CN101710098A - Method for measuring trace metal ion in high-purity metal organic zirconium - Google Patents
Method for measuring trace metal ion in high-purity metal organic zirconium Download PDFInfo
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- CN101710098A CN101710098A CN200910263103.6A CN200910263103A CN101710098A CN 101710098 A CN101710098 A CN 101710098A CN 200910263103 A CN200910263103 A CN 200910263103A CN 101710098 A CN101710098 A CN 101710098A
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- organic zirconium
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 29
- 239000002184 metal Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910021655 trace metal ion Inorganic materials 0.000 title claims abstract description 11
- 239000000523 sample Substances 0.000 claims abstract description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 239000012496 blank sample Substances 0.000 claims abstract description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 7
- 239000012498 ultrapure water Substances 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000005516 engineering process Methods 0.000 claims description 11
- 238000012360 testing method Methods 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 10
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 239000004809 Teflon Substances 0.000 claims description 3
- 229920006362 Teflon® Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000012086 standard solution Substances 0.000 abstract description 5
- 238000007865 diluting Methods 0.000 abstract 3
- 238000006864 oxidative decomposition reaction Methods 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 229910052735 hafnium Inorganic materials 0.000 description 9
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000013459 approach Methods 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 238000000120 microwave digestion Methods 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- TZMFJUDUGYTVRY-UHFFFAOYSA-N ethyl methyl diketone Natural products CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for measuring trace metal ion in high-purity metal organic zirconium, which comprises the steps of: putting compound of high-purity metal organic zirconium into a polytetrafluoroethylene screw opening bottle; putting the bottle on a ultra-clean work table, unscrewing a bottle cover, and performing oxidative decomposition; adding the solution into a microwave digesting apparatus for technical ultra-pure concentrated nitric acid to be digested into transparent and clear acid solution; and preparing 1 part of blank sample under the same condition; diluting the acid solution prepared by the last step with ultra-pure water, and diluting the blank sample under the same condition to be measured; diluting the metal unit standard solution which needs to be measured with hydrogen nitrate; correcting a plasma mass spectrometer with the diluted standard solution; respectively putting a parallel sample and a blank sample to be measured into the plasma mass spectrometer to be measured; measuring data Xi of each blank-deducted impurity element; and processing data, wherein Y=1-sigma Xi, and Y is the purity of the high-purity metal organic zirconium. The method is fast and reliable, and has high precision and accuracy.
Description
One, technical field
The present invention relates to the purity analysis of high pure metal organic zirconium, specifically measure trace metal ion wherein.
Two, background technology
In January, 2007,, indicate that the epoch of introducing new material in the CMOS manufacturing process formally arrive along with the issue of adopting 45nm technology microprocessor.The microprocessor of new issue takes the lead in having adopted hafnium base high-k dielectric material and novel gate metal electrode material, improves transistorized performance in the processor jointly.This transition mark semi-conductor industry and has been begun to select for use non-core element in the periodic table, i.e. element beyond silicon, oxygen, nitrogen and the carbon.It is generally acknowledged that simple dependence scaled down has been not enough to satisfy the sustainable growth of silicon device performance.Innovation is from the new element of introducing in the periodic table of elements, and this has become the major impetus that the driving element performance improves.
High dielectric constant material be owing to can allow thicker grid dielectric material, thereby reduces leakage current, and become essential.Therefore select appropriate hafnium, satisfy the requirement that specific inductive capacity, thermodynamic stability, gate electrode compatibility and contact bed stability etc. are produced.Search has the gate dielectric material of the alternative oxides of nitrogen of thermodynamic stability in the periodic table of elements; These materials just hafnium presoma are made up of hafnium, zirconium and scarce metallic compound.
