CN104070175A - Method for producing metal molybdenum spherical fine powder or superfine powder - Google Patents
Method for producing metal molybdenum spherical fine powder or superfine powder Download PDFInfo
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- CN104070175A CN104070175A CN201410305472.8A CN201410305472A CN104070175A CN 104070175 A CN104070175 A CN 104070175A CN 201410305472 A CN201410305472 A CN 201410305472A CN 104070175 A CN104070175 A CN 104070175A
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Abstract
The invention discloses a method for producing metal molybdenum spherical fine powder or superfine powder. The method comprises step 1, performing gas exchange on a production device to enable the original gas in the production device to be completely discharged; step 2, feeding the working gas and the auxiliary gas into a heating cylinder body through an insulation end cover; step 3, starting an electrical system to enable an induction coil to be energized and forming a gradient temperature field inside the heating cylinder body; step 4, adding molybdenum oxide powder into a spiral powder feeder when the circulating water is led into a first stage powder collecting tank, starting a first motor to drive the spiral powder feeder to run and leading the powder carried gas into a gas pipe, wherein the powder carried gas is hydrogen; step 5, shutting down the first motor and the electrical system and cutting off the supply of the powder carried gas, the auxiliary gas and the working gas. According to the method for producing the metal molybdenum spherical fine powder or superfine powder, the degree of sphericity of the molybdenum powder is improved, the integral process can be performed in a continuous and closed mode, the design is reasonable, the equipment is simple, the control is easy, the response speed is high, the production efficiency is high, and the method is suitable for mass production.
Description
Technical field
The invention belongs to field of powder metallurgy, be specifically related to a kind of method of preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder.
Background technology
The spherical powder of refractory metal molybdenum is because good mobility and high apparent density have extensive use in fields such as thermal spraying, injection moulding, powder metallurgy and welding.Adopt the porous molybdenum framework material of spherical preparation of molybdenum powder, its hole link, the infiltration passage that can guarantee molybdenum skeleton is unimpeded, prepare the molybdenum-copper material of even tissue, adopt the molybdenum copper contact material structure of spherical preparation of molybdenum powder even, ablation degree is basically identical, can prevent from producing because material structure is inhomogeneous local transition ablation or puncture, improve the performance of molybdenum-copper contact, improve its life-span.Spherical molybdenum powder because of its good fluidity, apparent density large, the coating that obtains of spraying more evenly, fine and close and there is good wearability.Because of good fluidity, the Song Bi great of spherical molybdenum powder, in powder metallurgy molybdenum product is produced, pressed compact shrinks evenly when sintering, and shrinkage factor is little, can realize good size Control, obtains desirable sintered body material, is beneficial to the following process of sintered blank.In addition, spherical molybdenum powder is applied to nearly forming technology, can makes molybdenum shaped piece, improve the utilization rate of raw material, cut down finished cost significantly.
At present, the spheronization process of molybdenum powder mainly contains spray granulation, atomization, rotary electrode method etc.The spherical molybdenum powder rough that spray granulation is produced, poor fluidity, pine are than low, in addition, in preparation spraying slip process, introduce organic binder bond, easily material is formed the pollution of the elements such as C, O, introduce organic binder bond, need the linking of the techniques such as follow-up binder removal, sintering, extended technological process, improved production cost; Water atomization technique is prepared spherical powder and is easy to form metal oxide, and gas atomization is easy to form disjunctor particle and granule interior has pore, and to powder, follow-up use is all disadvantageous for these; With rotary electrode method, prepare spherical powder, because the restriction of electrode rotating speed, the prepared powder size of rotation electrode technique is thicker, be generally greater than 100 orders, and bulky grain metal dust is difficult for melting in the follow-up use procedure of powder, easily " half-cooked ", the final performance that affect goods, and atomization plant and plasma apparatus invest hugely, and output is lower, cause product cost high, impact is promoted.
