喷雾干燥W-Cu前驱体粉末煅烧和还原中的物相变化特征

采用溶胶-喷雾干燥-氢气还原技术制备W-Cu复合粉末;采用X射线衍射分析技术(XRD)对喷雾干燥前驱体粉末在煅烧和还原过程中的物相特征进行了分析。研究表明:喷雾干燥W-Cu前驱体粉末煅烧后相组成转变为WO3和CuWO4;煅烧后氧化物粉末在还原过程中的相演变为低温下CuO相被还原、中温下WO3相还原成一系列钨的氧化物(WO2.90和WO2)以及高温下WO2相还原成W。     

水热还原法制备车电极用W-Cu复合粉末的特性表征

为了提高车电极的导电性,探索一种水热还原法制备的W-Cu复合粉末,并利用SEM、XRD等检测手段,对复合粉末的微观形貌以及物相组成进行特性表征,重点分析了水热反应后、煅烧后和还原后复合粉末的特性。结果表明:水热还原反应后,生成的沉淀物呈现大小不等的颗粒团聚状态,粉体颗粒呈球状,粒度在2.5μm左右,主要由CuWO_4H_2O与Cu_2WO_4(OH)_2组成,表明水热反应阶段生成的产物具有明显的晶态结构;煅烧后粉末中存在大量的Cu WO4-x,成为由Cu WO4-x、CuO和WO3组成的复合氧化物;还原后的粉末有团聚现象以及细小的初始颗粒,还原的Cu颗粒对WO3的还原起到促进作用,最终形成了弥散分布、颗粒细小的WCu复合粉末。     

水热合成-共还原法制备W-20%Cu复合粉体及其组织结构

以钨酸钠和硝酸铜为原料,通过水热合成反应及550℃/1.5 h焙烧得到氧化钨铜复合粉体,氢气还原后获得W-20%Cu复合粉体,采用X射线衍射(XRD)、扫描电镜(SEM)和高分辨透射电镜(HTEM),对该复合粉体的组织与结构进行表征。结果表明:采用水热合成法制备氧化钨铜的前驱体时混合溶液应调整为碱性,最好将pH值控制在9,水热反应产物主要是由CuWO4·2H2O与Cu2WO4(OH)2组成的复合络合物;550℃温度下焙烧时水热合成产物完全分解为由WO3、CuO和CuWO4-x组成的复合氧化物,粒度在2~5μm之间,分布均匀;复合氧化物在700~900℃下氢气还原成为典型的铜包钨结构的钨铜复合粉体,呈规则球形,晶粒度在70 nm左右,钨铜分布均匀,两相一体,保留了溶液中分子级的混合状态。     

一步还原法制备超细碳化钒铬粉末

以偏钒酸铵、氧化铬、纳米炭黑为原料,利用碳热还原法制备超细碳化钒铬粉末。采用X射线衍射仪、热重-差热分析仪和扫描电子显微镜对反应过程进行分析,结果表明:1 100℃时,氧化铬和氧化钒的碳化反应完成,得到碳化钒和碳化铬的混合粉末,粉末由平均粒径为0.6μm的类球形颗粒组成;1 200℃时,得到由V3Cr2C5和Cr2VC2组成的碳化钒铬固溶粉末,粉末颗粒均匀分散,形貌呈球形或类球形,平均粒径为0.8μm。     

水热共还原法制备W包Cu纳米粉体的工艺研究及表征

以钨酸钠(Na2WO4·2H2O)和硝酸铜(Cu(NO3)2·3H2O)为原料,采用水热反应结合连续煅烧还原工艺制备W/Cu纳米复合粉体,利用X射线衍射仪(XRD)、场发射扫描电镜(FE-SEM)、高分辨透射电镜(HRTEM)、能谱分析仪(EDS)等检测手段,分别对制备过程中各步骤的产物及最终复合粉的组成、形貌及微观结构进行表征,初步分析粉体合成的反应过程及合成机制。研究结果表明:在水热过程中,钨酸钠和硝酸铜发生共沉淀反应,生成类球形的Cu WO4·2H2O和Cu2WO4(OH)2复合络合物,该络合物粉末具有良好的分散性且无硬团聚,颗粒粒度均匀,平均粒径为10~15 nm。750℃煅烧后,水热产物脱水、分解,转变为由Cu WO4-x,Cu O和WO3组成的混合氧化物粉体。经800℃氢气还原,氧化物完全转化成W-Cu复合粉末,该W-Cu复合粉末呈一种特别的W包覆Cu的近球形结构,平均粒径为10~60 nm,且Cu的存在对氧化钨的还原起到了催化作用,致使钨相提早出现。     

