Thermoset composite having thermoplastic characteristics

Patent metadata

Field	Value
Publication number	US-10974463-B2
Application number	US-201916687140-A
Country	US
Kind code	B2
Filing date	Nov 18, 2019
Priority date	Jun 16, 2015
Publication date	Apr 13, 2021
Grant date	Apr 13, 2021

Abstract

A composite composition includes a thermoset resin and about 3 wt. % to about 35 wt. % of at least one material selected from the group consisting of cellulose nanofibrils (CNF), micro-sized cellulose fibers (MFC), and cellulose nanocrystals (CNC) dispersed therein as measured with respect to the overall weight of the composite composition. The cellulose nanofibrils and/or nanocrystals have an average diameter of about 5 nm to about 500 nm and an average aspect ratio in the range of about 5:1 to about 500:1. The cellulose micro-sized fibers have an average diameter of about 5 μm to about 100 μm and an average aspect ratio in the range of about 5:1 to about 250:1.

First claim

What is claimed is:

1. A method of making an article, the method comprising:
forming a composite composition comprising an uncured thermoset resin and 3 wt. % to 35 wt. % of at least one material selected from the group consisting of cellulose nanofibrils (CNF), micro-sized cellulose fibers (MFC), and cellulose nanocrystals (CNC) dispersed therein as measured with respect to an overall weight of the composite composition, wherein the cellulose nanofibrils and/or the nanocrystals have an average diameter in a range of 5 nm to 500 nm and an average aspect ratio in a range of 5:1 to 500:1, wherein the cellulose micro-sized fibers have an average diameter in a range of 5 μm to 100 μm and an average aspect ratio in a range of 5:1 to 250:1;
depositing the composite composition via a three-dimensional (3D) printing process to fabricate a green article comprising multiple layers of the composite composition; and
curing the green article to form an at least partially cured article.

2. The method of claim 1 , wherein the forming of the composite composition comprises:
providing the uncured thermoset resin;
providing the cellulose nanofibrils (CNF), the micro-sized cellulose fibers (MFC), and/or the cellulose nanocrystals (CNC); and
mixing the thermoset resin with the CNF, MFC, and/or CNC to form the composite composition.

3. The method of claim 2 , wherein the at least partially cured article comprises a tensile strength in a range of 35 MPa to 45 MPa.

4. The method of claim 2 , wherein the at least partially cured article comprises an elastic modulus in a range of 3 GPa to 3.6 GPa.

5. The method of claim 2 , wherein the curing is conducted at ambient temperature for a predetermined time.

6. The method of claim 2 , wherein the curing comprises heating the green article to a predetermined temperature for a predetermined time.

7. The method of claim 2 , wherein the forming of the composite composition further comprises:
providing a curing agent; and
mixing the thermoset resin and the curing agent when present with the CNF, MFC, and/or CNC to form the composite composition.

8. The method of claim 7 , wherein the at least partially cured article comprises a tensile strength in a range of 35 MPa to 45 MPa.

9. The method of claim 7 , wherein the at least partially cured article comprises an elastic modulus in a range of 3 GPa to 3.6 GPa.

10. The method of claim 7 , wherein the curing is conducted at ambient temperature for a predetermined time.

11. The method of claim 7 , wherein the curing comprises heating the green article to a predetermined temperature for a predetermined time.

12. The method of claim 7 , wherein the curing agent comprises a polyamide, an amidoamine, an aliphatic amine, a cycloaliphatic amine, or a combination thereof.

13. The method of claim 1 , wherein the composite composition comprises a thermoset resin selected from the group consisting of epoxy resins, vinyl ester resins, and polyester resins.

14. The method of claim 1 , wherein the thermoset resin comprises an epoxy resin, and
wherein the composite composition further comprises a curing agent.

15. The method of claim 14 , wherein the curing agent comprises a polyamide, an amidoamine, an aliphatic amine, a cycloaliphatic amine, or a combination thereof.

16. The method of claim 1 , wherein the at least partially cured article comprises a tensile strength in a range of 35 MPa to 45 MPa.

17. The method of claim 1 , wherein the at least partially cured article comprises an elastic modulus in a range of 3 GPa to 3.6 GPa.

18. The method of claim 1 , wherein the curing is conducted at ambient temperature for a predetermined time.

19. The method of claim 1 , wherein the curing comprises heating the green article to a predetermined temperature for a predetermined time.

Assignees

• Ut Battelle Llc

Inventors

• Ozcan Soydan
• Tekinalp Halil L

Classifications

• B33Y70/10

  Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials · CPC title

• B29K2105/124

  Nanofibers · CPC title

• C09D163/00

  Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins · CPC title

• B29K2067/00

  Use of polyesters {or derivatives thereof}, as moulding material · CPC title

• C08G59/245

  aromatic · CPC title