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

2021 ◽  
Vol 13 (2) ◽  
pp. 39-48
Author(s):  
Mohammad Abdullah ◽  
Triwikantoro Triwikantoro ◽  
Chairatul Umamah ◽  
Herman Jufri Andi
Keyword(s):  
Calcination Temperature ◽  
Magnetic Separation ◽  
Tetragonal Phase ◽  
Crystal Size ◽  
Central Kalimantan ◽  
Alkali Fusion ◽  
Zro2 Phase ◽  
Natural Zircon ◽  
Temperature Ranges ◽  
Zircon Sand

In this research ZrO2 has been synthesized from Kereng Pangi zircon sand in Central Kalimantan through alkali fusion-coprecipitation method. Firstly, zircon sand (ZrSiO4) 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. ZrO2 filtrate (ZrOCl2) precipitated with NH4OH 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 ZrO2. XRD results show that single tetragonal phase of ZrO2 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 ZrO2 with purity is at around 95.8 % at pH 4 and 96.3 % at pH 7 and pH 10.

Particle Size Analysis of the Synthesised ZrO2 from Natural Zircon Sand with Variation of pH Deposition Using Alkali Fusion-Coprecipitation Method

2019 ◽  
Vol 966 ◽  
pp. 89-94 ◽  
Author(s):  
Cahyaning Fajar Kresna Murti ◽  
Herman Aldila ◽  
Endarko ◽  
Triwikantoro
Keyword(s):  
Particle Size ◽  
Crystal Size ◽  
Precipitation Method ◽  
Size Analysis ◽  
Precipitation Process ◽  
Powder Particle Size ◽  
Alkali Fusion ◽  
Natural Zircon ◽  
Zircon Sand ◽  
Co Precipitation

Zirconia (ZrO2) is one of the refractory ceramic materials that have applications in several fields. The aim of this study was to synthesis ZrO2 from natural zircon sand collected from Kereng Pangi, Central Kalimantan with a variation of pH deposition using alkali fusion co-precipitation method. The synthesized ZrO2 began with the preparation process involved magnetic separation, milling, and leaching with HCl. Furthermore, the alkali fusion process was used KOH solution and heated in an electrical furnace at 700°C for 3 h whereas the co-precipitation process was carried out using a filtrate mixed with the NH4OH solution to reach a pH variation between 3–11 and then precipitated for 12 h. The precipitates were dried in an oven and then calcined at 800°C for 3 h. The structure of synthesized ZrO2 was characterized using XRD and the particle sizes were measured using particle size analyzer (PSA). The XRD analysis showed that the identified phase of zirconia powder is tetragonal with a crystal size in nanometer size. Result of PSA measurement revealed that the crystal size decreased in the range pH of 3 - 7, but increased in the range pH of 7 - 11. The biggest powder particle size could be achieved at 260 nm with pH 7 whereas the smallest size was at 143 nm occurred at pH 3.

Alkali fusion of zircon sand

2000 ◽  
Vol 109 (1) ◽  
pp. 49-56 ◽  
Author(s):  
K. A. El Barawy ◽  
S. Z. El Tawil ◽  
A. A. Francis
Keyword(s):  
Alkali Fusion ◽  
Zircon Sand

scholarly journals Synthesis of nanosized magnetic NiFe2O4 material by a coprecipitation method

2016 ◽  
Vol 19 (4) ◽  
pp. 137-143
Author(s):  
Tien Anh Nguyen ◽  
Dat Tien Nguyen
Keyword(s):  
Calcination Temperature ◽  
Crystal Size ◽  
Coprecipitation Method ◽  
Boiling Water ◽  
Cubic Structure ◽  
Hydrolysis Of

Nanosized NiFe2O4 spinel material has been synthesized by the coprecipitation method by hydrolysis of Ni(II) and Fe (III) cations in boiling water. The DTA/TGA, XRD, SEM, TEM, VSM results showed that NiFe2O4 crystals formed after calcinating at 700 oC for 2 h exhibited the cubic structure, with the size of 30-50 nM. Mr, Ms and Hc values were 1.06 emu/g, 14.94 emu/g and 61.57 Oe, respectively. The crystal size significantly increased with increasing calcination temperature.

