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2. METALLURGICAL AND MATERILAS ENGINEERING, DESIGN PROJECT, 2016-2017
PROPERTIES OF NANO ZINC BORATE – ADDED
POLYMER COMPOSITES
Ad SOYAD1*, Ad SOYAD1, Ad SOYAD1 and Danışman Ad SOYAD1
1Marmara University, Dept. of Metallurgical and Materials Eng., 34722, Kuyubasi, Istanbul, Turkey *
ABSTRACT
Zinc Borate is the most common commercially available boron-based fire-retardant with a chemical composition of xZnO.yB2O3.zH2O. The most widely used zinc borate types are 2ZnO.3B2O H2O and ZnO.B2O3.2H2O due to their excellent flame retardant property .1 Zinc borate has a relatively low toxicity with no demonstrated adverse public health effects following extensive long-term use as a fire-retardant in applications including carpet backing, fabric coating, wall covering, urethane foam, roofing poly vinyl chloride (PVC) tenting and awnings. Zinc borate slows down the degradation of the polymer creating a vitreous protective residual layer, which could act as a physical barrier and a glassy cage for polymer chains. Nano-sized zinc borate exhibits novel properties and application convenience that attract an increasing attention recently.
In this study, it is aimed to produce zinc borate - polymer nano-composites where zinc borate will be used as flame retardant additive. Since there are numerous zinc borates with different formulas, nano-sized zinc borate powders with the formulas of 2ZnO.3B2O H2O were successfully prepared by a wet chemical method using Zn(NO3)2.6H2O and Na2B4O7.5H2O as raw material in aqueous solution, and oleic acid as the modifying agent. The produced powders were blended with high density polyethylene (HDPE) by extruder and finally processed by iinjection machine to produce nano-composites. By using nano-sized zinc borate as flame retardant in HDPE systems, it is mainly aimed to improve the flame retardancy property of HDPE even using lower amount of additives without deteriorating the mechanical and other properties of polymeric systems. The content of nano-sized zinc borate powders of the designed composites varied between 1-5 wt.%. The microstructures and morphology of the as-obtained samples were studied by transmission electron microscopy (TEM). The flame retardancy properties of the nano-composites were investigated by LOI and compared with the micron sized particles.
Key words: Zinc borate, nano-composite, high density polyethylene, flame retardancy.
EXPERIMENTAL PROCEDURE
DISSOLVING Na2B4O7.5H2O AND Zn(NO3)2.6H2O
IN WATER
MIXING OF Na2B4O7.5H2O AND Zn(NO3)2.6H2O WITH OLEIC ACID at 70°C
PRODUCTION OF
2ZnO.3B2O H2O
COMPOUNDING OF wt% 2ZnO.3B2O H2O IN HDPE BY TWIN SCREW EXTRUDER
INJECTION MOULDING OF PRODUCED COMPOUNDS
PRODUCTION OF ZINC BORATE – POLYMER NANO COMPOSITE SAMPLES
XRD RESULT
COMPOSITION
MICROSTRUCTURE IMAGE
Composition
HDPE
(wt.%)
Nanosized ZB
Micronsized ZB
NPE-1 99 1 -
NPE-3 97 3
NPE-5 95 5
CPE-1
CPE-3
CPE-5
TEM images of synthesized 2ZnO.3B2O H2O powders a) c) b)
XRD of zinc borate (2ZnO.3B2O3.3.5H2O) a) nano powder synthesized in this study and b) powder produced by Tian.2
TGA RESULT
LOI TEST RESULT d) f) e) g) ı) h)
DTA-TG curve of the zinc borate powders indicated that they had a weight loss of around 14 wt% which is in close proximity with theoretical weight loss value of 2ZnO.3B2O3.3.5H2O (14.5 wt%).
The increase in LOI is possibly due to two reasons; 1) crystal water content of zinc borate which is released during firing, 2) B2O3 content of zinc borate that forms a strong protective layer against oxygen.
SEM images of zinc borate-HDPE composites containing nanosized zinc borate with 1wt% (a, b), 3 wt% (d, e) and 5 wt% (g, h), micronsized zinc borate with 1wt% (c), 3wt% (f) and 5 wt% (ı).
MECHANICAL PROPERTIES
CONCLUSION
Nano-sized zinc borate powders with the formula of 2ZnO.3B2O H2O were successfully produced by a wet chemical method using oleic acid as surfactant. XRD, FT-IR and DTA-TG results indicated that the powder had the zinc borate formula of 2ZnO.3B2O H2O. TEM and particle size measurements gave a particle size below 70nm. LOI results demonstrated that zinc borate addition into HDPE matrix improved the flame retardancy of HDPE. Furthermore, zinc borate addition into HDPE matrix improved the flame retardancy of virgin HDPE from 19.6% to 22.2% with addition of 5% nano-sized zinc borate. Although zinc borate addition into HDPE decreased the mechanical properties the results nano and micron sized zinc borate addition gave identical results.
