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Evonik VESTAKEEP i4 3DF-T PEEK

    • Название продукта: Evonik VESTAKEEP i4 3DF-T PEEK
    • Сайт Factroy: Округ Юду, Ганьчжоу, Цзянси, Китай
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    Спецификации
    Код ТН ВЭД 314414

    Как аккредитованный завод Evonik VESTAKEEP i4 3DF-T PEEK, мы соблюдаем строгие протоколы качества - каждая партия подвергается строгим испытаниям для обеспечения последовательных стандартов эффективности и безопасности.

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    Применение Evonik VESTAKEEP i4 3DF-T PEEK

    For cranial plate preforms and maxillofacial cutting guides, VESTAKEEP i4 3DF-T unfilled PEEK filament is printed on heated-chamber FFF systems fitted with a liquid-cooled all-metal hot end capable of sustained operation at 450 °C. The build chamber is held at 150 °C to 180 °C, and the build plate at 160 °C to 200 °C. Published processing guidance for this viscosity class recommends a 0.4 mm hardened nozzle, layer height between 0.15 mm and 0.25 mm, extrusion temperature between 400 °C and 430 °C, and a print speed not exceeding 40 mm/s. Under these conditions, interlayer bonding develops through chain re-entanglement across the melt interface; chamber temperatures below 150 °C produce anisotropic tensile strength loss exceeding 30% in the Z direction when tested according to ISO 527-2. Prior to clinical use, printed blanks are annealed in a circulating-air oven at 200 °C for 2 h, then slow-cooled at 5 °C/min to avoid residual stress cracking. The raw material is typically qualified to USP <88> Class VI for systemic injection, intracutaneous, and implantation extracts, but final device validation must be carried out under ISO 10993-1:2018, including cytotoxicity by ISO 10993-5:2009 and sensitization by ISO 10993-10:2010. Terminal components include patient-specific osteotomy guides, temporary implant prototypes, and surgical instrument handles. Warpage and delamination on production-scale systems are the dominant failure modes; these are controlled by maintaining chamber temperature uniformity within ±5 °C and by avoiding layers thinner than 0.15 mm, which can undergo preferential cooling at the nozzle tip.

    Biocompatibility and quality-system matrix for printed unfilled PEEK devices
    AssessmentStandard / methodConditionQualification note
    Biocompatibility endpointISO 10993-1:2018Device contact duration and tissue typeFinal printed geometry requires testing
    CytotoxicityISO 10993-5:2009MEM elution, L-929 fibroblastsUse extraction ratio according to surface area
    SensitizationISO 10993-10:2010Guinea pig maximization or LLNANo material change after annealing
    Material qualificationUSP <88> Class VINaCl, alcohol, PEG 400 extractsRaw-filament certificate only
    Quality systemISO 13485:2016Process validation IQ/OQ/PQTraceability for each build lot
    Risk managementISO 14971:2019Warpage, delamination, residual stressAnneal protocol documented

    How Does Print-Induced Crystallinity Shift Affect Aerospace Bracket Creep at 180 °C?

    The limiting factor for unfilled PEEK brackets in continuous air at 180 °C is not short-term oxidation but time-dependent creep of the amorphous fraction. As printed, the polymer contains a crystallinity level typically between 25% and 35% depending on build chamber temperature and cooling rate; post-annealing at 200 °C for 2 h raises the crystallinity to roughly 35% to 45%. Creep modulus measured at 150 °C under 10 MPa tensile stress according to ISO 899-1 shows a greater compliance reduction in unannealed samples than in annealed samples, because the glass transition at 143 °C separates the rubbery amorphous regions from the rigid crystalline domains. For airframe brackets replacing machined aluminium, the printed component is designed with continuous-load stress below 15 MPa at 150 °C to keep 1,000-hour strain below 2%. Flame-resistance qualification for cabin interiors uses 14 CFR 25.853(a) vertical-burn coupons; a 1.6 mm injection-moulded unfilled PEEK coupon has documented compliance with the vertical-burn pass criteria, but printed parts must be tested with edge surfaces oriented as manufactured because raster boundaries may alter flame spread. Smoke density and heat release are evaluated according to 15 CFR 25.853(d) OSU heat release, with a limit of 65 kW/m² peak and 65 kW·min/m² total. Terminal parts include low-velocity air duct flanges, clamp blocks, wire harness standoffs, and avionic bracket isolators. On production FFF machines with a 300 mm × 300 mm × 300 mm heated build volume, batch-to-batch variability in crystallinity is reduced by keeping chamber temperature above 150 °C and by using a controlled cooling phase at 2 °C/min to 5 °C/min after the final layer.