Effect of Heat Treatment Conditions on Microstructure and Infrared Transmission Property of Germanate Oxyfluoride Glass-Ceramics

2010 ◽  
Vol 663-665 ◽  
pp. 1285-1288
Author(s):  
Zhuo Hao Xiao ◽  
Sheng Long Wang
Keyword(s):  
Heat Treatment ◽  
Crystal Size ◽  
Structural Characteristics ◽  
Glass Ceramics ◽  
Infrared Transmission ◽  
Oxyfluoride Glass ◽  
Treatment Conditions ◽  
Ir Transmission ◽  
Temperature Ranges ◽  
Good Transparency

Germanate oxyfluoride glass in CaF2/BaF2-AlF3-SiO2-GeO2 was prepared by melt quenching technique and subsequently converted to glass-ceramics with microstructures comprised nano-crystallites in a residual glass matrix by two-step heat treatments process. DSC, XRD, SEM and IR transmission investigations were used to determine structural characteristics and optical property of the prepared germanate oxyfluoride glass-ceramics. The influences of heat treatment conditions on crystallization behaviors and infrared transmission were discussed. The results show that crystal phase in the glass-ceramics is only Ge2Al6O13 and the crystal size is about 20nm-80nm when treated temperature ranges from 900 oC to 960oC. Good transparency is exhibited in visible light band to midinfrared band (5.0um) when treated temperature is low than 940 oC.

scholarly journals Morphology-Controllable Hydrothermal Synthesis of Zirconia with the Assistance of a Rosin-Based Surfactant

2019 ◽  
Vol 9 (19) ◽  
pp. 4145 ◽  
Author(s):  
Chen Guo ◽  
Peng Wang ◽  
Shengliang Liao ◽  
Hongyan Si ◽  
Shangxing Chen ◽  
...  
Keyword(s):  
Hydrothermal Synthesis ◽  
Aqueous Solutions ◽  
Pore Size ◽  
Surface Area ◽  
Calcination Temperature ◽  
Pore Volume ◽  
Crystal Size ◽  
Edge Angle ◽  
Large Pore Volume ◽  
Hollow Cube

With the assistance of a rosin-based surfactant, dehydroabietyltrimethyl ammonium bromine (DTAB), well-dispersed hollow cube-like zirconia particles were firstly synthesized by the hydrothermal treatment of ZrOCl2 aqueous solutions. The introduction of DTAB is crucial for improving the dispersion and regularity of the as-synthesized sample. After calcination, the crystal size of the calcined samples increased, and the edge angle of the cube-like particles became round accordingly. Finally, a hollow spherical morphology was formed for the sample calcined at 923 K. The as-synthesized sample showed big surface area of 146.78 m2/g and large pore volume of 0.23 cm3/g. With the increase of calcination temperature, the surface area and pore volume of the samples decreased significantly, and the pore size increased accordingly.

High Purity Zirconia and Silica Powders via Wet Process: Alkali Fusion of Zircon Sand

2008 ◽  
Vol 591-593 ◽  
pp. 771-776 ◽  
Author(s):  
Chieko Yamagata ◽  
João B. Andrade ◽  
Valter Ussui ◽  
Nelson Batista de Lima ◽  
José Octavio Armani Paschoal
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
High Purity ◽  
High Specific Surface Area ◽  
Reactant Ratio ◽  
X Ray ◽  
Wet Process ◽  
Alkali Fusion ◽  
Zircon Sand

Zircon sand was reacted with liquid caustic soda (50% NaOH) in open vessel at 600 oC for 2h. The effect of NaOH/ZrSiO4 reactant ratio on the yield of zirconia recovery was verified. Samples of fusion products water washed were characterized by X-ray diffraction (XRD) to identify the main compounds formed. Silica powders were obtained via acid catalyzed reaction and zirconia powders were resulted from crystallization of zirconium oxychoride. Both zirconia and silica powders were analyzed by XRF (X-ray fluorescence) and BET method. Laser Quasi Elastic Light Scattering (QLS) technique was used for agglomerate size distribution determination. High purity and fine zirconia and silica powders were obtained. The specific surface area of zirconia calcined at 550 oC reached ~ 70m2g-1. Silica powder calcined at 800 oC presented a high specific surface area ~ 500 m2g-1.

scholarly journals Evaluasi Ketidakpastian Pengukuran Multi-Unsur Dalam Mineral Zirkon Dengan Metode Analisis Aktivasi Neutron

