WO2012169262A1 - Procédé de production d'une poudre granulée de molybdène et poudre granulée de molybdène - Google Patents

Procédé de production d'une poudre granulée de molybdène et poudre granulée de molybdène Download PDF

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Publication number
WO2012169262A1
WO2012169262A1 PCT/JP2012/057399 JP2012057399W WO2012169262A1 WO 2012169262 A1 WO2012169262 A1 WO 2012169262A1 JP 2012057399 W JP2012057399 W JP 2012057399W WO 2012169262 A1 WO2012169262 A1 WO 2012169262A1
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Prior art keywords
molybdenum
powder
granulated powder
producing
water
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English (en)
Japanese (ja)
Inventor
山口　悟
勉 森岡
斉 青山
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Toshiba Corp
Niterra Materials Co Ltd
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Toshiba Corp
Toshiba Materials Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/148—Agglomerating

Definitions

  • the present invention relates to a method for producing molybdenum granulated powder and molybdenum granulated powder.
  • Molybdenum (Mo) is used in various fields as a heat resistant material because it has a high melting point of 2620 ° C.
  • it is applied to thermal spray materials, sintering furnace plate materials, electrode parts, magnetron stems, sputtering targets, and the like.
  • the material for thermal spraying as a raw material in the state of Mo powder or Mo rod.
  • the plate material may be manufactured by sintering, or may be manufactured by combining rolling and forging.
  • electrode parts and the like may be manufactured by processing a plate material, drawing a wire by wire drawing, or manufacturing by a sintering method.
  • Mo powder or molten Mo is used as the initial raw material.
  • Mo molten metal is used by a method in which raw materials are melted and cast into a desired shape.
  • the method using the molten Mo is a method in which the molten metal is poured into a mold, and is a relatively simple method that can be processed into a large shape.
  • Patent Document 1 discloses a sintered electrode for a cold cathode tube having a U-shaped cross section (cup shape).
  • Patent Document 1 a cup-shaped electrode having a diameter of about 1 to 2 mm is manufactured using a sintering method.
  • molding process, a degreasing process, a sintering process, etc. are implemented with respect to Mo powder.
  • the sintering method has been progressed mainly by improving the degreasing process and the sintering process.
  • paragraph [0027] of Patent Document 1 it is disclosed that the degreasing step is performed in a wet hydrogen atmosphere while the sintering step is performed in a hydrogen atmosphere. As a result, the sinterability is improved and the production yield is improved.
  • Patent Document 2 of International Publication WO2011 / 004887A1 discloses a method for producing high-purity molybdenum powder having an average particle size of 0.5 to 100 ⁇ m.
  • Patent Document 2 discloses a molybdenum powder in which the proportion of primary particles is 50% or more.
  • improvements have been made on the Mo raw material powder, the degreasing process, and the sintering process.
  • the production yield did not necessarily reach 100%.
  • Such a phenomenon also occurred in the same way for a Mo sintered body using Mo powder to which a dopant such as potassium was added.
  • the present inventors have investigated the reason why the yield of a product using Mo powder added with a dopant as an initial raw material is not improved. As a result, it was found that the variation in the size, density, fluidity, etc. of the Mo granulated powder caused a variation in the filling density and supply amount in the molding process, which caused the product yield to decrease. In addition, when Mo granulated powder is used as the thermal spray powder, there is a problem that the supply amount to the thermal spray flame varies and the characteristics as the thermal spray film are not stable. As a result of pursuing this cause, it was found that there was a cause that the management according to the average particle size of the intended granulated powder was not performed in the granulation step. The present invention has been made to solve such problems, and provides a method for producing molybdenum granulated powder capable of stabilizing the quality of Mo products (powder or sintered body) and improving the yield. For the purpose.
  • a method for producing molybdenum granulated powder includes a step of injecting water into a container and heating the water to 50 to 80 ° C., a step of adding a binder to the heated water, A step of preparing a molybdenum-containing aqueous solution by adding a molybdenum powder having an average particle diameter of 1 to 10 ⁇ m to which at least one of a potassium component, an aluminum component and a silicon component is added while stirring, and a spray for dispersing the molybdenum-containing aqueous solution.
