Ag3O was synthesized by jet-milling magnetron-sputtered Ag–Ag2O thin films. Heating the jet-milled powders in air and N2 from 40 to 148 °C at ambient pressure produced Ag3O-rich powders. The phase composition and unit-cell parameters of the jet-milled powders were measured as a function of temperature with in situ X-ray powder diffraction experiments from −186 to 293 °C. Ag3O was also produced by ball milling and sonicating jet-milled films at ambient conditions. The phase composition, unit-cell parameters, and thermal-reaction rates indicate nonstoichiometric Ag3O was produced from the reaction of metastable, nonstoichiometric Ag2O (cuprite structure) and ccp Ag. The thermal expansion of Ag3O is anisotropic; below 25 °C, the a-axis expansion is about twice the c-axis expansion resulting in a negative slope of c/a(T). The reversal of the sign of c/a(T) near 25 °C is dramatic. The thermal reaction is arrested when the temperature is rapidly increased from ambient to 130 °C. Ag3O is metastable and decreases its unit-cell volume during kinetic decomposition to Ag when heated above ambient temperature in air and nitrogen. The relative volume expansion of Ag3O is about 80% less than Ag at room temperature and below. The suite of nonstoichiometric Ag3O produced by heating displays a linear relation between c/a and unit-cell volume at room temperature. The c/a and unit-cell volume of a hydrothermally grown Ag3O single crystal reported in a published structure determination was the Ag-rich, low-volume end member of the linear series. The c/a and unit-cell volume are sensitive indicators of the oxygen content and state of disorder.

中文翻译：

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从 Ag-Ag2O 薄膜环境压力合成非化学计量 Ag3O 的原位 XRPD 研究：相丰度、晶胞参数和 c/a 作为温度和时间的函数

银3O是通过喷射研磨磁控溅射Ag-Ag合成的2O 薄膜。在空气和 N 中加热喷射研磨的粉末2在环境压力下从 40 到 148 °C 产生 Ag3富氧粉末。测量喷射研磨粉末的相组成和晶胞参数作为温度的函数原位-186 至 293 °C 的 X 射线粉末衍射实验。银3O 也是在环境条件下通过球磨和对喷射研磨的薄膜进行超声处理来生产的。相组成、晶胞参数和热反应速率表示非化学计量的 Ag3O 是由亚稳态非化学计量 Ag 的反应产生的2O（紫铜矿结构）和 ccp Ag。Ag的热膨胀3O 是各向异性的；低于 25 °C 时，一种轴扩展大约是两倍C-轴扩展导致负斜率C/一种(吨）。符号的反转C/一种(吨) 接近 25 °C 是戏剧性的。当温度从环境温度迅速升高到 130 °C 时，热反应停止。银3当在空气和氮气中加热到环境温度以上时，O 是亚稳态的，并且在动力学分解为 Ag 的过程中会降低其晶胞体积。Ag的相对体积膨胀3在室温及更低温度下，O 比 Ag 低约 80%。非化学计量 Ag 套件3加热产生的 O 呈现线性关系C/一种和室温下的晶胞体积。这C/一种和水热生长的 Ag 的晶胞体积3在已发表的结构测定中报道的 O 单晶是线性系列的富含银的低体积末端成员。这C/一种和单细胞体积是氧含量和无序状态的敏感指标。