Reduction of outgassing rate and photon stimulated desorption yield
Transcription
Reduction of outgassing rate and photon stimulated desorption yield
IUVSTA WS-63 Workshop for “Surface phenomena limiting ultimate pressures inVacuum Systems”, Residencia Santo Tomás, Ávila, Spain, Sep. 14-19 (2010) Reduction of outgassing rate and photon stimulated desorption yield by ozonate water cleaning process for the large accelerator vacuum system Gao-Yu Hsiung Vacuum Group NSRRC, TAIWAN E-mail: [email protected] 1 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Outline Why the ozonate water cleaning How to do it What we have found Conclusions 2 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Why the Ozonate water cleaning A Synchrotron Light Source needs a vacuum vessel with extreme low pressure for accommodating the circulating electron (positron) beam, without the scattering or interactions with the residual outgas molecules, that allows the beam maintains a smallest emittance, highest stable qualities, and the long life time. The problem of the accelerator is limited space for the pumps to remove the outgas from the beam ducts effectively. The only solution for reaching a lowest pressure is to provide an extreme clean surface that results in an extreme low outgassing rate for the beam ducts. 3 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Synchrotron Light Sources in Taiwan Taiwan Light Source (TLS) is the 2nd third generation light source (1993) VUV SX HX 1E16 U9(1) Hsinchu Science Park Flux (Phot/s/0.1%bw) 1E15 (3) EPU5.6(1) SP8-IVXU3.2(1) U5(1) (3) (3) (5) (5) (7) SW6 1E14 1E13 (3) (5) (7) SP8-BM IASW6 W20 BM 1E12 SWLS Electron Storage Ring (1.5 GeV) 1E11 0.1 LINAC (50 MeV) Booster Ring (1.5 GeV) 1 10 HX VUV SX VUV SX Circumference – 120 m Critical Energy – 2.14 keV 1996 – Ramping to 1.5 GeV Natural Emittance – 25 n mrad 2000 – 1.5 GeV Full Energy Injection (200 mA) 2004 – Operation with Superconducting RF Cavity Average Pressure (200 mA) – 0.68 nTorr Accumulated Dose > 8000 Ah 2005 – Top-up Injection at 300 mA Life Time – 10 h 1993 – Operation 1.3 GeV 5 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 100 1000 10000 Photon Energy (eV) HX HX HX HX HX SX ID in operation W20 (1995) 4 ~ 15 keV U10 (1995) 3 ~ 500 eV U5 (1997) 60 ~ 1500 eV U9 (1999) 4 ~ 100 eV EPU5.6 (1999) 60 ~ 1400 eV SWLS (2002) 4 ~ 30 keV SW6 (2004) 6.5 ~ 19 keV IASW6 (2006) 6.5 ~ 19 keV New ID in planning 2nd IASW6 (2009) 3rd IASW6 EPU4.6 G.Y. Hsiung The major beam ducts for the electron storage ring is made of Al-alloys Undulator SC Wiggler SRF BM SR Front End e- SGV Vacuum Chambers NEG e6 SIP IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 Electron Storage Ring G.Y. Hsiung The pressure increases when installing new insertion Top-up devices and needs beam scrabble cleaning 1.3 GeV 200 mA Averaged Pressure per Beam Current (Pa/mA)_ 1.0E-09 Install ID W20 9.0E-10 1.5 GeV 1.5 GeV Replace new 300 mA Kicker Chambers Install SRF Cavity 200 mA Install ID-CH EPU5.6 + U5 Install ID-CH U9 8.0E-10 7.0E-10 Install New FE 6.0E-10 Install ID IASW6 Replace ID IASW6 Install ID Install ID SWLS SW6 5.0E-10 4.0E-10 3.0E-10 2.0E-10 1.0E-10 07/01/1993 YEAR/MONTH 15.5 years (iv) 2008/07 2007/07 (iii) 2006/07 2005/07 2004/07 2003/07 2002/07 2001/07 2000/07 (ii) 1999/07 1998/07 1997/07 1996/07 1995/07 (i) 1994/07 1993/07 0.0E+00 12/31/2008 Ref. G.Y. Hsiung, PAC’09 7 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung The beam life time reduces after installation of new Top-up vacuum devices (new absorbers) 1.3 GeV 1.5 GeV 1.5 GeV 200 mA 200 mA 300 mA 5000 Beam Current × Life Time (mA h)_ 4500 Install ID W20 4000 Install ID-CH