  • the molybdenum-containing aqueous solution is applied to the spray dryer in which A / B is in the range of 50 to 700.
  • a step of preparing a molybdenum granulated powder by dispersing and drying the molybdenum-containing aqueous solution is preferable to further carry out a sieving step of passing a sieve having a mesh size 2 to 3 times the average particle size B to the granulated powder after completion of the step by the spray dryer.
  • the average particle diameter B of the molybdenum granulated powder is preferably 20 to 150 ⁇ m.
  • the rotational speed A of the rotating plate of the spray dryer is preferably 5000 to 16000 rpm.
  • the potassium component is preferably added in the range of 100 to 1000 ppm by mass in terms of a potassium element simple substance.
  • the aluminum component is preferably added in the range of 100 to 1000 ppm by mass in terms of a single aluminum element.
  • the silicon component is preferably added in the range of 100 to 1000 ppm by mass in terms of silicon element.
  • the binder is preferably at least one of polyvinyl alcohol powder, polyethylene glycol powder and carbomethyl methylcellulose powder.
  • the volume of the binder is preferably 3 to 20 parts by volume.
  • the apparent density of the resulting molybdenum granulated powder is preferably 1.3 to 3.0 g / cc.
  • the molybdenum-containing aqueous solution preferably has a pure water amount of 0.2 to 1 liter when the amount of molybdenum powder is 100 parts by mass.
  • the spray dryer preferably dries the molybdenum granulated powder while supplying hot air of 150 to 300 ° C. Moreover, it is preferable that the spray dryer performs drying of the molybdenum granulated powder in a reduced-pressure atmosphere of atmospheric pressure or lower. Moreover, it is preferable that the fluidity of the obtained granulated powder is 50 sec / 50 g or less.
  • the molybdenum granulated powder of the present invention is characterized in that it contains at least one of a potassium component, an aluminum component, and a silicon component and has an apparent density of 1.3 to 3.0 g / cc.
  • the average particle diameter of the molybdenum granulated powder is preferably 20 to 150 ⁇ m. Further, when the total amount of molybdenum powder is 100 parts by volume, the volume of the binder is preferably 3 to 20 parts by volume. Further, the fluidity of the molybdenum granulated powder is preferably 50 sec / 50 g or less.
  • the method for producing molybdenum granulated powder according to the present invention in the granulation step, while adding water to a predetermined temperature and stirring, supplying the dopant-added molybdenum powder and binder, Since the average particle diameter and the rotational speed of the spray dryer are controlled within a predetermined range, molybdenum granulated powder having excellent average particle diameter, apparent density and fluidity can be produced.
  • a method for producing molybdenum granulated powder includes a step of injecting water into a container and heating the water to 50 to 80 ° C., a step of adding a binder to the heated water, A step of preparing a molybdenum-containing aqueous solution by adding molybdenum powder having an average particle diameter of 1 to 10 ⁇ m to which at least one of a potassium component, an aluminum component, and a silicon component is added while stirring, and a spray for dispersing the molybdenum-containing aqueous solution.
  • the molybdenum-containing aqueous solution is applied to the spray dryer in which A / B is in the range of 50 to 700. And a step of dispersing and drying the molybdenum-containing aqueous solution and preparing a molybdenum granulated powder. .
  • FIG. 1 shows an example of a process for preparing a molybdenum-containing aqueous solution.
  • reference numeral 1 is a container (a container for preparing a molybdenum-containing aqueous solution)
  • 2 is water
  • 3 is molybdenum powder (dope-containing molybdenum powder)
  • 4 is a binder
  • 5 is necessary.
  • 6 is a molybdenum-containing aqueous solution.
  • water is poured into the container. As this water, tap water, pure water, ultrapure water, or the like is used. Pure water and ultrapure water are water that contains almost no impurities.
