WO2018213256A1 - Procédé d'impression tridimensionnelle mettant en oeuvre des points quantiques - Google Patents

Procédé d'impression tridimensionnelle mettant en oeuvre des points quantiques Download PDF

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Publication number
WO2018213256A1
WO2018213256A1 PCT/US2018/032680 US2018032680W WO2018213256A1 WO 2018213256 A1 WO2018213256 A1 WO 2018213256A1 US 2018032680 W US2018032680 W US 2018032680W WO 2018213256 A1 WO2018213256 A1 WO 2018213256A1
Authority
WO
WIPO (PCT)
Prior art keywords
polymer
testing
quantum dot
filament
quantum dots
Prior art date
Application number
PCT/US2018/032680
Other languages
English (en)
Inventor
Cole BRUBAKER
Douglas E. Adams
Talitha M. FRECKER
Gannon Kane JENNINGS
Sandra J. Rosenthal
Original Assignee
Vanderbilt University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Vanderbilt University filed Critical Vanderbilt University
Publication of WO2018213256A1 publication Critical patent/WO2018213256A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B29B15/10—Coating or impregnating independently of the moulding or shaping step
    • B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
    • B29B15/14—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length of filaments or wires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
    • B29C64/10—Processes of additive manufacturing
    • B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites

Definitions

  • Embodiments relate to three-dimensional (3D) printing.
  • Three-dimensional (3D) printing may occur in a multi-step process including: ( 1) drafting and designing a part using computer-aided design (CAD) software; (2) converting the CAD file to an appropriate file type for printing; and (3) printing, via a 3D printer, the final part.
  • the final part may be printed using a variety of materials (for example, plastic, metal, polymer composites, etc.).
  • Enhancements may include, but are not limited to, enhanced optical characteristics, increased durability, enhanced strength, increased material toughness, and increased ductility.
  • one embodiment provides a method of incorporating quantum dots into a filament for use in three-dimensional (3D) printing.
  • the method includes dissolving polymer in a solvent, and adding quantum dots to the dissolved polymer to produce a polymer- quantum dot composite.
  • the method further includes drying the polymer-quantum dot composite to produce a polymer-quantum dot filament.
  • FIG. 1 is a flowchart illustrating a method, or process, for incorporating quantum dots into a filament for use in three-dimensional (3D) printing, according to some embodiments.
  • FIGS. 2A & 2B are graphs illustrating various properties of the filament of Fig. 1 according to some embodiments.
  • FIG. 3A is a top view of 3D printed parts created from the filament of Fig. 1 according to some embodiments.
  • FIG. 3B are transmission electron microscopy images for 3D printed parts created from the filament of Fig. 1 according to some embodiments.
  • FIG. 3C is a top view of 3D printed parts created from the filament of Fig. 1 according to some embodiments.
  • FIG. 4 is a graph illustrating various properties of the part of Fig. 3 according to some embodiments.
  • FIG. 5 is a graph illustrating various properties of the part of Fig. 3 according to some embodiments.
  • Fig. 1 is a flowchart illustrating a process, or operation, 100 according to some embodiments.
  • the process 100 incorporates quantum dots into a filament for use in three- dimensional (3D) printing. It should be understood that the order of the steps disclosed in process 100 could vary. Furthermore, additional steps may be added to the process and not all of the steps may be required.
  • An amount of polymer is dissolved in a solvent (block 105). In some
  • the polymer includes polymer pellets formed of a thermoplastic polymer, such as but not limited to, polylactic acid (PLA) or a similar polymer.
  • a thermoplastic polymer such as but not limited to, polylactic acid (PLA) or a similar polymer.
  • PLA polylactic acid
  • any polymer having compatibility with 3D printers may be used.
  • dichloromethane (DCM) or a similar solvent may be used.
  • Quantum dots are then added to the dissolved polymer to produce a polymer- quantum dot composite (block 1 10).
  • the quantum dots are formed of Cadmium Sulfur Selenide or a similar material.
  • the quantum dots before being added to the dissolved polymer, are synthesized and treated with an appropriate surface treatment or ligand (for example, oleic acid).
  • the quantum dots can be added at varying weight percents to the dissolved polymer in order to obtain the resultant polymer-quantum dot composite used for 3D printing applications.
  • the polymer-quantum dot composite is then dried, shredded, and/or extruded to form the polymer-quantum dot composite filament (block 1 15).
  • the drying process is used to remove the solvent. Additionally, in some embodiments, the drying process includes shredding the polymer-quantum dot composite (for example, a partially dried polymer-quantum dot composite) and further drying the shredded portions at a predetermined temperature (for example, approximately 100°C) for a predetermined time period (for example, approximately one hour).