EKSPLORIUM ◽  
2015 ◽  
Vol 36 (1) ◽  
pp. 45
Author(s):  
Sukirno Sukirno ◽  
Sri Murniasih ◽  
Rosidi Rosidi ◽  
Samin Samin
Keyword(s):  
Cross Sections ◽  
Uncertainty Estimation ◽  
Quantitative Composition ◽  
Central Kalimantan ◽  
Uncertainty Measurement ◽  
Real Concentration ◽  
Zircon Sand ◽  
Zircon Mineral ◽  
Confidence Rate

Evaluasi analisis multi-unsur yang disertai perhitungan ketidakpastian unsur pada mineral zirkon yang berasal dari Sampit, Kalimantan Tengah dan Pulau Bangka telah dilakukan dengan metode Analisis Aktivasi Neutron (AAN). Tujuan penelitian ini adalah menentukan komposisi dan nilai ketidakpastian multi-unsur dalam mineral zirkon untuk memenuhi persyaratan ISO/IEC guide 17025-2008 yang telah diterapkan pada laboratorium AAN. Analisis menggunakan spektrometri gamma dengan detektor HPGe menghasilkan 21 unsur terdeteksi yang dibagi menjadi tiga kelompok (mayor, minor, dan kelumit). Evaluasi ketidakpastian pengukuran perlu dilakukan untuk meningkatkan kualitas dan tingkat kepercayaan hasil analisis. Hasil pengujian tidak akan bermakna tanpa disertai perhitungan ketidakpastian. Oleh karena itu, dilakukan evaluasi nilai perhitungan ketidakpastian pada hasil analisis semua unsur yang terkandung dalam mineral zirkon. Hasil analisis kuantitatif tertinggi adalah zirkonium (Zr) dengan konsentrasi 38,986% dan mempunyai nilai ketidakpastian 0,33% sehingga nilai konsentrasi nyata adalah 38,986±0,33%, dalam oksida (ZrO2) mempunyai konsentrasi 52,661±0,45%. Unsur stibium (Sb) adalah unsur yang terdeteksi paling rendah dengan nilai konsentrasi dan ketidakpastian adalah 7±0,3 μg/g sedangkan dalam oksida (Sb2O3) mempunyai konsentrasi 17±0,9 μg/g. Komposisi oksida dan bahan kimia dalam mineral pasir zirkon yang lebih signifikan berasal dari Sampit dengan kandungan ZrO2+HfO2 (53-55%), F2O3 (5-6%), TiO2 (13-14%), Al2O3 (1,5-2%) dan SiO2. Unsur Si (SiO2) tidak dapat ditentukan dengan metode AAN sebab tampang lintang Si sangat kecil. The evaluation of multi-elements analysis has been carried out with calculation of element uncertainy in the zircon mineral from Sampit (Central Kalimantan) dan Bangka has been evaluated by the Neutron Activation Analysis (NAA) method. The purpose of this research is determination of composition and value of multi-elements uncertainty in the mineral of zircon to fulfil the requirements of ISO/IEC guide 17025-2008 that applied at NAA laboratory.  The result of analysis using gamma spectrometry with a HPGe detector showed of 21 detected elements, divided into three groups (major, minor, and trace). Evaluation of  uncertainty estimation should be done to increase quality and confidence rate of analysis results. The result of testing are not mean without calculation of uncertainty.  Therefore,  it was assessed the uncertainty measurement of all elements analysis in zircon mineral. The results of quantitative analysis is Zr with the highest concentration value of 38.986% and value of uncertainty is 0.331% so that value of real concentration is 38.986 ± 0.331%. In the form of oxide (ZrO2) has concentration of 52.661±0.45%. Sb element is the lowest element detected with value of concentration and uncertainty is 7±0,3 µg/g. In the form of oxide (Sb2O3) has concentration is 17±0.9 µg/g. The oxide composition and the must important of chemicals in the zircon sand mineral more significant from Sampit which quantitative composition areZrO2+HfO2 (53-55%), F2O3 (5-6%), TiO2 (13-14%), Al2O3 (1.5-2%) and SiO2.  Elements ofSi(SiO2) can not be determinedbyNAAmethodbecauseSi cross-sections is verysmall.

scholarly journals Analisis Mikrostruktur Partikel Zirkoniakalsia-silika (ZrO 2 -CaO-SiO ) Dari Pasir Zirkon Alam Indonesia Menggunakan Metode Spray Pyrolysis

