發(fā)布時(shí)間：2018-10-18 18:13

【摘要】：目前我國(guó)靶材用釕粉依賴進(jìn)口,成本高,含釕廢料直接制備靶材用高純釕粉具有十分重要的現(xiàn)實(shí)意義。論文針對(duì)含釕廢料的特點(diǎn),提出了采用堿熔-水浸-氧化蒸餾-離子交換除雜-沉淀-煅燒還原工藝直接制備濺射靶材用高純釕粉的研究。本論文取得結(jié)論如下:(1)釕廢料堿熔-水浸研究表明,在Na_2O_2+NaOH為熔劑、堿熔溫度750°C、Na_2O_2、NaOH及釕廢料質(zhì)量比為4:3:1、堿熔時(shí)間3h、水浸溫度95℃、水浸時(shí)間4h的條件下,釕的浸出率達(dá)到97%,獲得含釕溶液。(2)含釕溶液氧化蒸餾研究表明,采用硫酸為介質(zhì)體系,以氯酸鈉為氧化劑進(jìn)行氧化蒸餾,釕被氧化為四氧化釕揮發(fā),并用鹽酸吸收液吸收,達(dá)到初步除雜的目的,獲得氯釕酸溶液。在蒸餾溫度95℃、蒸餾負(fù)壓0.08MPa的條件下,釕的直收率達(dá)到94.4%。(3)離子交換除雜研究表明,實(shí)驗(yàn)中選擇D001與001×7為交換樹(shù)脂,溶液酸度為0.5mol/L(以H~+濃度計(jì)),溶液流速為2m L/min,交換級(jí)數(shù)為11級(jí),凈化后氯釕酸溶液中雜質(zhì)含量均低于0.0005g/L。(4)氯化銨沉淀研究表明,加入氧化劑將釕全部轉(zhuǎn)化為氯釕(IV)酸銨,達(dá)到進(jìn)一步除雜的目的;同時(shí)通過(guò)嚴(yán)格控制沉淀?xiàng)l件,制備出顆粒均勻、尺寸合適及分散性良好的顆粒。最佳工藝條件為:釕酸鹽的濃度為30g/L,沉淀過(guò)程中持續(xù)滴加氧化劑,氯化銨的加入方式為飽和溶液,溫度為90℃,反應(yīng)過(guò)程中持續(xù)攪拌。(5)煅燒-還原、混酸煮洗的研究表明,煅燒過(guò)程通入氮?dú)忪褵?氫氣還原的方式可將氯釕酸銨顆粒還原為形貌規(guī)整、尺寸均一的釕粉;用酸煮的方式進(jìn)一步深度除雜,釕粉純度可達(dá)99.995%。最佳工藝條件為:煅燒溫度500℃、煅燒時(shí)間2小時(shí)、還原溫度700℃、還原時(shí)間2小時(shí)。通過(guò)研究,確立了含釕廢料直接制備高純釕粉的工藝流程和參數(shù),該工藝原料適應(yīng)性強(qiáng),釕的回收率較高,制備出的釕粉粒度均一、形貌規(guī)整、純度較高。
[Abstract]:At present, ruthenium powder used for target in our country depends on import and its cost is high. It is very important to produce high purity ruthenium powder with ruthenium waste material. According to the characteristics of ruthenium waste material, the preparation of high purity ruthenium powder for sputtering target by alkali melting, water immersion, oxidation distillation, ion exchange removal, precipitation and calcination reduction process was studied in this paper. The conclusions obtained in this paper are as follows: (1) the results of alkaline melting and water leaching of ruthenium waste show that under the conditions of Na_2O_2 NaOH as flux, alkali melting temperature 750 擄C ~ (2 +) Na _ 2O _ 2 NaOH and the mass ratio of ruthenium waste 4: 3: 1, alkali melting time 3 h, leaching temperature 95 鈩，

本文編號(hào)：2279963