CN105954348A - Analysis and detection method for high purity indium - Google Patents
Analysis and detection method for high purity indium Download PDFInfo
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- CN105954348A CN105954348A CN201610571575.8A CN201610571575A CN105954348A CN 105954348 A CN105954348 A CN 105954348A CN 201610571575 A CN201610571575 A CN 201610571575A CN 105954348 A CN105954348 A CN 105954348A
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- G—PHYSICS
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- 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
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- G—PHYSICS
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- 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
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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
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Abstract
The invention discloses an analysis and detection method for high purity indium. The analysis and detection method includes the steps that ammonia water is prepared into ultra-pure ammonia water with the free diffusion method; nitric acid is prepared into ultra-pure nitric acid with the sub-boiling distillation method; high purity indium with the grade of 6N or above is dissolved with the ultra-pure nitric acid, then nitrogen oxide is removed through heating, the product is cooled, diluted with water and heated, the ultra-pure ammonia water is added dropwise, stirring and reacting are carried out, the pH value of 2 to 10 of the system serves as the reaction endpoint, and standing clarifying or centrifugal separation is carried out; supernatant liquid is taken, volatilized and concentrated, then the concentrated product is dissolved with the ultra-pure nitric acid, internal standard substances are added, constant volume is achieved, and to-be-detected liquid is obtained; According to ICP-MS measurement, the method is easy to operate, high in sensitivity, good in accuracy and specially suitable for detection of the purity of the high purity indium with the grade of 6N or above.
Description
Technical field
The present invention relates to the determination method of a kind of high purity indium, the analysis particularly to a kind of more than 6N high purity indium detects
Method；Belong to metal detection technical field.
Background technology
The development of New function material in modern material science, the most high-purity Indium and compounds, especially InP, InAs,
The exploitation application of large quantities of semi-conducting material such as InSb, developing rapidly of electron trade the most in recent years, more promote
The research and development of high purity indium.Owing to some impurity element has the biggest impact to the electrical properties of high purity indium compound semiconductor, because of
The quality control of this high purity indium is extremely important.In process of production, impurity trend, the removal journey of impurity in its preparation technology is related to
Degree, also requires that Instructing manufacture monitored at any time by high purity indium, is therefore badly in need of now the detection method of trace impurity in a kind of high purity indium.
The detection method of high purity indium, currently mainly based on glow discharge mass spectroscopy (GD-MS).Glow discharge spectrometry quilt
It is considered solid conductive material directly carries out trace and the maximally effective means of ultratrace element analysis at present.Owing to it is permissible
Direct solid sampling, is widely used to the analysis of the material such as high pure metal, alloy over nearly 20 years.GD-MS not only has superior
Detection limit and the advantage of wide dynamic linear response range, and sample preparation is simple, sensitivity difference is little between element, matrix effect
Low.GD-MS obtains extensively with its superior analytical performance in the fields such as electronics, chemistry, metallurgy, geology and material science
Application, high pure metal and Analysis of Semiconductor Materials have shown that its superiority, to it insulator, powder, liquid,
Application during Organic substance and biological material analysis and anion measure also is studied and perfect actively carrying out, and development prospect is very
Wide.
The main manufacturer of GD-MS: Sai Mo flies the ELEMENT GD Plus glow discharge mass spectroscopy of company, Britain's matter now
Spectrometer device high-resolution glow discharge mass spectroscopy Autoconcept GD90, the AstruM high-resolution aura of Nu Instruments
Electric discharge mass spectrograph, and the VG9000 (stopping production) of Qian Saimofei company.
Owing to GD-MS is expensive, operator quality level being also required that height, it is not a lot of that China is equipped now.And
And now the highest with GD-MS one sample expense of detection, spend the cycle long, to high purity indium development & production inapplicable and real
With.
YS/T 230-1994 high purity indium chemical analysis method, with organic reagent extract and separate indio body, after impurity enriched
AES measures.But organic reagent is difficult to purify, to measuring 6N and above indium improper.
Icp ms (ICP-MS) has assembling, detection sensitivity also may be used at Chinese large-sized laboratory
To reach requirement.YS/T 276.12-2011 indium chemical analysis method, icp ms (ICP-MS) is analyzed
Impurity element in smart indium (4N5), not matrix separation, diluted sample 2000 times.But for 6N and above high purity indium, by
Low in impurity content, it is impossible to use the method for not matrix separation to carry out impurity analysis detection.
Summary of the invention
The defect existed for the analyzing detecting method of existing high purity indium, it is an object of the invention to be to provide a kind of behaviour
Make the method analyzing detection high purity indium simple, highly sensitive, that accuracy is good.
