Vapor phase deposition and characterization of nanoporous films
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1 Vapor phase deposition and characterization of nanoporous films Cluster innovatieve coatings, March 23, 2018 Corda Campus Hasselt Rob Ameloot Center for Surface Chemistry and Catalysis KU Leuven University of Leuven Belgium
2 Leuven Chem&Tech and NanoCentre 2
3 Leuven Chem&Tech and NanoCentre Brand-new research facilities focused on interdisciplinary chemistry & nanotechnology 3
4 Leuven Chem&Tech and NanoCentre 4
5 Leuven Chem&Tech and NanoCentre Expertise in chemistry, chemical engineering, cleanroom fabrication and production processes in one location 5
6 Top down Bottom up 6
7 Introduction: Metal-organic frameworks? = crystalline and microporous materials based on coordination bonds Metal ion node Organic linker 5 Å 7
8 Introduction: Metal-organic frameworks? Well-controlled nano-environments in synthetic materials 5 Å 8
9 Example: ZIF-8 Zn 2+ + SOD 1 nm CH 3 Park, K. S. et al. PNAS, 103, (2006). 9
10 Introduction: Metal-organic frameworks? Modular structure Node Connector MOF structure A large diversity in composition, framework types and properties 10
11 Why are MOFs interesting? Adsorbents Sensors Dielectrics And many more: catalysts, nanoscaffolds, magnetic and spincrossover behavior, bio-molecule encapsulation and stabilization, CO 2 12
12 Match between synthesis and application Properties Applications The bulk approach 16
13 Making MOFs as powders Typically MOF synthesis is performed in a solvent and yields powders Ligand source Metal ion Source (salts) 50 m 17
14 Problems with MOF synthesis Corrosion of preformed circuitry Chemical contamination Solvent use: o Cost o Processability and safety concerns o In conflict with green fabrication (ITRS roadmap) Matching precursor dissolution and MOF crystallization o Roughness, pinholes, etc. o Particle contamination risk due to homogeneous nucleation Integration of MOFs in microelectronics fabrication is hard! 18
15 Match between synthesis and application Properties Applications Shape: defect-free layers and coatings, hollow capsules, nanoparticles, etc. Spatial control: surface patterns, crystallographic orientation, etc. Compatibility: with other functional components (electronics, etc.) 19
16 Atomic layer deposition (ALD) Hydroxyl-terminated substrate Metal oxide Organometallic Water Typical pressure: 1 mbar to atmospheric Typical temperature: RT C, typically C Chemicalsreact only at the surface. Surface-controlled, self-limiting growth extremely conformal, pinhole-free films Film thickness < 1 µm, more typically < 100 nm Sub-nm thickness control 20
17 ALD thin film materials Lu et al. Surface Science`Reports 71(2016)
18 ALD applications ALD high-k dielectrics in transistors Oxide (HfO 2 ) 5 μm IBM 22
19 ALD applications Thin film encapsulation and barriers Flexible electronics Rigid substrates OLED Solar energy Surface passivation Buffer layers Batteries & catalysts ALD possible on powders Industrial coatings Optical coatings Anti-reflective Glass strengthening Anti-tarnishing and more 23
20 Spatial ALD vs temporal ALD Spatial separation of half-reactions, instead of time-separation Efficient separation between the two half-reactions is needed: inert gas curtain Poodt, P. et al, Spatial atomic layer deposition: A route towards further industrialization of atomic layer deposition. J. Vac. Sci. Tech. A, 2012, 30,
21 MOF-CVD Stassen, Styles, Grenci, Van Gorp, Vanderlinden, De Feyter, Falcaro, De Vos, Vereecken & Ameloot, Nature Materials, 2016, 3, 304
22 MOF-CVD: vapor deposition approach Atomic layer deposition (ALD): Zn(C 2 H 5 ) 2 + H 2 O ZnO + 2 C 2 H 6, Reactive sputtering (PVD): Zn + O 2 (plasma) ZnO 27
23 MOF-CVD: vapor deposition approach Zn dissolution not possible! vapor-solid reaction ZnO + 2 HmIM Zn(mIM) 2 (=ZIF-8) + H 2 O ΔH r = ± 0.95 kj mol -1 Navrotsky et al. (2013). J. Am. Chem. Soc., 135(2),
24 MOF-CVD: vapor deposition approach HmIM CVD 100 C 30 min 2.5 cm Highly reflective and uniform ZIF-8 films over large areas (up to 200 mm) 29
25 X-ray diffraction Bragg-Brentano geometry 30
26 Cleanroom integration 32
27 MOF-CVD reactor optimized for in situ monitoring gravimetric + spectroscopic metrology to complement other characterization techniques 34
