Processing of Electroactive Components by means of Selective Laser Sintering / Melting (SLS/SLM) M. Gonon, N. Basile Fifteenth European Inter-Regional.

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Presentation transcript:

Processing of Electroactive Components by means of Selective Laser Sintering / Melting (SLS/SLM) M. Gonon, N. Basile Fifteenth European Inter-Regional Conference on Ceramics CIEC 15 5th-7th September 2016

Context Ceramic materials are the functional materials of a large number of electronic components. Complexes devices are composed of superimposed layers (conductors, semi-conductors, dielectrics, …) directly bounded over an insulating substrate. Processing such devices requires numerous deposition / firing steps : Time and energy consumption Firing conditions must be compatible with thermal stability of all already deposited materials. Compromises in terms of compositions and final microstructure and properties Substrate cleaning Ink serigraphy Drying Firing Final component x n conductors Functional layer Substrate

Context Laser source Cladding alloying Machining Welding / brazing Surface treatment (quenching , vitrification ; crystallization) Additive manufacturing

Context Would it be possible to consolidate and densify the different layers of an electronic component by mean of a laser beam ? Lasesurf projet Conductive metallic tracks Electroactive ceramics layers

Selective laser melting / sintering Laser treatments 0 Dimension dots 1 Dimension lines 2 Dimensions areas static dynamic static

Selective laser melting / sintering Grains bridging Densification Grain growth Phases transformation Sintering of a powder layer Mechanisms Parameters Temperature Time Temperature (°C) Relative density Specific surface (m²/g) Sintering Time Porosity Relative density Intermediate stage Initial stage Final stage Shrinkage (Porosity resorption) Temperature gradients Thermal expansion mismatch layer / substrate

Selective laser melting / sintering Sintering of a powder layer Temperature of the grains → true power density (absorbed) → grains size, shape, specific energy and thermal conductivity → interaction time Interaction time → dynamic or stationary Dynamic mode = Short interaction time → non stationary regime + complex thermal history → thermal gradient between surface and center of the grains. → compatibility with diffusion kinetics ? → Fast local heating and cooling = thermal chocks

Selective laser melting / sintering Processing parameters Power P (W) Speed s (mm/s) Vectorization v (µm) Beam diameter f (µm) Scan strategy 1 way or 2ways Power density (W/mm2) : Pw = P / (pφ2/4) Interaction time (s) : t* = ts x (Sbeam / Sscan) = p φ2/ (4 v s) Energy density (J/mm²) : J* = Pw t* = P / (s v) Overlapping (%) : Ov = 100 (f – v) / f

Selective laser melting / sintering Processing parameters Interaction time (s) Sintering ? Laser Cladding: Jan Gedopt, Marleen Rombouts Lasercentrum Vlaanderen

Selective laser melting / sintering Processing parameters Thermal history Example of the use of a laser beam as energy source to built up layer by layer a complex 3D monolithic structure (additive manufacturing).

Lasesurf Projet Challenge Application to thick powder layers deposited on a substrate ? Problems : Very short time of treatment Already dense substrate Multi materials Selected material : BaTiO3 Objective : process a 10 to 100 µm tick layer on an alumina substrate

Lasesurf Projet Procedure 1 : Treatment of BaTiO3 powder pellets. Parameters leading to a consolidation of the surface Characterize the microstructure Identify consolidation mechanisms 2 : Treatment of a BaTiO3 powder layer Powder deposited on an alumina substrate Ag coated or not. Influence on the scanning conditions BaTiO3 BaTiO3 Alumina BaTiO3 Ag Alumina

Treatment of BaTiO3 powder pellets Equipment / Characterization Trumark Station 5000 (Trumpf) Solid-state laser (Nd-YVO4) Pmax = 22,8 W (cw) l = 1064 nm f = 45 µm s = 0 to 7000 mm/s Characterization : Visual aspect XRD SEM

Treatment of BaTiO3 powder pellets BaTiO3 pellets Parametric investigation Tetragonal BaTiO3 Powders : micro, d50 = 0,44 µm (Sigma Aldrich) nano, d50 = 50 nm (Inframat Advanced Materials ) mixtures micro / nano Pw = P / (pφ2/4) t* = p φ2/ (4 v s) J* = Pw.t* Scanned area 10 x 10 mm2

Treatment of BaTiO3 powder pellets Influence of scan parameters Influence of s and v P = 100 % (22,8 W) Pw = 1,4 106 W/cm2 Pw = P / (pφ2/4) t* = p φ2/ (4 v s) J* = Pw.t* 15 % nano s = 80 mm/s v = 10 µm t* = 2 ms J* = 2,85 kJ/cm2 s = 1000 mm/s v = 10 µm t* = 0,16 ms J* = 0,228 kJ/cm2

Treatment of BaTiO3 powder pellets Influence of s and v t* = p φ2/ (4 v s) same s.v = same t* and then same J* High temperature forms of BaTiO3 if t* > 0,13 ms Amorphous phase if t* > 0,04 ms But differences in t* limits according to v and s

Treatment of BaTiO3 powder pellets Influence of s and v For given Pw and t*, the thermal profile of a given point of the scanned surface will be depending on it distance to the laser beam vs time. t* = p φ2/ (4 v s) v1, s1 2v1, s1/2 If speed is lowered and vectorisation increased, the laps of time between two close positions increases what favor cooling before reheating.

Treatment of BaTiO3 powder pellets Influence of s and v High amount of glassy phase. → Melting of nano and significant part of micro grains. High temperature crystal form of BaTiO3. → high rise in temperature of the core of the larger grains.