  • pure water has a specific resistance of 10 4 ⁇ ⁇ cm (25 ° C.) or higher
  • ultrapure water has a specific resistance of 18 ⁇ 10 6 ⁇ ⁇ cm (25 ° C.) or higher.
  • Examples of pure water and ultrapure water include distilled water, ion exchange water, and RO (Reverse Osmosis) water.
  • pure water or ultrapure water it is preferable to use pure water or ultrapure water.
  • pure water since the preparation of ultrapure water is complicated and causes cost increase, it is preferable to use pure water. Further, when it is not necessary to control the mixing of impurities, the cost merit is increased by using tap water.
  • the heating temperature of water is preferably 50 to 80 ° C., more preferably 60 to 70 ° C.
  • the material of the binder is not particularly limited, but is preferably at least one selected from polyvinyl alcohol (PVA) powder, polyethylene glycol (PEG) powder, and carbomethyl methylcellulose (CMC) powder.
  • PVA polyvinyl alcohol
  • PEG polyethylene glycol
  • CMC carbomethyl methylcellulose
  • Polyvinyl alcohol, polyethylene glycol, and carbomethyl methylcellulose are soluble in water because they are water-soluble. Also, for example, it is preferable because it does not remain as an impurity in the sintered body because it burns away in the sintering step.
  • the average particle size of the molybdenum powder is the average particle size of the primary particle size.
  • the value obtained by the FSSS method Fischer method is defined as the average particle size. If the average particle diameter of the molybdenum powder is less than 1 ⁇ m, the Mo powder is too small to be manufactured, which causes an increase in cost. On the other hand, if the average particle size exceeds 10 ⁇ m, the primary particle size is too large and it becomes difficult to stabilize the characteristics of the granulated powder.
  • the average particle diameter of the molybdenum powder is preferably 1 to 10 ⁇ m, more preferably 2 to 5 ⁇ m.
  • the molybdenum powder tends to aggregate more than necessary. Therefore, it is preferable to add a small amount, for example, 0.5 to 2 kg.
  • the molybdenum powder after confirming that the entire amount of the binder is dissolved in heated water. If the binder is added in a powder state, it can be visually discriminated whether or not it has been dissolved.
  • polyvinyl alcohol powder when used as the binder, when the polyvinyl alcohol powder is completely dissolved in water, the water before adding the molybdenum powder becomes translucent.
  • the molybdenum powder after the binder is added. The same is true for polyethylene glycol and carbomethyl methylcellulose. As shown in FIG.
  • the volume of the binder is reduced. It is preferably 3 to 20 parts by volume.
  • the binder serves as an adhesive that bonds the molybdenum powders together when forming the molybdenum granulated powder. Therefore, when the total amount of molybdenum powder is 100 parts by volume, if the amount of binder added is less than 3 parts by volume, the amount of binder is too small and uniform granulated powder may not be obtained.
  • the addition amount of a binder exceeds 20 volume parts and becomes excessive, a binder will enter too much into the clearance gap between molybdenum powders, and it will become a granulated powder with a large dispersion
  • the molybdenum-containing aqueous solution preferably has a water content of 0.2 to 1 liter when the amount of molybdenum powder is 100 parts by mass.
  • the spray dryer is charged with an aqueous solution containing molybdenum.
  • the amount of water is less than 0.2 liter with respect to 100 parts by mass of the molybdenum powder, the amount of water is too small and the viscosity of the molybdenum-containing aqueous solution increases, and it is difficult to stably supply it to the spray dryer.
  • the amount of water exceeds 1 liter, the amount of water is too large and it is difficult to stably supply water.
  • the supply of the molybdenum-containing aqueous solution to the spray dryer can be automated by mechanization.
  • water 5 may be added as necessary. Since the water is heated to 50 to 80 ° C., there is a possibility that the amount of water may change greatly due to the evaporation of the water when the binder and the molybdenum powder are added and mixed. If a large container with a volume of 20 liters or more is used as the container 1, the remaining amount of water is added to 70 to 40% after mixing the amount of water with the binder and molybdenum powder at 30 to 60% of the final amount. It is possible to adjust the amount of molybdenum powder and water by adding it. In order to make it easy to visually confirm whether or not the binder is completely dissolved in water, a method of additionally adding water is effective.
