THE EFFECT OF PH AND CALCINATION TEMPERATURE ON THE ZrO2 PHASE FORMATION FROM NATURAL ZIRCON SAND OF KERENG PANGI

Mohammad Abdullah, T. Triwikantoro, Chairatul Umamah, H. Andi
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Abstract

In this research ZrO 2 has been synthesized from Kereng Pangi zircon sand in Central Kalimantan through alkali fusion-coprecipitation method. Firstly, zircon sand (ZrSiO 4 ) was purified to reduce impurities by magnetic separation, cleaned using an ultrasonic cleaner, soaked/leached with HCl 2 M for 12 hours and leached with HCl at 60 oC for 3 hours. Secondly, alkali fusion was done with KOH as an alkali. This product was then washed by water and dried before leached with HCl 30% at 90 oC for 30 minutes to precipitate and seperate Silica from Zircon. ZrO 2 filtrate (ZrOCl 2 ) precipitated with NH 4 OH at pH 4, pH 7, and pH 10 forms Zr(OH) 4 gel. Zr(OH) 4 gel was dried and characterized by DTA-TGA, which was then followed by calcination based on DTA TGA results at temperature ranges of 550 oC - 700 oC to produce ZrO 2 . XRD results show that single tetragonal phase of ZrO 2 is formed in all variations of pH precipitation and calcination temperature. An analysis using MAUD software show that crystal size reduces as the increase in precipitation of pH. The crystal size results are 110 nm, 66 nm and 48 nm at pH 4, pH 7 dan pH 10 at 700 oC, respectively. Moreover, XRF results show that ZrO 2  with purity is at around 95.8 % at pH 4 and 96.3 % at pH 7 and pH 10.
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研究了PH和煅烧温度对克楞攀基天然锆石砂形成ZrO2相的影响
本研究以加里曼丹中部克钦邦吉锆石砂为原料,采用碱熔共沉淀法合成了氧化锆。首先对锆英砂(zrsio4)进行磁选提纯,减少杂质,超声波清洗机清洗,HCl 2m浸泡/浸出12小时,HCl 60℃浸出3小时。其次,以KOH为碱进行碱熔。然后用水冲洗干燥,再用30%盐酸在90℃下浸出30分钟,沉淀分离出锆石。ZrO - 2滤液(ZrOCl - 2)在pH 4、pH 7和pH 10下与nh4 OH沉淀形成Zr(OH) 4凝胶。对Zr(OH) 4凝胶进行干燥和DTA-TGA表征,然后根据DTA-TGA结果在550℃~ 700℃范围内进行煅烧,制得ZrO 2。XRD结果表明,在不同的pH沉淀和煅烧温度下,zro2均形成单一的四方相。MAUD软件分析表明,随着pH沉淀的增加,晶体尺寸减小。在700℃下,pH 4、pH 7和pH 10的结晶尺寸分别为110 nm、66 nm和48 nm。XRF结果表明,在ph4和ph7、ph10条件下,氧化锆的纯度分别为95.8%和96.3%。
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