In order to realize above-mentioned technical purpose, the invention provides a kind of Analysis of High-Purity Indium detection method, the method include with
Lower step:
1) ammonia prepares the impurity content super-pure ammonia water less than 0.1ppb by free diffusing method；
2) nitric acid uses sub-boiling distillation method to prepare the impurity content super-pure nitric acid less than 0.1ppb；
3), after using described super-pure nitric acid to dissolve above for 6N level high purity indium, heat abstraction nitrogen oxides is added, cooling, add water dilute
Releasing, be again heated to 55～65 DEG C, drip described super-pure ammonia water, stirring reaction, controlling system pH 2～10 is reaction end, quiet
Put clarification or centrifugation；Take the supernatant through volatilization concentrate after, concentrate use described super-pure nitric acid dissolve, add internal standard
Thing, constant volume, obtain liquid to be measured；
4) described liquid to be measured is measured by ICP-MS.
Preferably scheme, free diffusing method is realized by free diffusing device；Described free diffusing device includes base plate, close
Sealing cover, diffusion cell and absorption cell；Described base plate has groove in surface surrounding, and the bottom of described seal closure is embedded in described groove
In, make to be formed between seal closure and base plate closed area；Diffusion cell and absorption cell it is provided with in described closed area.
More preferably scheme, at the built-in ammonia of diffusion cell, at the built-in pure water of absorption cell；Diffusion cell and absorption cell are placed on
On base plate, seal closure on cover, in the groove of base plate, it is filled with pure water seals, stand, from absorption cell, obtain super-pure ammonia water stand-by.
In closed environment, the ammonia in ammonia slowly evaporates, and by absorbing pure water, thus purifies ammonia further.
Preferably scheme, sub-boiling distillation method is realized by sub-boiling distillation device；Described sub-boiling distillation device includes a stone
English container, acid receiving flask and acid collection funnel, described acid receiving flask is arranged on bottom described quartz container, and quartz container is received with acid
Being provided with acid collection funnel between collection bottle, acid collection funnel head stretches into quartz container internal upper part, and acid collection funnel cervical region stretches into institute
State inside acid receiving flask；
Described quartz container inner top is provided with acid-filling mouth and V-type condensing tube, middle part is provided with infrared heating pipe；Described V-type is cold
The top of solidifying pipe is arranged on directly over described acid collection funnel.
More preferably scheme, injects nitric acid from acid-filling mouth in quartz container, and the injecting height of nitric acid adds less than infrared ray
Heat pipe；In V-type condensing tube, inject condensed water, start infrared heating pipe simultaneously, control temperature in quartz container, make nitric acid be in
Sub-boiling state, the nitric acid of volatilization condenses enrichment on V-type condensing tube, flows in acid collection funnel, then flows into acid receiving flask, from acid
Receiving flask obtains super-pure nitric acid stand-by.
Preferably scheme, volatilization is concentrated by volatilization enrichment facility and realizes；Described volatilization enrichment facility includes a heating
Electric furnace, evaporation cover and evaporating device；Described evaporation cover is arranged on hot plate, and described evaporating device is placed in evaporation cover；Institute
Stating evaporation cover bottom and be provided with gas feed, top is provided with gas outlet.Evaporation cover uses the mode of bottom in and top out, can be effectively improved
The rate of volatilization of solution.Evaporation cover uses quartz material.
More preferably scheme, takes in the evaporating device that the supernatant is placed in volatilization enrichment facility, is passed through argon from gas feed,
Control hot plate temperature is at 75～85 DEG C, until evaporating in evaporating device completely.
More preferably scheme, argon flow velocity is 1～10 liter/min.
Preferably scheme, the speed of described stirring is 20～200rpm.Under agitation as appropriate speed, can effectively prevent precipitation
Thing adsorbing contaminant ion.Mixing time is preferably controlled in 5～30min.
The pH value of technical scheme control reaction end, between 2～10, not only can reduce the residual of matrix
Amount, can make again trace impurity stay in the solution.
Hinge structure, the Advantageous Effects that technical scheme is brought:
1, technical scheme, uses super-pure nitric acid to dissociate high purity indium, and employing super-pure ammonia water is on this basis
Regulator, makes indium be removed with indium hydroxide intermediate processing, and the method does not introduce new impurity, it is ensured that detect ultrapure indium
Accuracy.
2, technical scheme is during precipitation of indium, by strict control ph and employing alr mode, makes
Major part indium precipitation (removing more than 95%), and impurity stays solution, effectively prevents precipitation adsorption impurity, and cause impurity to damage
Lose；Preferably solve ICP-MS and be weak to matrix problem.
3, technical scheme is by precipitation major part indium, then is concentrated by volatilization, impurity carries out rich concentration, has
It is beneficial to improve the sensitivity that ICP-MS measures.
4, the technical method of the present invention detects based on ICP-MS, has easy and simple to handle, and detection speed is fast, the spy that expense is few
Point, it is adaptable to Quality Control Analysis and quality arbitration.
