WO2012169258A1 - 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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WO2012169258A1
WO2012169258A1 PCT/JP2012/057355 JP2012057355W WO2012169258A1 WO 2012169258 A1 WO2012169258 A1 WO 2012169258A1 JP 2012057355 W JP2012057355 W JP 2012057355W WO 2012169258 A1 WO2012169258 A1 WO 2012169258A1
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molybdenum
granulated powder
powder
producing
average particle
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PCT/JP2012/057355
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English (en)
Japanese (ja)
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山口　悟
勉 森岡
斉 青山
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株式会社東芝
東芝マテリアル株式会社
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Publication of WO2012169258A1 publication Critical patent/WO2012169258A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals

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 used for thermal spraying materials, sintering furnace plate materials, electrode parts, magnetron stems, sputtering targets, and the like.
  • the material for thermal spraying is a material supplied by 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 Mo molten metal will be used as an 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 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.
  • a sintering method When producing a sintered compact by a sintering method, a granulation process, a formation process, a degreasing process, a sintering process, etc. are implemented with respect to Mo powder.
  • the conventional sintering methods have been advanced 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. Thereby, the sinterability is improved and the 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.
  • the improvement regarding Mo raw material powder, a degreasing process, and a sintering process was performed. However, even if the improvement is advanced, the product yield has not necessarily reached 100%. Such a phenomenon also occurred in the same way for a Mo sintered body using Mo powder to which cobalt or the like was added.
  • the inventors have investigated the reason why the yield of products using Mo powder as an initial raw material is not improved. As a result, it was found that the size, density, fluidity, etc. of the granulated powder were dissolved and dissolved, but if they were large, the filling density and supply amount in the molding process were varied and dissolved, causing the product yield to decrease. . In addition, when Mo granulated powder is used as the thermal spray powder, the amount of supply to the thermal spray flame (supply speed) varies and dissolves, resulting in problems such as unstable properties as the thermal spray film. 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 is for solving such problems, and realizes stabilization of the quality of Mo products (powder or sintered body) and improvement of yield, and enables molybdenum granulated powder to be efficiently produced with high yield. It aims at providing the manufacturing method of the molybdenum granulated powder which can be manufactured.
  • the method for producing molybdenum granulated powder according to the present invention includes a step of injecting an organic solvent into a container, a step of adding polyvinyl butyral as a binder to the organic solvent, and stirring the organic solvent while stirring the tin component and cobalt.
  • a sieving step of passing a sieve having a mesh diameter 2 to 3 times the average particle size B of the granulated powder with respect to the granulated powder after completion of the granulating 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.
  • an organic solvent is ethanol.
  • the content (addition amount) of the cobalt component is preferably in the range of 50 to 500 mass ppm (wtppm) in terms of cobalt elemental element.
  • the content of the tin component is in the range of 50 to 500 ppm by mass in terms of tin element. Moreover, it is preferable to add both a tin component and a cobalt component.
  • 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 solution preferably has an organic solvent amount of 0.2 to 1 liter when the molybdenum powder amount is 100 parts by mass.
  • the spray dryer preferably dries the molybdenum granulated powder while supplying hot air at 100 to 300 ° C. Moreover, it is preferable that the spray drier carries out the drying of the molybdenum granulated powder in a reduced-pressure atmosphere below atmospheric pressure. Moreover, it is preferable that the fluidity
  • the molybdenum granulated powder according to the present invention is characterized by containing at least one of a tin component and a cobalt component and having 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 a molybdenum granulated powder in the granulation step, while stirring an organic solvent, a molybdenum powder and a binder to which a tin component or / and a cobalt component are added are supplied, and the intended granulation is further performed. Since the ratio of the average particle size of the powder and the rotation speed of the rotating plate of the spray dryer is controlled within a predetermined range, it is possible to produce molybdenum granulated powder with excellent average particle size, apparent density and fluidity. it can.
  • a method for producing molybdenum granulated powder according to an embodiment of the present invention includes a step of injecting an organic solvent into a container, a step of adding polyvinyl butyral as a binder to the organic solvent, and stirring the organic solvent while tin is used.
