity of Cr in described solid etalon material, draw Cr standard working curve;
3) laser ablation inductively coupled plasma-mass spectrometry detection is carried out to the Cr of mixing zinc sulfide crystal material sample to be measured, obtain content and the distribution of Cr in testing sample.
2. method according to claim 1, is characterized in that, prepares described solid etalon material and comprises: obtain ZnS host material by CVD (Chemical Vapor Deposition) method growth; Cr film is plated at ZnS host surface by Magnetic filter ion plating method; Spread plating the ZnS host material after Cr film more than 14 days at 950 DEG C in vitreosil pipe, diffusion terminates rear sanding and polishing, obtains described solid etalon material.
3. method according to claim 1 and 2, is characterized in that, described solid etalon material is at least 3.
4. according to the method in any one of claims 1 to 3, it is characterized in that, step 2) in, laser ablation inductively coupled plasma-mass spectrometry measures the response signal intensity of Cr on Cr:ZnS solid etalon material diverse location, each time of degrading of degrading position is more than 50 seconds, and the response signal intensity relative deviation RSD obtained is less than 10%.
5. method according to any one of claim 1 to 4, it is characterized in that, step 2) comprising: obtain solution with solid etalon material described in aqua regia dissolution, measure Cr concentration in described solution by ICP-AES or inductively coupled plasma mass spectrometry, calculate the content of Cr in solid etalon material.
6. method according to any one of claim 1 to 5, is characterized in that, in described Cr standard working curve, the linear relationship between Cr content and response signal intensity is more than 0.99.
7. method according to any one of claim 1 to 6, it is characterized in that, described laser ablation adopts optical maser wavelength 213 nanometer, laser energy 30% ~ 80%, laser frequency 10 ~ 20Hz, laser beam spot 100 ~ 200 microns, the micro-meter per second of sweep speed 20 ~ 50, helium gas flow 0.6 ~ 0.8L/ minute.
8. method according to any one of claim 1 to 7, is characterized in that, described laser ablation adopts line to degrade and/or mode is degraded in face.
9. method according to any one of claim 1 to 8, is characterized in that, described inductivity coupled plasma mass spectrometry adopts argon gas to be carrier gas, argon flow amount 0.6 ~ 0.8L/ minute.
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| CN113186602A (en) * | 2021-04-29 | 2021-07-30 | 杭州光学精密机械研究所 | Cr-doped II-VI compound homogeneous edge-coated polycrystalline laser material and preparation method thereof |
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