Treatment of BaTiO3 powder pellets Influence of s and v Low amount of glass phase. → Melting of nano grains ? Low temperature crystal form of BaTiO3 and weak grain growth of the unmelted grains. → limited elevation of temperature of the core of the larger grains.

Treatment of BaTiO3 powder pellets Influence of s and v Comparison mix micro + nano / pure micro weak cohesion of sanned surfaces for s > 200 mm/s s < 200 mm/s → glassy surface. → melting of a large part of the grains. → phase transformation and growth of unmelted grains.

Treatment of BaTiO3 powder pellets Influence of P and s v = 10 µm Pw = P / (pφ2/4) t* = p φ2/ (4 v s) J* = Pw.t* Higher t* limits if Pw decreases from 100 % down 95% and 90%. However, no cohesion of scanned surface if P < 90 % (Pw = 1,3 106 W/cm2). → the increase in t* thorough a decrease in s doesn't compensate the decreased in Pw (a cte J* is not sufficient to lead to a same result).

Treatment of BaTiO3 powder pellets Conclusion influence of scan parameters Possible to obtain consolidated t-BaTiO3 layers. Need of a fraction of fine grains that melt for “low” energetic conditions. Interaction time t* must be short enough to limit the melted fraction and avoid phase transformation of the larger grains. t* limit depend on vectorisation v and speed s. Energy density J* is not a pertinent parameter : Pw cannot be lowered below 1,3 106 W/cm2.

Consolidation of a BaTiO3 powder layer Procedure 1 : Treatment of BaTiO3 powder pellets. Parameters leading to a consolidation of the surface. Characterize the microstructure. Identify consolidation mechanisms. 2 : Treatment of a BaTiO3 powder layer Powder deposited on an alumina substrate Ag coated or not. Influence on the scanning conditions. BaTiO3 BaTiO3 Alumina BaTiO3 Ag Alumina

Treatment of BaTiO3 powder layers Interaction during a line scan 25 µm BaTiO3 layers P = 100 % ; s = 1.000 mm/s

Treatment of BaTiO3 powder layers Interaction during a line scan 80 µm 20 µm P = 100 % ; s = 1.000 mm/s 80 µm Pellets Substrate

Treatment of BaTiO3 powder layers Surface scan BaTiO3 layer on alumina substrate P = 100 % ; s = 1.000 mm/s ; v = 40 µm P = 100 % ; s = 2.000 mm/s ; v = 20 µm P = 100 % ; s = 4.000 mm/s ; v = 10 µm 40 µs t* = p φ2/ (4 v s)

Treatment of BaTiO3 powder layers Conclusion powder layers Problem of interaction with the substrate. High temperatures reach by the powder layer not compatible with low temperature melting conductors as Ag. Thermal gradients between the layer and the substrate cause dilatation / shrinkage mismatches generating stresses and cracks. Target : more homogeneous heating. Avoiding melting (real solid state sintering). Thermal characterization of the scanned surface during the laser treatment

Thermal characterization of a laser scan Infrared camera : FLIR AGEMA 750 PAL objectif FOV 24, acquisition time : 2 s Scanned Surface : 10 x 10 mm2 Spatial resolution : 12 x 8 mm2 Number of cells : 96 (8 x 12)

Thermal characterization of a laser scan Power density : 1,4 106 W/cm2 Vectorisation : 40 µm Scan speed : s = 10 mm/s Interaction time : t* = 3,5 10-3 s 20s Vectorisation

Thermal characterization of a laser scan Power density : 1,4 106 W/cm2 Vectorisation : 40 µm Scan speed : s = 10 mm/s Interaction time : t* = 3,5 10-3 s Vectorisation

Thermal characterization of a laser scan Scan speed : s = 30 ; 10 ; 5 mm/s t* = p φ2/ (4 v s) Vectorisation

Thermal characterization of a laser scan Vectorisation Scan speed : s = 10 mm/s t* = p φ2/ (4 v s) 10 x 10 mm2 20 x 10 mm2 10 x 20 mm2

Thermal characterization of a laser scan At high speed, time resolution of IR camera (2 s) doesn't allow to follow temperature of a selected zone during 1 cycle. Repeated cycles : Min ; Average and Max temperature of the scanned surface vs time. Influence of speed. 1000 mm/s 5000 mm/s

Thermal characterization of a laser scan High temperature gradient over the scanned surface a low speed. Limited gradient at high speed. Weak heating of the cells during the first cycles. Heating is limited to a little area around the laser beam. 1000 mm/s 5000 mm/s

Thermal characterization of a laser scan A temperature plateau is reached after 80 s. The maximum temperature is not influenced by the speed. The heating rate at sort time is higher for high speeds.

Thermal characterization of a laser scan Conclusion thermal characterization Interaction time t* is not a characteristic parameter. short vectorisation v and high speed s = more progressive and homogeneous heating. Possibility of increasing interaction time by mean of a multiscan strategy. = very short interaction time during one cycle (very high speed) but repeated several times. = control of the heating profile of the scanned surface. t* = p φ2/ (4 v s)

Thermal characterization of a laser scan Conclusion thermal characterization 100 µm BaTiO3 Layer P = 100 % ; v = 40 µm s = 2500 mm/s ; s = 5.000 mm/s ; X 60 s Consolidation but no densification

Thermal characterization of a laser scan Conclusion / outlooks Possibility to consolidate and densify a BaTiO3 layer through the melting of a low volume fraction of small powder grain. But not compatible with other materials. Mismatch with the substrate leading to cracks. A real solid state sintering requires an increase of the total time of treatment while keeping a homogenous controlled heating of the surface : = Mutiscan strategy The maximum temperature reached in the stationary regime do not depend on the scanning speed but on the power density of the laser beam. Limit of the equipment

Thank you for your attention