  • a step of preparing a molybdenum-containing solution by introducing molybdenum powder having an average particle diameter of 1 to 10 ⁇ m to which at least one of a component and a cobalt component is added, and rotation of a rotating plate of a spray dryer for dispersing the molybdenum-containing solution
  • the molybdenum-containing solution is put into a spray dryer in which A / B is in the range of 50 to 700.
  • FIG. 1 shows an example of a process for preparing a molybdenum-containing solution.
  • reference numeral 1 is a container (a container for preparing a molybdenum-containing solution)
  • 2 is an organic solvent
  • 3 is a molybdenum powder (a molybdenum powder to which a tin component or a cobalt component is added)
  • 4 is a binder.
  • 5 is an organic solvent to be recharged as necessary
  • 6 is a molybdenum-containing solution.
  • the organic solvent 2 is injected into the container 1.
  • alcohol or the like is used.
  • the alcohol ethanol (ethyl alcohol: C 2 H 5 OH) is preferable.
  • Ethyl alcohol is preferable because it easily dissolves a binder (polyvinyl butyral) described later.
  • a step of adding the binder 4 to the organic solvent 2 is performed.
  • Polyvinyl butyral (PVB) is used as the material of the binder.
  • Polyvinyl butyral is well soluble in organic solvents, especially ethanol.
  • a binder stirring an organic solvent.
  • a step of preparing a molybdenum-containing solution 6 is performed by adding molybdenum powder 3 having an average particle diameter of 1 to 10 ⁇ m while stirring organic solvent 2.
  • the average particle size of the molybdenum powder 3 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.
  • the average particle diameter of the molybdenum powder 3 is 1 to 10 ⁇ m, and more preferably 2 to 5 ⁇ m. Further, when a large amount of molybdenum powder is added at once, the molybdenum powder tends to aggregate more than necessary, so 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 the organic solvent. If the binder is added in the state of powder, it can be discriminated with the naked eye whether or not it is dissolved.
  • the organic solvent (ethanol) before adding the molybdenum powder becomes translucent. In order to easily determine whether or not the binder is completely dissolved in the organic solvent (ethanol), it is preferable to add the molybdenum powder after the binder is added.
  • the volume of the binder is 3 to 20 parts by volume. It is preferable that 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 becomes too small, and uniform granulated powder may not be obtained.
  • the added amount of the binder is 3 to 20 parts by volume with respect to 100 parts by volume of the molybdenum powder, and more preferably 5 to 15 parts by volume.
  • the molybdenum-containing solution preferably has an organic solvent amount of 0.2 to 1 liter when the molybdenum powder amount is 100 parts by mass.
  • the spray dryer is charged in a molybdenum-containing solution.
  • the amount of the organic solvent is less than 0.2 liters with respect to 100 parts by mass of the molybdenum powder, the amount of the organic solvent is too small, the viscosity of the molybdenum-containing solution increases, and it can be stably supplied to the spray dryer. Have difficulty.
  • the amount of the organic solvent exceeds 1 liter, the amount of the organic solvent becomes excessive, and it is difficult to stably supply the organic solvent.
  • a stable supply method can also be adopted by supplying it with stirring.
  • the supply of the molybdenum-containing solution to the spray dryer can be mechanized and automated.
  • ethanol since ethanol has a relatively low boiling point of 78.3 ° C., ethanol may evaporate and the amount of solvent may change greatly when a binder and molybdenum powder are added and mixed.
  • the amount of organic solvent is mixed with the binder and molybdenum powder at 30 to 60% of the final amount, and then the remaining organic
  • a method of adjusting the blending ratio between molybdenum powder and the amount of organic solvent by additionally adding a solvent amount of 70 to 40% can also be employed.
  • a method of adding the organic solvent is also effective.
  • the molybdenum powder of the present invention is a molybdenum powder to which at least one of a tin component and a cobalt component is added.
  • a tin component or the cobalt component compounds such as simple elements, oxides, and complex oxides can be used.