  • the dried polymer-quantum dot composite is extruded and spooled to form the filament prior to 3D printing. In such an embodiment, the dried polymer-quantum dot composite may be extruded at a specified temperature dependent on the polymer-quantum dot composite (for example, approximately 170°C).
  • FIGS. 2A & 2B are graphs 200, 205 illustrating properties of a 3D printed polymer-quantum dot composite film (PLA/QD Film) compared to a 3D printed pure polymer film (Pure PLA Film) and quantum dot solution (CdSSe QD Solution).
  • Graph 200 illustrates the absorbance of the PLA/QD Film, the Pure PLA Film, and the CdSe QD Soln.
  • the 3D printed PLA/QD Film maintained the absorbance behavior of quantum dots in solution (CdSSe Solution).
  • Graph 205 illustrates a PL emission spectra of the PLA/QD Film, the Pure PLA Film, and the quantum dot solution (CdSSe Solution).
  • 3D printed PLA/QD Films also maintains the overall optical characteristics and monotonic emissive behavior associated with quantum dots in solution, while the 3D printed Pure PLA Film displayed no emissive characteristics due to the lack of embedded quantum dots.
  • the emission and resulting color of the 3D printed polymer-composite parts can be tuned by varying the overall weight percent of quantum dots in the polymer-quantum dot composite system.
  • FIG. 3A illustrates various 3D printed parts 300 containing increasing concentrations of embedded quantum dots by weight according to some embodiments.
  • the concentrations of quantum dots by weight may be, but are not limited to approximately 0.1% QD to PLA by weight, approximately 0.5% QD to PLA by weight, approximately 1.0% QD to PLA by weight, approximately 3.0% QD to PLA by weight, approximately 5.0% QD to PLA by weight, and approximately 7.0% QD to PLA by weight.
  • the 3D printed part may include concentrations of approximately 7% to approximately 60% QD to PLA by weight (for example, approximately 20% QD to PLA by weight).
  • parts 300a are exposed to ambient light, while parts 300b are excited with ultraviolet (UV) light.
  • UV ultraviolet
  • FIG. 3B illustrates examples of resultant transmission electron microscopy images for 3D printed parts 300 and quantum dots in solution according to some embodiments.
  • image 305a is a microscopy image of as synthesized quantum dots
  • image 305b is a microscopy image of part 300 having approximately 0.5% QD to PLA by weight
  • image 305c is a microscopy image of part 300 having approximately 3.0% QD to PLA by weight
  • image 305d is a microscopy image of part 300 having approximately 7.0% QD to PLA by weight.
  • the parts 300 may be 3D printed using polymer-quantum dot filament. Although parts 300 are illustrated as rectangles, in other embodiments, the parts may be other shapes (for example, dog bone shaped parts 310 of FIG. 3C). 3D printed parts 300, 310 may be used for testing of the polymer-quantum dot filament. The testing may include, but is not limited to, tensile load testing, testing for average maximum load, testing for average maximum displacement, testing for average stress, testing for average strain at failure, testing for elastic modulus, as well as testing for toughness in addition to other optical, chemical and thermal considerations.
  • Fig. 4 is a graph 400 illustrating a load versus displacement curve for a 3D printed part (for example, parts 300, 310) and a 3D printed part using polymer filament.
  • 3D printed parts for example, parts 300, 310) may have altered mechanical strength and responses dependent on the overall concentration of embedded quantum dots.
  • such properties may be a result of interactions between individual polymer chains and encapsulated quantum dots as well as aggregation between individual quantum dots in the final 3D printed structure (for example, parts 300, 310).
  • Fig. 5 is a graph 500 illustrating differential scanning calorimetry (DSC) curves for a 3D printed PLA/QD part (for example, parts 300, 310) and a 3D printed part manufactured using Pure PLA polymer filament.
  • DSC differential scanning calorimetry
  • T g glass transition temperature
  • T c crystallization temperature
  • T m melting temperature
  • 3D printed PLA/QD part for example, parts 300, 310 and the 3D printed Pure PLA part
  • 3D printed polymer-quantum dot composite parts may have a lower glass transition temperature (T g ) due to the inclusion of quantum dots in the composite 3D printing material.
  • the application provides, among other things, a method for incorporating quantum dots into a filament for use in three-dimensional (3D) printing.
  • 3D printed parts which are printed using polymer-quantum dot composite filament, as described above, displayed changes in absorbance and emissive behavior compared to parts which are printed using an unmodified filament.
  • 3D printed parts, printed using polymer- quantum dot filament, as described above may display an altered mechanical response compared to parts printed using an unmodified polymer filament.
  • these behaviors are a result of quantum dots dispersion and aggregation occurring within the polymer chain network of the 3D printed polymer-quantum dot composite parts.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Civil Engineering (AREA)
  • Composite Materials (AREA)
  • Structural Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)