EPU5.6 + U5 Replace new Kicker Chambers Install ID SWLS Install SRF Cavity Install ID-CH U9 3500 Install ID SW6 3000 Install New FE 2500 Install ID IASW6 Replace ID IASW6 2000 1500 1000 07/01/1993 YEAR/MONTH 15.5 years (iv) 2008/07 2007/07 (iii) 2006/07 2005/07 2004/07 2003/07 2002/07 2001/07 2000/07 (ii) 1999/07 1998/07 1997/07 1996/07 (i) 1995/07 1993/07 0 1994/07 500 12/31/2008 Ref. G.Y. Hsiung, PAC’09 8 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Aluminum Alloys (Al) Vacuum Chambers for the TLS Storage Ring Downstream chamber wall of B-chamber, act as the photon absorber, absorbs the non-used synchrotron light. B-Chamber • CNC machining in pure alcohol • Freon cleaning before welding • TIG welding in clean room S-Chamber • Al Extrusion • Chemical cleaning by acid • TIG welding in clean room ID-Chamber • Al Extrusion • Chemical cleaning by acid 9 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Oil-free manufacturing process for Al Bending chambers provides high reliable quality 3) Surface Cleaning 1) NC Machining with Ethyl Alcohol 4) DIP Installation 2) Dimension Check After Machining 5)Welding in Clean Room 9) Installation in the Tunnel 8) Pre-assembly In Lab 10 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 7) Leak Test 6) Deformation Check AfterWelding G.Y. Hsiung Assembly, Welding and Testing (at NSRRC) for the BChamber Assembly TIGWelding Vacuum Test 11 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Need to request the commission period for Beam-cleaning to reduce the PSD yields (dynamic pressure) (weeks ~ months) Pressure rise per beam current and Desorption coefficient in B-ch (ηB) during beam cleaning. Desorption coefficient at S-ch (ηS) and B-ch (ηB) TMP pumps were useful for removing the large amount of PSD outgas during the commissioning. (a) (b) 100 Ah 12 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 Ref. G.Y. Hsiung et al, J.Vac. Sci.Technol. A13, 2569 (1995) G.Y. Hsiung TLS Operation Experiences - Pressure Requirement 200 mA × 10 hours 100 Ah 13 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Residual Gases of PSD from TLS Major PSD Outgas : H2 (93%) > CO (4.4%) > CO2 (1.2%) > CH4 (0.5%) ~ H2O (0.5%) Ref. G.Y. Hsiung et al, J.Vac. Sci.Technol. A12(4), 1639 (1994) 14 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 Ref. G.Y. Hsiung et al, J.Vac. Sci.Technol. A13, 2569 (1995) G.Y. Hsiung The 3 GeV TPS Vacuum System Vacuum system for TPS (e-beam) storage ring (SR): Lattice : 24 DBA, ξ= 2 nmrad Straight : 12m (6)+7m (18) E = 3 GeV, Imax = 400 mA (top-up) Booster (concentric with SR) : 3 GeV full energy injection Design safety margin: 28% (heat load from 3.3 GeV, 350 mA) Requirements of SR vacuum system: Ultra-high vacuum (UHV) High reliability High stability 15 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Layout of 1/6 Super periods (L = 86.4 m) 12 m 1 7m 7m 2 3 1. 2. 3. 4. 16 One Cell (1/24) Vacuum System Bending beam ducts Straight beam ducts Beam ducts for Insertion Devices (ID) IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 4 7m G.Y. Hsiung 24 Arc Cells of Vacuum System SGV S3 B1 S4 B2 SGV 17 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Vacuum Design of One Cell Simple structure of vacuum beam ducts along the beam channel, no flange, few absorbers, few bellows, for lowering the impedance. Completely oil-free and precise CNC machining for the B-chambers and TIG welding in the clean room to obtain a clean surface with lowest surface outgassing rate and the consequent lowest pressure. Strong back supports for the BPM fixed on the girders for positioning the BPM precisely and cooling channels drilled through the B-chambers provides an uniform temperature control for assuring the BPM shift < 0.1 micron against the thermal stress. 