  • the content (addition amount) of the tin component is preferably in the range of 50 to 500 ppm by mass in terms of the tin (Sn) element alone.
  • the content (addition amount) of the cobalt component is preferably in the range of 50 to 500 ppm by mass in terms of cobalt (Co) element alone.
  • the tin component or the cobalt component when the tin component or the cobalt component is less than 50 ppm by mass in terms of a simple metal element, the effect of addition is small.
  • the addition of a tin component or a cobalt component increases the recrystallization temperature and increases the high-temperature strength as compared with high-purity molybdenum.
  • Secondary workability such as a drawing process to a wire, improves.
  • 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, the wire characteristics can improve non-sag, high-temperature vibration resistance, and blackening resistance.
  • ammonium dimolybdate (NH 4 ) 2 ⁇ Mo 2 O 7 )
  • Mo oxide ammonium dimolybdate
  • tin chloride and / or cobalt chloride is added so as to be 50 to 500 mass ppm in terms of a metal simple substance.
  • pure water is added, kneaded, heated to 100 to 140 ° C. with stirring and dried to obtain a molybdenum component-added molybdenum oxide powder.
  • the molybdenum component-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 molybdenum powder to which the tin component and / or cobalt component is added. .
  • the purity of the molybdenum powder to which the tin component or cobalt component is added is not particularly limited, but the sum of Mo and tin or / and cobalt may be 99% by mass or more, and further 99.9% by mass or more. preferable.
  • Main impurities of the molybdenum powder include Fe (iron), Al (aluminum), Ca (calcium), Mg (magnesium), and Si (silicon). Other impurities include Ni (nickel), Na (sodium), K (potassium), Pb (lead), Bi (bismuth), Cd (cadmium), Cu (copper), and Mn (manganese). It is done.
  • the measurement of the purity of molybdenum is Fe (iron), Al (aluminum), Ca (calcium), Mg (magnesium), Si (silicon), Ni (nickel), Na (sodium), K (potassium), Pb (lead). ), Bi (bismuth), Cd (cadmium), Cu (copper), and Mn (manganese) are subtracted from 100% by mass.
  • Fe iron
  • Al aluminum
  • Ca calcium
  • Mg manganesium
  • Si silicon
  • Ni nickel
  • Na sodium
  • K potassium
  • Pb lead
  • Bi Bismuth
  • Cd cadmium
  • Cu copper
  • Mn manganesese
  • gas components such as oxygen, are mentioned as impurities other than the said metal impurity. While the amount of oxygen is 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 solution
  • 6 is a molybdenum-containing solution
  • 7 is an inlet for a molybdenum-containing aqueous solution
  • 8 is a rotating plate
  • 9 is a molybdenum granulated powder.
  • Reference numeral 10 denotes an outer wall of the spray dryer
  • reference numeral 11 denotes a molybdenum granulated powder collection container.
  • the molybdenum-containing solution 6 adjusted in the above process is poured into the charging port 7.
  • the input amount (input speed) to the input 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 input speed exceeds 80 cc / min, the input amount becomes excessive, and the characteristics of the resulting granulated powder vary.
  • the charged molybdenum-containing solution 6 is supplied onto the rotating plate 8.
  • the rotating plate 8 rotates at a constant rotational speed.
  • the molybdenum-containing solution 6 is supplied to the rotating rotating plate, it is repelled by a certain amount to form spherical molybdenum granulated powder 9 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 8 of the spray dryer.
  • the present invention is characterized in that A / B is controlled in the range of 50 to 700 when the rotational speed of the rotating plate 8 is A (rpm) and the average particle diameter of the granulated powder is B ( ⁇ m). It is what.
  • a / B is controlled in the range of 50 to 700 when the rotational speed of the rotating plate 8 is A (rpm) and the average particle diameter of the granulated powder is B ( ⁇ m). It is what.
  • the molybdenum-containing solution 6 is supplied to the rotating plate 8, the molybdenum-containing solution 6 is repelled on the rotating plate by a certain amount, and the repelled molybdenum-containing solution 6 becomes spherical molybdenum granulated powder 9 due to surface tension.