Summary of the invention
For the defect existing in above-mentioned prior art or deficiency, the object of the invention is to, a kind of method of preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder is provided.The present invention adopts following technical scheme:
A method of preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder, specifically comprises the steps:
1) preparation facilities is carried out to gas displacement, original gas in it is discharged completely;
2) through working gas entrance and auxiliary gas entry, in heating cylindrical shell, send into working gas and assist gas; Working gas, assist gas all adopt hydrogen;
3) open electrical system and make to heat the induction coil energising on cylindrical shell, in heating inner barrel, form gradient temperature field;
4) to one-level powder collecting tank, pass into recirculated water, to packing auger, add molybdenum oxide powder, open the first motor and drive packing auger operation simultaneously; From tracheae, pass into powder and carry gas, powder carries gas and adopts hydrogen; Powder carries gas and carries the molybdenum oxide powder of being exported by packing auger, successively through powder uniforming device and powder feeding flue, be transported in heating cylindrical shell, molybdenum oxide powder, at cartridge heater precursor reactant, obtains spherical molybdenum micro mist or Ultramicro-powder and is collected successively by one-level powder collecting tank and secondary powder collecting tank;
5) while preparing task amount and complete, first close the first motor to stop carrying oxidation molybdenum powder, then close the electrical system being connected with the induction coil that heats cylindrical shell, final cutting powder carries the supply of gas, assist gas and working gas.
Further, described step 1) concrete operations: utilize aspiration pump to make to form negative pressure in it by vacuumizing in preparation facilities, then pass into hydrogen from tracheae, auxiliary gas entry and working gas entrance simultaneously and realize gas displacement.
Further, described step 2) in, the flow of described working gas is 6～9m
3/ h; The flow of described assist gas is 2～3m
3/ h.
Further, described step 3) in, the high-tension electricity loading on described induction coil is 6kV～9kV, electrical system input power is 20～100kW.
Further, described step 4) in, the particle diameter of described molybdenum oxide powder is 50～200 μ m, it is 1.0～3kg/h that molybdenum oxide powder adds speed.
Further, described step 4) in, it is 0.3～1.5m that described powder carries gas flow
3/ h.
Further, described step 4) in, described in the spherical molybdenum micro mist that obtains or the particle size range of Ultramicro-powder be 0.1～100 μ m.
Further, described preparation facilities comprises powder uniforming device, tracheae, packing auger, feed bin, the first motor, the collection of one-level tank powder, powder feeding flue, insulated end cover, heating cylindrical shell, cartridge heater body support frame, secondary powder collecting tank, aspiration pump and the second motor, wherein:
Described the first motor connects packing auger provides driving force for it; Feed bin connects the feed end of packing auger, and packing auger connects heating cylindrical shell by powder feeding flue; Between described packing auger and powder feeding flue, powder uniforming device is installed, this powder uniforming device is with two tracheaes; Powder uniforming device adopts the cylinder that a caliber is larger than the powder feeding pipe caliber of packing auger;
On the outer wall of described heating cylindrical shell, uniform winding has the induction coil being connected with electrical system; The upper end of heating cylindrical shell is removably provided with insulated end cover; The middle part that described powder feeding flue enters insulated end cover and extends to heating cylindrical shell enters the top of gradient temperature field; Cartridge heater external body suit cartridge heater body support frame, and be arranged on one-level tank powder collection top by cartridge heater body support frame; Heating cylindrical shell lower end is communicated with one-level powder collecting tank;
The outlet of one-level powder collecting tank is connected with the entrance of secondary powder collecting tank by tube connector, and tube connector is along the powder direction of motion certain angle that is inclined upwardly; The exit of secondary powder collecting tank is provided with Waste gas outlet, and this outlet connects the aspiration pump with the second motor.