Accompanying drawing explanation
[Fig. 1] is free diffusing device sketch；
[Fig. 2] is sub-boiling distillation device sketch；
[Fig. 3] is volatilization enrichment facility sketch；
1 is seal closure, and 2 is absorption cell, and 3 is diffusion cell, and 4 is base plate, and 5 export for V-type condensing tube, and 6 is quartz container, 7
For acid receiving flask, 8 is infrared heating pipe, and 9 export for V-type condensing tube, and 10 is acid collection funnel, and 11 is acid-filling mouth, and 12 is gas
Import, 13 is evaporation cover, and 14 is gas outlet, and 15 is evaporating device, and 16 is hot plate.
Detailed description of the invention
Below in conjunction with embodiment, the present invention and detailed description of the invention thereof are described in further detail.
Embodiment 1
1) diffusion method purifies ammonia, and free diffusing device sketch is as shown in Figure 1.
Open on reeded clean politef sheet material a surrounding, with a big polytetrafluoroethylene beaker cup
Enter ammonia to be purified, in adjacent position placement one equipped with the polytetrafluoroethylene beaker of pure water, cover teflon seal cover,
In under teflon seal cover, edge is placed on the groove that surrounding opens reeded clean politef sheet material, groove is filled with few
Amount pure water seals, and after certain time (general 1 time-of-week), ammonia in polytetrafluoroethylene beaker is loaded clean polytetrafluoroethyl-ne
In alkene bottle stand-by.
ICP-MS detects ammonia quality:
Before and after table 1 ammonia purifies, impurity content contrasts
2) sub-boiling distillation method purifies nitric acid, and sub-boiling distillation device sketch is as shown in Figure 2.
Injecting a certain amount of volume nitric acid to be purified from acid-filling mouth in quartz cylinder container, nitric acid height can not be with infrared
Add heat pipe contact, connect V-shape coolant intake and cooling water outlet mouth, start infrared heating pipe, control power, with acid surfaces not
Boiling is advisable.Tube-surface liquid to be cooled flows in acid collection funnel, then flows into acid receiving flask, starts about 50 milliliters and gives up,
Collect the further part loading clean politef of knot stand-by.
ICP-MS detects nitric acid quality:
Before and after table 2 nitric acid purifies, impurity content contrasts
3) sample dissolves and precipitation.
Weighing 1.5 grams of high purity indiums in high-purity politef cup, add 8 milliliters of nitric acid purified, low-temperature heat is dissolved
Completely, continue heating and catch up with most nitrogen oxides, cooling, add water to 80 milliliters.Beaker is placed on magnetic stirring apparatus, is heated to 60 and takes the photograph
Family name's degree, puts into polytetrafluoro stirrer, stirring, dropwise drips the ammonia of purification, adjusts pH and is about 8, takes off cooling, be settled to 100
Milliliter, stands (or centrifugation)；
4) concentrate.Such as Fig. 3.
Take 20 milliliters of supernatant in evaporating device, cover evaporation cover, be passed through high-purity argon gas from gas feed, control certain stream
Amount (about 5 liters/min), gas is from gas outlet's discharge, and gas outlet is twice than the bore of gas feed, controls hot plate
Temperature 80 degrees Celsius, does not seethe with excitement with liquid in evaporating device and is advisable, and volatilization is near dry, 0.2 milliliter of nitric acid purified, and adds a certain amount of interior
Mark, is settled to 10 milliliters；
5) ICP-MS measures.
ICP-MS condition is as follows:
INSTRUMENT MODEL: THERMO company, X-SERIES 2；
Table 3 ICP-MS canonical analysis condition
Table 4 elementary analysis to be measured condition
Table 5 ICP-MS canonical analysis condition requires and actual measurement
Table 6 ICP-MS typical element analysis detection limit
| Analyze isotope | Analytical model | Analyze detection limit |
| 9Be | Hot flame | 3.06ppt |
| 59Co | Hot flame | 0.62ppt |
| 115In | Hot flame | 6.5ppt |
| 238U | Hot flame | 0.15ppt |
| 56Fe | CCT | 1.8ppt |
| 23Na | Cool flame | 14.9ppt |
ICP-MS detection high purity indium quality is as follows:
Certain batch 6N indium ICP-MS testing result of table 7
This batch 6N indium from the point of view of testing result reaches requirement.
Claims (9)
1. an Analysis of High-Purity Indium detection method, it is characterised in that: comprise the following steps:
1) ammonia prepares the impurity content super-pure ammonia water less than 0.1ppb by free diffusing method；
2) nitric acid uses sub-boiling distillation method to prepare the impurity content super-pure nitric acid less than 0.1ppb；
3), after using described super-pure nitric acid to dissolve above for 6N level high purity indium, heat abstraction nitrogen oxides is added, cooling, dilute,
Being again heated to 55～65 DEG C, drip described super-pure ammonia water, stirring reaction, controlling system pH 2～10 is reaction end, stands clear
Clear or centrifugation；Take the supernatant through volatilization concentrate after, concentrate use described super-pure nitric acid dissolve, add internal standard substance,
Constant volume, obtains liquid to be measured；
4) described liquid to be measured is measured by ICP-MS.