  • the molybdenum powder of the present invention is a molybdenum powder to which at least one of a potassium component, an aluminum component, and a silicon component is added.
  • a potassium component the aluminum component, and the silicon component, compounds such as single elements, oxides, and complex oxides are used, respectively.
  • the potassium component is preferably in the range of 100 to 1000 mass ppm in terms of potassium element simple substance.
  • the aluminum component is preferably in the range of 100 to 1000 ppm by mass in terms of a single aluminum element.
  • the silicon component is preferably in the range of 100 to 1000 ppm by mass in terms of a silicon element. If the amount is less than 100 ppm by mass, the effect of addition is small.
  • a dopant may be 1 type or may add 2 or more types.
  • a potassium component, an aluminum component, and a silicon component are components called a dopant.
  • the recrystallization temperature is increased and the high temperature strength is increased as compared with high purity molybdenum.
  • Secondary processing includes wire bending processing, wire bending processing, plate material (plate material made of Mo sintered body) rolling processing, bending processing, punching processing, and the like. Further, when a wire is used, non-sag, high-temperature vibration resistance, and blackening resistance can be improved.
  • ammonium dimolybdate (NH 4 ) 2 ⁇ Mo 2 O 7 )
  • Mo oxide ammonium dimolybdate
  • Potassium silicate is added to the Mo oxide so that the amount of elemental potassium element per elemental Mo is 100 to 1000 ppm by mass.
  • pure water is added, kneaded, heated to 100 to 140 ° C. with stirring and dried to obtain a molybdenum oxide powder to which a dopant is added.
  • the dopant-added molybdenum oxide powder can be heated and reduced at 1000 to 1200 ° C. for 2 to 5 hours in a hydrogen atmosphere to obtain a dopant-added molybdenum powder.
  • the above shows an example in which potassium is added as a dopant.
  • silicon or aluminum is added as a dopant, silicon alone or a silicon compound, and aluminum alone or an aluminum compound are added, respectively.
  • potassium silicate was used as the potassium component, the invention is not limited to this, and other potassium compounds may be used.
  • when adding 2 or more types of potassium, aluminum, and silicon what is necessary is just to add each element or compound and to obtain a dopant addition molybdenum powder.
  • the purity of the dopant-added molybdenum powder is not particularly limited, but the total of Mo and the dopant is preferably 99% by mass or more, and more preferably 99.9% by mass or more.
  • Main impurities of the molybdenum powder include Fe (iron), Ca (calcium), and Mg (magnesium).
  • Other impurities include Ni (nickel), Na (sodium), Pb (lead), Bi (bismuth), Cd (cadmium), Cu (copper), Mn (manganese), and Sn (tin). It is done.
  • the measurement of the purity of molybdenum is Fe (iron), Ca (calcium), Mg (magnesium), Ni (nickel), Na (sodium), Pb (lead), Bi (bismuth), Cd (cadmium), Cu (copper) ), Mn (manganese) and Sn (tin) are subtracted from 100% by mass.
  • Fe iron
  • Ca calcium
  • Mg manganesium
  • Ni nickel
  • Na Sodium
  • Pb lead
  • Bi bismuth
  • Cd cadmium
  • Cu copper
  • Mn Manganese
  • Sn tin
  • gas components such as oxygen, are mentioned as impurities other than the said metal impurity.
  • the amount of oxygen is preferably 7% by mass or less, and the amount of nitrogen is preferably 7% by mass or less.
  • FIG. 2 shows an example of a granulation process using a spray dryer.
  • reference numeral 1 is a container containing a molybdenum-containing aqueous solution
  • 6 is a molybdenum-containing aqueous solution
  • 7 is an inlet for the molybdenum-containing aqueous solution
  • 8 is a rotating plate that disperses the molybdenum-containing aqueous solution 6 into fine droplets.