28 Spectroscopic ellipsometry is suitable for MOF thin films - ex situ and in situ Non-destructive optical technique Measures the change in polarization state of the beam Characterized by ellipsometric Ψ and Δ 35
29 Ellipsometry measures changes in polarization and is highly sensitivity to very thin films Reflectometry vs Ellipsometry 36
30 Spectroscopic ellipsometry is suitable for MOF thin films - ex situ and in situ Ellipsometry measurement Ψ, f( ) Build model Effective media approximation Si substrate Fit ZIF-8 ZnO Si substrate Results: thickness, refractive index ( )! Poor fit results are meaningless! 37
31 Ellipsometry applied to porous thin films 1 Ideal MOF film 2 porous MOF + unconverted oxide 3 Distributed crystals 4 as a porosimetric tool 38
32 Ellipsometry as a porosimetry tool Overall (polarizability and) refractive index can be expressed as a summation of the refractive indices of materials comprising the system (Lorentz-Lorenz / Clausius-Mossotti) B = σ N i α i = c n2 1 n 2 +2 V filled with adsorbate V total = n 2 e 1 n 2 e + 2 n n n 2 ads 1 n 2 ads + 2 n e : measured refractive at a certain adsorbate partial pressure n o : measured refractive index at vacuum n ads : refractive index of adsorbate e.g. MeOH, H 2 O 39
33 A complementary technique: QCM for MOF-CVD kinetic + adsorption studies with nanogram precision Mass variation unit area change in frequency of a quartz crystal resonator Quartz crystal Oscillator circuit 41
34 Many parameters can / need to be optimized Reaction and crystallization Adsorption - desorption Transport phenomena (heat) MOF-CVD = f temperature, precursor, reaction time Layer thickness Nature of precursor Deposition process Others: Pressure Flow rate Co-reactants Substrate surface chemistry Reaction kinetics Transport phenomena (mass) Crystal growth process 42
35 Monitoring different reactor configurations MOF-CVD = f temperature, precursor, reaction time In situ ellipsometry growth from 3nm ZnO, T=gradient, P starting =0.2 mbar 44
36 HmIM exposure time Optimal time depends on precursor thickness (and temperature) MOF-CVD = f temperature, precursor, reaction time starting ZnO thickness full coverage region smooth films MOF-CVD sweet spot ZnO Substrate HmIM vapor ZnO Substrate full conversion region Substrate ZIF-8 crystals ZnO Substrate ZnO Substrate 47
37 HmIM exposure time Optimal conditions yield high-quality films MOF-CVD = f temperature, precursor, reaction time 14.8 starting ZnO thickness full coverage region 35nm MOF film from 3nm ZnO 800nm smooth films (Phase AFM) nm ZIF film from 3nm ZnO full conversion region Reference (100 nm ZIF) 3 nm 48
38 Towards application: Sensors Example: nerve agent simulants Kelvin probing (macroscopic test) ChemFET (integrated device) Exposure guideline (AEGL-2): 15 ppb Chem. Sci. 7, (2016). 53
39 Attacking nerve agents: help from nature Phosphotriesterase Zn-OH-Zn motif Phosphotriesterase 54
40 Towards application: Sensors Material selection: literature Zn-OH-Zn bonds Phosphotriesterase Zr-OH-Zr bonds UiO-66 family Original context: degradation of chemical warfare stocks O. Farha & J. Hupp (Northwestern) Angew. Chem. 126, , 2014, Nat Mater 14, ,
41 Towards application: Sensors Example: nerve agent simulants Chem. Sci. 7, (2016). Detection limit (3 noise level): 0.3 ppb (!) 56
42 Towards application: Sensors Example: nerve agent simulants High performance in the presence of water! Chem. Sci. 7, (2016). 57
43 Roadmap for MOFs in devices Stassen, Burtch, Talin, Falcaro, Allendorf & Ameloot Chem. Soc. Rev., 2017, 46, R. Ameloot - Self-assembling a smarter world: the hole story 59
44 Status of MOFs & microelectronics? Cleanroom integration Sensor demonstration Film growth Dielectric properties Remaining: film roughness, mechanical properties, thermal expansion behavior, further compatibility and integration testing, 60
45 Thanks to the team! 61
46 5 µm KU Leuven (Belgium): Prof. Dirk de Vos Prof. Steven de Feyter Ivo Stassen Alex Cruz Timothee Stassin Imec (Belgium): Prof. Philippe Vereecken ESTORE team & MCA Dept Ghent University (Belgium) Prof. V. Van Speybroeck Juliana Hajek TU Graz (Austria) Prof. Paolo Falcaro CSIRO (Australia): Dr. Mark Styles National University of Singapore: Dr. Gianluca Grenci Ivo Stassen Interested in a PhD / postdoc position? Rob.Ameloot@kuleuven.be LMU Munich (DE): Alex Cruz Prof. Thomas Bein Dr. S. Wuttke & Dr. D. Medina 62
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