    In centrifugal pump wear rings and valve seats handling aggressive aqueous streams, the filament is printed with 100% infill, a 0.2 mm layer height, and a 0.4 mm nozzle, then machined on the sealing face to Ra 0.8 µm. Chemical compatibility for unfilled PEEK is evaluated by prolonged immersion according to ASTM D543-21 in 20 wt% sulfuric acid at 80 °C; the design acceptance criterion is set at 90% tensile strength retention after 1,000 h. Published data for injection-moulded PEEK under non-oxidizing dilute acid conditions supports this criterion, but printed coupon qualification is mandatory because layer interfaces can act as preferential diffusion paths. The main processing limitation is not chemical attack but seal-path porosity at layer interfaces; a hydrostatic leak test at 3 bar with water is used to reject parts with connected voids. For gaskets and sensor housings in steam lines and ethylene oxide sterilizers, the grade withstands hot steam at 120 °C to 134 °C without significant hydrolysis, but continuous exposure to concentrated nitric acid, concentrated sulfuric acid, or free chlorine at temperatures above 80 °C should be excluded from design. Stress cracking in chlorinated solvents is evaluated by ISO 22088-3:2006; unfilled PEEK is resistant in most low-polarity oils but requires coupon screening when mixed aromatic fractions exceed 5%. Terminal parts include wear rings, valve seats, gasket rings, sensor bodies, and pump casing inserts in chemical metering circuits.

    When Semiconductor Test Socket Tooling Must Stay Below 0.10% Collected Volatile Condensable Material

    Printed tooling for semiconductor contactors, wafer combs, and handler end effectors is qualified by total mass loss and collected volatile condensable material according to ASTM E595-15; acceptance limits are typically 1.00% TML and 0.10% CVCM after 24 h at 125 °C and 5×10⁻⁵ Torr. Unfilled PEEK can pass these limits after a pre-bake at 150 °C for 4 h, because absorbed water from equilibrium at 23 °C/50% RH otherwise contributes to the TML value. The coefficient of linear thermal expansion of unfilled PEEK is approximately 50×10⁻⁶ K⁻¹ below the glass transition, roughly ten times that of silicon; wafer contact tooling therefore uses slotted or segmented designs rather than rigid full-contact plates. Surface resistivity of unfilled PEEK remains above 10¹³ Ω according to IEC 62631-3-2, so the material is not suitable for static-dissipative nests unless a carbon-filled grade or external grounding path is introduced. Dimensional stability of printed alignment pins is maintained by printing at 100% infill and by annealing to complete crystallinity relaxation, then finish-machining to a tolerance of ±0.05 mm. In test socket bodies carrying pogo pins at 150 °C, creep under side load is controlled by specifying wall thickness not less than 2.0 mm and by orienting the load against the crystalline flow direction. Terminal parts include handler contact blocks, wafer combs, test socket frames, and high-temperature electrical insulators.

    Outgassing acceptance for semiconductor tooling
    ParameterStandardAcceptance limitPrinted part verification
    Total mass lossASTM E595-151.00% maxPre-bake at 150 °C for 4 h, test per coupon
    Collected volatile condensable materialASTM E595-150.10% maxQuartz collector at 25 °C
    Water vapor regainedASTM E595-15ReportedDistinguish water from organic outgassing
    Surface resistivityIEC 62631-3-2Insulative categoryNo static-dissipative claim for unfilled grade