Analysis of High-Purity Indium detection method the most according to claim 1, it is characterised in that:
Described free diffusing method is realized by free diffusing device；
Described free diffusing device includes base plate, seal closure, diffusion cell and absorption cell；
Described base plate has groove in surface surrounding, and the bottom of described seal closure is embedded in described groove, makes seal closure and the end
Closed area is formed between plate；Diffusion cell and absorption cell it is provided with in described closed area.
Analysis of High-Purity Indium detection method the most according to claim 1 and 2, it is characterised in that: at the built-in ammonia of diffusion cell,
The built-in pure water of absorption cell；Diffusion cell and absorption cell are placed on, seal closure on cover, in the groove of base plate, are filled with pure water
Seal, stand, from absorption cell, obtain super-pure ammonia water stand-by.
Analysis of High-Purity Indium detection method the most according to claim 1, it is characterised in that:
Described sub-boiling distillation method is realized by sub-boiling distillation device；
Described sub-boiling distillation device includes a quartz container, acid receiving flask and acid collection funnel；Described acid receiving flask is arranged on
Bottom described quartz container, being provided with acid collection funnel between quartz container and acid receiving flask, acid collection funnel head stretches into quartz
Container internal upper part, acid collection funnel cervical region stretches into inside described acid receiving flask；
Described quartz container inner top is provided with acid-filling mouth and V-type condensing tube, middle part is provided with infrared heating pipe；Described V-type condensing tube
Top be arranged on described acid collection funnel directly over.
5. according to the Analysis of High-Purity Indium detection method described in claim 1 or 4, it is characterised in that: from acid-filling mouth toward quartz container
Interior injection nitric acid, the injecting height of nitric acid is less than infrared ray heating tube；In V-type condensing tube, inject condensed water, start red simultaneously
Pipe heater outside, controls temperature in quartz container, makes nitric acid be in sub-boiling state, and the nitric acid of volatilization condenses richness on V-type condensing tube
Collection, flows in acid collection funnel, then flows into acid receiving flask, obtains super-pure nitric acid stand-by from acid receiving flask.
Analysis of High-Purity Indium detection method the most according to claim 1, it is characterised in that: described volatilization is concentrated by volatilization
Enrichment facility realizes；Described volatilization enrichment facility includes a hot plate, evaporation cover and evaporating device；Described evaporation cover is arranged
On hot plate, described evaporating device is placed in evaporation cover；Described evaporation cover bottom is provided with gas feed, and top is provided with gas
Outlet.
7. according to the Analysis of High-Purity Indium detection method described in claim 1 or 6, it is characterised in that: the supernatant is placed in volatilization
In the evaporating device of enrichment facility, it is passed through argon from gas feed, controls hot plate temperature at 75～85 DEG C, until in evaporating device
Evaporate completely.
Analysis of High-Purity Indium detection method the most according to claim 7, it is characterised in that: argon flow velocity is 1～10 liter/min.
Analysis of High-Purity Indium detection method the most according to claim 1, it is characterised in that: the speed of described stirring 20～
200rpm。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108572213A (en) * | 2018-04-24 | 2018-09-25 | 株洲科能新材料有限责任公司 | A kind of high purity tellurium impurity enriched device and its method for 5N grades of tellurium analysis detections |
| CN109592656A (en) * | 2019-01-31 | 2019-04-09 | 内蒙古通威高纯晶硅有限公司 | A kind of preparation method of impurity analysis acid |
| KR20210024778A (en) * | 2019-08-26 | 2021-03-08 | 호서대학교 산학협력단 | Purifying reagent apparatus for obtaining ultrapure nitric acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108572213A (en) * | 2018-04-24 | 2018-09-25 | 株洲科能新材料有限责任公司 | A kind of high purity tellurium impurity enriched device and its method for 5N grades of tellurium analysis detections |
| CN109592656A (en) * | 2019-01-31 | 2019-04-09 | 内蒙古通威高纯晶硅有限公司 | A kind of preparation method of impurity analysis acid |
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Address after: 412000 Jinshan private science and Technology Park, Hetang District, Zhuzhou City, Hunan Province Patentee after: Zhuzhou Keneng New Material Co.,Ltd. Address before: 412000 Jinshan private science and Technology Park, Hetang District, Zhuzhou City, Hunan Province Patentee before: ZHUZHOU KENENG NEW MATERIAL Co.,Ltd. |