18 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 1. Button : φ6.9 mm 2. Gap : 0.3 mm 3. Distance : 17.5 mm 4. Angle : 6.7° G.Y. Hsiung Main Chambers for One Cell S3 BPM Pumping port Bellows B1 S4 B2 19 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung The electron storage ring request an extreme low outgassing rate Vacuum system for 3 GeV TPS electron storage ring requests an average pressure (P) < 1×10-9 Torr in the chambers, which depends on the rate of thermal outgas (QTH), the rate of photon stimulated desorption (QPSD), and the effective pumping speed (S). P (QTH Where QPSD ) / S K1 q A K2 I q : surface outgassing rate (Torr·l·s-1·cm-2) of chambers A : area (cm2) of chamber surface produces outgas η: yield (molecules/photon) of photon stimulated desorption of photon absorbers I : electron beam current (mA) K1, K2 : proportional constants Typically in case of P < 1 nTorr : q < 1×10-13 Torr·L/(s·cm2) η < 1×10-4 Molecules/photon 20 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Cleaning methods for the chambers The popular cleaning methods: Aluminum chambers Chemical cleaning with HNO3/HF acid (CERN*, TLS) for Al extrusion chambers Oil-free CNC machining in pure alcohol and Freon cleaning (TLS) for Al bending chambers Copper chambers Chemical cleaning with Citranox (APS) Cleaning processes with the solutions of HF, Freon, etc. will be replaced by the ones without polluting the environment. * Ref. A.G. Mathewson et al, J.Vac. Sci.Technol. A7(1), 77 (1989) 21 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Chemical cleaning for Al extrusion chambers 1. Immersion in NaOH (45 g/L) at 45 ºC for 1~2 minutes. 2. Rinsing in demineralized water. 3. Immersion in an acid bath containing HNO3 (50% by volume) and HF (3% by volume). 4. Rinsing in demineralized water. 5. Ultrasonic bath in demineralized water (R > 10 MΩ) for ~ 20 minutes. 6. Drying. * Ref. A.G. Mathewson et al, J.Vac. Sci.Technol. A7(1), 77 (1989) 22 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung AES of Al samples after Chemical cleaning 3.0E+04 “F” is resided on the surface after chemical cleaning 2.0E+04 1.0E+04 0.0E+00 0 -1.0E+04 -2.0E+04 C 500 F 1000 O 1500 Al 5.0E+04 O 4.0E+04 -3.0E+04 F 3.0E+04 Al O 2.0E+04 F 1.0E+04 C Al C 0.0E+00 0 23 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 1 2 3 4 G.Y. Hsiung Motivations of using Ozonate water An effective cleaning method with ozone gas for the reduction of carbon contamination from the surface has been investigated by T. Momose [1]. Another method of ozonate water cleaning for the superconducting rf cavities studied by K. Asano [2] shows good results of removing the surface contaminations. Replace the Freon cleaning process with ozonate water cleaning for Aluminum B-chambers after ethanol machining. Ozonate water may remove the residual F atom from the Al extrusion chambers [1] T. Momose, Y. Maeda, K. Asano and H. Ishimaru, J. Vac. Sci. Technol. A13(3), 515 (1995). [2] K. Asano, T. Furuya, S. Mitsunobu, T. Tajima and T. Takahashi, “Stable Performance of 508-MHz Superconducting RF Cavities for KEK B-Factory”, KEK Preprint 95-191 (1996). 