Method of microcrystalline powder of ittrium receiving

FIELD: metallurgy.

SUBSTANCE: double complex chlorides of ittrium and potassium is reduced by lithium at temperature 450-720°C in inert atmosphere and high pressure. Received reacting mass is heated at a rate 3-5°C/min up to the temperature for 60-300°C higher the reduction temperature and then it is implemented vacuum separation at a temperature 750-780°C and evacuation 1·10-4 millimetres of mercury.

EFFECT: it is provided receiving of microcrystalline metallic powder of itrrium with minimal content of oxygen and gas-producing admixtures, described by high dispersity.

5 cl, 1 tbl, 1 dwg, 1 ex

 

The invention relates to the metallurgy of rare metals, and in particular to methods of microcrystalline high-purity powders of yttrium.

The relevance of the technology of metal powders of rare metals is determined by the peculiarity of their physico-chemical properties that allow you to create materials with new and unique properties.

The technical problem solved by the invention is to obtain microcrystalline powders of yttrium, which, depending on the quality characteristics can be used in various fields of technology.

Such characteristics of metal powders of yttrium as particle size distribution, content of impurities, the value of specific surface area depend on the way they are received and, accordingly, determines the possibility of their application in a particular field of technology.

One of the promising directions in the use of microcrystalline powders of yttrium are low-temperature pyronaridine multi-purpose, used especially in space technology. Used powder of yttrium must meet specified technical requirements: the minimum oxygen content (for maximum calories while burning); the minimum content of gas-forming impurities, particularly hydrogen (to minimize clicks the education of gaseous impurities on the condition of combustion in a confined space); high dispersion (for the corresponding speed of combustion of piracetamum).

One of the most common ways to obtain microcrystalline metal powders is a mechanical method, which consists in grinding the starting material. The degree of reduction largely depends on the fragility of the source material.

Obtaining mechanical methods of powders ductile metals such as yttrium, carried out by crushing their fragile compounds that are easily decomposed.

One of the starting materials to obtain a microcrystalline powder of yttrium hydride is yttrium, having a structure similar to the structure of intermetallic compounds, and therefore has sufficient brittleness at room temperature.

The known method of microcrystalline yttrium, including hydrogenation metal yttrium hydrogen with getting brittle hydride yttrium, grinding yttrium hydride in a ball mill and dehydrogenation of the resulting powder at a temperature of ≥850°C (See Antonov A.I., Morozov R.A., "preparative chemistry of the hydrides, Directory, Kiev: Naukova Dumka, 1976, 95. with or B. müller, Damacles and Glebovic "metal Hydrides", Per. s angl., M: Atomizdat, 1973, 429 S.).

The method allows to obtain powders of yttrium varies the fragility, including fine, but the resulting powder contains a significant amount of hydrogen. Due to the high thermal stability of yttrium hydride process of dehydrogenation may be carried out at high temperatures (≥850°C)in which the hydrogen content in yttrium iron powder cannot be below 0.1%.

The known method of producing metal powder of yttrium, including heat treatment of yttrium chloride in the presence of lithium hydride or calcium hydride with obtaining the reaction mass, the cooling and hydrometallurgical processing of obtaining powder of yttrium hydride. Powder of yttrium hydride is subjected to thermohydraulic at a temperature of 900°C To produce metal powder of yttrium (see RF patent № 2013460, SW 59/00, publ. 1994).

The disadvantage of this method is the production of a material with a high content of hydrogen and oxygen and a high particle size due to their agglomeration in thermohydrolysis.

The known method of producing metal powder of yttrium from the sponge, consisting in the regenaration of yttrium and scandium potassium, lithium, magnesium, zinc, calcium, cadmium in the autoclave heated. The yttrium chloride is poured into the autoclave with metal-reducing agent taken in excess of 20%, and heated to 800-1000°C in a vacuum of 0.1-0.001 mm Hg within 2-8 hours with sublimation of the resulting chloride IU the Alla-reductant and purification of the obtained sponge yttrium (see description method similar to that described in the patent of Russian Federation № 2013460). The method adopted for the prototype.

