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Preparation and Characterization of Biodegradable Zinc-

Based alloys by Laser Powder Bed Fusion Technology
Dec.06, 2021 Beijing, China

By Muhammad 导师
Waqas 贺定勇教授
• School of Materials Science and Manufacturing
 Contents
1. Introduction

2. Pure Zn and Zn10Mg preparation and characterization

3. Zn–Li-Mg alloy preparation

4. Conclusion and future plan

 1 Research Background

Ti Mg Zn Fe
Montani, M., et al., Processability of pure Zn and pure Fe by SLM for biodegradable metallic implant manufacturing. Rapid Prototyping Journal,
2017.
 Applications and Advantages of Zinc

Zinc

High impact strength

Fully Bioresorbable
Good Biocompatibility
Low toughness
Durable
Cost effective
Degradable
Mostly used in cardiovascular stents,
vascular stents, bioresorbable stents.

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 Advantages of Zinc Alloys

Zinc Alloys
Mg and Fe alloys were first
studied as biodegradable metals

Mg corrosion is too fast and Fe The degradation rate of Zn is slower

corrosion is too slow, limiting its than that of Mg, and the degradation
applications to biomedical rate of Fe is faster.
implants

Pure zinc has weak mechanical properties and can’t fulfil the needs of implants.
Adding magnesium to zinc alloy greatly enhances the alloys mechanical
properties and biocompatibility.
 Zn10Mg Alloy and its Advantages

Zn10Mg

Most commonly used as Good biocompatibility Moderate

an implants materials with tissues Young’s Modulus

Providing higher strength

compared pure zinc Low density Low Toxicity

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 Technical Route Map
Zn alloys melting
Study on additive manufacturing and

Degradation and corrosion mechanism

Atomization process of Zn alloy Prepared by SLM
for Zn alloy powder

Study on Experimental
properties of Zn alloys

Experimental arrangement electrochemical study on

of SLM equipment corrosion degradation

SLM process optimization

Microstructure and Biocompatibility of Zn alloy fabricated

Mechanical properties by SLM
 Goals and novelty of this study

1) Explore a method for densification of pure zinc and zinc alloy powders by selective laser melting.
Reveal the effect of Zn mechanism on morphology and flowability of Zn-0.6Li-0.5Mg alloy powder via
selective laser melting

2) Establish the connection between the preparation process and the developments of Zn-0.6Li-
0.5Mg zinc alloy and examine its mechanical properties using selective laser melting and Casting
techniques

3) The evolution of electrochemical process and biocompatibility of Zn-Li-Mg alloy through selective
laser melting will discuss
 Key Problems

I. Find a densification method for selective laser melting of pure zinc powder forming

II. To reveal the influence of process parameters on the densification of selective laser
melting pure zinc and zinc alloy forming

III. The development of Zn-0.6Li-0.5Mg alloy powder via atomization process and fabricate
the samples through selective laser melting

IV. To reveal the mechanism of electrochemical test and biocompatibility of Zn-Li-Mg alloy
 Response Surface Method (RSM)
Explanatory variable
To obtain an optimal
& response variable
response
Geometries

Cubes Response
surface
Sphere Methodology

Mixture of
Experiments
Maximize the
Orthogonality Centered Composite Design (CCD) Production
Uniformity Box Behnken Design (BBD)
Rotatability Orthogonal Design (OD)
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Pure Zinc Samples by Archimedes Method

 B A 
P 100  Dw
 ( B  F ) Do 
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 Pure Zinc Samples Before and After Heat Treatment
99.98%
(a) (b)

Pure Zinc samples (a) before and (b) after heat-treatment of the samples

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Relative Density of Zn10Mg Alloy by Archimedes Method

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Graphical representation of Table Data Zn10Mg samples