24 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung How to do it? Key is to produce a very clean surface from the beginning! Completed oil-free manufacturing process for Al B-chamber Oil-free CNC machine in dust controlled clean room Ethanol machining environment with pure alcohol spray Dry ambient atmosphere for the machined chambers Dry compressed air (H2O < 1 ppm) for spray system Dry N2-filled aluminum bag for wrapping the machined chambers Ozonate water cleaning for unpacked Al chambers prior to the TIG welding in the clean room 25 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Machining for the TPS Al B-chambers (~ 4 m) Oil-free CNC Machining in Clean Room CNC Machining Processes (sprayed with pure alcohol) 26 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Ozonate water Cleaning for the B-chamber Aluminum half plates, for 4 m Bending chambers, packed after oil-free machining Ozonated Water Cleaning (> 20 ppm) 4. Transport to Welding room 1. Ozonate water vessel 2. Immerse chamber in Ozonate water (30 min) Unpack and Prepare for Cleaning 27 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 3. Drying in Clean booth G.Y. Hsiung Welding for the B-chamber in clean room Upper and Lower Halves B-Chamber Alignment Alignment with Pins 28 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Welding for B-chambers Manual welding for rest parts Auto welding for straight sides B1 29 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Summary of welding procedure for Bchambers 1. Manual TIG welding for pumping ports of each halves. 2. Auto TIG welding for both non-parallel straight sides, with 6 torches ignited simultaneously. 3. Manual TIG welding for rest curved sides. 4. Machining the end ports. 5. Manual TIG welding for end ducts, flanges, and cooling tubes. 30 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Assembly of 14m vacuum cell, in-situ welding, and vacuum baking (150°C, 24h) 31 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung What we have found Prepare the Aluminum and Copper test samples AES - Surface analysis, depth profile SIMS - Surface contaminations Kevin Probe – Surface Work function Thermal outgassing rate Photon stimulated desorption yield 32 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Sample preparation for cleaning test • Ethanol machining : only Ethanol machining • Chemical cleaning : regular machining and chemical cleaning • Ozonate water cleaning : Ethanol machining and immerse in ozonate water for 30 minutes • Citranox cleaning (Cu) : regular machining and citranox cleaning Chemical cleaning process: NaOH (45 g/L) at 45 ℃ for 2 min → bubble bath in DI water for 10 min → (50 % HNO3 + 3 % HF) for 2 min → bubble bath in DI water for 10 min → ultrasonic rinsing for 2 min → drying with pure nitrogen gas Citranox cleaning process: 2% Citranox in 60℃ DI water and ultrasonic rinsing for 10 min → DI water rinsing for 10 min → drying with pure nitrogen gas 33 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung AES surface inspection Surface analysis of AES for Al samples without photon exposure Chemical cleaning 6.7ppm ozonated water cleaning Only ethanol machining 34 The Al samples with ozonate water cleaning provide lowest carbon resided on the surface in comparison with those samples cleaned with either chemical cleaning or ethanol machining. IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Al samples - (a) Original (CNC machining) ; (b) O3 water cleaning (a) Original O C (31%) Al Al O C (b) O3 water cleaning O C (7%) Al O Al C Low Carbon 35 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Thermal Outgassing Rate (Aluminum) 1.0E-07 (a) (b) 1.0E-08 (c) 1.0E-09 q(torr L/sec cm2) ♦♦♦ (a) O3 Water Cleaning 臭氧水清洗 ---- (b) Ethanol CNC Machining 酒精加工 xxx (c) Chemical Cleaning 化學清洗 1.0E-10 After Baking : 1.0E-11 (c) Chemical cleaning q72 = 9.5×10-14 Torr·L/s·cm2 1.0E-12 (b) Ethanol CNC Machining q72 = 1.4×10-14 Torr·L/s·cm2 1.0E-13 1.0E-14 1.0E-15 1.E-04 (a) O3 Water Cleaning q72 = 4.8×10-15 Torr·L/s·cm2 1.E-03 1.E-02 1.E-01 1.E+00 1.E+01 1.E+02 1.E+03 1.E+04 * 1 Torr·L/(s·cm2) ~ 1330 Pa·m/s TIME (hour) 36 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Photon exposure experiments taken at 19B(PSD) Beam Line of TLS Sample Ion gun Safety Shutter Photon Shutter X-Y Slits SR QMS Yield of photon stimulated desorption η = 3.5 × 1019.S.