    To qualify downhole electrical connectors and seal backup rings, rapid gas decompression resistance is tested by NORSOK M-710 Annex B after saturation in a 90/10 CO₂/CH₄ mixture at 100 bar and 100 °C. Published data for printed PEEK under these specific conditions is limited, so coupon qualification must be performed for each build orientation and annealing protocol. Compatibility with aliphatic hydrocarbons, brine, and sour gas is evaluated by immersion testing under ISO 23936-2:2011; the unfilled PEEK grade is generally accepted for such service below its chemical degradation threshold, but each field fluid requires coupon verification. Continuous contact with amine-based corrosion inhibitors above 150 °C is excluded because amine absorption can reduce glass transition temperature and accelerate creep. Seal backup rings are printed with spiralized outer contours and then machined to a square or bevelled cross-section; a compression set test at 200 °C for 24 h according to ASTM D395-18 is used to assess dimensional recovery. On FFF machines, residual thermal stress from a 150 °C chamber can produce radial cracking in thick rings exceeding 6 mm wall thickness; this is reduced by using a post-print annealing step at 200 °C for 4 h and slow cooling. Terminal parts include downhole connector housings, seal backup rings, sensor mounts, and packer wear shoes.

    Combustion Gas Path Sealing, 0.5 mm Wall Thickness, and Continuous-Use Rating Under UL 746B

    Below 0.5 mm wall thickness, combustion gas path sealing parts and EGR sensor housings are printed with a 0.25 mm layer height and 100% infill to minimize void content. Unfilled PEEK in sheet or injection-moulded form is rated UL 94 V-0 at 3.0 mm; printed coupons can meet the same classification when edge surfaces are machined to remove raster notches, but the rating is not automatically transferable to FFF parts and must be re-established by UL 94 vertical burn testing on printed bars. Continuous-use temperature in air is assessed by UL 746B relative thermal index; unfilled PEEK typically carries an RTI of 240 °C for mechanical impact and 260 °C for electrical. Short-term excursions to 260 °C are allowed only under mechanical load below 5 MPa as determined by creep testing per ISO 899-1. Short-term dielectric strength of unfilled PEEK is approximately 20 kV/mm when tested by IEC 60243-1; printed parts with internal delamination may show breakdown below 12 kV/mm, so a withstand test at 1.5 kV for 60 s is applied to motor end-bell insulators. For press-fit electrical insulator rings, the high coefficient of thermal expansion requires radial clearance of 0.20 mm to 0.30 mm per 25 mm diameter to avoid cracking of mating steel housings after heat aging. Terminal parts include EGR sensor flanges, PCV valve seats, motor end-bell insulators, and high-temperature terminal blocks.

    After 100 steam sterilisation cycles at 134 °C for 5 min with 0.21 MPa gauge pressure, tensile modulus retention can be tracked by ISO 527-2 coupon testing; reported differences for unfilled PEEK are typically within measurement scatter. Sterilisation trays, autoclave racks, and dental instrument holders are printed in open-lattice structures to reduce thermal mass and to allow condensate drainage; critical load-bearing struts are designed with a minimum cross-section of 3 mm to prevent creep during the 30 min drying phase at 120 °C. Validation of steam sterilisation for printed devices is performed according to ISO 17665-1:2006, with biological indicators and temperature mapping of the load. Repeated exposure to steam above 140 °C can accelerate hydrolysis at layer interfaces, so the upper use temperature for sustained steam service is limited to 134 °C. For dental autoclave trays sterilized daily, water absorption at 23 °C/50% RH remains below 0.5 wt%, preventing significant dimensional shift after drying. Terminal parts include sterilisation trays, autoclave racks, dental instrument holders, and load-bearing fixtures in central sterile processing departments.