La_2O_3/Y_2O_3对水热法制备W-Cu粉体的影响

采用水热-共还原法制备了稀土氧化物(La_2O_3,Y_2O_3)掺杂W-Cu混合粉末。通过改变稀土的添加量及添加种类,设定不同的还原温度和还原时间,在N_2/H_2还原气氛中得到还原产物。借助SEM、TEM、XRD等手段分析了复合粉末的物相、形貌、成分和微观结构,探讨了稀土掺杂对复合粉体还原温度、还原时间以及还原产物的影响。结果表明,加入稀土La_2O_3后,复合粉末的煅烧温度降低、还原温度升高,还原时间变长,稀土适合添加量为2%;单一加入La_2O_3得到复合粉末分散性好,颗粒为均匀的圆形和多边形,且相较于单一加入Y_2O_3和加入La_2O_3+Y_2O_3复合还原粉中W,Cu混合最为均匀。     

La_2O_3对超细钨复合粉末烧结性能与钨合金显微组织的影响

采用溶胶喷雾干燥-煅烧还原方法制备超细/纳米W-La2O3复合粉末,将粉末压制成形后在1 950℃烧结,制备La2O3弥散强化钨合金,检测合金的密度与强度,并采用SEM对超细粉末形貌、合金的组织结构、断口形貌进行分析,结果表明:随La2O3加入量增加,粉末颗粒显著细化,W-0.7%La2O3复合粉末的粒径仅为0.1μm;制备的W-La2O3超细/纳米复合粉末具有很高的烧结活性,烧结后,合金最高相对密度达到99.1%;La2O3均匀弥散分布于钨晶界,抑制钨合金的晶粒长大,提高材料的强度,W-0.7%La2O3合金中钨平均晶粒尺寸仅为8.7μm,抗弯强度达到548 MPa;合金的断裂形式表现为穿晶-沿晶共有的复合断裂形式。     

Fe-Cr-W复合氧化物粉末共还原工艺研究

通过H2-CO共还原法对Fe-18Cr-9W复合氧化物粉末进行还原，控制还原工艺的参数制得纳米级Fe-18Cr-9W复合粉末。采用XRD对粉末进行物相分析，并计算晶粒尺寸；采用高倍SEM观察粉末形貌；对复合粉末的费氏粒度、比表面面积、氧含量等进行测定与分析，研究还原温度和还原时间对粉末性能的影响。结果表明：当还原温度高于650℃时制得的复合粉末由Fe和Fe-（Cr，W）两相组成；粉末颗粒呈球形或近球形：还原温度和还原时间都对Fe-18Cr-9复合粉末的性能有显著影响，当还原温度为700℃，还原时间为90min时。制备的颗粒为平均费氏粒度低于0．58μm。平均BET粒度小于80nm，晶粒粒径小于50nm，粉末氧含量小于0．14％的纳米级Fe-18Cr-9复合粉末。     

不同钨源原料制备WC-Co复合粉的形貌研究

以WC-6%Co为基本成分,计算原料醋酸钴,超纯炭黑、有机碳分别与WO2.72,WO3,APT,AMT配料量,称量后加入装有适量纯水的可倾斜式滚动球磨机,湿磨混匀形成料浆,然后充分搅拌料浆进行喷雾干燥,将喷雾干燥的前驱体粉末煅烧、过筛,称量装舟,推入1 100℃通有氢气的高温钼丝炉中制备出WC-6Co复合粉末.结果表明:以WO2.72为原料制备WC-6Co复合粉,粉末粒度在1~45μm,平均粒度为23.38μm;以WO3为原料制备粉末粒度在8~35μm,平均粒度为22.58μm;以APT为原料制备粉末粒度在1~34μm,平均粒度为12.81μm;以AMT为原料制备粉末粒度在3~45μm,平均粒度为17.83μm;粉末球形度由好到差顺序为:WO3、WO2.72、AMT、APT;松装密度由大到小顺序为:WO3、WO2.72、APT、AMT;流动性由好到差顺序为:WO2.72、WO3、APT、AMT;通过测量粉末BET,换算对应WO2.72、WO3、APT和AMT为原料时制备粉末的WC晶粒度分别为400 nm、252 nm、255 nm和26 nm.     