The disadvantage of this method is to obtain a powder of yttrium increased size, not less than 20 μm.

The technical result of the claimed invention to provide a microcrystalline powders of yttrium for low temperature pyronaridine.

The technical result is achieved in that in a method of producing microcrystalline metal powders of yttrium, including latimeriidae recovery of yttrium chloride when heated, vacuum separation of the reaction mixture and grinding yttrium sponge according to the invention as chloride of yttrium use double complex yttrium chloride and potassium, restoration carried out at a temperature 450-720°C in an inert atmosphere and high pressure, vacuum separation of the resulting reaction mass is carried out at a temperature of 750-780°C and pressure up to 1·10-4mm Hg, while maintaining the temperature of the vacuum separation at 60-300°C above the temperature recovery and speed of heating of the reaction mass temperature to recover to a temperature separation of 3-5°C/min; the recovery of yttrium chloride are 10-12%excess reductant; the recovery process is carried out at a pressure of inert gas of 1.1-1.4 kg/cm2as the inert atmosphere is s used argon; before unloading yttrium sponge cooled to a temperature of 550-600°C in vacuum, then to a temperature of 200-250°C cooling are in the inert gas atmosphere and then in an air atmosphere.

The invention consists in that the microcrystalline high-purity metal powders of yttrium method and the mode of its implementation, in which the source material for grinding yttrium get through the recovery process chloride yttrium, lithium, followed by vacuum separation of the resulting reaction mass.

The stated temperature parameters of the process of recovery and vacuum separation and their interaction provide, on the one hand, the formation of the microcrystalline structure of particles recovered yttrium on the stage of recovery, and save the resulting structure and particle size of the yttrium in the formation of yttrium sponge on stage vacuum separation of the reaction mass with a favorable combination of the specific surface of the particles and the open and closed porosity.

The new method is that the recovery process is carried out at elevated pressure, and separation in a vacuum.

The declared modes, the method provides not only the fragility of yttrium sponges, but also its high quality content of impurities, and especially in Dorada.

This quality meets the requirements of materials used in low-temperature pyronaridine.

Substantiation of the parameters.

During the process latimeriidae recovery of yttrium chloride at a temperature below 450°C, the recovery process is slower and the possible passivation of the surface of the melt of lithium and incompleteness of interaction.

During the process latimeriidae recovery of yttrium chloride at temperatures above 720°C coarsens the structure of the particles recovered yttrium and, therefore, obtaining microcrystalline powder is difficult.

When conducting vacuum separation of the reaction mass at a temperature below 750°C, the pressure below 1·10-4mm Hg in the obtained powder possible presence of residual lithium content (potassium)

When conducting vacuum separation of the reaction mass at a temperature above 780°C and a vacuum higher than 1·10-4mm Hg possible escalation of grain and complicated vacuum diagram.

The process of obtaining yttrium sponge should be carried out with the difference of the temperature of the recovery process and temperature vacuum separation of not less than 60°C, the maximum temperature recovery and not more than 300°C while the minimum temperature recovery.

When the difference in temperatures less than 60°With increasing BP the two separation and possible consolidation of the powder particles.

When the difference of temperatures over 300°C increases the total recovery time and possible escalation of particles in the sponge.

The heating rate of temperature recovery to the temperature of the vacuum separation should not exceed 5°C/min, the higher the heating rate will lead to the enlargement of the particles to the closure of pores and, as a consequence, contamination of the lithium chloride/potassium.

The heating rate is less than 3°C/min slows down the process and may increase the size of the grain.

The optimal parameters of the recovery process are 10-12% of excess reductant. Less excess of reducing agent will reduce extraction of yttrium in the sponge, and more to unproductive expenditure reductant, increase the time separation and increase the fire risk in the process.

