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“氢气脱氧预烧结+放电等离子烧结”两步法制备低氧高致密超细晶钼

Preparation of low-oxygen, high-density ultrafine-grained molybdenum by a two-step method: hydrogen deoxidation pre-sintering + spark plasma sintering

  • 摘要: 以超细钼粉(0.40 μm)为原料,采用“氢气脱氧预烧结+放电等离子烧结”两段式烧结法制备了高致密超细晶钼。研究发现,通过在1000 ℃的氢气中预烧结2 h,超细钼粉中氧的质量分数从0.237%降低至0.066%。预烧结后形成了大量烧结颈,晶粒尺寸没有明显增大。将预烧结样品在1200 ℃下进行放电等离子烧结(SPS),烧结压力为50 MPa,烧结时间10 min。在放电等离子烧结过程中,样品经历了致密化烧结,相对密度达到了99.2%。由于放电等离子烧结温度较低(1200 ℃),钼晶粒没有出现显著生长,平均晶粒尺寸为0.88 μm。得益于较低的氧含量、较高的相对密度、以及较小的晶粒尺寸,钼金属的维氏硬度和抗弯强度分别为HV 300和523 MPa。然而,降低放电等离子烧结温度至1100 ℃会导致样品烧结不充分,相对密度仅为91.3%,维氏硬度和抗弯强度分别降低至HV 215和343 MPa。提高放电等离子烧结温度至1300 ℃导致晶粒尺寸显著增大至6.95 μm,维氏硬度和抗弯强度分别降低至HV 197和467 MPa。

     

    Abstract: High-density ultrafine-grained molybdenum was prepared using ultrafine molybdenum powder (0.40 μm) as the raw material by a two-stage sintering method of hydrogen deoxidation pre-sintering and spark plasma sintering (SPS). The research found that by pre-sintering at 1000 ℃ in hydrogen for 2 hours, the mass fraction of oxygen in ultrafine molybdenum powder decreased from 0.237% to 0.066%. After pre-sintering, a large number of sintering necks were formed, but the grain size did not significantly increase. Then, the pre-sintered samples were sintered by SPS at 1200 ℃, with a sintering pressure of 50 MPa for 10 min. During the spark plasma sintering process, the sample underwent densification sintering and the relative density reached 99.2%. Due to the relatively low SPS sintering temperature (1200 ℃), the average grain size was 0.88 μm, which is not grow significantly. Benefiting from the low oxygen content, high relative density, and small grain size, the Vickers hardness and bending strength of the Mo metal prepared in this work were HV 300 and 523 MPa, respectively. However, reducing the SPS sintering temperature to 1100 ℃ would result in insufficient sintering of the sample, with the relative density being only 91.3%, and the Vickers hardness and bending strength dropping to HV 215 and 343 MPa respectively. Increasing the SPS sintering temperature to 1300 ℃ caused the grain size to increase significantly to 6.95 μm, and the Vickers hardness and bending strength decreased to HV 197 and 467 MPa, respectively.

     

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