  • 9 is a granulated molybdenum powder
  • 10 is an outer wall of the spray dryer
  • 11 is a recovery container for the molybdenum granulated powder.
  • the molybdenum-containing aqueous solution 6 adjusted in the above process is poured into the charging port 7.
  • the charging speed to the charging port 7 is preferably 10 to 80 cc / min.
  • the input speed is less than 10 cc / min, the input amount is too small and the mass productivity is deteriorated.
  • the charging speed exceeds 80 cc / min, the charging amount becomes excessive, and the characteristics of the resulting granulated powder vary.
  • the charged molybdenum-containing aqueous solution 6 is supplied onto the rotating plate 8 via the charging port 7.
  • the rotating plate 8 rotates at a constant rotational speed.
  • the molybdenum-containing aqueous solution 6 is supplied to the rotating rotating plate 8, it is repelled by a certain amount, and spherical molybdenum granulated powder 9 is formed by surface tension.
  • the molybdenum granulated powder 9 falls along the outer wall 10 of the spray dryer and is collected in a molybdenum granulated powder collection container 11.
  • the average particle diameter of the molybdenum granulated powder is highly related to the rotation speed of the rotating plate.
  • the present invention is characterized in that A / B is controlled in the range of 50 to 700, where A (rpm) is the rotational speed of the rotating plate and B ( ⁇ m) is the average particle diameter of the molybdenum granulated powder.
  • a (rpm) is the rotational speed of the rotating plate
  • B ( ⁇ m) is the average particle diameter of the molybdenum granulated powder.
  • a / B which is the ratio of the rotational speed A of the rotating plate to the average particle diameter B of the granulated powder, is less than 50, the rotational speed of the rotating plate is insufficient with respect to the average particle diameter of the intended granulated powder. Therefore, the average particle size B of the intended granulated powder cannot be obtained. Moreover, when A / B is less than 50, it becomes a granulated powder having a larger average particle diameter than the average particle diameter B of the intended granulated powder. On the other hand, when A / B exceeds 700, the rotation speed A of the rotating plate is too high with respect to the average particle diameter B of the intended granulated powder, and thus the average particle diameter B of the intended granulated powder is obtained. Absent.
  • a / B exceeds 700, it becomes a small average particle diameter with respect to the average particle diameter B of the intended granulated powder.
  • a / B By controlling the value of A / B in the range of 50 to 700, a granulated powder having an average particle diameter within a range of ⁇ 50% with respect to the average particle diameter B of the intended granulated powder can be obtained.
  • the average particle size B of the intended granulated powder is 50 ⁇ m
  • the average particle diameter of granulated powder uses an enlarged photograph, and makes the maximum diameter of the granulated powder reflected there the particle diameter, and the average value of 100 granulated powder is the average particle diameter of the granulated powder.
  • the average particle size B of the granulated powder is preferably 20 to 150 ⁇ m. If the average particle diameter of the granulated powder is in the range of 20 to 150 ⁇ m, it can be applied to various applications. Further, the rotational speed A of the rotating plate 8 is preferably 5000 to 16000 rpm. When the rotational speed A is in the range of 5000 to 16000 rpm, the molybdenum-containing aqueous solution 6 is effectively repelled efficiently on the rotating plate 8, and molybdenum granulated powder having a target average particle diameter is easily obtained.
  • the spray dryer preferably dries the molybdenum granulated powder while supplying hot air of 150 to 300 ° C. Supplying hot air of 150-300 ° C into the outer wall of the spray dryer to dry the molybdenum granulated powder, thereby evaporating the moisture in the granulated powder and strengthening the bonding force between the molybdenum powders by the binder Can do. As a result, it is possible to effectively produce molybdenum granulated powder having a target average particle diameter. Hot air is supplied into the outer wall 10 of the spray dryer from a hot air supply port (not shown) and exhausted from an exhaust port (not shown).
  • the spray drier carries out the drying of the molybdenum granulated powder in a reduced-pressure atmosphere below atmospheric pressure.