Further, described insulated end cover comprises upper cover and lower cover two parts; Wherein, described upper cover is circular and there is discoid projection at its middle part, and the bottom of projection is cylindrical cavity, and the center of projection is provided with central through hole; Described lower cover is a disk with mesopore, and lower cover below is provided with a cylinder; This barrel bore with the internal diameter of lower cover, the internal diameter of upper cover is all identical; Upper cover and lower cover form a working gas transport tube between the two after fastening; On the sustained height of the sidewall of upper cover, being arranged with two working gas entrances, is starting point by these two working gas entrances, along the inwall of above-mentioned working gas transport tube, is provided with two helical grooves that parallel as working gas transfer passage; On the sustained height of the sidewall of lower cover the latter half, be arranged with two auxiliary gas entries; The central spot of the lower end of described cylinder and heating cylindrical shell is in sustained height; Between the outer wall of cylinder and heating cylinder inboard wall, form a toroidal cavity; This toroidal cavity can make the assist gas that is entered heating cylindrical shell by auxiliary gas entry form gas curtain on heating cylinder inboard wall, in case metal powder sticks on the inwall of heating cylindrical shell.
Further, described one-level powder collecting tank is a cylinder, its sidewall is double-layer stainless steel structure, between this double-decker, form the cavity of even thickness, this cavity is connected with the coolant outlet of cooling water inlet on the sidewall of one-level powder collecting tank lower end and its opposite side wall upper end, and this cavity is for passing into recirculated water to the high temperature powder rapid condensation nodularization in one-level powder collecting tank.
Compared with the conventional method, the present invention acts on heating cylindrical shell by induction field, and will heat cylindrical shell and use circulating water, the temperature field that cylindrical shell is heated and then portion produces within it, take hydrogen as working gas, assist gas and powder carry gas, molybdenum oxide material powder is sent into inner barrel, molybdenum oxide powder is under the effect of gradient temperature field, moment cracking, gasification is superfine powder, and be molybdenum powder particle by hydrogen reducing, molybdenum powder particle continues to shrink under gradient temperature field action, and obtain spherical molybdenum micro mist or Ultramicro-powder through rapid condensation nodularization, its particle size range is 0.1～100 μ m.The method has overcome the deficiency of current spherical molybdenum powder preparation method, has simplified production procedure, realizes one-step method and produces spherical molybdenum powder, has reduced production cost, for spherical molybdenum powder, promotes and has established solid foundation.
Accompanying drawing explanation
Fig. 1 is the generalized section of the preparation facilities that uses of method of the present invention.
Fig. 2 is the structural representation of insulated end cover.Wherein, Fig. 2 (a) is the overall structure schematic diagram of insulation lid; The schematic diagram that Fig. 2 (b) is upper cover; The schematic diagram that Fig. 2 (c) is lower cover.
Fig. 3 is the schematic diagram of working gas entrance in insulated end cover.
Fig. 4 is raw material molybdenum oxide electromicroscopic photograph.
Fig. 5 is the molybdenum powder obtaining after spheroidising.
Each mark title in figure: 1, powder uniforming device, 2, tracheae, 3, packing auger, 4, feed bin, 5, the first motor, 6, cooling water inlet, 7, coolant outlet, 8, gradient temperature field, 9, assist gas, 10, working gas, 11, powder feeding flue, 12, working gas entrance, 13, insulated end cover, 14, auxiliary gas entry, 15, heating cylindrical shell, 16, cooling water inlet, 17, coolant outlet, 18, tube connector, 19, secondary powder collecting tank, 20, aspiration pump, 21, Waste gas outlet, 22, the second motor, 23, metal filtration post, 24, upper cover, 25, lower cover, 26, projection, 27, central through hole, 28, working gas transfer passage, 29, cylinder, 30, powder carries gas.
Below in conjunction with the drawings and specific embodiments, the present invention is further explained.
The specific embodiment
As shown in Figure 1, in the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder of the present invention, the preparation facilities structure adopting is as follows:
Comprise powder uniforming device 1, tracheae 2, packing auger 3, feed bin 4, the first motor 5, one-level tank powder collection 7, powder feeding flue 11, insulated end cover 13, heating cylindrical shell 15, cartridge heater body support frame 16, secondary powder collecting tank 19, aspiration pump 20 and the second motor 22, wherein:
The first motor 5 connects packing auger 3 provides driving force for it; Feed bin 4 connects the feed end of packing auger 3, and packing auger 3 connects heating cylindrical shell 15 by powder feeding flue 11.
