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Preparation of Coarse and Spherical Tungsten Powders by Ammonium Paratungstate

Category: Tungsten Information
Published on 07 December 2015
Ammonium paratungstate (or APT) is a white crystalline salt of ammonium and tungsten, with the chemical formula (NH4)10(H2W12O42)·4H2O.
 
Ammonium paratungstate is produced by separating tungsten from its ore. Once the ammonium paratungstate is prepared, it is heated to its decomposition temperature, 600 °C. Left over is WO3, tungsten(VI) oxide. From there, the oxide is heated in an atmosphere of hydrogen, reducing the tungsten to elemental powder, leaving behind water vapor. From there, the tungsten powder can be fused into any number of things, from wire to bars to other shapes.
 
Coarse and spherical tungsten powders were prepared by wet hydrogen reduction. Ammonium tungstate solutions with the additives of Li, Na and K alkali metal salts were used as raw materials. The effects of the type and content of the alkali metal salts as well as reduction time on the microstructure, chemical composition, phase composition, and particle size of ammonium paratungstate (APT) and coarse tungsten powders were investigated by scanning electronic microscopy, energy dispersive spectroscopy, X-ray diffraction, and test sieves. It is shown that ideal tungsten powders with good fluidity, sphericity, integrity and even distribution can be obtained by using the ammonium tungstate solution with 3 g·L-1 NaCl, KC1 and Li2CO3 and reducing at 1000°C for 180 min in wet hydrogen atmosphere. The average particle size of the obtained tungsten powders is 67 μm, the maximum particle size is 150 μm, the biggest loose density is 13.41 g·cm-3, and the best powder flowability is 9 s for 50 g tungsten powders.
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Direct Solid State Synthesis of W–Al2O3 Nanostructured Composite Using Ammonium Paratungstate (APT) and Al Powder Mixture

Category: Tungsten Information
Published on 04 December 2015
Mechanical processing can be used to obtain metastable crystalline phases, e.g., phases that can only be reached at equilibrium using high temperatures and/or pressures, or even amorphous phases from crystalline phases that are stable at room temperature and pressure. Such transformations, also called mechanical alloying, can be produced by ball milling.
 
W–Al2O3 nanostructured composite has been produced by mechanical milling of ammonium paratungstate (APT) and Al powder mixture at room temperature. The milled products have been characterized by X-ray diffraction (XRD), and scanning electron microscopy (SEM) equipped with energy dispersive spectrometry (EDS). The XRD and EDS results confirmed that direct reduction of APT to α-W took place after 25 min milling. It was observed that α → β phase transition took place after 24 h mechanical milling. SEM micrographs showed that alumina matrix composite reinforced with W could be obtained by one step MSR (mechanically induced self-propagation reaction) process. X-ray diffraction peak broadening equation confirmed that the mean grain size of these particles was in nanometer range which gradually decreased with increasing the milling time.
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Growth and Morphology of W18O49 Crystals Produced by Microwave Decomposition of Ammonium Paratungstate

Category: Tungsten Information
Published on 04 December 2015
Growth and morphology of W18O49 crystals produced by microwave decomposition of ammonium paratungstate
 
By microwave irradiation of ammonium paratungstate (APT, (NH 4)10 H 2Wi 2042 ' 4H 20), needle crystals of W 18 049 with a wide variety of size and morphology were formed. Their sizes and morphologies varied depending on various facets of individual APT pseudomorphous particles on which whiskers were grown, and among neighbouring decomposed APT pseudomorphous particles. Based on scanning electron and transmission electron-microscopic observations, it has been concluded that individual whiskers were monocrystalline and grew by a root growth mechanism from a nucleus formed in the amorphous layer, and that a rapid leader-like whisker growth in length was followed by a subsequent slower growth in thickness. Any evidence supporting a screw dislocation mechanism or tip growth by vapour-liquid-solid have not been detected.
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Co-doped Effects on Tungsten Copper Electrode

Category: Tungsten Information
Published on 03 December 2015

Tungsten copper electrodes are usually activated sintered by porous tungsten skeleton pre-sintering or mixed powder with active elements. Generally, due to tungsten does not dissolved in the liquid phase copper, which lead to the porosity of high tungsten content of the composite material and has a bad effect on the process of densification. In order to reduce the porosity, we can take advantage of additives which dissolves tungsten.

