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Controlling High-T Ceramic Grain Boundaries with E Fields Understanding the Mechanisms of Flash Sintering and Beyond

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Controlling High-T Ceramic Grain Boundaries with E Fields Understanding the Mechanisms of Flash Sintering and Beyond 2018 Aerospace Materials for Extreme Environment Program Review Controlling High-T Ceramic Grain Boundaries with E Fields Understanding the Mechanisms of Flash Sintering and Beyond Jian Luo University of California, San Diego May 16, 2018 The Phillips Technology Institute Collaboration Center Acknowledgement: Students: Jiuyuan Nie (Ph.D. student), Yuanyao Zhang (Ph.D., Sept 2016; currently employed at Lam Research) and Tao Hu (partial postdoc; TEM) AFOSR Program Manager: Dr. Ali Sayir AFOSR Grant no. FA9550-14-1-0174 September 2014 – August 2019 Jian Luo Background: Prior Studies & Motivation Selected AFOSR Project Achievement (I) Innovative Sintering 3YSZ Cold Sintering Clive Randall et al. (e.g., ACS AMI 2016) Flash Sintering 3YSZ Rishi Raj et al. higher JACerS 2010 Specimen T <200 C, H2O-assisted (hydrothermal), ~1 h Typically Needed: Post Annealing at Reduced T From This AFOSR Project: Water-Assisted Flash Sintering (WAFS) ZnO Nie, Zhang, Chan, Huang, Luo Scripta Materialia 142: 79-82 (2018) Jian Luo Background: Prior Studies & Motivation Selected AFOSR Project Discoveries (II) Electric Fields on Microstructural Development? Inhibit Grain Promote Grain Growth? Growth? 3YSZ Raj et al. Conrad (JACerS 2011) (JACerS 2009) Bi2O3-doped ZnO To induce space charges at GBs? Our Most Recent AFOSR Work Jian Luo The Scientific Questions and Technological Opportunities of Our Example of ZnO Flash Sintering Flash Sintering Acta Mater. 2017 + Viewpoint: Scripta Mater. 2018 More Open Scientific Q’s Scientific Open More 2% (1) How does flash start? 0% -2% Einitial = 300 V/cm -4% Conventional (2) How does rapid densification occur? -6% Sintering -8% (E = 0) -10% 5 C/m (3) Can we control microstructures? 20 mA/mm2 ~89% E.g., nano ceramics? Bimodal microstructures? -12% -14% Linear Shrinkage Linear 30 mA/mm2 ~94% -16% (4) Can we start a flash at room temperature? J = 39 mA/mm2 -18% max ~97% density in 30 s Water-Assisted Flash Sintering (WAFS) -20% 0 200 400 600 800 1000 1200 Furnace Temperature (T , oC) (5) Can electric field/current/potential affect F microstructural development? Jian Luo (1) How does a flash start? Differential Heat 2 d VS Generation Rate E Per Unit Surface Area dTSS A 3 4Stefan TS Differential Heat Dissipation Rate Per Unit Surface Area An unstable temperature rise or a Coupled Thermal & Electric Runaway will occur if: Specimen & Surface Area 23dQ EVTASSS4Stefan dTSS T If heat radiation dominates… Differential Differential Heat Heat Generation Dissipation Rate Rate Zhang et al., Acta Materialia 2015 & 2017 Viewpoint: Luo, Scripta Materialia 2018 Jian Luo (1) How does the flash start? Testing Our Model: “Onset Flash = Coupled Thermal and Electric Runaway” Three Notes (Open Q’s): We showed that a flash can start as a thermal runaway (for ~ 20 cases), but: 1) it does not exclude the possibility that a discontinuous increase