On the outer wall of heating cylindrical shell 15, uniform winding has the induction coil being connected with electrical system, and induction coil for making to heat the cylindrical shell 15 gradient temperature fields 8 that temperature changes in gradient of inner generation after energising; The upper end of heating cylindrical shell 15 is removably provided with insulated end cover 13; The outside suit of heating cylindrical shell 15 cartridge heater body support frames 16, and by cartridge heater body support frame 16, be arranged on one-level tank powder and collect 7 tops; Heating cylindrical shell 15 lower ends are communicated with one-level powder collecting tank 7.
Referring to Fig. 2 a, insulated end cover 13 comprises upper cover 24 and lower cover 25 two parts.Wherein, as shown in Figure 2 b, upper cover 24 is discoid protruding 26 for circular and its middle part have, and the bottom of projection 26 is cylindrical cavity, and the center of projection 26 is provided with central through hole 27; As shown in Figure 2 c, lower cover 25 is a disk with mesopore, and lower cover 25 belows are provided with a cylinder 29; These cylinder 29 internal diameters with the internal diameter of lower cover 25, the internal diameter of upper cover 24 is all identical; Upper cover 24 forms a working gas transport tube between the two after fastening with lower cover 25; On the sustained height of the sidewall of upper cover 24, being arranged with two working gas entrances 12, is starting point by these two working gas entrances 12, along the inwall of above-mentioned working gas transport tube, is provided with two helical grooves that parallel as working gas transfer passage 28; Working gas transfer passage 28 in powder preparation process to heating cylindrical shell 15 interior winding-up working gas 10, form spiral helicine distribution of gas field, constraint material powder is in the holdup time of gradient temperature field 8, make powder absorb the heat content of temperature field maximum, realize the thermodynamics reduction of powder and the micro-variations of pattern, finally obtain spherical molybdenum micro mist or Ultramicro-powder.On the sustained height of the sidewall of lower cover 25 the latter halfs, be arranged with two auxiliary gas entries 14.
The central spot of the lower end of cylinder 29 and heating cylindrical shell 15 is in sustained height; Between the outer wall of cylinder 29 and heating cylindrical shell 15 inwalls, form a toroidal cavity; This toroidal cavity can make the assist gas 9 that is entered heating cylindrical shell 15 by auxiliary gas entry 14 form gas curtain on heating cylindrical shell 15 inwalls, in case metal powder sticks on the inwall of heating cylindrical shell 15;
The middle part that powder feeding flue 11 enters insulated end cover 13 by the central through hole 27 of upper cover 24 and extends to heating cylindrical shell 15 enters the top of gradient temperature field 8;
For the powder of pulsed flow that packing auger 3 is sent here mixes, realize powder and be transported to heating cylindrical shell 15 inside with uniform flow, between packing auger 3 and powder feeding flue 11, powder uniforming device 1 is installed, this powder uniforming device 1 is with two tracheaes 2; Tracheae 2 carries gas 30 for passing into powder to powder uniforming device 1, and powder carries gas 30 and adopts hydrogen, and it is not only for carrying powder, and for the powder that is entered powder uniforming device 1 by packing auger 3 is blown out to disperse state; Powder uniforming device 1 adopts the caliber cylinder larger than the powder feeding pipe caliber of packing auger 3.
One-level powder collecting tank 7 is a cylinder, its sidewall is double-layer stainless steel structure, between this double-decker, form the cavity of even thickness, this cavity is connected with cooling water inlet 6 on one-level powder collecting tank 7 lower end sidewalls and the coolant outlet 17 of its opposite side wall upper end, and this cavity is for passing into recirculated water to the high temperature powder rapid condensation nodularization in one-level powder collecting tank 7.In secondary powder collecting tank, 19 adopt filter cylinders, are provided with metal filtration post 23 in it, identical with existing product.