Adding activate element to promote tungsten dissolution, and of the solid phase sintering and liquid phase diffusion densification during sintering tungsten particles dissolved in the liquid phase precipitation, round and accumulation, to obtain a high density. Its addition can remarkably improve the material properties, reduce the sintering temperature and shortening the sintering time. However, the addition of these elements will be activated in a certain extent, reduce the thermal conductivity and electrical conductivity of tungsten copper electrode. Therefore, this kind of method is suitable for the occasions, which has lower demands of thermal conductivity and electrical conductivity.

tungsten copper electrode

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Annealing Process Effect on Tungsten Copper Electrode Properties II

Category: Tungsten Information
Published on 03 December 2015

Some experiments shows that annealing process has a great influence on the electrical conductivity of tungsten copper electrode, there is a table of the electrical conductivity of W-25Cu tungsten copper electrode at different temperature in the part one.

The table shows that when the annealing temperature reaches 800 ℃, the electrical conductivity of tungsten copper electrode is the highest, after which the temperature continues to rise, the conductivity decreased. Theoretically, this is due to the elimination of internal stress and the Cu phase recrystallization.

On the one hand, when tungsten skeleton is starting cooling process after infiltrated at high temperature, it produce large internal stress because of the a great difference between the coefficient of thermal expansion of tungsten (W) and copper (Cu), which affects the electrical conductivity of tungsten copper electrodes. On the other hand, copper phase recrystallized at 400 ℃, and when the temperature rises to 800 ℃, copper atom lattice distortion reduced, the crystal defects supplemented and improved conduction mechanism of Cu is further reflected. However, with further increase of annealing temperature, changes in Cu phase grain boundaries will gradually slow, the impact on the conductivity becomes negligible.

More infomation about annealing process effect on tungsten copper electrode properties, click here:

http://news.chinatungsten.com/en/tungsten-information/80963-ti-10443

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Humidity Sensor Using A Mixture of Ammonium Paratungstate Pentahydrate and Aluminium Sulphate

Category: Tungsten Information
Published on 03 December 2015
This paper describes an attempt to develop a ceramic humidity sensor having an approximately exponential dependency of its AC conductance on relative humidity and having a short response time. Ammonium paratungstate pentahydrate [(NH4)10W12O41.5H2O] and aluminium sulphate [Al2(SO4)3.16H2O] mixed in different wt% are used to make thick films. It is found that the AC conductance of the thick film with 40 wt% of ammonium paratungstate pentahydrate shows an almost exponential relationship with relative humidity. SEM and XRD studies are also carried out on the film to look at the nature and constituents of the samples.
 
Studies on ceramics for use as humidity sensors have been a field of research for the last two decades. Porous ceramics have been investigated and used as humidity sensors for consistency and durability. In particular, ammonium paratungstate pentahydrate (APT.5H2O) has consolidated its position as a humidity sensing material  and a humidity sensor. On the other hand, recent studies on aluminium sulphate, Al2(SO4)3.16H2O also enhance the possibility of its use as a humidity sensor. Here, the humidity dependency of the AC electrical conductance of thick films of APT mixed with aluminium sulphate in different proportions is investigated. The response time of the sensor is also measured. The SEM and XRD studies on the sample are carried out in order to know the structure of the samples and to identify the constituents of the samples. The results are presented and discussed in this paper.
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Determination of Bismuth in High Purity Ammonium Paratungstate by Coprecipitation-Hydride Generation-Atomic Fluorescence Spectrometry

Category: Tungsten Information
Published on 03 December 2015
A method for the determination of bismuth in high purity ammonium paratungstate by coprecipitation-hydride generation-atomic fluorescence spectrometry has been proposed. Coprecipitation of bismuth with lanthanum hydroxide was to be separated and concentrated. It was found that the bismuth could be recovered after two times of coprecipitation. The optimum experimental parameters,and the effect of coexistent elements on the determination of bismuth were investigated. The detection limit and determination limit of Bi were 0.020ng/mL and 0.012 μg/g respectively. The recoveries were 92.8%~108.4% and the RSD was 4.6%.The method can be applied to analyzing the trace bismuth in high purity ammonium paratungstate.
 