The high pure metal organic zirconium is at the following technology node great scale integrated circuit of 32-22nm CMOS Technology Need at present, the metal organic compound of developing with independent intellectual property right, as compounds such as zirconium base amino-contained, cyclopentadienyl and pentanedione classes, can be with such presoma in order to prepare the hafnium that is used for 32-22 nanometer cmos device gate medium, the passive MIM device of RF circuit and advanced storer of function admirable.From the microstructure angle, explore hafnium and metal gate material with the channel material integrating process in interfacial characteristics and interfacial effect, realize in the growth course modification and regulation and control to the interface.Developing with compatible mutually ald (ALD) hafnium of semiconductor technology and prepare gordian technique, by antetype device material is verified, finally be great scale integrated circuit industry great-leap-forward development, and the hafnium and the technology of preparing support of key are provided.
Because the pollutant in the high pure metal organic zirconium can cause component failure and influence yield rate, and can be applied to purity requirement height on the great scale integrated circuit, generally all more than 99.99%, at semicon industry, the detection of purity is a standard with the trace metal ion in the detection compound generally, as detected metal ion content summation＜100ppm, represent that then purity reaches 99.99%.The exploitation of high pure metal organic zirconium and purification need the sensitive analytical approachs that measure trace amounts of metal contaminants concentration reliably.
Three, summary of the invention
Goal of the invention: the present invention is directed to above-mentioned technological gap, a kind of method of measuring trace metal ion in the high pure metal organic zirconium is provided, reach fast, reliable, precision and accuracy height.
Technical scheme: a kind of method of measuring trace metal ion in the high pure metal organic zirconium, determination step is: 3 parts of compounds getting high pure metal organic zirconium to be measured are in teflon screw socket bottle, place in 10000 grades of ultra-clean chambers unscrew on 100 grades of superclean benches the bottle cap oxygenolysis fully after, add the ultrapure red fuming nitric acid (RFNA) of technology and clear up into transparent clarification acid solution with microwave dissolver, amount to 3 parts of parallel samples, do 1 part of blank sample under the equal conditions; With 18.2M Ω cm
-1Ultrapure water will go up the acid solution that makes of step and be diluted to the solution that matrix concentration is 1000 μ g/g, described matrix element is a zirconium, amounts to 3 parts of parallel samples, also the equal conditions dilution is to be measured for blank sample; The plain titer acidity of metal unit that needs are detected is that 2% nitric acid is diluted to 10ng/mL or 20ng/mL, and with the dilution after titer icp ms is proofreaied and correct, then parallel sample to be measured and blank are put into icp ms respectively and test, record the data Xi of each impurity element after the deduction blank; Data processing: Y=1-∑ Xi, Y are the purity of high pure metal organic zirconium.
Described high pure metal organic zirconium oxygenolysis fully after, place the withstand voltage polytetrafluoroethyltank tank of configuration microwave dissolver, 120 ℃, 5 atmospheric pressure, 3 minutes; 150 ℃, 10 atmospheric pressure, 3 minutes; 180 ℃, 15 atmospheric pressure, 3 minutes; Dividing three program segment totally-encloseds to add nitric acid clears up.
All experiment containers are used 12M Ω cm more all through the chloroazotic acid washing by soaking
-1Pure water and 18.2M Ω cm
-1Ultrapure water soaks ultrasonic cleaning, places infrared lamp oven dry on 100 grades of superclean benches at last.
Beneficial effect:
The present invention compares with existing analytical approach has following remarkable advantage:
(1) in sample sample preparation and detection link, environment there is very high requirement, possesses 10000 grades of ultra-clean chambers, 100 grades of superclean benches, 18.2M Ω cm
-1Ultrapure water and technology extra pure regent, only the purity of the accurate reflection of ability high pure metal organic zirconium in the environment of cleaning guarantees precision of test result.
(2) in the pre-treating method of sample, adopt Microwave Digestion, under suitable temperature, pressure condition, the polytetrafluoroethyltank tank totally-enclosed adds nitric acid and decomposes sample, than normal temperature and pressure resolution method commonly used in the past, reduce the link of staiing, guaranteed not losing of volatile element, can accurately reflect the content of metallic ion in the sample; And general of Microwave Digestion needed 10 minutes just can become clear solution to Specimen eliminating fully, and conventional normal temperature and pressure resolution method is looked the complexity that organic sample decomposes, at least need 4-6 hour, so Microwave Digestion possesses fast and reliable advantage accurately.
