Synthesis of Pure Bulk Fe3C under High Temperature and High Pressure
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摘要: Fe3C（渗碳体）是一种用途广泛、力学和磁学性能优良的材料，因而其制备方法一直受到人们的关注。通过高温高压下铁和碳的固相反应，成功制备出大块、致密、高纯的Fe3C样品，探索了原料种类、颗粒大小、合成温度、合成压力、保温时间等因素对烧结样品的影响。结果表明：当Fe粉粒径为9
$ {\text{μ}}{\rm{m}}$ ，石墨粒径为1.3$ {\text{μ}}{\rm{m}}$ ，在4 GPa、1000 ℃条件下烧结的Fe3C最为致密。Abstract: Fe3C (cementite) is a widely used material with excellent mechanical and magnetic properties; therefore the preparation method of Fe3C has been widely concerned. In this paper, dense and high-purity bulk Fe3C samples were prepared based on the solid-phase reaction of iron and carbon under high temperature and high pressure, and the influence of raw material type, particle size, sintering temperature, pressure, and holding time are investigated for the sintered samples. It shows that the densest samples were produced under the sintering pressure and temperature of 4 GPa and 1000 ̊C when the Fe and graphite particles were 9$ {\text{μ}}{\rm{m}}$ and 1.3$ {\text{μ}}{\rm{m}}$ respectively.-
Key words:
- Fe3C /
- cubic anvil press /
- high temperature and high pressure /
- sintering
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图 5 样品的背散射电子图和能谱分析图
Figure 5. Backscattered electron map and energy spectrum analysis of the sample
图 6 碳的
${{K_{\text{α}}}}$ 峰值计数率随碳质量分数的变化（标准样品Fe3C和样品4中C的质量分数分别为(6.67±0.01)%和(6.58±0.01)%）Figure 6. The
${{K_{\text{α}}}}$ peak count rate of carbon varies with carbon mass fraction (The mass fraction of C in the standard sample Fe3C and Sample 4 are (6.67±0.01) % and (6.58±0.01)%, respectively.)
图 7 Fe3C的横波声速(a)和纵波声速(b)的超声测量结果
Figure 7. (a) Shear wave and (b) compressional wave of Fe3C measured using ultrasonic equipment
表 1 Fe3C原料及烧结参数
Table 1. Fe3C raw material and sintering parameters
No. dFe/$ {\text{μ}}{\rm{m}}$ dC/$ {\text{μ}}{\rm{m}}$ T/℃ t/min p/GPa Product Density/(g·cm–3) 1 149 74 (Acticarbon) 800 10 4 Fe3C 6.869 2 149 1.3 (Graphite) 800 10 4 Fe-C 3 9 1.3 (Graphite) 800 10 4 Fe-C 4 9 1.3 (Graphite) 1000 10 4 Fe3C 7.533 5 0.03 1.3 (Graphite) 1000 10 4 Fe3C 6.931 
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