in (T) (due to a 1st-order transition or defect avalanche) can trigger a thermal runaway a flash; 2) it explains how flash starts, but not the fast densification (that is indeed faster than expected) mechanisms; and 3) it does not exclude possible • AtmosphereAl“Flash”TiOelectric2O2:3 adoping systematic of single field/current/potential dependenceincreases8YSZ crystals validation(vs. the ZnO ((new newconductivity of): discoveryourdiscovery model of)) •ZnOnewwithSurfaceseffects, tosurfacemethoddifferent promote are which 2 to -more Dphases control electronflash. insulatingindeed (anatase gas exist(~10( vs.vs.12 conductiverutile)e/cm and2 ):&can ) •smallerReducingdopingArbeor significant H (undoped,particles2 reducesatmosphere ( cation,vs.more increases moreconductiveanionic) )conductive conductivity Jian Luo (2) How does rapid densification occur? Flash The First 30 Seconds! Einitial = 300 V/cm 2% Conventional E = 0% Sintering initial 2 (E = 0) 100 Jmax ≈ 30 mA/mm 0.015 Specimen -2% 300 V/cm 0.8 2 90 -4%Jmax = 20 mA/mm 5 C/m 0.7 Conductivity Imax = 0.5 A ~89% 80 -6% 0.6 0.010 2 70 J = 30 mA/mm 0.5 -8%max 60 Imax = 0.75 A ~94% 0.4 -10% 50 2 0.3 0.005 Jmax = 39 mA/mm Voltage (V) Voltage ~97% density in 30 s Current (A) Current -12% I = 1 A 40 0.2 max 30 -14% Conductivity (S/cm) Conductivity σ 0.1 I Shrinkage Linear V 0.000 20 0.0 -16% -10 0 10 20 30 -10 0 10 20 30 -10 0 10 20 30 -18% Time (sec) Time (sec) Time (sec) -20% 0J 200 T400 Final600 Density!800 1000 1200 Power max S o 1 Furnace Temperature (T , C) ~120 nm ~260 nm F Density 2% ) 3 ~61% density 0% ~400 nm W/mm ( 0.1 -2% -4% Power Density Density Power -6% 0.01 -10 0 10 20 30 -8% Time (sec) -10% 5 s ) C o 1600 -12% , s Linear Shrinkage Linear T ( Estimated 1400 -14% Densification levels off after ~20-30s TS ~1200 C 1200 -16% 20 s 30 s 1000 ~200 C/s -10 0 10 20 30 ~1 μm 800 Time (sec) 600 EstimatedSpecimen Temperature -10 0 10 20 30 Time (sec) Jian Luo (2) How does rapid densification occur? Rapid Thermal Annealing (RTA) to Mimic the T(t) Profile in Flash Sintering Comparable T(t) Profiles Densification Similar Densification & Grain Growth Rates Flash Sintering TSteady-State (Imax = 0.75 A) = ~ 1040°C – 1160°C TSteady-State (Imax = 0.5 A) = ~ 920°C – 1050°C Rapid Thermal Annealing (RTA) Grain Growth Intense IR Heating Heating @ 200°C/s; Isothermal for 0-30 s Jian Luo (2) How does rapid densification occur? Controlled (Step-wise) Heating Rate Experiments Importance of Ultrahigh dT/dt 1.0 1 step 0.9 Conventional 0% 0.8 0.7 0.6 -5% 0.5 0.4 -10% 0.3 Shrinkage Current (A) Current 7 steps 0.2 86.7% density 0.1 0.1 A/100 s -15% 0.0 94% density (in 20 s) -100 0 100 200 300 400 500 600 700 800 -100 0 100 200 300 400 500 600 700 800 Time (sec) Time (sec) 2 Identical Emax = 300 V/cm and the final Imax = 0.75 A (Jmax = 30 mA/mm ) Reducing effective ramp rate: by increasing Imax in 7 steps, or 0.1A/100s The Benefits of Ultrahigh dT/dt (Detailed Discussion in the Next 2 Slides…): 1) helping a competition between densification (via GB diffusion at high T) vs. particle coarsening (via surface diffusion at low T) to keep sintering driving force 2) leading to non-equilibrium defects, e.g., non-equilibrium grain boundaries, with higher diffusivities ? Zhang et al. Acta Mater. 