Tool IPA Recycling Technology *Takashi Futatsuki, Hiroki Narita, Kazushige Takahashi, and Hiroshi Sugawara

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1 Tool IPA Recycling Technology *Takashi Futatsuki, Hiroki Narita, Kazushige Takahashi, and Hiroshi Sugawara *Deputy General Manager, Electronics Industry BU, Plant Division, ORGANO Corporation

2 OUTLINE 1. Background and Purpose 2. Quality Target 3. System and Apparatus 4. Analytical Result 5. Operating Cost 6. Summary

3 Background and Purpose

4 Wafer Drying Technologies Method IPA Vapor Marangoni Rotagoni IPA Liquid SCCO2 Tool Type Batch Batch Single Single Single IPA Phase Vapor Vapor Vapor Liquid Liquid (Replacement) IPA Consumption Discharge Volume Large Very Large Large Very Large Discharged Concentration High (>20wt%) Very High (>80wt%) 1. IPA consumption and discharge volume is getting larger. 2. Discharged concentration is getting higher. Requirement of IPA recycling. 3. IPA is the final liquid chemicals contacted with wafer in new methods. Requirement of IPA (fresh as well) purification, because of final contact.

5 Purpose of this study Recycling IPA discharged from silicon wafer drying process Conventional recycling technology is distillation - Well established technology - The recycled IPA quality is fine - However, it needs high distillation tower and huge energy for evaporation - Distillation tower cannot be installed by the process tools (never in the same building) To develop a compact IPA recycling system with low energy consumption.

6 Quality Target

7 Quality Target of recycled IPA Raw Materials (waste IPA from drying process) Quality Target (Recycled IPA) IPA Concentration 20 80wt% >99.9wt% Metals 10ppb < 0.1ppb Si - < 1ppb Anions 10ppb < 0.4ppb Particles 200nm - < 100#/mL note Assumption EL-IPA grade On-site IPA recycling and purification system.

8 System and Apparatus

9 Schematic Flow Diagram of the System UPW Wafer Dryer Discharged IPA Ultrasonic Atomization Pre-conc. (>80wt%) Vapor Permeation Conc./ Purification (>99.9wt%) Fresh IPA 99.99wt% <Features> 1. Compact (small space). 2. On-site treatment 3. Low energy consumption. 4. Quick start up.

10 Ultrasonic Atomization H 2 O IPA Atomization Vaporization Mist generation by ultrasonic. Mist separation by size. Smaller energy than evaporators

11 Laboratory System of Ultrasonic Atomization Recovery Rate 95% B Mist or Gas Liquid Cyclone Ultrasonic Atomization Heater Chiller P Condenser IPA: >85wt% IPA Treated IPA/H 2 O solution IPA: 20wt%

12 Laboratory System of Ultrasonic Atomization Condenser Cyclone Air Pump IPA treatment : 0.2 kg/h Atomizing Unit (magnification)

13 System Flow Example of Ultrasonic Atomization Ultrasonic Atomization Ultrasonic Atomization Ultrasonic Atomization IPA: 85wt% Product Drainage IPA: <1wt% Discharged IPA IPA: 20wt%

14 Comparison Evaporator and Ultrasonic Atomization Stopping Operating Operating Evaporator Whole Operation High Temperature Long Starting Time Ultrasonic Atomization Flexible Operation Low Temperature Short Starting Time

15 VP (Vapor Permeation) Separation Image Zeolite Membrane IPA/H 2 O (Vapor) H 2 O(Vapor) Vacuum IPA <Dewatering by zeolite membrane> 1. Selective adsorption on the membrane. 2. Selective diffusion in the membrane. 3. Desorption from the membrane by vacuum.

16 VP Test Apparatus Front Back Zeolite membrane IPA treatment : 2 kg/h

17 System Flow of VP and Purification Recovery Rate 93% MF P.O.U (Tool) IPA: >99.9wt% Ion adsorption membrane Tank VP membrane Tank Pump Condenser Condenser Ion exchange resin No.1 Evaporator No.2 Evaporator IPA: 85wt% IPA Waste

18 Analytical Result

19 Analytical Results unit Fresh IPA - spec Fresh IPA - data Recycled IPA - data IPA Conc. % >99.99 > >99.9 Water % < <0.1 Cl ppb <5 <0.3 <0.3 SO4 ppb <5 <0.3 <0.3 Al ppb <0.1 <0.05 <0.05 Ca ppb <0.2 <0.10 <0.10 Cu ppb <0.1 <0.05 <0.05 Fe ppb <0.3 <0.10 <0.10 Na ppb <0.2 <0.10 <0.10 Ni ppb <0.1 <0.05 <0.05 Pb ppb <0.1 <0.05 <0.05 Zn ppb <0.1 <0.05 <0.05 Particle >30 nm /ml <

20 Operating Cost

21 Pre-concentration by Ultrasonic Atomization - Cost <Conditions> Starting Treated :IPA=20wt%, 250kg/h :IPA=85wt%, 56kg/h IPA loss :5% <Cost Estimation> Ultrasonic Atomization (Pre-conc.) Operating Cost :12 JPY/kg Foot Print (m) W1.5 L2.0 H3.0

22 VP & IEX Purification - Cost <Conditions> Starting Treated :IPA=85wt%, 56kg/h :IPA>99wt%, 44kg/h IPA loss :7% <Cost Estimation> VP & IEX Purification Operating Cost :30 JPY/kg Foot Print (m) W4.0 L3.0 H2.5

23 Total Cost (Ultrasonic Atomization +VP & Purification) <Conditions> Starting Treated :IPA=20wt%, 250kg/h :IPA>99wt%, 50kg/h IPA loss :12% Fresh IPA cost :200 JPY/kg <Estimation> Pre-conc. VP & Purification Fresh IPA Total : 12 JPY/kg : 30 JPY/kg : 23 JPY/kg : 65 JPY/kg

24 Total Cost Evaluation Starting : IPA=20.0wt% 250kg/h Treated : IPA>99.9wt% 50kg/h IPA recovery cost = Initial cost + Operating costs

25 Summary

26 Summary Recycling IPA discharged from silicon wafer drying process Ultrasonic Atomization +VP & Purification - Pre-concentration by Ultrasonic Atomization (to 85%) - Concentration by Vapor Permeation (to 99.5%) - Purification (metal removal) by Ion Exchange (less than 0.05 ppb) Featuring compact and low energy consumption, the system can recycle IPA by the process tools with economical benefits.

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