PLA: The Effects of Annealing & Autoclaving on Mechanical Behavior of Desktop FDM Parts

Researchers from the University of California delve into a very important area of 3D printing for the medical field, experimenting with how sterilization processes affect materials. They released their findings in the recently published ‘Identifying a commercially-available 3D printing process that minimizes model distortion after annealing and autoclaving and the effect of steam sterilization on mechanical strength.’

3D printed models are currently changing the face of medicine in terms of patient-specific treatment, allowing for better diagnosis, education for patients and their families (and medical students), along with acting as pre-planning tools and surgical guides.

In relation to FDM 3D printing in medicine, the authors refer back to previous studies concluding that PLA was weakened by sterilization yet strengthened in annealing, explaining that the next viable step would be to find a 3D printing material that can withstand heat treatment and steam sterilization.

The team fabricated four 30 mm cubes as samples for the study, each featuring different infill—designed in Tinkercad and then 3D printed on a LulzBot Mini 3D printer.

Manufacturer temperature (°C) recommendations for FDM 3D printing materials

Samples were printed all at once, using 0.38 mm layer height and a 0.5 mm printhead nozzle. Materials tested included:

  • ColorFabb Woodfill
  • Dragons Metallic PLA in All That Glitters Gold
  • Essentium PLA in Gray
  • Maker Series PLA in Food Safe FDA OK Clear
  • Maker Series PLA in White HOT White
  • Proto-Pasta HTPLA in White
  • Raptor Series PLA in HD Vivid Blue

a) Infill geometries clockwise beginning from top-left: tetrahedral, triangles, grid, zig-zag and b) 3D printed cubes

Each sample was bathed in hot water, with the annealing treatment performed via an 800 W Strata Home sous vide circulating precision cooker.

“The cubes were removed from the hot water-bath and allowed to cool to room temperature without interference. The X, Y, and Z dimensions of the cubes were measured again to quantify deformation and calculate percent changes, a positive percent change indicating expansion and a negative percent change indicating shrinkage,” explained the researchers.

“In order to quantify distortion in either direction, we took the absolute value of these percentages. Subjective observations were noted such as spherical ‘balloon-like’ expansion. We also analyzed whether certain materials consistently expanded or contracted in every axes.”

Samples were then placed in autoclave sterilization pouches and deposited into a Tuttnauer 2540 M autoclave for 45 minutes at 134 °C and a pressure of 375 PSI. Afterward, the samples were cooled to room temperature and then examined for any signs of deformation.

a) Standard Army-Navy retractor and b) strength-optimized Army-Navy retractor designs in inches created in AutoDesk Fusion 360 obtained from Chen et al. c Retractor orientation on the build plate to eliminate need for support material

a) Standard retractors warping after hot water-bath annealing and b) after autoclaving. c) Strength-optimized retractor without intervention (right) and warping after hot water-bath annealing (left)

The material exhibiting the least amount of deformation was Essentium PLA Gray. The highest deformation was noted in Maker Series PLA White HOT White.

Quantifying absolute deformation in 30 mm cubes across 3D printing materials after annealing

“After hot water-bath annealing for 30 mm cubes, the infill that deformed the least was ‘grid,’ and the infill pattern that deformed the most was ‘zig-zag.’ After both annealing then autoclaving for 30 mm cubes, the material that deformed the least was Essentium PLA Gray. The material that deformed the most was Maker Series PLA White HOT White. After both annealing then autoclaving for 30 mm cubes, the infill pattern that deformed the least was ‘grid,’ and the infill pattern that deformed the most was ‘tetrahedral.’”

Quantifying absolute deformation in 30 mm cubes across 3D printing materials after annealing then autoclaving

Quantifying absolute deformation in 30 mm cubes across infill geometries after annealing then autoclaving

Maker Series PLA White HOT White was the only material noted to expand in every axis—despite the infill geometry or intervention. Every other material showed variances due to infill. Expansion after annealing usually seemed to suggest ‘direction of distortion’ after autoclaving.

“We acknowledge that dimensional changes and strength limitations may not be a challenge at a lower autoclave cycle, which would require further testing. We have also yet to understand the mechanical behavior of the 3D printed models in this study when they are subjected to multiple cycles of autoclaving and whether they will continue to undergo dimensional change. However, regardless of whether 3D printed PLA surgical instruments are determined to be single or multi-use, these instruments may still be valuable in fields such as aerospace medicine where space limitations exist, or in resource-limited situations where additional instruments are needed,” stated the researchers.

“This study is intended as a pre-clinical evaluation of the mechanical behavior of FDM 3D printing materials following hot water-bath annealing treatment and autoclave sterilization. For FDM 3D printed Army-Navy retractors, further sterilization and biocompatibility validation will be necessary for it to be applied clinically.”