  • ⁇ Granulated powder in the range of 50% can be obtained.
  • the apparent density of the resulting molybdenum granulated powder is preferably 1.3 to 3.0 g / cc.
  • the average particle diameter of the molybdenum granulated powder is measured using an enlarged photograph. If it is this measuring method, the average particle diameter on an external appearance can be judged.
  • the variation in the amount of molybdenum inserted into the molding die occurs, and the pores in the sintered compact may become larger than necessary. If the apparent density of the molybdenum granulated powder is less than 1.3 g / cc, the amount of molybdenum in the granulated powder is too small, and this causes a variation in quality in the subsequent commercialization. On the other hand, when the apparent density exceeds 3.0 g / cc, the molybdenum powder is tightly packed, and it is difficult to stably manufacture with a spray dryer. The apparent density is measured by a measuring method based on JIS-Z-2504.
  • the fluidity of the obtained granulated powder is 50 sec / 50 g or less.
  • the fluidity is measured by a measuring method based on JIS-Z-2504.
  • the fluidity is an index indicating how smoothly the granulated powder moves (flows).
  • the fluidity is good (fluidity 50 sec / 50 g or less)
  • the supply to the molding die at the time of commercialization can be carried out smoothly and rapidly.
  • the granulated powder has good handleability.
  • liquidity is favorable means that the shape of granulated powder is close to a sphere.
  • the aspect ratio is 1.5 or less.
  • FIG. 3 shows an example of the shape of molybdenum granulated powder.
  • reference numeral 3 denotes molybdenum powder
  • 9 denotes molybdenum granulated powder
  • L1 denotes a short diameter of the molybdenum granulated powder
  • L2 denotes a long diameter.
  • the aspect ratio is obtained by “major axis L2 / minor axis L1”.
  • An aspect ratio of 1.0 indicates a state close to a true sphere.
  • the molybdenum granulated powder of this invention excellent in average particle diameter, apparent density, and fluidity
  • a method of carrying out a sieving step is also effective. Excessive granulated powder can be removed by carrying out the sieving step. As a result, the average particle diameter can be further controlled.
  • molybdenum granulated powder having excellent average particle diameter, apparent density, and fluidity can be efficiently produced with high yield. Therefore, the granulated powder according to each product can be manufactured with a good yield.
  • the use of the granulated powder include thermal spraying powder, raw powders of various sintered bodies, and the like.
  • the production yield can be further improved by changing the average particle size according to the shape of the molding die. For example, in a sintered body having a thickness of 1 mm or less, the average particle diameter of the granulated powder is about 50 ⁇ m, and in a sintered body having a thickness of about 5 mm, the average particle diameter of the granulated powder is about 100 ⁇ m. It is possible to efficiently fill the molding die.
  • Example 1 (Examples 1 to 7 and Comparative Example 1) A dopant-added molybdenum powder shown in Table 1 and polyvinyl alcohol (PVA) powder and pure water were prepared as binders. Water was poured into a stainless steel container, and while the water was heated and stirred, the polyvinyl alcohol powder was added and all the added polyvinyl alcohol powder was dissolved. When all the polyvinyl alcohol powder was dissolved, it was confirmed that the solution was a translucent aqueous solution. Thereafter, a total of 40 kg of molybdenum powder was added in an amount of 1-2 kg. When the molybdenum powder was agitated, pure water was added as needed for the amount of water that was insufficient due to evaporation.
  • PVA polyvinyl alcohol
  • Example 1 Samples using polyvinyl alcohol powder as a binder were designated as Examples 1 to 5. Further, a sample using polyethylene glycol powder as a binder was Example 6, and a sample using carbomethylmethylcellulose powder was Example 7. On the other hand, the molybdenum containing aqueous solution which concerns on the comparative example 1 was prepared by processing like Example 1 except the heating temperature of water having been 35 degreeC. Table 2 below shows the conditions of the adjustment process of the molybdenum-containing aqueous solution so far.
