ICP-MS分析太阳级硅中杂质含量及分析实例-杜嘉斌

1、ICP-MS分析太阳级硅中杂质含量及分分析太阳级硅中杂质含量及分析实例析实例杜嘉斌杜嘉斌 赛维赛维LDK-技术研究院技术研究院 赛维赛维LDK检测中心检测中心ICP-MS实景实景Elements Analyzed by ICP-MS - D.L. of ELAN DRCD.L. range 1 ppt 1 100 ppt 0.1 1 ppbSchematic Diagram of ELAN DRCOptional PFA Sample Introduction SystemSpray ChamberPt InjectorIonization Process in PlasmaMoleculeA

2、tomIonAerosolParticlesNebulizationDesolvationVaporizationDissociationIonizationCa(OH)2Ca Ca+Ionization Efficiency of Elements in Ar Plasma0102030405060708090020406080100Atomic numberIonisation efficiency (%)LiBeBCBaMgAlSiPSClKCaScVTiCrMnZnGaGeCuFeNiCoAsSeBrRbSrYZrNbMoTcRuRhPdAgCdInSnSbTeIXeCsNaLanth

3、anoidesHfTaWReOsIrPtAuHgTl PbBiPoRnRaAcNFKrHeONeArElectron temperature : 6,680KElectron density : 1.4714 x 10 cm-1First Ionization Potential of ElementsAr 15.75eV01020304050607080900510152025Atomic numberIonisation potential(eV)He 24.58eVLiBeBCBaMgAlSiPSClKCaScVTiCrMnZnGaGeCuFeNiCoAsSeBrRbSrYZrNbMoT

4、cRuRhPdAgCdInSnSbTeIXeCsNaLanthanoidesHfTaWReOsIrPtAuHgTlPbBiPoRnRaAcNFKrHeONeAr8 eVInside DRCNH3+ArO+Fe+Mn+NH3 gas in+Ion-Molecule Reaction In DRCM IP(M)Ar 15.76 eVNH310.16 eVCa 6.11 eVAr+ + NH3 NH3+ + ArD D Hr = D D IP = - 5.6 eV (Exothermic reaction)k = 1.60 X 10-9 cm-3 molecule-1 second-1(*)Ca+

5、+ NH3 no reactionD D Hr = D D IP = + 4.0 eV (Endothermic reaction)k 10-13 cm-3 molecule-1 second-1 (*)+Ca+Ar+NH3+ELAN DRC Quadrupole Mass Filter Binary gold metallized ceramic rods for hyperbolic quadrupole field. Proven rock-solid mass calibration stability. Rapid scanning characteristics. On-the-f

6、ly custom resolution. ELAN DRC Dual-Stage Discrete Dynode DetectorPrinciple of Dual Mode DetectorAnalog countingPulse countingAmpDiscriminatorCounterAmpV/F converterP/A factorLow conc.High conc.GatePulse mode is used for lower concentration.Analog mode is used for higher concentration.Gate closes wh

7、en signals are too high.Sample preparation（1）1 Environment Major elements found in atmospheric particles include Al, K, Ca, Fe, Na, Mg and B. These same elements are also critical impurities in the solar grade silicon industry. In order to analyze ultra-trace levels of these elements, a class 1000 o

8、r better cleanroom is recommended for the ICP-MS.2 Sample bottlesSample bottles must be thoroughly cleaned prior to useResistivity:18.2M.CM 253 Ultrapure Water4 SEMI grade ultrapure HNO3 and HF Sample preparation（1）l Remove the first few surface layersl Digest the silicon in sealed PFA bottlesl Adju

9、sting the silicon matrix concentration at 1000-2000 ppm level by ultrapure waterl Analyze this solution (including boron)Sample preparation（2）Sample preparation（2）Separate analysis of phosphorus Interference: 30SiH, 14N16OHlThe sample solutions were heat to near dryness. lThe residues were then adde

10、d with several drops of concentrated HFlheat to near dryness againl These procedures was repeated for two more times then dissolved in diluent HFlAnalyze this solutionSupplierABCDEFGTypechunkchunkchunkchunkchunkchunkchunkElement B 13.844 28.935 20.713 25.069 31.061 21.446 17.386 Na 219.474 122.776 1

11、08.849 143.016 102.592 N.D.N.D. Mg 76.576 64.488 55.718 47.368 63.901 93.822 33.662 Al 318.064 379.558 374.141 337.526 401.566 392.710 378.378 K 54.802 43.436 42.053 48.913 46.189 32.108 27.972 Ca 727.083 548.591 372.136 1091.401 785.584 88.631 46.271 Cr 22.974 23.083 25.569 26.912 21.503 43.304 30.999 Fe 38.600 46.697 54.158 36.698 65.974 427.567 38.288 Ni 25.314 23.929 27.580 16.852 22.833 48.799 21.180 Cu 33.029 36.775 38.847 37.640 38.721 34.787 32.698 Zn 28.470 32.021 25.536 47.188 45.603 77.210 26.437