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VPD-ICPMS – ICPMS trace metals analysis for bare Si

Cerium Labs’ VPD-ICPMS starts with the vapor phase decomposition sample preparation technique by which trace elements on the surface of a silicon wafer are …

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Source: ceriumlabs.com

Date Published: 11/15/2021

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Vapor Phase Decomposition – VPD ICPMS Online Monitoring …

Radian VPD ICPMS (Vapor Phase Decomposition) is a high-throughput, completely automated production tool for online monitoring of metal contamination on …

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Date Published: 1/16/2021

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VPD-ICP-MS Analysis Service – Aystorm Scientific

Wafer Testing, Trace Metal Contamination, Nobel Metals,VPD-ICP-MS and TXRF Analysis, Process Monitoring.

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Analysis of Metallic Impurities in Si Wafers Using Fully …

Schematic diagram of the VPD-ICP-MS system. Page 3. 3. The Expert_PS VPD system was designed to be compatible with.

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VPD ICP-MS presentation to CIMPACA members_v2

Automated VPD drasticallly improve detection limits! Unit 108/cm²on. 8 in wafer. TXRF. Manual VPD. ICP-MS. Automated.

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주제와 관련된 이미지 vpd icp ms

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P10-2 Agilent 7700 Series ICP MS Animation
P10-2 Agilent 7700 Series ICP MS Animation

주제에 대한 기사 평가 vpd icp ms

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Cerium Labs – ICPMS trace metals analysis for bare Si

Cerium Labs‘ VPD-ICPMS starts with the vapor phase decomposition sample preparation technique by which trace elements on the surface of a silicon wafer are collected into a liquid sample to be analyzed by HR-ICP-MS. The silicon wafer (150, 200 and 300 mm) is exposed to hydrofluoric acid vapor in a sealed chilling chamber. The hydrofluoric acid vapor forms a condensate on the chilled wafer surface. This condensate etches the oxide layer off of the wafer surface along with any trace metals that are present. The condensate is then collected by rolling a drop of scan solution (a dilute mixture of hydrogen peroxide, nitric acid, and hydrofluoric acid) across the surface of the wafer. The drop is transferred from the wafer surface into a clean sample vial. The liquid sample is then analyzed for trace metals using HR-ICP-MS. The VPD technique is capable of measuring metallic contaminants at concentrations ranging from 1E6 to 1E14 atoms/cm2. It is particularly useful in measuring light elements (e.g., lithium, beryllium, boron, sodium, magnesium and aluminum) on bare silicon or in hydrofluoric acid soluble thin films.

VPD ICPMS Online Monitoring of Silicon Wafer Top/ Bottom Surface and Edge for Metal Contamination

Online Monitoring of Silicon Wafer Surface and Edge for Metal Contamination

The Radian VPD-ICPMS (Vapor Phase Decomposition) is a high-throughput, completely automated production tool for online monitoring of metal contamination on semiconductor wafers with ultra-low detection limits. The Radian’s single process station design, ultrafast scanner, and fully integrated ICPMS makes it the fastest, most automated Vapor Phase Decomposition in the world.

Vapor Phase Decomposition, VPD and ICPMS, VPD ICP MS, icpms analysis, semiconductor wafer analysis, VPD ICPMS, metal contamination, VPD monitor

[PDF] Fully Automated VPD ICP-MS System. Rousset Technology Center STMicroectronics

Fully Automated VPD ICP-MS System. Rousset Technology Center STMicroectronics

DOWNLOAD PDF (2.8MB)

Short Description

Description

Fully Automated VPD ICP-MS System

P.Maillot Rousset Technology Center STMicroectronics October 2011

Outline

Area of interest

? Standard industry monitoring Principle of VPD and ICP-MS CIMPACA equipment description Acceptance test Applications Conclusion

Acknowledgements • Success of this project was made possible thanks to the 2009 evaluation team – – – – – – – – –

E. Lattard LFoundry C. Galvez Tera D. Goguenheim IM2NP H. Wortham LCP F. Michel Vegatec C.Grosjean ST/CIMPACA A. Planchais ST/CIMPACA C. Martin ST P. Maillot ST

Acknowledgements • Installation and qualification was made possible thanks to – – – – – –

I. Poulet Tera D.Vacher Air Liquide S. Giorgi Air Liquide A. Planchais ST/CIMPACA C. Martin ST P. Maillot ST

– And the local ST EES/facilities/hook-up team!