  • the average particle diameter, aspect ratio, apparent density, fluidity, and yield of the molybdenum granulated powder obtained by the production methods of Examples 1A to 7A and Comparative Examples 2 to 3 were investigated.
  • the average particle diameter extracted arbitrary 100 grains of the obtained molybdenum granulated powder took the enlarged photograph, calculated
  • the yield was calculated from the ratio of (the total amount of the granulated powder / 40 kg) ⁇ 100% of the amount of the molybdenum powder 40 kg and the total amount of the granulated molybdenum powder.
  • the measurement results are shown in Table 4 below.
  • the molybdenum granulated powder produced by the method for producing molybdenum granulated powder according to this example has a small deviation from the target average particle diameter B, and has an aspect ratio and an apparent appearance. The density and fluidity were excellent. In addition, it can be said that this is an efficient manufacturing method with a high yield.
  • Comparative Example 2 and Comparative Example 3 in which A / B is outside the range of the present invention showed characteristics in which both parameters deteriorated.
  • Container Container for preparing molybdenum-containing aqueous solution
  • Container Container for preparing molybdenum-containing aqueous solution
  • Molybdenum powder Molybdenum powder with added dopant
  • Binder 5 ... Water to be recharged as required 6
  • Molybdenum-containing aqueous solution 7 ...
  • Molybdenum-containing aqueous solution inlet 8 ...
  • Rotary plate 9 ... Molybdenum granulated powder 10 ... Outer wall 11 of spray dryer ... Recovery of molybdenum granulated powder container

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Abstract

L'invention concerne un procédé de production d'une poudre granulée de molybdène caractérisé en ce qu'il comporte : une étape consistant à injecter de l'eau dans un contenant, et à la chauffer jusqu'à une température allant de 50 à 80°C ; une étape consistant à ajouter un liant dans l'eau chauffée ; une étape consistant à préparer une solution aqueuse contenant du molybdène en chargeant de la poudre de molybdène, qui a une taille moyenne des particules de 1 à 10 μm, à laquelle au moins l'un parmi un composant de potassium, un composant d'aluminium et un composant de silicium a été ajouté, tout en mélangeant l'eau ; et une étape consistant à charger la solution aqueuse contenant du molybdène dans un sécheur par pulvérisation où, quand la vitesse de rotation d'un rotateur du sécheur par pulvérisation dans lequel la solution aqueuse contenant du molybdène doit être dispersée est considérée comme étant A (tr/min), et quand la taille moyenne des particules de la poudre granulée devant être préparée est considérée comme étant B (μm), le rapport A/B va de 50 à 700, et à disperser et sécher la solution aqueuse contenant du molybdène pour préparer la poudre granulée de molybdène. Le procédé mentionné ci-dessus permet de produire une poudre granulée de molybdène activée ayant la taille moyenne de particules prévue à haut rendement.
PCT/JP2012/057399 2011-06-08 2012-03-22 Procédé de production d'une poudre granulée de molybdène et poudre granulée de molybdène Ceased WO2012169262A1 (fr)

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JPS59150073A (ja) * 1983-02-10 1984-08-28 Toshiba Corp 高温熱処理用モリブデン治具の製造方法
JPS59150070A (ja) * 1983-02-10 1984-08-28 Toshiba Corp モリブデン材の製造方法
JPH0198764A (ja) * 1987-10-08 1989-04-17 Teikoku Piston Ring Co Ltd シリンダとピストンリングとの組合わせ
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JPH11199948A (ja) * 1998-01-06 1999-07-27 Toshiba Corp 低温延性材料
JP2004052020A (ja) * 2002-07-17 2004-02-19 Matsushita Electric Ind Co Ltd タングステン重合金からなる振動子の製造方法
JP2005120400A (ja) * 2003-10-15 2005-05-12 Sumitomo Electric Ind Ltd 顆粒状の金属粉末
JP2005291530A (ja) * 2004-03-31 2005-10-20 Tdk Corp 噴霧乾燥装置、粉体の乾燥方法およびフェライト粒の製造方法

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