References
C. Ting, D. Jian-Cheng, W. Long-Shuo and F. Gang, Journal of Materials Processing Technology 209 (2009) 4076–4079.
Tian Y, Guo Y, Jiang M, Sheng Y, Hari B, Zhang G, Jiang Y, Zhou B, Zhu Y, Wang Z. Synthesis of hydrophobic zinc borate nanodiscs for lubrication, Materials Letters 2006;60:
The effects of nano-sized zinc borate addition on mechanical properties of HDPE composites were compared with micron-sized zinc borate-HDPE and virgin HDPE. These results indicated that the addition of micron-sized zinc borate on mechanical properties led to higher negative effect. Although elongation at fracture of zinc borate - HDPE composites was higher than virgin HDPE, no substantial difference was observed in elongation at fracture of micron and nano-sized zinc borate added HDPE composites.
Acknowledgements
I would like to give my great thanks to Arçelik A.Ş. Research and Development Centre and Marmara University Research Fund (Grant No: FEN-B ) for financial support of this investigation.
METALLURGICAL AND MATERILAS ENGINEERING, DESIGN PROJECT,

3. PROPERTIES OF NANO ZINC BORATE – ADDED
POLYMER COMPOSITES
Ad SOYAD1*, Ad SOYAD1, Ad SOYAD1 and Danışman Ad SOYAD1
1Marmara University, Dept. of Metallurgical and Materials Eng., 34722, Kuyubasi, Istanbul, Turkey *
Abstract
Zinc borate is a boron containing chemical material that is used in polymeric materials, dyes, cables, fabrics, carpets, internal parts of automobiles and planes, textile and paper industry to increase the flame retardancy. Commercially, the most widely used zinc borate has a formula of 2ZnO.3B2O3.3,5H2O and particle size about 10-20m. Recent studies have showed that nano sized flame retardants have more superior flame retardancy and other properties (mechanical properties, surface quality etc.) than micron sized flame retardants.
In this study, effect of cationic (CTAB), anionic (oleic acid) and non ionic (Triton 114) surfactants on the size and shape of zinc borate powders was investigated. Nano sized zinc borate powders (2ZnO.3B2O H2O) that have almost homogenous particle size distribution and rod-shaped structure were synthesized
FT-IR Results: The FTIR spectrum of CBA-0 powder (without surfactant), which was produced at 45°C, under 300 rpm mixing speed for 15 hours, exhibits O—H bonds at about 3231 cm-1. The peak at 1634 cm-1 wavelenght points the formation of H—O—H crystal water. B(3)—O bonds can be seen at, 1340 cm-1 and 676 cm-1 where as B(4)—O bonds were seen at cm-1. FT-IR results showed that zinc borate was successfully synthesized..
Experimental
Solution I:
0.05 mole of Zn(NO3)2.6H2O ml distilled water
Solution II:
0.05 mole of Na2B4O7.5H2O + 60 ml distilled water
Mixing
Washing the precipitate 3 times
Drying the precipitate at 70°C
Adding %25 concentrated ammonia solution
Precipitating
Surfactant
XRD Results: CBA 0 powder was examined with XRD and it gave an amorphous structure. Thus, the powder was annealed at 600°C for 4h and some crystalline phases were observed
TG-DTA Results: TG-DTA analysis of CBA 0 powder indicated that the powder had 14% weight loss between °C. This result exhibits that a zinc borate powder with a formula of 2ZnO.3B2O3.3-3,5H2O was produced. The theoretical weight loss of zinc borates with the formulas of 2ZnO.3B2O3.3H2O and 2ZnO.3B2O3.3,5H2O varies as 12.7% and 14.5%, respectively. The powder also resisted until 550°C-600°C.
TEM Results
The flow diagram for the wet chemical precipitation with ammonia in a batch reactor.
Conclusion
When two solutions were mixed, a white sediment was formed instantaneously. Then 25 ml of ammonia solution was added to the mixture to adjust the solution pH to 11. At this pH, the sediment was dissolved and a clear solution occured. The clear solution was mixed in a batch type glass reactor with heating jacket for 16 hours at 45°C. Ammonia was slowly evaporated and when the pH of the reaction became 10 as a result of the evaporation, zinc borate powder was precipitated as a fine powder. The resultant powder was washed with distilled water three times to get a pure zinc borate powder. Then pure zinc borate precipitate was dryed at 70°C. A B C D
Powder
Length (nm)
Width (nm)
A: without surfactant
>1000
<50
B: with CTAB
50-200
5-10
C: with Triton-114
15-40
D: with oleic acid
<500 nm B C D
Acknowledgement: We would like to give our great thanks to National Boron Research Institute (BOREN) (Project No: 2008-Ç0154) for financial support.
METALLURGICAL AND MATERILAS ENGINEERING, DESIGN PROJECT,