3D Scatterplot of LP vs SS vs H D
Density
97.7775
97.8624
97.9337
98.0282
98.0936
98.1849
98.1950
98.2429
70 98.2594
98.4211
98.6809
LP 60 98.9618
99.0818
60 0
99.3074
99.5639
50 50 0 SS
70
75 400
HD 80
The Density of Pure Zn and Zn10Mg by Image-J Software
Density= 98.3
Density= 99.5 Density= 98.4

Density= 98.8 Density= 97.3 Density= 94.8

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 Compressive Strength and Hardness Test of Zn10Mg Alloy
2. Compressive Strength Test
1. Vickers Hardness Test LP (W) 60
SS (mm/s) 600
#4
HD (mm) 0.07

#3 LP (W) 50
SS (mm/s) 700
HD (mm) 0.07

LP (W) 50 LP (W) 50 LP (W) 50

SS (mm/s) 500 SS (mm/s) 600 SS (mm/s) 700
HD (mm) 0.07 HD (mm) 0.07 HD (mm) 0.07

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Zn10Mg EDS Test

Elements Wt.%
Zn 90.29
Mg 09.71
Zn10Mg Fractography Analysis

Cracks Cleavage Planes

 Powder Morphology of Zn-0.6Li-0.5 Mg Alloy

Materials Verified By Zn Li Mg

Weight% ICP Bal. 0.6 0.5

Materials Verified By Zn Li Mg

Weight% XRF Bal. Undetectable 0.7

The size of the powder particles varied from

an average diameter of 15-55µm; however,
some particles had diameters smaller and
larger than the mentioned range and had
different spherical and elliptical shapes.
 XRD Test for Zn-Li-Mg Alloy
1. Phase identification
(b)

Fig. (a) is a phase analysis using JADE software. Fig. (b) is the XRD spectrum of Zn-0.6Li-0.5Mg
powder. Further verification of the elements quantities we perform ICP and XRF test. After verified
through three Methods we can say that results are highly reliable.
 Density of Zn-0.6Li-0.5Mg Alloy Using Archimedes Method

 B A 
P 100  Dw
 ( B  F ) Do 

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Relative Density of Zn-0.6Li-0.5Mg by Image-J
Density= 92.2
Density= 99.7 Density= 98.1
Hardness comparison of Zn, Zn10Mg and Zn-0.6Li-0.5Mg
 Tensile properties of LPBF-built and Casted specimen
(a) (b) Casting

SLM

Young Modulus E= 55.84Gpa Young Modulus E= 85.84Gpa

SLM- Process Cast- Process
Tensile properties of LPBF-specimen after heat-treatment
 Summary
(1) The pure Zn powder performed well in the SLM process. When printing the samples (pure Zn
and Zn10Mg), severe fume and spatter were observed during SLM. An especially designed gas
circulation system effectively prevents this phenomenon.

(2) This research indicates that pure Zn metal coupons have a high density above 99.98% after heat
treatment at temperature of 200°C for 3 hours.

(3) For Zn10Mg alloy, all produced samples are very similar to a maximum density between 97.7 ⁓
99.6%, because the accurately designed table via RSM. The most precise value for relative density
was attained at a laser power of 70W, the scan speed of 600mm/s, and the hatch distance of
0.07mm. In addition, the authenticity of the two methods (Archimedes & Image J) results obtained
from this experiment are accurate.

(4) Verify the composition of Zn-Li-Mg alloy powder by ICP, XRF and XRD. The results are almost
similar to this mixture Zn-0.6Li-0.5Mg. The results of the density verified by Archimedes and ImageJ
methods. The maximum density obtained 99.6% at laser power 50W, a scan speed of 700mm/s and
hatch distance of 0.07mm.
Further Research Plan of Zn-Li-Mg Alloy

1. Powder characterization 2021 .12 - 2022 .2

2. Mechanical Properties SLM/Cast 2022 .2 - 2022 .4

3. Electrochemical property 2022 .4 - 2022 .8

4. Biocompatibility / Bio-activity 2022 .8 - 2023 .2

Thank you for your attention, and your suggestion will be
helpful to accomplish this research