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INEEL/CON-2000-00104PREPRINTSpray-Formed Tooling for Injection Molding andDie Casting ApplicationsK. M. McHughB. R. WickhamJune 26, 2000 June 28, 2000International Conference on Spray Depositionand Melt AtomizationThis is a preprint of a paper intended for publication in ajournal or proceedings. Since changes may be madebefore publication, this preprint should not be cited orreproduced without permission of the author.This document was prepared as a account of worksponsored by an agency of the United States Government.Neither the United States Government nor any agencythereof, or any of their employees, makes any warranty,expressed or implied, or assumes any legal liability orresponsibility for any third partys use, or the results ofsuch use, of any information, apparatus, product orprocess disclosed in this report, or represents that itsuse by such third party would not infringe privatelyowned rights. The views expressed in this paper arenot necessarily those of the U.S. Government or thesponsoring agency.B E C H T E L B W X T I D A H O , L L C1Spray-Formed ToolingFor Injection Molding and Die Casting ApplicationsKevin M. McHugh and Bruce R. WickhamIdaho National Engineering and Environmental LaboratoryP.O. Box 1625Idaho Falls, ID 83415-2050e-mail: kmm4inel.govAbstractRapid Solidification Process (RSP) Tooling is a spray forming technology tailored forproducing molds and dies. The approach combines rapid solidification processing and net-shapematerials processing in a single step. The ability of the sprayed deposit to capture features of thetool pattern eliminates costly machining operations in conventional mold making and reducesturnaround time. Moreover, rapid solidification suppresses carbide precipitation and growth,allowing many ferritic tool steels to be artificially aged, an alternative to conventional heattreatment that offers unique benefits. Material properties and microstructure transformationduring heat treatment of spray-formed H13 tool steel are described.IntroductionMolds, dies, and related tooling are used to shape many of the plastic and metal components weuse every day at home or at work. The process involves machining the negative of a desired partshape (core and cavity) from a forged tool steel or a rough metal casting, adding coolingchannels, vents, and other mechanical features, followed by grinding. Many molds and diesundergo heat treatment (austenitization/quench/temper) to improve the properties of the steel,followed by final grinding and polishing to achieve the desired finish 1.Conventional fabrication of molds and dies is very expensive and time consuming because: Each is custom made, reflecting the shape and texture of the desired part. The materials used to make tooling are difficult to machine and work with. Tool steels arethe workhorse of industry for long production runs. Machining tool steels is capitalequipment intensive because specialized equipment is often needed for individual machiningsteps. Tooling must be machined accurately. Oftentimes many individual components must fittogether correctly for the final product to function properly.2Costs for plastic injection molds vary with size and complexity, ranging from about $10,000 toover $300,000 (U.S.), and have lead times of 3 to 6 months. Tool checking and part qualificationmay require an additional 3 months. Large die-casting dies for transmissions and sheet metalstamping dies for making automobile body panels may cost more than $1million (U.S.). Leadtimes are usually greater than 40 weeks. A large automobile company invests about $1 billion(U.S.) in new tooling each year to manufacture the components that go into their new line of carsand trucks.Spray forming offers great potential for reducing the cost and lead time for tooling byeliminating many of the machining, grinding, and polishing unit operations. In addition, sprayforming provides a powerful means to control segregation of alloying elements duringsolidification and carbide formation, and the ability to create beneficial metastable phases inmany popular ferritic tool steels. As a result, relatively low temperature precipitation hardeningheat treatment can be used to tailor properties such as hardness, toughness, thermal fatigueresistance, and strength. This paper describes the application of spray forming technology forproducing H13 tooling for injection molding and die casting applications, and the benefits of lowtemperature heat treatment.RSP ToolingRapid Solidification Process (RSP) Tooling, is a spray forming technology tailored forproducing molds and dies 2-4. The approach combines rapid solidification processing and net-shape materials processing in a single step. The general concept involves converting a molddesign described by a CAD file to a tooling master using a suitable rapid prototyping (RP)technology such as stereolithography. A pattern transfer is made to a castable ceramic, typicallyalumina or fused silica (Figure 