  • uniform granulated powder can be manufactured also from having added the binder.
  • a / B which is the value of the above ratio is less than 50, the rotation speed of the rotating plate is insufficient with respect to the average particle diameter of the intended granulated powder, and therefore the average particle diameter 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 of the rotating plate is too high with respect to the average particle diameter of the intended granulated powder, and thus the average particle diameter B of the intended granulated powder cannot be obtained.
  • 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 in the range of 50 to 700, a granulated powder having an average particle diameter in the 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.
  • the rotation speed A of the rotary plate 8 of the spray dryer is preferably 5000 to 16000 rpm. When the rotational speed A is in the range of 5000 to 16000 rpm, the molybdenum-containing solution is efficiently repelled on the rotating plate, and a granulated powder having a target average particle diameter is easily obtained.
  • the spray dryer preferably dries the molybdenum granulated powder while supplying hot air at 100 to 300 ° C.
  • hot air having a temperature of 100 to 300 ° C.
  • the organic solvent in the granulated powder can be evaporated and the binding force between the molybdenum powders by the binder can be enhanced.
  • molybdenum granulated powder having a target average particle diameter can be produced.
  • 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 dryer performs drying of the molybdenum granulated powder in a reduced-pressure atmosphere of atmospheric pressure or lower.
  • a reduced-pressure atmosphere of atmospheric pressure or lower By setting the inside of the outer wall 10 of the spray dryer to a reduced-pressure atmosphere of atmospheric pressure or less, the organic solvent in the granulated powder can be easily evaporated.
  • the rotation speed of the rotating plate of the spray dryer is adjusted in accordance with the average particle diameter of the granulated powder, ⁇ A granulated powder having an average particle size in the range of 50% can be obtained efficiently.
  • 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 abundance ratio of the molybdenum powder partially varies. Arise. Variation in the existence ratio leads to variation in the product. For example, when granulated powder is used as a thermal spraying powder, if there are granulated powders with significantly different densities, the amount of molybdenum powder charged into the thermal flame flame will vary, resulting in variations in the thermal sprayed Mo film. Cause. Moreover, when producing a sintered compact, 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.
  • the apparent density is less than 1.3 g / cc, the amount of molybdenum in the molybdenum granulated powder is too small, which causes a variation in quality in the subsequent commercialization.
  • the apparent density exceeds 3.0 g / cc, the molybdenum powder is tightly packed, so that it is difficult to stably manufacture with a spray dryer.
  • the apparent density is measured according to a measurement method based on JIS-Z-2504.
  • liquidity of the obtained molybdenum granulated powder is 50 sec / 50g or less. This fluidity measurement is also carried out by a measurement method based on JIS-Z-2504.
  • the fluidity is an index indicating how smoothly and quickly the granulated powder moves (flows).
  • the fluidity is good (fluidity 50 sec / 50 g or less)
  • the filling and filling of the molding die can be smoothly and rapidly performed when commercialized.
  • the granulated powder has good handleability.
  • liquidity is good 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 molybdenum granulated powder.
  • 3 is a molybdenum powder
  • 9 is a molybdenum granulated powder
  • L1 is a short diameter of the molybdenum granulated powder
  • L2 is a long diameter.
  • the aspect ratio is obtained from the formula “major axis L2 / minor axis L1”.
  • An aspect ratio of 1.0 indicates a state close to a true sphere.
  • the molybdenum granulated powder excellent in average particle diameter, apparent density, and fluidity
  • a process for controlling the average particle diameter of the molybdenum granulated powder, especially the particle size distribution it has a mesh diameter 2 to 3 times the average particle diameter B of the granulated powder after completion of the granulation process by a spray dryer.
  • a method of further carrying out a sieving step through a sieve is also preferred. By carrying out this sieving step, excessive granulated powder can be removed. As a result, the average particle diameter can be further controlled.
  • this sieving step is effective because it can remove excessive granulated powder.