ΔP/ΔN ΔN = 8.05 × 1017.E.Ie.θ/2π 37 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 • Sample has been installed at the 19B(PSD) beam line for exposure test. • The synchrotron radiation is white light with critical energy 2.14 keV. • To measure the surface concentration by in situ SIMS. S the effective pumping speed of system ΔP pressure increasing when photon exposure E electron beam energy (1.5 GeV) Ie electron beam current (300 mA) θ horiz. photon span on sample (0.0033rad) G.Y. Hsiung PSD yield for Aluminum samples Yield of photon stimulated desorption (η) for various cleaning processes : 38 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 • η of ozonate water cleaning is more than one order of magnitude lower than those of only ethanol machining or chemical cleaning at 1mAh. • η decreases with beam dose increases. • Al samples with ozonate water cleaning maintain the lowest η at the beam dose through 1000 mAh. G.Y. Hsiung Comparison of PSD partial pressure - w/wo ozonate water cleaning Partial pressure rise during photon exposure • Ethanol machining • 6.7 ppm ozonate water cleaning CO CO2 H2 C CH4 At the beginning of photon exposure, all the major outgases of ozonate water cleaning are lower than those of ethanol machining. The major difference comes from carbon related outgases, e.g. CO, CO2, CH4. 39 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Comparison of PSD partial pressure - different concentration of ozonate water Partial pressure rise during photon exposure • 6.7 ppm ozonate water cleaning CO2 • 30 ppm ozonate water cleaning H2 CO C CH4 The major PSD outgases are H2 ~ CO ~ CO2 > CH4 ~ C2H6. The denser ozonated water effectively reduces all the major PSD outgases. 40 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Can the PSD of Crotch Absorber (OFHC) in Bchamber be reduced with ozonate water cleaning? For Beam line < 204 °C (at 3.3 GeV, 350 mA) BM fan I.D. fan < 190 MPa (at 3.3 GeV, 350 mA) • Crotch absorbers ( > 2.3 m) takes BM fan only. • 100% I.D. fan will be penetrated through. Courtesy: Albert Sheng (NSRRC) 41 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung SIMS for ethanol machined Cu cleaned with (a) Citranox, (b) Ozonate water Cu-X : Copper cleaned with Citranox CH C C 2H2 C2 CH CC2H2 2 C F Cl F Cu-O3 : Copper cleaned with Ozonate water NEGATIVE ION MASS (a.m.u.) Na K Ca Cu POSITIVE ION MASS (a.m.u.) 42 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 Cl NEGATIVE ION MASS (a.m.u.) Na Al CxHy- ,Cl- : reduced Na+, K+ ,Ca+ : reduced Al K Ca Cu POSITIVE ION MASS (a.m.u.) G.Y. Hsiung PSD for ethanol machined Cu samples cleaned with (a) citranox, (b) O3-water Yield of photon stimulated desorption (η) for different cleaning processes : • η of ozonate water (20 ppm) cleaning is lower than that of citranox cleaning at the beam dose through 400 mAh. • η deceases with beam dose increases. 43 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung PSD-RGA for ethanol machined Cu cleaned with (a) Citranox, (b) Ozonate water Partial pressure rise during photon exposure • 20 ppm ozonate water cleaning • Citranox cleaning CO2 H2 CO C CH4 C2H6 The major PSD outgases are CO2 > H2 ~ CO > CH4 ~ C2H6. The ozonated water cleaning effectively reduces all the major PSD outgases. 