1). This is followed by spray forming a thick deposit of tool steel(or other alloy) on the pattern to capture the desired shape, surface texture and detail. Theresultant metal block is cooled to room temperature and separated from the pattern. Typically,the deposits exterior walls are machined square, allowing it to be used as an insert in a holdingblock such as a MUD frame 5. The overall turnaround time for tooling is about three days,stating with a master. Molds and dies produced in this way have been used for prototype andproduction runs in plastic injection molding and die casting.Figure 1. RSP Tooling processing steps.3An important benefit of RSP Tooling is that it allows molds and dies to be made early in thedesign cycle for a component. True prototype parts can be manufactured to assess form, fit, andfunction using the same process planned for production. If the part is qualified, the tooling can berun in production as conventional tooling would. Use of a digital database and RP technologyallows design modifications to be easily made.Experimental ProcedureAn alumina-base ceramic (Cotronics 780 6) was slurry cast using a silicone rubber master die,or freeze cast using a stereolithography master. After setting up, ceramic patterns weredemolded, fired in a kiln, and cooled to room temperature. H13 tool steel was induction meltedunder a nitrogen atmosphere, superheated about 100C, and pressure-fed into a bench-scaleconverging/diverging spray nozzle, designed and constructed in-house. An inert gas atmospherewithin the spray apparatus minimized in-flight oxidation of the atomized droplets as theydeposited onto the tool pattern at a rate of about 200 kg/h. Gas-to-metal mass flow ratio wasapproximately 0.5.For tensile property and hardness evaluation, the spray-formed material was sectioned using awire EDM and surface ground to remove a 0.05 mm thick heat-affected zone. Samples wereheat treated in a furnace that was purged with nitrogen. Each sample was coated with BN andplaced in a sealed metal foil packet as a precautionary measure to prevent decarburization.Artificially aged samples were soaked for 1 hour at temperatures ranging from 400 to 700C, andair cooled. Conventionally heat treated H13 was austenitized at 1010C for 30 min., airquenched, and double tempered (2 hr plus 2 hr) at 538C.Microhardness was measured at room temperature using a Shimadzu Type M Vickers HardnessTester by averaging ten microindentation readings. Microstructure of the etched (3% nital) toolsteel was evaluated optically using an Olympus Model PME-3 metallograph and an AmrayModel 1830 scanning electron microscope. Phase composition was analyzed via energy-dispersive spectroscopy (EDS). The size distribution of overspray powder was analyzed using aMicrotrac Full Range Particle Analyzer after powder samples were sieved at 200 m to removecoarse flakes. Sample density was evaluated by water displacement using Archimedes principleand a Mettler balance (Model AE100).A quasi 1-D computer code developed at INEEL was used to evaluate multiphase flow behaviorinside the nozzle and free jet regions. The codes basic numerical technique solves the steady-state gas flow field through an adaptive grid, conservative variables approach and treats thedroplet phase in a Lagrangian manner with full aerodynamic and energetic coupling between thedroplets and transport gas. The liquid metal injection system is coupled to the throat gasdynamics, and effects of heat transfer and wall friction are included. The code also includes anonequilibrium solidification model that permits droplet undercooling and recalescence. Thecode was used to map out the temperature and velocity profile of the gas and atomized dropletswithin the nozzle and free jet regions.4Results and DiscussionSpray forming is a robust rapid tooling technology that allows tool steel molds and dies to beproduced in a straightforward manner. Examples of die inserts are given in Figure 2. Each wasspray formed using a ceramic pattern generated from a RP master.Figure 2. Spray-formed mold inserts. (a) Ceramic pattern and H13 tool steel insert. (b) P20 toolsteel insert.Particle and Gas BehaviorParticle mass frequency and cumulative mass distribution plots for H13 tool steel sprays aregiven in Figure 3. The mass median diameter was determined to be 56 m by interpolation ofsize corresponding to 50% cumulative mass. The area mean diameter and volume meandiameter were calculated to be 53 m and 139 m, respectively. Geometric standard deviation,d=(d84/d16) , is 1.8, where d84 and d16 are particle diameters corresponding to 84% and 16%cumulative mass in Figure 3.5Figure 3. Cumulative mass and mass frequency plots of particles in H13 tool step sprays.Figure 4 gives computational results for the multiphase velocity flow field (Figure 4a), and H13tool steel solid fraction (Figure 4b), inside the nozzle and free jet regions. Gas velocity increasesuntil reaching the location of the shock front, at which point it precipitously decreases,eventually