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[Source / Images: ‘Identifying a commercially-available 3D printing process that minimizes model distortion after annealing and autoclaving and the effect of steam sterilization on mechanical strength’]

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Safety Suggestions for 3D Printing Medical Parts at Home: FDM Polymers

This does not constitute medical advice or indeed is meant to convey any particular indication that it would be safe to print medical parts at home. In a moment bereft of optimal choices however people are printing medical and ancillary medical things at home using desktop FDM systems. In order to make this safer, we’ve penned a number of articles encouraging you to do no harm, some safety suggestions on your print room setup and how to keep it clean and the relevant safety guidelines available including if you’ll print what category of items you’ll print. GMP plus the right materials and certifications is the only way to safely make a medical product or a quasi-medical product. If you print irresponsibly or cough on a face shield that you give to a hospital you may, in fact, kill someone who would have lived without you face shield. Please be careful.

Cleaning

1, Parts should be cleaned with soap and water. This is a guide on cleaning for COVID.

Disinfectant 

2. Subsequently, you can disinfect them. This is a list of EPA approved disinfectants. You should make sure that you yourself are clean and wearing gloves before doing this step. A newly washed apron, gloves, mask, and a face shield should be worn before disinfecting. All surfaces should be cleaned and disinfected before doing this step. Do not eat, drink, let people or pets in the room before this step.

Sterilization

3. Sterilization is a required step. There are a number of different processes that can all kill the living things that will inhabit your parts. Here is a quick guide, here are the CDC guidelines on sterilization and this is a practical guide.

Autoclaving

Autoclaving is the most common form of sterilization for a lot of polymer 3D printed parts. This gives you a good overview. Essentially your parts are sterilized under pressurized steam at around 121C. Immediately you’ll know that PLA won’t fare well under these conditions. These parts will often delaminate and fail.

In fact, most FDM materials do not fare well when autoclaved as their heat deflection temperatures are too low. Materials such as PPSU/PSU/PPSF are good candidates for autoclaving and can be exposed to repeated cycles. Their print temperatures range in the 380C range and 100C bed temperature however and this is beyond the reach of many desktop machines. The material is also around $380 per 500g or $216 per 500g, depending on approvals and the vendor. You could also consider materials such as PEEK or PEKK which also are expensive and high performance. PEI also withstands repeated cycles. PEEK is very difficult to print, PEKK and PEI are generally easier. To process these materials well you will have to have a highly modded printer or a high-temperature printer with a nozzle print temp of 400C, bed temp 100C and chamber temperature of 100C.

ABS is generally not a good candidate for autoclaving and ABS parts often fail in the autoclave. All other materials not mentioned here are also not good. This is a guide specifying which polymers are good candidates for the autoclave.

Should you wish to go the low-cost route then Polypropelene is also an alternative. Some polycarbonates could work but parts may warp and strength is reduced. Stratasys’ PC-ISO material is a good candidate for autoclaving. Polyamide filaments (but only really PA6) can, in a limited way, be autoclaved and are more accessible. POM (Acetal) is a risk in terms of fumes but with sufficient industrial ventilation could be managed. I personally wouldn’t print POM at home even with an enclosed system, filters and good ventilation.

WARNING: Please never 3D print PVC filament, it is too high risk to use, even in an industrial setting with HVAC and high safety standards. Fumes are highly toxic and dioxins may remain on your printer or on parts. There is no safe way to 3D print PVC. 3D printed PVC parts may have highly toxic dioxin residue on or in them. Here are articles on dioxins and PVC and thermal decomposition and in fires. During the 3D printing of PVC: hydrogen chloride may be released, cancer causing PAH’s may be released, as may toxic and carcinogenic dioxins.

Never use CF or GF or carbon nanotube or carbon black filaments for this application and try for the natural color if possible. Please note that even natural color filaments do often contain undisclosed not MSDS listed processing additives but generally no colorants. Please purchase filaments with the relevant approvals.

Other Options 

Typically the users will have their very own processes and adhere to them. There are some other options as well. Prusa has done a great job on identifying them for their face shield designs. They’ve found that for their shields autoclaving specifically will deform them. With some different materials this may not be the case. I’d always go with a part that can work in an autoclave. This is a readily available sterilization technology.

Also, the nice thing about an autoclave is that it is a very well understood, widely practiced, reliable technology. For the other methods above the processes could be less controllable. So design parts that work in materials that work in an autoclave, If this is impossible then I’d move to other sterilization methods.

What is encouraging for parts made in the home for the home or for you sterilizing a mask before you give it to your brother for example, is that a 5 minute bath in IPA seems to do the trick. Bleach could also be a solution. This means that with care, there are methods by which you could do a rudimentary sterilization at home. Now rudimentary sterilization is a bit like saying you’re half pregnant. Especially with cleaning, disinfecting and sterilizing we want to be incredibly careful.

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