The pressure of the inert gas should be maintained in the range of 1.1-1.4 kg/cm2. More pressure complicates the instrumentation process. Less pressure leads to increased evaporation of the reducing agent and to improve the fire safety of the process.

Parameters passivation yttrium sponge before discharge associated exclusively with proforest sponges and are necessary for the safety of the unloading process.

The method is illustrated by an example.

Obtaining microcrystalline powder of yttrium includes the following stages: obtaining espagnole double chloride of yttrium and potassium with formula K 3Yl6, latimeriidae double recovery of yttrium chloride and potassium, vacuum separation of yttrium sponge grinding and classification of the obtained powder of yttrium.

To obtain the dual of yttrium chloride and potassium source components: yttrium oxide, potassium chloride and ammonium chloride, taken in a molar ratio of 1:6:13, mixed and loaded into XLERATOR preheated to 650°C. After loading the batch temperature was raised to 900 to 1000°C. the Process is finished after the complete melting of the formed chloride. The resulting chloride is poured into the mold. After complete solidification of the chloride it is removed from the mold and placed in a sealed container.

The interaction of yttrium chloride and lithium occurs by the reaction:

YCl3+3Li=Y+3LiCl.

The setup diagram for latimeriidae recovery of yttrium from anhydrous chloride shown in the drawing, where

1 - cover the working chamber; 2 - thermal insulation; 3 - water jacket; 4 - bake resistance; 5 - heater; 6 - retort; 7 - the screen; 8 - the crucible with the charge; 9 - funnel; 10 - thermop.

The installation consists of a resistance furnace, sealed working chamber and the vacuum system. For carrying out the recovery process complex yttrium chloride and potassium in the form of lumps in the amount of 2 kg and lithium taken with a 10%excess, is placed in a niobium crucible located in the working chamber in the system. Lithium pre-cleaned of protective grease. The chamber is pressurized and vacuum. To remove the protective grease downloaded the mixture is heated to a temperature of 300°C and maintained at this temperature for about 1 hour, not stopping pumping. Then the chamber is filled with argon to a pressure of 1.1 kg/cm2. The temperature in the chamber was raised to 720°C and maintained for 1 hour.

In the recovery of the formed reaction mass containing slag, which is a double chloride of lithium and potassium in equimolar ratio, yttrium sponge and the remains of lithium. Vacuum separation of the reaction mixture is carried out at a temperature of 780°C and a vacuum of 1-10-4mm Hg, with a heating rate of temperature recovery to the temperature of separation is 5°C/min, Slag and residues lithium condensed on a water-cooled cover of the retort. The duration of the vacuum separation was 1 hour.

To prevent fire sponge before unloading spend passivation. With this purpose, after the separation process sponge in the plant is cooled first in vacuum to a temperature of 550°C, and then until a temperature of 250°C in an atmosphere of technical argon. The moisture and oxygen in argon, interact with the recovered metal and Passepartout its surface. When reaching those is the temperature of 200°C. further passivation is carried out in air atmosphere.

For grinding yttrium sponge use a rotating ball mill dry grinding with stainless steel balls. The grinding time is 6 hours. The grain size of yttrium sponge is 200 nm.

The grain size of yttrium sponges were determined using raster scanning electron microscope JSM-6480LV.

The content of impurities in the powder of yttrium was determined by the method of the spark mass spectrometry mass spectrometer JMS-01-BM2.

Yttrium sponge, obtained by the claimed method, has the highest specific surface area and the smallest grain size that allows for subsequent mechanical grinding to obtain crystalline yttrium powder.

After grinding sponge ball mill and conducting screening found that the resulting powder fraction is not more than 200 nm has a yield of 40%.

Received yttrium powder was analyzed for content of some impurities. The results are presented in the table.