decaying exponentially outside the nozzle. Small droplets are easily perturbed by thevelocity field, accelerating inside the nozzle and decelerating outside. After reaching theirterminal velocity, larger droplets (150 m) are less perturbed by the flow field due to theirgreater momentum.It is well known that high particle cooling rates in the spray jet (103-106 K/s) and bulk deposit (1-100 K/min) are present during spray forming 7. Most of the particles in the spray haveundergone recalescence, resulting in a solid fraction of about 0.75. Calculated solid fractionprofiles of small (30 m) and large (150 m) droplets with distance from the nozzle inlet, areshown in Figure 4b.Spray-Formed DepositsThis high heat extraction rate reduces erosion effects at the surface of the tool pattern. Thisallows relatively soft, castable ceramic pattern materials to be used that would not be satisfactorycandidates for conventional metal casting processes. With suitable processing conditions, fine6Figure 4. Calculated particle and gas behavior in nozzle and free jet regions. (a) Velocity profile.(b) Solid fraction.7surface detail can be successfully transferred from the pattern to spray-formed mold. Surfaceroughness at the molding surface is pattern dependent. Slurry-cast commercial ceramics yield asurface roughness of about 1 m Ra, suitable for many molding applications. Deposition of toolsteel onto glass plates has yielded a specular surface finish of about 0.076 m Ra. At the currentstate of development, dimensional repeatability of spray-formed molds, starting with a commonmaster, is about 0.2%.ChemistryThe chemistry of H13 tool steel is designed to allow the material to withstand the temperature,pressure, abrasion, and thermal cycling associated with demanding applications such as diecasting. It is the most popular die casting alloy worldwide and second most popular tool steel forplastic injection molding. The steel has low carbon content (0.4 wt.%) to promote toughness,medium chromium content (5 wt%) to provide good resistance to high temperature softening,1 wt% Si to improve high temperature oxidation resistance, and small molybdenum andvanadium additions (about 1%) that form stable carbides to increase resistance to erosive wear8. Composition analysis was performed on H13 tool steel before and after spray forming.Results, summarized in Table 1, indicate no significant variation in alloy additions.Table 1. Composition of H13 tool steelElementCMnCrMoVSiFeStock H130.410.395.151.410.91.06Bal.Spray Formed H130.410.385.101.420.91.08Bal.MicrostructureThe size, shape, type, and distribution of carbides found in H13 tool steel is dictated by theprocessing method and heat treatment. Normally the commercial steel is machined in the millannealed condition and heat treated (austenitized/quenched/tempered) prior to use. It is typicallyaustenitized at about 1010C, quenched in air or oil, and carefully tempered two or three times at540 to 650C to obtain the required combination of hardness, thermal fatigue resistance, andtoughness.Commercial, forged, ferritic tool steels cannot be precipitation hardened because after electroslagremelting at the steel mill, ingots are cast that cool slowly and form coarse carbides. In contrast,rapid solidification of H13 tool steel causes alloying additions to remain largely in solution andto be more uniformly distributed in the matrix 9-11. Properties can be tailored by artificialaging or conventional heat treatment.A benefit of artificial aging is that it bypasses the specific volume changes that occur duringconventional heat treatment that can lead to tool distortion. These specific volume changes occuras the matrix phase transforms from ferrite to austenite to tempered martensite and must beaccounted for in the original mold design. However, they cannot always be reliably predicted.Thin sections in the insert, which may be desirable from a design and production standpoint, areoftentimes not included as the material has a tendency to slump during austenitization or distort8during quenching. Tool distortion is not observed during artificial aging of spray-formed toolsteels because there is no phase transformation.An optical photomicrograph of spray-formed H13 is shown in Figure 5 together with an SEMimage, in backscattered electron (BSE) mode. Energy dispersive spectroscopic (EDS)composition analysis of some features in the photomicrographs is also given. While exactquantitative data is not possible due to sampling volume limitations, results suggest that grainboundaries are particularly rich in V. Intragranular (matrix) regions are homogeneous and richin Fe. X-ray diffraction analysis indicates that the matrix phase is primarily ferrite (bainite) withvery little retained austenite, and that the alloying elements are largely in solution. Discreteintragranular carbides are relatively rare, very small (about 0.1 m) and predominatelyvanadium-rich MC carbides. M2C carbides are not observed.ElementSiVCrMnMoFeSpot #1 (wt%)0.6132.136.680.172.0558.36Spot #2 (wt%)1.590.795.350.282.2889.72Figure 5. Photomicrographs of as-deposited H13 tool steel. 