3Y-TZP DLP Additive Manufacturing: Solvent-free Slurry Development and Characterization

Vat photopolymerization (VP) stands out among ceramic additive manufacturing processes for its ability to print sub-100 micrometer complex features. One of the main challenges of this process is the preparation of a homogeneous and stable ceramic slurry with a high solid load and low viscosity. In this work, different dispersants and resins were tested, aiming to provide a solvent-free slurry suitable for DLP additive manufacturing. Disperbyk-111 and PEGDA 250 stood out in the tests, providing a 40 vol% ceramic slurry with no noticeable sedimentation and viscosity of 2.3 Pa.s at 30 s^-1 despite the relatively high specific surface area (15 m²/g) of the 3Y-TZP powder used compared to powders usually used for VP slurries. The adsorption of Disperbyk-111 on ceramic particles surface was investigated by FTIR. Finally, ceramic bodies were 3D printed, debound and sintered at 1500 ºC for 2 h, confirming the ability to manufacture detailed dense ceramic parts.

Keywords:
Rheological behavior; Stereolithography; 3d printing; Digital light processing; Zirconia

Authorship

Italo Leite de Camargo ^**e-mail: italo.camargo@usp.br

Universidade de São Paulo – USP, Departamento de Engenharia Mecânica – EESC, Trabalhador São Carlense, 400, São Carlos, SP, Brasil.Universidade de São PauloBrasilSão Carlos, SP, BrasilUniversidade de São Paulo – USP, Departamento de Engenharia Mecânica – EESC, Trabalhador São Carlense, 400, São Carlos, SP, Brasil.

Instituto Federal de Educação, Ciência e Tecnologia de São Paulo – IFSP, Primeiro de Maio, 500, Itaquaquecetuba, SP, Brasil.Instituto Federal de EducaçãoBrasilItaquaquecetuba, SP, BrasilInstituto Federal de Educação, Ciência e Tecnologia de São Paulo – IFSP, Primeiro de Maio, 500, Itaquaquecetuba, SP, Brasil.

https://orcid.org/0000-0001-8329-6799

Rogério Erbereli

https://orcid.org/0000-0003-0753-8172

Hayden Taylor

University of California, Berkeley, Department of Mechanical Engineering, 6159 Etcheverry Hall, Berkeley, CA 94720, USAUniversity of CaliforniaUSABerkeley, CA, USAUniversity of California, Berkeley, Department of Mechanical Engineering, 6159 Etcheverry Hall, Berkeley, CA 94720, USA

https://orcid.org/0000-0001-9810-6505

Carlos Alberto Fortulan

https://orcid.org/0000-0002-2259-9910

*e-mail: italo.camargo@usp.br

SCIMAGO INSTITUTIONS RANKINGS

Figures | Tables | Formulas

Figures (9)
Tables (1)
Formulas (2)

Thumbnail

Figure 1
Comparison of the viscosity of published zirconia photosensitive slurries with their specific surface area labeled¹1 Komissarenko DA, Sokolov PS, Evstigneeva AD, Shmeleva IA, Dosovitsky AE. Rheological and curing behavior of acrylate-based suspensions for the DLP 3D printing of complex zirconia parts. Materials. 2018;11(12):2350.^,³²32 Borlaf M, Serra-Capdevila A, Colominas C, Graule T. Development of UV-curable ZrO2 slurries for additive manufacturing (LCM-DLP) technology. J Eur Ceram Soc. 2019;39(13):3797-803. http://dx.doi.org/10.1016/j.jeurceramsoc.2019.05.023.
http://dx.doi.org/10.1016/j.jeurceramsoc...

33 Li X, Zhong H, Zhang J, Duan Y, Bai H, Li J, et al. Dispersion and properties of zirconia suspensions for stereolithography. Int J Appl Ceram Technol. 2020;17(1):239-47.

34 Xing B, Cao C, Zhao W, Shen M, Wang C, Zhao Z. Dense 8 mol% yttria-stabilized zirconia electrolyte by DLP stereolithography. J Eur Ceram Soc. 2020;40(4):1418-23. http://dx.doi.org/10.1016/j.jeurceramsoc.2019.09.045.
http://dx.doi.org/10.1016/j.jeurceramsoc...