  • molybdenum granulated powder having excellent average particle diameter, apparent density, and fluidity can be efficiently produced with a high yield. Therefore, the granulated powder according to each product can be manufactured with a good yield.
  • Applications of this granulated powder include thermal spraying powder, raw powders of various sintered bodies, and the like.
  • the use of molybdenum granulated powder with excellent average particle diameter, apparent density and fluidity ensures uniform filling in the mold.
  • the density of the sintered body can be stabilized.
  • the 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 set to about 50 ⁇ m, whereas in a sintered body having a thickness of about 5 mm, the average particle diameter of the granulated powder is set to about 100 ⁇ m. As a result, it is possible to efficiently fill the molding die. Moreover, since the high temperature characteristic is excellent, the workability at the time of processing into a wire is also improved.
  • Example 2 (Examples 1 to 5 and Comparative Examples 1 and 2) A molybdenum powder added with a tin component and / or a cobalt component shown in Table 1, and polyvinyl butyral (PVB) powder and ethanol were prepared as binders. First, ethanol was poured into a stainless steel container, and while stirring at room temperature, polyvinyl butyral powder was added, and all the added polyvinyl butyral powder was dissolved. When all the polyvinyl butyral powder was dissolved, it was confirmed that the solution was a translucent solution. Thereafter, a total of 40 kg of molybdenum powder was added in an amount of 1-2 kg.
  • Examples 1 to 5 were molybdenum-containing solutions using polyvinyl alcohol powder as a binder. The conditions for the preparation steps of the molybdenum-containing solution so far are shown in Tables 1 and 2 below.
  • the average particle diameter, aspect ratio, apparent density, fluidity and product yield of the granulated molybdenum powders obtained by the production methods of Examples 1A-5B and Comparative Examples 1-2 were investigated.
  • the average particle size was obtained by extracting 100 arbitrary particles of the obtained molybdenum granulated powder, taking an enlarged photograph, obtaining the maximum diameter reflected therein, and taking the average value of 100 particles as the average particle size.
  • the aspect ratio used the same enlarged photograph, calculated
  • the apparent density and fluidity were measured according to a measuring method based on JIS-Z-2504.
  • the product yield was calculated from the ratio of the amount of molybdenum powder charged to 40 kg and the total amount of recovered molybdenum granulated powder ((total amount of granulated powder / 40 kg) ⁇ 100%). The measurement results are shown in Table 4 below.
  • the molybdenum granulated powder added with the tin component and / or the cobalt component, produced by the method for producing the molybdenum granulated powder according to each example has a target average particle size.
  • the deviation with respect to the diameter B was small, and the aspect ratio, the apparent density, and the fluidity were excellent.
  • this is an efficient manufacturing method with a high yield.
  • Comparative Example 1 and Comparative Example 2 where A / B is outside the specified range in the present invention both parameters showed a deteriorated characteristic.

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 un solvant organique dans un contenant ; une étape consistant à ajouter du butyral polyvinylique dans le solvant organique pour servir de liant ; une étape consistant à préparer une solution contenant du molybdène en chargeant de la poudre de molybdène ayant une taille moyenne des particules de 1 à 10 μm, à laquelle un composant d'étain et/ou un composant de cobalt a été ajouté, tout en mélangeant le solvant organique ; et une étape consistant à charger la solution 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 contenant du molybdène doit être dispersée est considérée comme étant A (tr/min), et quand la taille moyenne des particules de la poudre granulée est considérée comme étant B (μm), le rapport A/B va de 50 à 700, et à disperser et sécher la solution contenant du molybdène pour préparer la poudre granulée de molybdène. Le procédé mentionné ci-dessus permet de produire une poudre granulée de molybdène ayant la taille moyenne de particules prévue, et contenant un composant d'étain et/ou un composant de cobalt, de manière efficace à haut rendement.
PCT/JP2012/057355 2011-06-08 2012-03-22 Procédé de production d'une poudre granulée de molybdène et poudre granulée de molybdène WO2012169258A1 (fr)

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