Basic Metal behavior

Segregation

Ex: Ti

SiO2

Precipitation Diffusion

Ex: Fe

Ex: Cu

Si

Basic Metal behavior Wet Clean, Plasma Implant/Recoil or Diffusion Bulk monitoring

Surface monitoring

SiO2

Si

Standard industry monitoring • Surface – Sweeping TXRF • Bulk : – Post anneal SPV (or equivalent lifetime measurement technique)

7

Drawbacks TXRF Limited in terms of detection limits 3 beam needed to cover all elements Edge exclusion No bevel capability SPV No specie ID except for Fe Indirect techniques / Artifacts / Data interpretation Edge exclusion No bevel capability 8

Thus we needed Improved detection limits Specie identification over the whole atomic table VPD ICP-MS combines both capabilities

9

VPD principle Vapor Phase Decomposition

Etching of SiO2 Layer with HF Vapor

ICP-MS principle Inductively Coupled Plasma Mass Spectrometry

Limitation of Conventional VPD • Loss of scan solution during scan due to poor holding capacity. • Thicker bulk-Si or poly-Si etching difficult • Recovery of thicker nitride film impossible. • Full wafer collection only giving average value • Manual wafer handling and manual transferred of droplet to ICP-MS / cross contamination risk • A separate system is required to perform bevel scan.

Standard VPD is blind to energetic or diffused contaminants • Thus post implant or diffusion requires bulk VPD monitoring

Specie Calcium Sodium Magnésium Aluminum Potassium Titanium Chromium Iron Cobalt Nickel Copper Zinc Molybdenum

Surface 1.13 2.91 0.57 27.24 0.65 0.32 0.22 1.43 ND 0.08 ND 0.3 0.29

Bulk 3.34 1.29 0.85 34.67 0.35 12.59 0.1 0.92 ND 0.14 3.18 0.11 278.9

0.13 1.45 *Maillot/ Roux (STMicroelectronics) . Tungsten 18th international conference on ionVPD ICP-MS data in units of 1010at/cm² implantation technology (IIT2010), Kyoto , Japan, June 2010

Automated VPD ICP-MS • • • • • • •

Risk of loss of scan solution drastically reduced No edge exclusion Bulk-Si or poly-Si analysis Thick nitride analysis Bevel analysis Partial analysis , local analysis SMIF enclosure , automation of wafer handling , scan and droplet transfer to ICP-MS minimize risk of cross contamination

CIMPACA equipment overview VPD : ExpertTM from IAS ICP-MS : NexIonTM from Perkin-Elmer

VPD ICP-MS CIMPACA lab

ExpertTM VPD system

NexIonTM ICP-MS

Interface between VPD and ICP-MS

Sas for chemicals

Inside ExpertTM

Inside ExpertTM

Operation sequence (1/3)

Operation sequence (2/3)

Operation sequence (3/3)

VPD chamber Local Exhaust

EPD Sensor Port

Wafer Load Sensor

VPD Chamber

VPD chamber

HF vapor in

Si wafer with various film layer

HF vapor in

Si wafer is placed in a VPD chamber, where HF vapor is introduced and HF vapor etches layers of films on bare-Si wafer. Metallic impurities remain on the bare Si wafer. VPD can etch various types of film on bare-Si wafer.

Qualification test and tool capabilities

Acceptance specification and results N o.

Parameter

Specification

Result

>90% all elements listed in Table 7, except Au and Passed Ag < 0.2%, less than 1 out of 500 wafers. Continued. Depending on the wafer Remarks 1 Collection efficiency 2 Droplet loss: wafer surface and edge 3 Bevel capability Functional. Passed 4 Droplet drying for TXRF : positioning Within 1mm from wafer centre Passed 5 Detection limit : VPD (8” wafer) As per supplier specifications Passed (Table 5 - 6) 6 Detection limit : LPD As per supplier specifications Passed (Table 7) 7 Partial analysis (ring, sectors..) N/A Passed Demonstration on 31-May 8 Process of several wafers with different recipes in the same run Capability Passed Demonstration on 31-May 9 Auto calibration ICP-MS Choice among 1/wfs Passed Demonstration on 31-May 10 Particle contamination Continued. 11 Metal contamination from handling 12 Overall throughput < 2 added per load/unload < 10% of added contaminant per specie after VPD + load /unload cycles (Need to clarify how to perform the test) Bare-Si: > 6 wafers/hr