In chemistry, coprecipitation (CPT) or co-precipitation is the carrying down by a precipitate of substances normally soluble under the conditions employed. Analogously, in medicine, coprecipitation is specifically the precipitation of an unbound "antigen along with an antigen-antibody complex".
 
Coprecipitation is an important issue in chemical analysis, where it is often undesirable, but in some cases it can be exploited. In gravimetric analysis, which consists on precipitating the analyte and measuring its mass to determine its concentration or purity, coprecipitation is a problem because undesired impurities often coprecipitate with the analyte, resulting in excess mass. This problem can often be mitigated by "digestion" (waiting for the precipitate to equilibrate and form larger, purer particles) or by redissolving the sample and precipitating it again.
 
On the other hand, in the analysis of trace elements, as is often the case in radiochemistry, coprecipitation is often the only way of separating an element. Since the trace element is too dilute (sometimes less than a part per trillion) to precipitate by conventional means, it is typically coprecipitated with a carrier, a substance that has a similar crystalline structure that can incorporate the desired element. An example is the separation of francium from other radioactive elements by coprecipitating it with caesium salts such as caesium perchlorate. Otto Hahn is credited for promoting the use of coprecipitation in radiochemistry.
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Annealing Process Effect on Tungsten Copper Electrode Properties

Category: Tungsten Information
Published on 02 December 2015

After infiltration cooling rate has a great impact on the copper layer quality, too fast cooling will be easy to produce pores and tiny cracks. Meanwhile, due to the furnace temperature unevenness, the copper layer thickness of products are not easy to be uniform, so it requires the use of a copper infiltrated after annealing treatment, which further improving the performance of a tungsten-copper electrode. Some experiments shows that annealing process has a great influence on the electrical conductivity of tungsten copper electrode, there is a table of the electrical conductivity of W-25Cu tungsten copper electrode at different temperature.

tungsten copper electrode

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Infiltration Time Effect on Tungsten Copper Electrode Properties III

Category: Tungsten Information
Published on 02 December 2015

Viewed from the electrical conductivity of tungsten copper electrode, it is increasing with the infiltration time. We can learn from the graph that infiltration time from 30 min to 80min, the conductivity of tungsten copper alloy from 32.12% IACS to 38.6% IACS. While the infiltration time continues to increase, the conductivity was reduced from 38.6% IACS to 32.58% IACS.

This is due to the conductive properties of tungsten-copper depends mainly on the copper content and connectivity, as time increases, the amount of copper was infiltrated increases, more evenly distributed organizations tungsten copper, tungsten copper electrode conductivity correspondingly improved. But if infiltration time continued to increase, after that tungsten particles begin to grow up and there may arise organization copper pool, which causes the uneven distribution, so the hardness and conductivity of tungsten copper electrode will decrease.

tungsten copper electrode

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Thermal Polycondensation of Ammonium Paratungstate

Category: Tungsten Information
Published on 02 December 2015

Connected with the examination of the thermal polycondensation of ammonium paratungstate pentahydrate the chemical and morphological properties of intermediate phases formed during the thermal decomposition of APT have been investigated. We have studied the pH and the turbidity of the aqueous solutions of the intermediate phases, the solubility of the phases, and their rehydratation capability as well as the morphology of the crystallite granules and the grain size distribution. These properties of the original APT have been related to the same properties of the products of decomposition formed between different temperature ranges. The results obtained show unambiguously that each of the above mentioned properties suddenly changes in the temperature range 225 to 250°C. This temperature range coincides with the formation temperature of a new phase called APT II. The most probable formula of APT II is (NH4)8 [H2W13O43(OH)2]·H2O.

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