2017; Luo, Scripta Mater. 2018 Jian Luo (2) How does rapid densification occur? How Does Ultrahigh dT/dt Help? Ultrahigh dT/dt (~ 200 C/s for ZnO): Helpping a competition between densification (via GB diffusion @ high T) vs. coarsening (via surface diffusion @ low T) to keep high sintering driving force E.g., 10% less coarsening 2X the sintering rate ( G4) Zhang et al. Acta Mater. 2017; Luo, Scripta Mater. 2018 Demonstrated also for 3YSZ by Professor Todd & co-workers (Oxford) Ultra-fast heating can accelerate the sintering of 3YSZ by >100X without E Jian Luo (2) How does rapid densification occur? Todd et al.: Ultrahigh dT/dt Non-Equilibrium Grain Boundaries w/ Increased Diffusion How to probe non-equilibrium grain boundaries? • In situ (seems difficult)? • Doping & quenching? • Modeling? ? Grain Boundary Structural Transitions? Jian Luo (3) Can we control microstructures? Fast Densification of Nanocrystalline Ceramics w/ Suppressed Grain Growth? Two-Step Flash Sintering (TSFS) ❷ There❷ 3 A is also30 s a97.6% competition between: ❹ • grain growth (via diffusion // GB at relatively❶ ❸ high T) vs. • densification (via diffusion ⊥ GB at relatively low T), which5 µm is in part responsible for two-step sintering. 1.75 ± 0.16 µm ❶ 3 A 6 s 90.3% ❸ 3 A 6 s + 2 A 150 s ❹ 3 A 6 s + 2 A 300 s Nie et al. Recall Ultrahigh dT/dt: To help a competition between 96.5% Scripta Mater. 94.7% 141: 6 (2017) • densification (via GB diffusion at high T) vs. • particle coarsening (via surface diffusion at low T) 2 µm 2 µm 2 µm to keep sintering267 ± 30 nm driving force.330 ± 28 nm 370 ± 17 nm Jian Luo (3) Can we control microstructures? Two-Step Flash Sintering (TSFS): >200X Faster Than Conventional Two-Step Sintering Better Results, Nie et al. Scripta Materialia 141: 6-9 (2017) >200X Faster Conventional Two-Step Sintering of ZnO to Achieve Similar Results in ~72,000 s Mazaheri, Zahedi, & Sadmezhaad J. Am. Ceram. Soc. 91: 56 (2008) Jian Luo (3) Can we control microstructures (& defects)? Beyond Two-Step Flash Sintering (TSFS)? The flash sintering scheme allow Flash Sintering Bimodal Microstructures a direct control of I(t) and T(t) profiles to much better precisions and higher speeds! Open Questions (Future Studies or Opportunities): 1) Can we control I(t) and T(t) to achieve more exotic microstructures, e.g., bimodal misconstrues? 2) Can we pattern the electrodes to achieve graded microstructures? 3) Can we use flash sintering to make highly-defective materials? Jian Luo (4) Can we start a flash at room temperature? Water-Assisted Flash Sintering (WAFS) 2% Optimization0% Guided by the Model in Ar – 5% H2 Our Example of ZnO (Tmelting = 1975 C) -2% Flash Flash at TF = 108 C! -4%~97% Density in <30 s -6% Einitial = 300 V/cm -8%(Grain Size: ~1 m) Conventional -10% Sintering (E = 0) -12% 5 C/m -14% Linear Shrinkage Linear -16% -18% -20% 0 200 400 600 800 1000 1200 Jmax = ~97% density in 30 s 2 Furnace Temperature (T , oC) 39 mA/mm (Tfurnace < 650 C) F Zhang & Luo, Scripta Mater. 2015 Cold Sintering Our Recent Attempt (following Randall et al.): JPS 2018 Clive Randall et al.
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