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Acta Metall Sin  2014, Vol. 50 Issue (6): 727-736    DOI: 10.3724/SP.J.1037.2013.00712
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DEVELOPMENT OF MASTER SINTERING CURVE FOR SPARK PLASMA SINTERING OF 93W-5.6Ni-1.4Fe HEAVY ALLOY
HU Ke, LI Xiaoqiang(), QU Shengguan, YANG Chao, LI Yuanyuan
National Engineering Research Center of Near-Net-Shape Forming for Metallic Materials, South China University of Technology, Guangzhou 510640
Cite this article: 

HU Ke, LI Xiaoqiang, QU Shengguan, YANG Chao, LI Yuanyuan. DEVELOPMENT OF MASTER SINTERING CURVE FOR SPARK PLASMA SINTERING OF 93W-5.6Ni-1.4Fe HEAVY ALLOY. Acta Metall Sin, 2014, 50(6): 727-736.

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Abstract  

Tungsten heavy alloys are used for a number of applications, including radiation shields, counter weights, electrical contacts, vibration dampeners and kinetic energy penetrators. The most common compositions consist of W along with some combination of Ni, Fe, or Cu. The alloys are usually fabricated by the conventional powder metallurgy technique, in which the elemental blended powders are first compacted and then followed by a high temperature sintering. An important processing goal for this alloy is to obtain a high density with fine grain size. It is therefore desirable to predict its densification behavior and final density. Recently, the master sintering curve (MSC) theory provides a better understanding of whole sintering process. In previous work, the densification and grain growth mechanisms during spark plasma sintering (SPS) of 93W-5.6Ni-1.4Fe heavy alloy were investigated. In this investigation, the master sintering curve approach was first extended theoretically to spark plasma sintering of 93W-5.6Ni-1.4Fe heavy alloy. Two master sintering curves of 93W-5.6Ni-1.4Fe heavy alloy in different heating rate stages (with heating rate of 100 ℃/min as division point) during SPS process were developed. Both of the master sintering curves can effectively predict the densification behavior of 93W-5.6Ni-1.4Fe heavy alloy during SPS process, as well as the shrinkage and final density. The calculated densification function c quantitatively shows that the densification process increases with temperature when heating rate is higher than 100 ℃/min. In addition, the apparent densification activation energies calculated by MSC are roughly identical to those obtained by Arrhenius method.

Key words:  W-Ni-Fe heavy alloy      SPS      master sintering curve      heating rate      apparent densification activation energy     
Received:  07 November 2013     
ZTFLH:  TF12  
Fund: Supported by Support Program of Ministry of Education of China (No.62501036011), Fundamental Research Fund for the Central Universities (No.2012ZG0006), Program for New Century Excellent Talents in University (No.NCET-10-0364) and Open Foundation of National Engineering Research Center of Near-Net-Shape Forming for Metallic Materials (No.2013006)

URL: 

https://www.ams.org.cn/EN/10.3724/SP.J.1037.2013.00712     OR     https://www.ams.org.cn/EN/Y2014/V50/I6/727

Fig.1  SEM micrograph of the blended powders
Element
Purity
%
Particle size μm Mass fraction of main impurity / %
C O P N
W 99.9 2.4~2.6 0.002 0.07 0.0008 -
Ni 99.5 2.2~2.5 ≤0.25 ≤0.11 0.0003 -
Fe 99.5 3.0~5.0 ≤0.10 ≤0.30 - ≤0.10
Table 1  Characteristics of the raw powders
Fig.2  ρ-Θ curves of 93W-5.6Ni-1.4Fe heavy alloys when heating rates are lower than 100 ℃/min with apparent densification activation energy Q of 200 kJ/mol (a), 300 kJ/mol (b), 400 kJ/mol (c), 500 kJ/mol (d), 600 kJ/mol (e) and 800 kJ/mol (f) ( ρ—relative density, Θ—work of sintering)
Fig.3  Plot of mean residual square versus apparent densification activation energy when heating rates are lower than 100 ℃/min
Fig.4  S-shaped master sintering curve of 93W-5.6Ni-1.4Fe heavy alloys when heating rates are lower than 100 ℃/min (Q=438 kJ/mol)
Fig.5  ρ-Q curves of 93W-5.6Ni-1.4Fe alloy when heating rates are higher than 100 ℃/min with apparent densification activation energy Q of 100 kJ/mol (a), 200 kJ/mol (b), 300 kJ/mol (c), 400 kJ/mol (d), 500 kJ/mol (e) and 600 kJ/mol (f)
Fig.6  Plots of mean residual square versus apparent densification activation energy during two different sintering stages of 93W-5.6Ni-1.4Fe heavy alloys when heating rates are higher than 100 ℃/min
Fig.7  Plot of mean residual square versus apparent densification activation energy during the whole sintering process of 93W-5.6Ni-1.4Fe heavy alloys, when heating rates are higher than 100 ℃/min
Fig.8  S-shaped master sintering curve of 93W-5.6Ni-1.4Fe heavy alloys during the whole sintering process when heating rates are higher than 100 ℃/min (Q=234 kJ/mol)
Fig.9  Validation of master sintering curve for 93W-5.6Ni-1.4Fe heavy alloy during spark plasma sintering (SPS) (Solid symbols represent the 93W-5.6Ni-1.4Fe powders are isothermally sintered at 960~1320 ℃ with a heating rate (HR) of 90 ℃/min; hollow symbols represent the 93W-5.6Ni-1.4Fe powders are nonisothermally sintered at 960~1360 ℃ with heating rates lower than 100 ℃/min; point-within hollow symbols represent the 93W-5.6Ni-1.4Fe powders are nonisothermally sintered at 960~1360 ℃ with heating rates higher than 100 ℃/min)
Fig.10  Effect of heating rate on densification function c during SPS of 93W-5.6Ni-1.4Fe heavy alloy (Solid symbols represent the 93W-5.6Ni-1.4Fe powders are isothermally sintered at 960~1320 ℃ with heating rate of 90 ℃/min; hollow symbols represent the 93W-5.6Ni-1.4Fe powders are nonisothermally sintered at 960~1360 ℃ with heating rates lower than 100 ℃/min; point-within hollow symbols represent the 93W-5.6Ni-1.4Fe powders are nonisothermally sintered at 960~1360 ℃with heating rates higher than 100 ℃/min; Ψ—densification ratio, Θ ref—work of sintering at ρ= (ρ0+1)/2, ρ0 —initial green density)
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