Abstract

L'invention concerne un procédé d'incorporation de points quantiques dans un filament, destiné à être utilisé dans l'impression en trois dimensions (3D). Le procédé selon l'invention consiste à dissoudre un polymère dans un solvant et à ajouter des points quantiques au polymère dissous afin de produire un composite polymère-points quantiques. Ce procédé consiste également à sécher le composite polymère-points quantiques afin de produire un filament polymère-points quantiques.
PCT/US2018/032680 2017-05-15 2018-05-15 Procédé d'impression tridimensionnelle mettant en oeuvre des points quantiques WO2018213256A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201762506042P 2017-05-15 2017-05-15
US62/506,042 2017-05-15

Publications (1)

Publication Number Publication Date
WO2018213256A1 true WO2018213256A1 (fr) 2018-11-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112247141A (zh) * 2020-10-21 2021-01-22 吉林大学 一种用于挤出3d打印的纤维增强金属基复合材料的料浆及其制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120241646A1 (en) * 2011-03-21 2012-09-27 East China University Of Science And Technology Polymer-conjugated quantum dots and methods of making the same
CN105602546A (zh) * 2015-12-30 2016-05-25 量子光电科技（天津）有限公司 用于3d打印的量子点发光复合物及其制备方法
US20160325491A1 (en) * 2013-12-26 2016-11-10 Texas Tech University System Microwave-induced localized heating of cnt filled polymer composites for enhanced inter-bead diffusive bonding of fused filament fabricated parts

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120241646A1 (en) * 2011-03-21 2012-09-27 East China University Of Science And Technology Polymer-conjugated quantum dots and methods of making the same
US20160325491A1 (en) * 2013-12-26 2016-11-10 Texas Tech University System Microwave-induced localized heating of cnt filled polymer composites for enhanced inter-bead diffusive bonding of fused filament fabricated parts
CN105602546A (zh) * 2015-12-30 2016-05-25 量子光电科技（天津）有限公司 用于3d打印的量子点发光复合物及其制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112247141A (zh) * 2020-10-21 2021-01-22 吉林大学 一种用于挤出3d打印的纤维增强金属基复合材料的料浆及其制备方法
CN112247141B (zh) * 2020-10-21 2022-07-12 吉林大学 一种用于挤出3d打印的纤维增强金属基复合材料的料浆及其制备方法

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