Table.
The content of impurities in yttrium iron powder
ppm mass.ppm mass. ppm mass.
YbaseMg<0,05Cr2
N250Al4Mn2
Li6Si6Fe30
In0,08P<0,1Co1
NDS0,4Ni9
N500Cl600Cu0,8
07500K100Nb<0,5
F 2Ca0,5Mo<0,6
Na0,1V0,3W<0,6

Thus, the claimed invention allows to obtain a microcrystalline metal powder of yttrium with the desired characteristics in accordance with the scope of its application and may be a promising method to obtain microcrystalline powders of other REE.

1. The method of microcrystalline metal powders of yttrium, including latimeriidae recovery of yttrium chloride when heated, vacuum separation of the reaction mixture and grinding yttrium sponge, characterized in that the recovery of yttrium conduct of the dual complex of yttrium chloride and potassium, restoration carried out at a temperature 450-720°C in an inert atmosphere and high pressure, vacuum separation of the resulting reaction mass is carried out at a temperature of 750-780°C and pressure of 1·10-4mm Hg, while maintaining the temperature of the vacuum separation at 60-300°C above the temperature recovery and speed of heating of the reaction mass temperature to recover to a temperature separat and 3-5°C/min

2. The method according to claim 1, characterized in that the recovery of yttrium chloride are 10-12% of excess reductant.

3. The method according to claim 1, characterized in that the recovery process is carried out at a pressure of inert gas of 1.1-1.4 kg/cm2.

4. The method according to claim 1, characterized in that an inert atmosphere using argon.

5. The method according to claim 1, characterized in that before unloading yttrium sponge cooled to a temperature of 550-600°C in vacuum, then to a temperature of 200-250°C cooling of lead in the atmosphere of inert gas, and then in air atmosphere.



 

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1 tbl, 1 ex

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10 cl, 1 dwg

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EFFECT: enhanced efficiency of method.

1 tbl, 3 ex

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9 cl, 1 tbl, 4 ex

The invention relates to the metallurgy of tungsten, in particular the production of metallic tungsten from wolframalpha compounds, in particular SelidovUgol concentrate
The invention relates to powder metallurgy and can be used to obtain powder for capacitor production

The invention relates to ferrous metallurgy and can be used to obtain alloy powders of tantalum or niobium

FIELD: non-ferrous metallurgy, possibly production of highly purified powders of tantalum and niobium with large specific surface by metal thermal reduction.

SUBSTANCE: method is realized at using as corrosion protection means layer of halide of alkali metal formed on inner surface of vessel before creating in reaction vessel atmosphere of inert gas. Charge contains valve metal compound and halide of alkali metal. It is loaded into reaction vessel and restricted by protection layer of halide of alkali metal having melting temperature higher than that of charge by 50 - 400°C. Before loading charge, valve metal compound and alkali metal halide may be mixed one with other. Mass of protection layer of alkali metal halide Ml and charge mass Mc are selected in such a way that that to satisfy relation Ml = k Mc where k - empiric coefficient equal to 0.05 - 0.5. Gas atmosphere of reaction vessel contains argon, helium or their mixture. Fluorotantalate and(or) oxyfluorotantalate or fluoroniobate and(or) oxyfluoroniobate of potassium is used as valve metal compound. Sodium, potassium or their mixture is used as alkali metal. Chloride and(or) fluoride is used as alkali metal halide. Valve metal compound and alkali metal halide may contain alloying additives of phosphorus, sulfur, nitrogen at content of each additive in range 0.005 - 0.1% and 0.005 - 0.2% of mass valve metal compound respectively. Invention lowers by 1.3 - 2 times contamination of powder with metallic impurities penetrating from vessel material. Value of specific surface of powder is increased by 1.2 - 1.8 times, its charge is increased by 10 - 30 %, leakage current are reduced by 1.2 - 1.5 times.

EFFECT: improved quality of valve metal powder, enhanced efficiency of process due to using heat separated at process of reducing valve metal for melting protection layer.

9 cl, 1 tbl, 4 ex

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