3% nital etch. (a) Opticalphotomicrograph. (b) SEM image (BSE mode) near a grain boundary. Table gives EDScomposition of numbered features.9Figure 6 illustrates the microstructure of spray-formed H13 aged at 500C for 1 hr. Duringaging, grain boundaries remain well defined, perhaps coarsening slightly compared to as-deposited H13 (Figure 5). The most prominent change is the appearance of very fine (0.1 mdiameter) vanadium-rich MC carbide precipitates. The precipitates are uniformly distributedthroughout the matrix and increase the hardness and wear resistance of the tool steel.Increasing the soak temperature to 700C results in prominent carbide coarsening, the formationof M7C3 and M6C carbides, and a decrease in hardness. The photomicrographs of Figure 7illustrate the dramatic change in carbide size. BSE imaging clearly differentiates Mo/Cr-richcarbides from V-rich carbides, shown as light and dark areas, respectively, in Figure 7. EDSanalysis of these carbides is also given in Figure 7.ElementSiVCrMnMoFeSpot #1 (wt%)0.0613.807.202.642.4473.86Spot #2 (wt%)1.520.825.480.232.3889.57Figure 6. Photomicrographs of spray-formed/aged H13 tool steel. 500C soak for 1 hr. 3% nitaletch. (a) Optical photomicrograph. (b) SEM image (BSE mode) near a grain boundary. Tablegives EDS composition of numbered features.10ElementSiVCrMnMoFeSpot #1 (wt%)082.279.0104.334.39Spot #2 (wt%)05.3025.70055.5513.45Spot #3 (wt%)1.600.886.320.282.9288.00Figure 7. SEM Photomicrograph (BSE mode) of spray-formed/aged H13 tool steel showingadjacent V-rich (dark) and Mo/Cr-rich (light) carbides. 700C soak for 1/2 hr, 3% nital etch.Table gives EDS composition of numbered features.Material PropertiesPorosity in spray-formed metals depends on processing conditions. The average as-depositeddensity of spray-formed H13 was 98-99% of theoretical, as measured by water displacementusing Archimedes principle.As-deposited hardness was typically about 59 HRC, harder than commercial forged and heattreated material (28 to 53 HRC depending on tempering temperature), and significantly harderthan annealed H13 (200 HB). The high hardness is attributable to lattice strain due to quenchingstresses and supersaturation.As shown in Figure 8, hardness can be varied over a wide range by artificial aging. 59 HRC as-deposited samples were given isochronal (1 hr) soaks at 50C increments from 400 to 700C, aircooled, and evaluated for microhardness. At 400C, a small decrease in hardness was observed,presumably due to stress relieving. As the soak temperature was further increased, hardness roseto a peak hardness of approximately 62 HRC at 500C. Higher soak temperature resulted in adrop in hardness as carbide particles coarsened.Peak age hardness in spray-formed H13 tool steel is notably higher than that of commercialhardened material. Normally, commercial H13 dies used in die casting are tempered to about 40to 45 HRC as a tradeoff since high hardness dies, while desirable for wear resistance, are proneto premature failure via thermal fatigue as the dies surface is rapidly cycled from 300C to700C during aluminum production runs.11Figure 8. Hardness of artificially aged spray-formed H13 tool steel following one hour soaks attemperature. Hardness range of conventionally heat treated H13 included for comparison.As-deposited spray-formed material was also hardened following the conventional heat treatmentcycle used with commercial material. Samples of forged/mill annealed commercial and spray-formed materials were austenitized at 1010C, air quenched, and double tempered (2 hr plus2 hr) at (538C). The microstructure in both cases was found to be tempered martensite with afew spheroidal particles of alloy carbide. Hardness values for both materials were very nearlyidentical.Table 2 gives the ultimate tensile strength and yield strength of spray-formed, cast, andforged/heat treated H13 tool steel measured at test temperatures of 22 and 550C. Values forspray formed H13 are given in the as-deposited condition and following artificial aging andconventional heat treatments. Values for the spray-formed material are comparable to those offorged and are considerably higher than those of cast tool steel. The spray-formed material seemsto retain its strength somewhat better than forged/heat treated H13 at higher temperatures.12Table 2. H13 tool steel mechanical properties.Sample/Heat TreatmentUltimateTensile Strength(MPa)YieldStrength(MPa)TestTemperature(C)Spray formed/as-deposited106195122Spray formed /aged at 540C1964188122Spray formed /aged at 540C16471475550Spray formed /conventional heat treatment*1358115822Cast60022Cast/conventional heat treatment*88222Commercial forged/ heat treated*1799168122Commercial forged/ heat treated*13231247550* austenitized at 1010C, double tempered (2hr+ 2hr) at 590C. no yield at 0.2% offset.Summary Spray forming is a r
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