44 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung PSD beam cleaning for Cu cleaned with (a) Citranox, (b) Ozonate-water Cu-X : Copper cleaned with Citranox H2 1.0E-08 1.0E-09 1.0E-07 CO2 CO C CH3 0.01Ah 0.1Ah 1Ah 1.0E-10 1.0E-11 • 45 PARTIAL PRESSURE (Arbi. Unit) PARTIAL PRESSURE (Arbi. Unit) 1.0E-07 Cu-O3 : Copper cleaned with Ozonate water CO2 H2 1.0E-08 1.0E-09 CO C 0.01Ah CH3 0.1Ah 1Ah 1.0E-10 1.0E-11 2 12 13 14 15 16 17 18 27 28 29 32 44 2 12 13 14 15 16 17 18 27 28 29 32 44 MASS (a.m.u.) MASS (a.m.u.) Pressure rises (dP/I) of H2, CH4, CO, CO2 are lower for Cu (Ozonate water cleaning) IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Yield of PSD with Beam cleaning Comparison of Al and Cu samples Aluminum samples Copper samples 1.0E-02 1.0E-02 Ethanol machining only Citrinox Chemical cleaning 20ppmO3-30min 6.7ppm O3 cleaning YIELD of PSD, η (molecules/photon)… YIELD of PSD, η (molecules/photon)... 30ppm O3 cleaning 1.0E-03 1.0E-04 1.0E-05 1.0E-03 1.0E-04 1.0E-05 1.0E-06 1.0E-06 0.001 0.001 0.01 0.1 1 10 0.01 0.1 1 BEAM DOSE (Ah) BEAM DOSE (Ah) • • 46 η < 5 × 10-5 molecules/photon at beam dose of 0.1 A·h (for ozonate water cleaned samples) η of Cu (ozonate water cleaning) < η of Cu (citranox cleaning) IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung 10 Summary of cleaning effect for Al and Cu cleaned with Ozonate water Comparison of η(PSD) : η(Al) & η(Cu) (Ozonate water cleaning) < η(Al) & η(Cu) (Ordinary cleaning methods) Partial pressure of outgas from PSD for Cu : Major outgas of H2 ~ CO ~ CO2 > CH4 : Cu-O (Ozonate water) < Cu-X (Citranox) Surface analysis for Cu by SIMS Negative ions of CxHy, Cl : Cu-O < Cu-X Positive ions of Na, K, Ca : Cu-O < Cu-X The lower carbon resided on surface layers results in the lower yield of PSD. Ozonate water cleaning method provides lower carbon on surface layer than other cleaning methods. Recommend : OFHC Cu with Ethanol CNC machining can be cleaned with ozonate water. OFHC Cu with oil machining can be cleaned with acid (Citranox etc.) prior to ozonate water (rather than DI water) rinsing. Next experiments will analyze the Cu samples with various cleaning methods after vacuum baking. 47 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Try to understand the surface condition after various cleaning methods Ethanol machining Ozonate water cleaning Chemical cleaning Work function (mV) Surface Roughness (µm) Thickness of Oxide layer (nm) 48 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 Courtesy: Ivan Liu, Master thesis of NTHU,Taiwan, Sep. 12 (2006) G.Y. Hsiung A super dry N2 exposure to 1 atm for the baked Al chamber (Ethanol CNC + 20 ppm O3-water cleaning) recovers to the UHV in 10 Hours (non-bake) • q ~ 2 E-13, • P1 < 2 nTorr at 10 hours after pumping (before vacuum baking) 49 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung Conclusions Ozonate water cleaning process after oil-free ethanol machining provides the lowest thermal outgassing rate and the least yield of the photon stimulated desorption for both aluminum and copper samples. The surface analysis by SIMS or AES shows the less contaminants of C, Na, K, etc. resided on the surface after ozonate water cleaning which results in the lowest PSD yield of carbonaceous outgases such as CO, CO2 and CH4. The work function and surface roughness have been measured on Alsamples for various cleaning methods. The machined surface provides thinner oxide layer and less roughness which gives lower rate of surface desorption. A further cleaning with ozonate water is helpful for removing the residual carbon on the surface layer and the reduction of carbonaceous molecular desorption. Thanks for your attention. 50 IUVSTA WS-63, Avila, Spain, Sep. 14-19, 2010 G.Y. Hsiung