(3) Pei Zhi a certain amount of matrix (with zirconium as matrix element) concentration solution, when going up test, icp ms (ICP-MS) can eliminate of the influence of high matrix concentration to test result, can improve the method detection limit of instrument again as much as possible, obtain result fast and accurately.
(4) with the ICP-AES test, the matrix element zirconium is big and complicated to the interference of other impurity elements, and the instrument detection limit will carry out trace detection and have certain degree of difficulty in the ppb level; And test with ICP-MS, the instrument detection limit is low, in the ppq-ppt level, disturbs and lacks, and can satisfy the mensuration of trace metal ion.
Four, embodiment
Embodiment 1
(1) pre-treatment of sample:
Instrument: microwave dissolver
Because the hafnium presoma is the bigger zirconium metalloid-organic compound of coordinating group, meet air, aqueous vapor can be decomposed, determine amount metal ion content wherein so be as the criterion, sample must be taken a sample in anaerobic anhydrous inert glove box, the 0.10XX that weighs gram, take a sample 3 parts altogether as parallel sample, place on the interior 100 grades of superclean benches of 10000 grades of ultra-clean chambers, unscrew the sampling jar bottle cap by sample oxygenolysis slowly, sample after decomposing fully adds the ultrapure red fuming nitric acid (RFNA) of 3mL technology and is transferred in the withstand voltage counteracting tank of the teflon of ultrapure cleaning, 3 parts in parallel sample is done blank 1 part under the equal conditions, set (120 ℃ of the suitable conditions of clearing up, 5 atmospheric pressure, 3 minutes; 150 ℃, 10 atmospheric pressure, 3 minutes; 180 ℃, 15 atmospheric pressure, 3 minutes), Specimen eliminating is become clear solution, more per sample sampling amount with 18.2M Ω cm
-1Ultrapure water to be diluted to matrix concentration (with zirconium as matrix element) be that 1000 μ g/g solution examples are to be measured.
(2) test of sample:
When testing on ICP-MS, according to technical requirement, selected abundance height, noiseless, mass number that detection limit is low are tested by optimized analytical approach and instrument condition.
Instrument: icp ms
Reagent: ultrapure water--Millipore produces 18.2M Ω cm
-1Water; The technology super-pure nitric acid
Standard solution: will need the plain standard 1mg/mL of metal unit (national standard material center provides) that detects to be made into mixing stock solution 1 μ g/mL, acidity is 2% nitric acid (standby).
During use the standard solution of being prepared is diluted to 10ng/mL, 20ng/mL.
Test: the standardization that ICP-MS tests is proofreaied and correct with the standard solution that contains 10ng/mL, 20ng/mL.Parallel sample of 3 duplicate samples and blank are measured on the ICP-MS after the correction respectively, counted extension rate when method of testing is set up, record the data (Xi) after each impurity element is deducted blank.
Data processing: Y=1-∑ Xi (Y is the purity of high pure metal organic zirconium).
Claims (3)
1. method of measuring trace metal ion in the high pure metal organic zirconium is characterized in that determination step is:
A. 3 parts of compounds getting high pure metal organic zirconium to be measured are in teflon screw socket bottle, place in 10000 grades of ultra-clean chambers unscrew on 100 grades of superclean benches the bottle cap oxygenolysis fully after, add the ultrapure red fuming nitric acid (RFNA) of technology and clear up into transparent clarification acid solution with microwave dissolver, amount to 3 parts of parallel samples, do 1 part of blank sample under the equal conditions;
B. use 18.2M Ω cm
-1Ultrapure water will go up the acid solution that makes of step and be diluted to the solution that matrix concentration is 1000 μ g/g, described matrix element is a zirconium, amounts to 3 parts of parallel samples, also the equal conditions dilution is to be measured for blank sample;
C. will need the plain titer acidity of the metal unit that detects is that 2% nitric acid is diluted to 10ng/mL or 20ng/mL, and with the dilution after titer icp ms is proofreaied and correct, then parallel sample to be measured and blank are put into icp ms respectively and test, record the data Xi of each impurity element after the deduction blank;