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    Evonik VESTAKEEP i4 3DF-T is a natural-colour polyether ether ketone monofilament for fused filament fabrication of high-temperature and medical components. The product is manufactured from VESTAKEEP i4 G resin, a medium-viscosity unfilled PEEK grade that meets ASTM F2026 for raw polyether ether ketone feedstock intended for surgical implant applications. The filament is supplied in two diameters, 1.75 mm and 2.85 mm, on sealed spools with net weights of 250 g and 500 g. The base resin density is 1.30 g/cm³ when tested to ISO 1183-1. The melting peak is 340 °C and the glass transition temperature is 143 °C, both determined by differential scanning calorimetry per ISO 11357-1 and ISO 11357-3. These values place the material in the semicrystalline high-temperature thermoplastics class and require extrusion hardware that can sustain melt temperatures above 400 °C. The filament is not a direct drop-in for amorphous 3D-printing polymers: it must be dried before processing, deposited into a heated chamber, and typically annealed if maximum crystallinity and dimensional stability are required. The product designation separates the filament format from granulate; the i4 suffix identifies the medium-viscosity base resin, while the 3DF-T suffix indicates a filament product with controlled diameter, ovality, and spool winding for reliable FFF feeding.

    What Melt-Viscosity and Thermodynamic Values Govern Nozzle Deposition?

    Extrusion of VESTAKEEP i4 3DF-T through a 0.4 mm hardened steel or tungsten carbide nozzle is constrained by the medium-viscosity melt behaviour of the i4 base resin. Evonik technical documentation for VESTAKEEP i4 G reports a melt volume-flow rate of approximately 25 cm³/10 min at 380 °C and 5 kg load when tested to ISO 1133-1. This is higher than high-viscosity PEEK grades such as VESTAKEEP 4000 G but lower than melt-extrusion grades optimized for high-throughput fused granulate fabrication. The practical consequence is that the filament can be extruded at linear deposition speeds typical of high-temperature FFF machines without excessive melt pressure, provided the hot end can maintain a continuous setpoint between 400 °C and 430 °C. A heated build plate is required in the range of 130 °C to 150 °C, and a closed build chamber should be held at a temperature that prevents rapid cooling of the deposited bead below the glass transition. Machine-specific chamber setpoints from 90 °C to 150 °C are encountered; published data for the exact minimum chamber setpoint for VESTAKEEP i4 3DF-T is limited, and the optimal value depends on part cross-section, layer time, and whether the printer uses active side heaters or passive enclosure heating. Hardened steel or tungsten carbide nozzles are preferred over brass when long campaigns are run because PEEK melt at 400 °C accelerates copper-alloy wear in carbon-filled grades; for this unfilled grade the primary nozzle concern is thermal stability of the thermistor and heater block rather than abrasive wear. The extruder drive system should be capable of maintaining filament feed force without buckling the filament; a constrained or dual-drive filament path is commonly specified on production high-temperature printers with actively heated chambers. The viscosity data also govern die swell and road width control: the first layer height is typically set at 0.20 mm to 0.25 mm for a 0.4 mm nozzle, and extrusion multipliers are reduced if the melt temperature is raised above the 400 °C reference setpoint because viscosity falls with increasing temperature. The residence time of the melt inside the hot end should be minimized because PEEK can degrade if held at 430 °C for extended periods; short melt zones and hardened nozzles reduce the risk of gel formation and black specks.

    Prior to extrusion, the filament must be dried to prevent hydrolytic degradation and steam-induced porosity in the deposited road. PEEK has a low equilibrium moisture uptake, but filament wound onto spools can acquire surface moisture during shipping and handling at relative humidity above 60%. Drying in a desiccant or vacuum oven at 150 °C for 3 h is a typical pre-processing condition for PEEK filament, with the dried spool transferred directly to a dry-feed enclosure maintained below -40 °C dew point. Printed parts that exhibit intermittent surface pits, steam bubbles at the nozzle, or a hissing sound during extrusion are usually indicators of residual moisture. The spool should not be left uncovered in an uncontrolled production room for more than 4 h after drying; if longer exposure occurs, re-drying is required. The winding tension and layer-to-layer spooling pattern of VESTAKEEP i4 3DF-T are specified to avoid filament cross-over and buckling in long-bowden or direct-drive feed paths. Excessively tight feed-path bends can cause elastic energy storage and slip at the drive gear; for 1.75 mm filament, the machine-specific minimum bend radius supplied by the printer builder should be followed rather than a universal value. A filament run-out sensor and an enclosed spool holder with desiccant pack reduce batch-to-batch moisture variation in production.