2017 ◽  
Vol 6 (1) ◽  
pp. 23
Author(s):  
Elin Karlina ◽  
Nina Djustiana ◽  
I Made Joni ◽  
Renny Febrida ◽  
Camellia Panatarani ◽  
...  
Keyword(s):  
Spray Pyrolysis ◽  
Calcium Silicate ◽  
Precursor Solution ◽  
Spray Pyrolysis Method ◽  
Natural Sand ◽  
Zirconium Silicate ◽  
Silicate Structure ◽  
Natural Zircon ◽  
Zircon Sand ◽  
The One

Indonesian Natural Sand, Zircon, is an Indonesia’s natural resource that contains zirconia, silica, titania and alumina. In Dentistry, zirconia as one of the content in natural zircon sand, have the potential to be the material for filler composites. The purpose of this research was to analyze the Zirconia-Calcium-Silicate Particle (ZrO2CaO-SiO2) synthesized from Indonesia natural sand, zircon, in microstructural way. Methods: By synthesizing ZirconiaCalcium-Silicate particle (ZrO2-CaO-SiO2) from Indonesia natural zircon sand, using spray pyrolysis method. A precursor solution that is used consists of zirconil nitrate (Zr (NO3) 2), sodium silicate (Na2SiO3), and calcium hydroxide (Ca (OH) 2). Variations in the temperature of the reactor that are used were 4000C, 4500C, and 5000C with a feed rate of 6 L / min and a piezoelectric frequency of 1.7 MHz. Result showed  that the better content in zirconia-calcium-silicate is the one  that was synthesized at a temperature of 4500C, based on the results of EDS, SEM and XRD. The composition that is obtained in the zirconia-calcium-silicate particle has a ratio of 1: 14: 4 with the size of 500-1000nm, and has a tetragonal crystal zirconium silicate structure and dicalcium monoclinic silicate. From this research it can be concluded that the result that was synthesized at a temperature of 4500C is adequate to use as a filler based on the characterization result of SEM and XRD.

Study on Sodium-Calcining of Boron Concentrate

2013 ◽  
Vol 813 ◽  
pp. 403-406 ◽  
Author(s):  
Tao Jiang ◽  
Lu Yin ◽  
Lei Zhu ◽  
Xiang Xin Xue
Keyword(s):  
Chemical Analysis ◽  
Calcination Temperature ◽  
Magnetic Separation ◽  
Processing Parameters ◽  
Leaching Rate ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid Ratio ◽  
Theoretical Mass ◽  
Suitable Processing

Boron concentrate obtained from paigeite mineral by magnetic separation was treated by using sodium-calcining method. Mass of NaOH, calcination temperature and time that influence the leaching rate of B2O3 was investigated. Phase compositions and B2O3 leaching rate of sodium roasting products were analyzed by X-ray diffraction and chemical analysis. The results showed that the suitable processing parameters were addition of NaOH 10 times by theoretical mass, calcination temperature 600°C, holding time 4h. Under the above conditions, the leaching rate of B2O3 reached 92.94% when the leaching temperature, leaching time and liquid-solid ratio is 99°C, 2h and 10:1, respectively.

Factors influencing the stability of the tetragonal form of zirconia

1986 ◽  
Vol 1 (4) ◽  
pp. 583-588 ◽  
Author(s):  
Ramachandra Srinivasan ◽  
Robert De Angelis ◽  
Burton H. Davis
Keyword(s):  
Size Effect ◽  
Crystallite Size ◽  
Calcination Temperature ◽  
Tetragonal Phase ◽  
Line Broadening ◽  
X Ray ◽  
Factors Influencing ◽  
Tetragonal Crystals ◽  
Tetragonal Form ◽  
The Stability

The pH of the solution that zirconia is precipitated from defines the crystal phase formed after calcination of the material at 400°to 600°C. A metastable tetragonal form is obtained for either low (less than about 5) or high (greater than about 13) pH. The tetragonal phase formed at high pH is much more stable at the calcination temperature than the material obtained at a low pH is. For a material obtained by precipitation at a low pH, monoclinic crystallites, determined by x-ray line broadening, were obtained that were smaller than the tetragonal crystals that produced them. A crystallite size effect, based on x-ray line broadening, is not responsible for the formation or stabilization of the tetragonal phase.

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