Specification to be changed. Table 9

13

VPD , ICP-MS and VPD ICP-MS communication and handling failures

< 0.2%, less than 1 out of 500 wafrers. Continued. 14 Software VPD and ICP-MS Fully functional as per supplier specifications Passed Demonstration on 31-May 15 Security As per specifications Passed Demonstration on 31-May 16 Wafer counter Capability to log the number of processed wafers and provide pareto per user Passed Demonstration on 31-May Passed Table 1 Table 2 - 4 Demonstration on 31-May Au exempted because of no standard solution. Au exempted because of no standard solution. Table 8 Automated VPD drasticallly improve detection limits! Unit 108/cm²on 8 in wafer TXRF Manual VPD ICP-MS Automated VPD ICP-MS Al 5000 18 0.6 Ti 150 10 1.7 Cr 225 9 0.9 Fe 60 9 0.5 Co 60 8 0.2 Ni 100 8 0.3 Cu 60 8 0.08 Zn 150 7 0.3 Mo 580 3 0.3 W 1250 3 0.04 Recovery Test Results (Bare Wafer) Elements 1st Scan 2nd Scan 3rd Scan Total Recovery (%) Li 4.688 0.002 0.001 4.690 99.9 Na 7.737 0.034 0.007 7.778 99.5 Mg 6.700 0.101 0.024 6.824 98.2 Al 32.598 0.900 0.030 33.529 97.2 K 7.179 0.041 0.004 7.223 99.4 Ca 7.105 0.352 0.304 7.761 91.5 Ti 3.403 0.003 0.001 3.406 99.9 Cr 5.188 0.045 0.007 5.240 99.0 Mn 5.105 0.006 0.001 5.112 99.9 Fe 9.465 0.311 0.062 9.838 96.2 Co 3.067 0.002 0.001 3.070 99.9 Ni 5.357 0.019 0.001 5.377 99.6 Cu 2.861 0.429 0.001 3.291 86.9 Zn 4.322 0.012 0.001 4.335 99.7 Ge 3.294 0.003 0.001 3.297 99.9 As 2.865 0.004 0.001 2.869 99.8 Cd 3.293 0.001 0.001 3.295 99.9 In 3.272 0.002 0.001 3.275 99.9 Ba 2.197 0.130 0.019 2.346 93.6 Ta 3.660 0.001 0.001 3.662 99.9 W 3.712 0.036 0.001 3.749 99.0 Pb 2.791 0.053 0.003 2.847 98.0 Matching with manual VPD (AL Crolles) - Deposition on wafer of 1 ml droplet with 1000 ppb by element Global incertitude includes Wafer contamination (droplet deposition) Wafer drying Wafer transportation Wafer analysis Element Li:7 Na:23 Mg:24 Auto 1 1138 1137 Auto 2 1140 Auto 3 Al:27 K:39 Ca:40 Ti:48 Cr:52 Fe:56 Ni:58 882 836 998 708 899 846 745 938 922 922 1127 1038 1698 955 1118 832 871 1028 715 894 804 728 911 926 926 1128 1062 1671 945 1158 1159 873 777 1045 689 895 818 711 903 912 959 1123 1073 1721 967 Man 1 NA 1728 1476 1018 1120 1648 1156 684 1296 692 684 908 1180 888 NA 916 Man 2 NA 1352 1284 856 736 1028 868 648 876 684 700 960 760 960 NA 1024 Man 3 NA 1412 1280 924 720 836 952 652 884 696 684 1032 744 948 NA 960 21% 49% 13% 16% 32% 11% 20% 21% 25% 25% 3% 21% 12% Delta % Co:59 Cu:65 Zn:66 Mo:95 Ta:181 W:184 1% Various Scan Patterns X Z (1) Full (2) Radial (3) Square Sector (4) Radial Sector Y R • Synchronized operation and works on the same method (5) Bevel Partial scan exemple : ONO contamination , partitioning • Suspicion of ONO furnace contamination – – – – – Outer sector VPD : OK Inner sectors VPD : Metal x identified Full wafer NO : nOK Full wafer O : OK Full wafer N : nOK – Great added value for root cause analysis , in this case using only 4 test wafers Partial scan exemple : Post implant Al monitoring Metal y concentration was found to be 2x higher in outer sector Qualified recipes • • • • • • • • • Bare wafer : native oxide Oxyde : up to 500nm Nitride : up to 100nm Poly : 100 and 250nm ONO Radial analysis : 5 sectors Bevel Bulk Si : full wafer down to 1µ µm Local bulk (20mm) : down to 20µ µm by 3µ µm steps (still in qualification mode) Bulk-Si and Poly-Si Etching 2 • Using ozone introduced into VPD chamber together with HF • Air based Ozone : 2.5nm/min • Oxygen based Ozone : 25nm/min • Wafer is cooled during VPD • Wafer is dried after VPD 3 4 Exemple : Poly-Silicon VPD 1 Poly 400 Å + Oxide 1,000Å 2 after 5min 3 4 after 10min after 15min Full Bulk-Si Etching 1 2 3 4 Typical VPD Etching Rate Film Etch rate (nm/min) SiO2 (LPCVD) 70 SiO2 (CVD) (HDP) 80 Si3N4 (LPCVD) 3 – 14 SiON (CVD) 90 Poly-Si (LPCVD) 7 - 14 Bulk-Si 15 - 25 BPSG (CVD) 100 PSG (CVD) 90 . Detection Limit, LPD (Bulk Etching) Unit: Atom/cm3 Bulk etching type Etched Area (cm2) Etched Depth (cm) Etched volume (cm3) Scan Volume (uL) Li Na Mg Al K Ca Ti Cr Mn Fe Co Ni Cu Zn As Mo Ag Ba Ta W Au 12" Full surface 707 0.00001 (0.1µm) 0.00707 250 Spec Measured 4.00E+13 2.70E+12 1.00E+13 4.65E+12 1.20E+13 4.29E+12 1.00E+13 4.82E+12 1.20E+13 1.89E+12 8.00E+12 3.51E+12 4.00E+13 5.23E+12 8.00E+12 2.87E+12 2.00E+12 1.84E+12 6.00E+12 1.62E+12 2.00E+12 6.81E+11 4.00E+12 8.66E+11 4.00E+12 2.40E+11 4.00E+12 8.27E+11 1.60E+12 1.40E+12 1.20E+12 8.55E+11 1.00E+12 2.61E+11 6.00E+11 2.10E+11 6.00E+11 3.02E+11 1.00E+12 1.37E+11 8.00E+11 4.67E+11 Local area 3.14 0.0001 (1µm) 0.000314 250 Spec Measured 9.00E+14 6.08E+13 2.25E+14 1.05E+14 2.70E+14 9.66E+13 2.25E+14 1.08E+14 2.70E+14 4.26E+13 1.80E+14 7.90E+13 9.00E+14 1.18E+14 1.80E+14 6.46E+13 4.50E+13 4.14E+13 1.35E+14 3.64E+13 4.50E+13 1.53E+13 9.00E+13 1.95E+13 9.00E+13 5.40E+12 9.00E+13 1.86E+13 3.60E+13 3.14E+13 2.70E+13 1.92E+13 2.25E+13 5.88E+12 1.35E+13 4.72E+12 1.35E+13 6.80E+12 2.25E+13 3.08E+12 1.80E+13 1.05E+13 Local area 3.14 (20µm) 0.002 0.00628 250 Spec Measured 4.50E+13 3.04E+12 1.13E+13 5.23E+12 1.35E+13 4.83E+12 1.13E+13 5.42E+12 1.35E+13 2.13E+12 9.00E+12 3.95E+12 4.50E+13 5.89E+12 9.00E+12 3.23E+12 2.25E+12 2.07E+12 6.75E+12 1.82E+12 2.25E+12 7.66E+11 4.50E+12 9.75E+11 4.50E+12 2.70E+11 4.50E+12 9.31E+11 1.80E+12 1.57E+12 1.35E+12 9.62E+11 1.13E+12 2.94E+11 6.75E+11 2.36E+11 6.75E+11 3.40E+11 1.13E+12 1.54E+11 9.00E+11 5.25E+11 Local Bulk Etching Dual Scan Nozzle holds the scan solution at a spot size of 20 mm and etches around 20 um within 15 minutes. Local Bulk Etching Depth Profile 40 um depth 20 um depth Drying + post analysis • Collected droplet deposition in center of cleanwafer • Drying • Wafer unload • Then droplet residue can be analysed by ToF-SIMS Calibration and SPC Calibration Item Setup Calibration 5 /week 4 concentrations all elements Redo if QC is OOC Detection Limits 2/week QC 1 concentration , every 15 wfs Blank Every 2h or after contaminated wafer Rince After contaminated Wafer – ASAS automatically adds internal standard solution that compensates matrix effect – Droplet volume in data report SPC • Wafer type 1 : post wet bench class 1 RCA clean , to validate the whole measurement chain contamination level . Reusable • Wafer type 2 : post As implant in oxyde. To validate VPD cycle ( dissolution and collection) • Wafer type 3 : Post load /unload added particule Software Expert Software Main Screen Expert Recipe Set Up Screen MCM Recipe Set Up Screen Type wafer information MCM Main Screen VIS Main Screen Results of Radial Scan VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD Radial results Results of S-Sector Scan VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD VPD S-Sector results Typical report Numéro d'analyse et référence de l’échantillon Unités 10^10at/cm2 Eléments Symbole Lithium Li Comments 1 Fully Automated ICP-MS System P.Maillot Rousset Technology Center STMicroectronics October 20112 Outline? Area of inte...

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