    Thermal Transitions Alone Do Not Prevent Z-Axis Delamination

    The melting point of 340 °C and glass transition of 143 °C define the thermal window, but they do not guarantee sufficient interlayer fusion in FFF parts. In the molten state, the i4 base resin flows at the extrudate surface and begins to cool immediately after deposition. If the chamber temperature is too low, the previously deposited layer remains below the glass transition, and chain diffusion across the weld interface is incomplete. The result is a plane of weakness that is measurable as a reduction in tensile strength when specimens are printed in the Z orientation and tested to ASTM D638-14 or ISO 527-2. Published data for the specific Z-direction properties of VESTAKEEP i4 3DF-T is limited, but fused filament fabrication of PEEK is known to produce anisotropic mechanical behaviour; the interlayer bond is the critical process variable, not the bulk resin tensile strength. Annealing at 200 °C for 2 h is commonly used to increase crystallinity, relieve residual stress, and restore a proportion of the lost interlayer strength. The annealing cycle should be applied after printing with the part fixtured or supported, because PEEK parts can distort as the residual stress relaxes. Crystallization kinetics also influence this step: PEEK crystallizes slowly from the melt, and the cooling rate in the build chamber controls whether the as-printed matrix is predominantly amorphous or semicrystalline. A chamber held near 150 °C slows the cooling rate and shifts the crystallinity toward the equilibrium semicrystalline state, whereas a chamber below the glass transition freezes in a largely amorphous structure that later sinters and changes dimensions during annealing. This is why the same nominal print temperature can produce different final crystallinity and different mechanical response from one printer to another.

    Chemical Resistance, Moisture Uptake, and Sterilization Workflow Boundaries

    The unfilled PEEK chemistry of VESTAKEEP i4 3DF-T provides broad resistance to aqueous process fluids, aliphatic and aromatic hydrocarbons, alcohols, esters, and many halogenated solvents under ambient conditions; specific chemical compatibility of printed parts should be verified by immersion testing per ISO 175. The base resin absorbs less than 0.5% water at saturation when tested to ISO 62, which supports repeated steam sterilization cycles. Steam sterilization at 134 °C for minimum hold times of 18 min should be performed on printed parts only after annealing, because residual amorphous zones can undergo secondary crystallization and small dimensional shifts during the first autoclave exposure. Gamma irradiation at 25 kGy to 50 kGy is also applied to PEEK medical devices; mechanical evaluation per ISO 527-2 after irradiation is required because the dose rate and oxygen exposure affect the measured retention. Ethylene oxide sterilization is acceptable provided that the printed part is fully degassed after the cycle and the process validation confirms residual gas limits. Concentrated sulfuric acid and concentrated nitric acid attack PEEK at elevated temperatures and are outside the operational compatibility envelope. The use of strong oxidizing acids or combinations of chlorinated solvents with high temperatures should be excluded from cleaning protocols because the ketone and ether linkages in the polymer backbone are susceptible to chain scission. Machining coolants containing chlorinated paraffins should be removed before annealing or sterilization because thermal decomposition of the coolant at 400 °C is a potential source of surface contamination. The chemical inertness of the base resin does not eliminate the need for post-printing cleaning validation under the applicable medical-device quality system.

    Support removal and machining are governed by the semicrystalline nature of the printed matrix. VESTAKEEP i4 3DF-T parts can be machined on standard CNC mills using carbide tooling; water-based coolant is preferred to dry machining because PEEK has low thermal conductivity and can generate localized heat at the cut surface. Drilling and tapping should be performed after annealing, because the as-printed amorphous regions can smear and produce burrs at the hole edge. Support structures printed in PEEK are difficult to remove; breakaway supports are practical only if the support interface is designed with a small contact area. Soluble support materials are generally incompatible with the high chamber temperatures required for PEEK, so mechanical removal is the standard route. Sanding and polishing require gentle pressure because PEEK is notch-sensitive; a sharp machined surface or scratch can reduce notched impact strength measured to ISO 179-1/1eA. Surface roughness and residual stress after machining should be checked before cleaning and packaging.