D. data processing: Y=1-∑ Xi, Y are the purity of high pure metal organic zirconium.
2. the method for trace metal ion in the mensuration high pure metal organic zirconium according to claim 1, it is characterized in that described high pure metal organic zirconium is after oxygenolysis is complete, place the withstand voltage polytetrafluoroethyltank tank of configuration microwave dissolver, 120 ℃, 5 atmospheric pressure, 3 minutes; 150 ℃, 10 atmospheric pressure, 3 minutes; 180 ℃, 15 atmospheric pressure, 3 minutes; Dividing three program segment totally-encloseds to add nitric acid clears up.
3. the method for trace metal ion is characterized in that in the mensuration high pure metal organic zirconium according to claim 1, and all experiment containers are used 12M Ω cm more all through the chloroazotic acid washing by soaking
-1Pure water and 18.2M Ω cm
-1Ultrapure water soaks ultrasonic cleaning, places infrared lamp oven dry on 100 grades of superclean benches at last.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102565182A (en) * | 2011-12-16 | 2012-07-11 | 天津中环领先材料技术有限公司 | Method for testing content of metal ions on surface of 8-inch silicon polished wafer for insulated gate bipolar transistor (IGBT) |
| CN104597110A (en) * | 2015-01-23 | 2015-05-06 | 河北钢铁股份有限公司 | ICP-MS measuring method of microelement impurities in high-purity chromium |
| CN107782779A (en) * | 2017-11-28 | 2018-03-09 | 苏州市苏测检测技术有限公司 | Heavy metal component quick detection pre-processing device in food |
| CN108267498A (en) * | 2017-12-28 | 2018-07-10 | 中核北方核燃料元件有限公司 | The assay method of boron aluminium impurity content in a kind of uranium gadolinium zircaloy |
| CN110361376A (en) * | 2019-06-27 | 2019-10-22 | 上海宝钢工业技术服务有限公司 | The measuring method of zirconium and its compound in workplace air |
| CN113504291A (en) * | 2021-06-16 | 2021-10-15 | 宁波锦越新材料有限公司 | Sample preparation method and detection method for determining impurities in ultra-high-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
| CN114764085A (en) * | 2021-05-31 | 2022-07-19 | 上海赛夫特半导体材料有限公司 | Method for analyzing trace metal impurities of ultra-pure resin material and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101339103B (en) * | 2008-08-07 | 2011-10-05 | 云南烟草科学研究院 | Flue gas trapping and absorption apparatus and its uses in cigarette flue gas heavy metal element determination |
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2009
- 2009-12-16 CN CN200910263103.6A patent/CN101710098B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565182A (en) * | 2011-12-16 | 2012-07-11 | 天津中环领先材料技术有限公司 | Method for testing content of metal ions on surface of 8-inch silicon polished wafer for insulated gate bipolar transistor (IGBT) |
| CN104597110A (en) * | 2015-01-23 | 2015-05-06 | 河北钢铁股份有限公司 | ICP-MS measuring method of microelement impurities in high-purity chromium |
| CN107782779A (en) * | 2017-11-28 | 2018-03-09 | 苏州市苏测检测技术有限公司 | Heavy metal component quick detection pre-processing device in food |
| CN108267498A (en) * | 2017-12-28 | 2018-07-10 | 中核北方核燃料元件有限公司 | The assay method of boron aluminium impurity content in a kind of uranium gadolinium zircaloy |
| CN110361376A (en) * | 2019-06-27 | 2019-10-22 | 上海宝钢工业技术服务有限公司 | The measuring method of zirconium and its compound in workplace air |
| CN114764085A (en) * | 2021-05-31 | 2022-07-19 | 上海赛夫特半导体材料有限公司 | Method for analyzing trace metal impurities of ultra-pure resin material and application thereof |
| CN113504291A (en) * | 2021-06-16 | 2021-10-15 | 宁波锦越新材料有限公司 | Sample preparation method and detection method for determining impurities in ultra-high-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
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| CN101710098B (en) | 2012-12-12 |
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