H2O2氧化水热晶化法制备超细钨粉

通过H2O2氧化工业级钨粉颗粒制备出纳米级WO3粉体,采用两段还原法对所得的产物进行氢还原后得到超细钨粉。用XRD、SEM、BET等对所得产物进行了一系列的表征。结果表明:工业级钨粉经氧化水热晶化处理后所得产物为单斜相WO3,平均粒径约为60 nm;将制得的WO3在氢气氛下还原,800℃下保温45 min后得到颗粒分布较窄、平均粒径约150 nm的立方相钨粉。当还原温度升高至900℃时,所得的钨粉颗粒明显长大,部分粒径长大至2~3μm,但颗粒的球形度更好。     

Chinalco Signed Framework Agreement for Strategic Cooperation with Harbin Municipal Government

正Last month,Chinalco signed framework agreement for strategic cooperation with Harbin Municipal Government in Harbin Xiong Weiping,Chairman of Chinalco,said that based on the strategic deployment to build world top-class mining company with the highest growth potential,Chinalco was now concentrating all efforts on making strategic transition and structural adjustment,strategic cooperation with the local governments where     

Jiangxi Promotes Jiangxi Copper Corporation To Become The World's Most Competitive Mining Company

<正>According to the latest info from Jiangxi Province State-owned Assets Supervision and Administration Commission,Jiangxi Copper Corporation was approved to become the first pilot enterprise for deepening reform.Contents of the pilot work is"Three Self"(self expansion,self decision-making,self     

Journal of Rare Earths Contents List of Vol.32(2014)

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Contributions to Baosteel Technical Research wanted

正Baosteel Technical Research,a quarterly journal,which is issued domestically and abroad,is run and sponsored by Baosteel Group Corporation.Baosteel Technical Research mainly reports the achievements in technological innovation,academic research,new product development and industrial equipment improvement by Baosteel.It will continue to follow up on hot topics and serve the company’s technological development and progress.Its readers include experts in     

Ministry of Industry and Information Technology: No Short Term Solution For Our Country’s Excess Nonferrous Metal Smelting Capacity

【正】According to the Ministry of Industry and Information Technology,the Ministry has released the 2013 Operation Report on China’s Industrial Communication Indu...     

Chinalco Signed Framework Agreement for Strategic Cooperation with Gansu Province

正Recently,Chinalco and Gansu Provincial People’s Government signed"Framework Agreement for Strategic Cooperation on Reform,Restructuring and Transition Development of Chinalco’s Electrolytic Aluminum Enterprises in Gansu",signifying that the strategic cooperation between Chinalco and Gansu Province had made new substantive progress.     

Unavoidable Economic Cycle:30% Of Nonferrous Metal Companies Were Involved In Restructuring

正Owing to continual downturn in real estate and bulk commodity markets,a number of traditional industries in China suffered unfavorable impact in performance.With the progressive disclosure of third quarter report,the no-pleasant-surprise performance of     

Baotou Rare Earth Became the World's Biggest High Performance Magnetic Material Base

正The High Performance Magnetic Material Phase II Project,an industry upgrading project implemented by Inner Mongolia Baotou IronSteel Rare Earth(Group)Hi-tech Co.,Ltd,recently basically finished equipment commissioning,signifying that the enterprise had developed the production capacity of15000 t/a Nd-Fe-B strip casting alloy and 5000t/a Nd-Fe-B magnet,thus becoming the world’s     

Introducing Two Central Enterprises to Integrate Rare Earth Industry,Shandong Rare Earth Group Breaks Surface

正With the signing of"Letter of intention for Propelling Integration of Shandong Rare Earth Enterprises"between Shandong Province Commission Of Economy and Informatization,China IronSteel Research Institute Group("China Steel Institute"),and China Rare MetalsRare Earth Co.,Ltd("China Rare Earth"),the"Shandong Rare Earth Group"jointly set up by the 3 units thus broke surface.On August 9,reporters of the China Economic Herald learned from Shandong Province     

Aluminium Production by Province or City in 2014

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