    Because the filament is intended for medical and implant manufacturing, the regulatory documentation chain matters as much as the thermal and mechanical data. VESTAKEEP i4 G, the base resin for VESTAKEEP i4 3DF-T, is specified against ASTM F2026, which establishes chemical identity, density, tensile properties, and melt flow requirements for PEEK used in surgical implants. The medical-device manufacturer remains responsible for final biocompatibility evaluation under ISO 10993-1:2018 with endpoints selected according to contact duration and tissue type; cytotoxicity testing to ISO 10993-5 and sensitization or irritation testing to ISO 10993-10 are common for implant-grade PEEK, but material certification alone does not exempt the final device from testing. For devices sold in Europe, the finished implant must comply with EU MDR 2017/745; for the United States, the device must comply with 21 CFR Part 820 and applicable premarket requirements. For industrial and non-implant applications, documentation is frequently evaluated under REACH and RoHS obligations, but the applicability depends on the final article and its intended market. The filament format introduces additional process-controlled variables—extrusion temperature, build orientation, layer height, annealing temperature, and chamber atmosphere—that are not present in injection-moulded PEEK. Therefore, the quality system must treat the filament lot, printer lot, and build cycle as interacting variables. A compliance checklist for the documentation chain that typically accompanies the material supply is provided below.

    Documentation chain for VESTAKEEP i4 3DF-T and VESTAKEEP i4 G base resin
    StandardTitle or endpointScope
    ASTM F2026Standard specification for PEEK polymers for surgical implant applicationsRaw resin conformance
    ISO 1133-1Melt volume-flow rate, 380 °C/5 kgViscosity control
    ISO 1183-1DensityMaterial identity
    ISO 11357-1/-3Melting and glass transition temperaturesThermal processing window
    ISO 527-2Tensile propertiesBase resin and printed-part characterization
    ISO 179-1/1eACharpy notched impact strengthImpact resistance
    ISO 10993-1:2018Biological evaluation planningFinished-device responsibility
    ISO 10993-5In vitro cytotoxicityBiocompatibility endpoint
    ISO 10993-10Sensitization and irritationBiocompatibility endpoint

    Representative base resin values reported by Evonik for VESTAKEEP i4 G include tensile modulus of 4100 MPa, tensile stress at yield of 100 MPa, elongation at yield of 5%, elongation at break of 20%, Charpy notched impact strength of 6.0 kJ/m² to ISO 179-1/1eA. These values apply to injection-moulded test plaques and are not automatically transferred to FFF parts without build-orientation correction.

    When the Filament Must Be Distinguished from VESTAKEEP i4 G Granulate and Other PEEK Grades

    The distinction between VESTAKEEP i4 3DF-T and VESTAKEEP i4 G granulate is process-format based, not bulk-chemistry based. The i4 G granulate is supplied for injection moulding and other melt-processing methods; the i4 3DF-T filament is converted from the same resin chemistry into a controlled-diameter filament for FFF. The conversion step adds spool winding, diameter tolerance, and moisture control requirements that do not apply to granulate. VESTAKEEP i4 3DF-T should not be ground and fed as granulate into an injection moulding machine, because the winding process and thermal history of the filament are not validated for injection moulding process control. Conversely, i4 G granulate cannot be directly used in a filament-fed FFF machine without a pellet-fed extruder head and filament winding system. When compared to other Evonik PEEK grades such as VESTAKEEP 4000 G or high-viscosity grades, the i4 medium-viscosity designation shortens the time required for interlayer wetting but reduces the melt strength needed for very large unsupported horizontal spans; in FFF, these properties are balanced by nozzle temperature, chamber heating, and deposition strategy. When compared to carbon-fibre-reinforced PEEK filaments, the unfilled i4 3DF-T has lower wear on machine hardware but lower modulus and lower dimensional stability at elevated load; if compressive or flexural stiffness is the controlling design variable, carbon-filled grades should be evaluated with the appropriate flexural test method such as ISO 178 or ASTM D790. Published data for direct mechanical comparisons between VESTAKEEP i4 3DF-T and other PEEK filaments under identical FFF processing conditions is limited, so any substitution should be preceded by a designed experiment using the same printer, toolpath, chamber temperature, and annealing cycle.

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