35 Li X, Zhong H, Zhang J, Duan Y, Li J, Jiang D. Fabrication of zirconia all-ceramic crown via DLP-based stereolithography. Int J Appl Ceram Technol. 2020;17(3):844-53.

36 Borlaf M, Szubra N, Serra-Capdevila A, Kubiak WW, Graule T. Fabrication of ZrO2 and ATZ materials via UV-LCM-DLP additive manufacturing technology. J Eur Ceram Soc. 2020;40(4):1574-81. http://dx.doi.org/10.1016/j.jeurceramsoc.2019.11.037.
http://dx.doi.org/10.1016/j.jeurceramsoc... ^-³⁷37 Chen F, Zhu H, Wu JM, Chen S, Cheng LJ, Shi YS, et al. Preparation and biological evaluation of ZrO2 all-ceramic teeth by DLP technology. Ceram Int. 2020;46(8):11268-74. http://dx.doi.org/10.1016/j.ceramint.2020.01.152.
http://dx.doi.org/10.1016/j.ceramint.202... at a shear rate of 30 s^-1 and volume fraction. The dotted rectangle identifies the preferred characteristics for suspensions (solid loading ≥ 40 vol% and viscosity ≤ 3 Pa.s).

Thumbnail

Figure 2
Rheological behavior of ceramic slurries with 15 vol% solid loading (a) with different dispersants with varying concentrations at a shear rate of 30 s^-1. (b) Viscosity curve with different dispersants in the concentration which provided the lowest viscosity (c) Shear stress vs shear rate with different dispersants fitted by the Herschel-Bulkley model.

Thumbnail

Figure 3
Rheological behavior of ceramic slurries with 30 vol% solid loading (a) viscosity curve with different monomers (b) Shear stress vs shear rate with different monomers fitted by the Herschel-Bulkley model.

Thumbnail

Figure 4
Influence of solid loading in 3Y-TZP ceramic slurries with 2wt% of Disperbyk-111 at a shear rate of 30 s^-1

Thumbnail

Figure 5
Rheological behavior of 40 vol% solid loading ceramic slurries. (a) Viscosity curve with different monomers; (b) Shear stress vs shear rate with different monomers fitted by the Herschel-Bulkley model.

Thumbnail

Figure 6
Sedimentation test of ceramic slurries with 15 vol% solid loading with different dispersants: Retained volume fraction as a function of the time.

Thumbnail

Figure 7
FTIR spectroscopy (a) Disperbyk-111. (b) As received and modified (with Disperbyk-111) 3Y-TZP powders

Thumbnail

Figure 8
Printed adaptation of Christ the Redeemer Statue (Rio de Janeiro – Brazil). (a) Green part. (b) Sintered part.

Thumbnail

Figure 9
Sintered printed bars with magnified view of the layers.

Thumbnail

Table 1
Monomers used in this study

Thumbnail

(1)

Thumbnail

(2)

Figure 1 Comparison of the viscosity of published zirconia photosensitive slurries with their specific surface area labeled¹1 Komissarenko DA, Sokolov PS, Evstigneeva AD, Shmeleva IA, Dosovitsky AE. Rheological and curing behavior of acrylate-based suspensions for the DLP 3D printing of complex zirconia parts. Materials. 2018;11(12):2350.^,³²32 Borlaf M, Serra-Capdevila A, Colominas C, Graule T. Development of UV-curable ZrO2 slurries for additive manufacturing (LCM-DLP) technology. J Eur Ceram Soc. 2019;39(13):3797-803. http://dx.doi.org/10.1016/j.jeurceramsoc.2019.05.023.
http://dx.doi.org/10.1016/j.jeurceramsoc...

33 Li X, Zhong H, Zhang J, Duan Y, Bai H, Li J, et al. Dispersion and properties of zirconia suspensions for stereolithography. Int J Appl Ceram Technol. 2020;17(1):239-47.

34 Xing B, Cao C, Zhao W, Shen M, Wang C, Zhao Z. Dense 8 mol% yttria-stabilized zirconia electrolyte by DLP stereolithography. J Eur Ceram Soc. 2020;40(4):1418-23. http://dx.doi.org/10.1016/j.jeurceramsoc.2019.09.045.
http://dx.doi.org/10.1016/j.jeurceramsoc...

