兰钨的相组成与工艺参数的关系

The Relationship Between the Phase of Tungsten Blue Oxides and the Processing Parameters

  • 摘要: 用氢轻度还原仲钨酸铵(APT)所得兰钨的组成随还原温度不同而变化。在275℃为非晶态铵钨青铜(ATB);在325℃为结晶态ATB;随着还原温度升高,ATB含量逐渐减少,在575℃的试样中不存在ATB。超过325℃时,出现W20O58,其含量随温度升高而增加,在525℃达到最大值,然后随温度继续升高而迅速减少。在525℃至575℃之间,还原产物的相组成发生显著变化,由ATB和W20O58组成的物相迅速转变为由WO2、β-W和α-W所组成的物相。本文给出了兰钨的相组成与APT还原温度的定量关系。与用氢还原WO3相比,在APT的轻度氢还原过程中,β-W出现的温度范围广,且含量高。
    在450℃用氢还原APT,当还原时间为5min时,产物是结晶态ATB;随着还原时间延长,将出现W20O58,并逐渐增多,而ATB的含量则逐渐减少。本文实验地研究了在450℃用氢还原APT时所得兰钨的相组成与还原时间的关系。

     

    Abstract: The phases of tungsten blue oxides produced by the light reduction of ammonium paratungstatc (APT) with hydrogen vary with the reduction temperature. The product reduced at 275℃ is noncrystalline ammonium tungsten bronze (ATB) and at 325℃ is crystalline ATB. The content of ATB in the reduced product gradually decreases with increasing the reduction temperature. There is no ATB in the product reduced at 575℃. The phase W20O58 appears above 325℃. Its content increases with the reduction temperature and reaches its maximum at 525℃, and then it decreases sharply above 525℃. The phases WO2 and β-W appear at 525℃. The phase α-W appears between 525℃and 575℃.The phases of the products reduced at 525-575℃change remarkably from ATB andW20O58 to WO2, β-W and α-W. The quantitative relationship between the phases of tungsten blue oxide and the reduction temperature of APT has been studied in this paper.
    When WO3 is lightly reduced by hydrogen, W20O58 appears at certain temperature between 425℃ and 525℃; W18O49 appears between 475℃ and 525℃; A little β-W appears at 625℃. When the reduction temperature is higher than 625℃, the content of α-W in the reduction product rapidly increases with the reduction temperature.
    When APT is lightly reduced by hydrogen, β-W can be obtained at a very wide temperature range, compared with WO3also reduced by hydrogen. The content of β-W obtained from APT is more than that obtained from WO3.
    When APT is reduced by hydrogen at 450℃ for five minutes, the product is crystalline ATB.If the reduction time is longer than five minutes, W20O58 phase will appear. The content of W20O58 increases gradually with the reduction time and at the same time the content of ATB decreases gradually. When the reduction of APT with hydrogen is carried out at 450℃, the relationship between the phases of tungsten blue oxide and the reduction time has been experimentally investigated in this article.

     

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