35 Li X, Zhong H, Zhang J, Duan Y, Li J, Jiang D. Fabrication of zirconia all-ceramic crown via DLP-based stereolithography. Int J Appl Ceram Technol. 2020;17(3):844-53.

36 Borlaf M, Szubra N, Serra-Capdevila A, Kubiak WW, Graule T. Fabrication of ZrO2 and ATZ materials via UV-LCM-DLP additive manufacturing technology. J Eur Ceram Soc. 2020;40(4):1574-81. http://dx.doi.org/10.1016/j.jeurceramsoc.2019.11.037.
http://dx.doi.org/10.1016/j.jeurceramsoc... ^-³⁷37 Chen F, Zhu H, Wu JM, Chen S, Cheng LJ, Shi YS, et al. Preparation and biological evaluation of ZrO2 all-ceramic teeth by DLP technology. Ceram Int. 2020;46(8):11268-74. http://dx.doi.org/10.1016/j.ceramint.2020.01.152.
http://dx.doi.org/10.1016/j.ceramint.202... at a shear rate of 30 s^-1 and volume fraction. The dotted rectangle identifies the preferred characteristics for suspensions (solid loading ≥ 40 vol% and viscosity ≤ 3 Pa.s).

Figure 2 Rheological behavior of ceramic slurries with 15 vol% solid loading (a) with different dispersants with varying concentrations at a shear rate of 30 s^-1. (b) Viscosity curve with different dispersants in the concentration which provided the lowest viscosity (c) Shear stress vs shear rate with different dispersants fitted by the Herschel-Bulkley model.

Figure 3 Rheological behavior of ceramic slurries with 30 vol% solid loading (a) viscosity curve with different monomers (b) Shear stress vs shear rate with different monomers fitted by the Herschel-Bulkley model.

Figure 4 Influence of solid loading in 3Y-TZP ceramic slurries with 2wt% of Disperbyk-111 at a shear rate of 30 s^-1

Figure 5 Rheological behavior of 40 vol% solid loading ceramic slurries. (a) Viscosity curve with different monomers; (b) Shear stress vs shear rate with different monomers fitted by the Herschel-Bulkley model.

Figure 6 Sedimentation test of ceramic slurries with 15 vol% solid loading with different dispersants: Retained volume fraction as a function of the time.

Figure 7 FTIR spectroscopy (a) Disperbyk-111. (b) As received and modified (with Disperbyk-111) 3Y-TZP powders

Figure 8 Printed adaptation of Christ the Redeemer Statue (Rio de Janeiro – Brazil). (a) Green part. (b) Sintered part.

Figure 9 Sintered printed bars with magnified view of the layers.

Table 1 Monomers used in this study

Monomer	Density (g/cm³)	Viscosity (mPa.s)
1,6-Hexanediol diacrylate (HDDA)	1.01	8
Poly (ethylene glycol) diacrylate with average M_n 250 (PEGDA 250)	1.11	15
Poly (ethylene glycol) diacrylate with average M_n 575 (PEGDA 575)	1.12	48

(1)

τ = τ_{e} + K {\dot{γ}}^{n}

(2)

η_{r} = \frac{η}{η_{0}} = {(1 - \frac{ϕ}{ϕ_{m}})}^{- B * ϕ_{m}}

How to cite

copy

ABM, ABC, ABPol UFSCar - Dep. de Engenharia de Materiais, Rod. Washington Luiz, km 235, 13565-905 - São Carlos - SP- Brasil. Tel (55 16) 3351-9487 - São Carlos - SP - Brazil
E-mail: pessan@ufscar.br

Acompanhe os números deste periódico no seu leitor de RSS

Versão para download de PDF

PDF

Inglês

Versões e tradução automática

Versão original do texto

English

Tradução automática

Google Translator
Microsoft Translator

Como citar

RIS

BIBTEX

Outros formatos de citação e exportação:

SciELO - Scientific Electronic Library Online
Rua Dr. Diogo de Faria, 1087 – 9º andar – Vila Clementino 04037-003 São Paulo/SP - Brasil
E-mail: scielo@scielo.org

Leia a Declaração de Acesso Aberto

Métricas

3Y-TZP DLP Additive Manufacturing: Solvent-free Slurry Development and Characterization

PlumX

Mensagem

[1] *e-mail: italo.camargo@usp.br