The outlet of one-level powder collecting tank 7 is connected with the entrance of secondary powder collecting tank 19 by tube connector 18, and tube connector 18 is along the powder direction of motion certain angle that is inclined upwardly, object is that larger particles powder in order to drain into tube connector 8 at one-level powder collecting tank 7 is because self gravitation can be got back to one-level powder collecting tank along tube connector 18; In the present invention, this angle is greater than 30 °; The exit of secondary powder collecting tank 19 is provided with Waste gas outlet 21, and this outlet connection is with the aspiration pump 20 of the second motor 22, for being discharged by Waste gas outlet 21 after the gas extraction of secondary powder collecting tank 19.
The spherical molybdenum powder of the large-size of heating cylindrical shell 15 outputs completes collection in one-level powder collecting tank 7, more tiny molybdenum powder particle with air-flow through tube connector 18 to secondary powder collecting tank 19, adhere to metal filtration post 23, increase along with adhesive capacity, land and realize and collecting in secondary powder collecting tank 19 bottoms, waste gas is discharged through Waste gas outlet 21.
The material of insulated end cover 13 is silicon nitride or similar insulating materials; The material of heating cylindrical shell 15 is chromium base, nickel-bass alloy material or similar material; The material of cartridge heater body support frame 16 is pottery.
The method of preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder of the present invention, specifically comprises the steps:
1) said apparatus is carried out to gas displacement, original gas in it is discharged completely; Specifically utilize aspiration pump 20 to make to form negative pressure in it by vacuumizing in device, then from tracheae 2, auxiliary gas entry and working gas entrance, pass into the hydrogen of a period of time simultaneously and realize gas displacement; Then by detonation, test and guarantee that device is inner for hydrogen atmosphere, to avoid raw material molybdenum powder to contact with air;
2) through working gas entrance 12 and auxiliary gas entry 14, in heating cylindrical shell 15, send into working gas and assist gas, the flow of working gas is 6～9m
3/ h, the flow of assist gas is 2～3m
3/ h; Working gas and assist gas all adopt hydrogen;
3) open electrical system and make induction coil energising, in the inner gradient temperature field 8 that forms of heating cylindrical shell 15, the high-tension electricity loading on induction coil is 6kV～9kV, and electrical system input power is 20～100kW; The temperature of above-mentioned gradient temperature field is 1500～2000 ℃;
4) to one-level powder collecting tank 7, pass into recirculated water, to packing auger 3, add molybdenum oxide powder simultaneously, open the first motor 5 and drive packing auger 3 operations, the particle diameter of the molybdenum oxide powder adding is 50～200 μ m, and it is 1.0～3kg/h that molybdenum oxide powder adds speed to control; From tracheae 2, pass into powder and carry gas 30, powder carries gas 30 and adopts hydrogen, and its flow is 0.3～1.5m
3/ h; Powder carries gas 30 for carrying the sheet exported by packing auger 3 and the molybdenum oxide powder of irregular polyhedrons, successively through powder uniforming device 1, powder feeding flue 11, is transported to the gradient temperature field 8 in heating cylindrical shell 15;
Molybdenum oxide powder is under the effect of gradient temperature field 8, moment cracking, gasification are superfine powder, and be molybdenum powder particle by hydrogen reducing, molybdenum powder particle continues to shrink under 8 effects of gradient temperature field, and through one-level powder collecting tank 7, obtain rapid condensation nodularization and obtain spherical molybdenum micro mist or Ultramicro-powder, its particle size range is 0.1～100 μ m, wherein, the spherical molybdenum powder of large-size completes collection at one-level powder collecting tank 7, and more tiny molybdenum powder particle arrives in secondary powder collecting tank 19 and is collected with air-flow.
5) while preparing task amount and complete, first close the first motor 5 to stop carrying oxidation molybdenum powder, then close the electrical system being connected with the induction coil that heats cylindrical shell 15, final cutting powder carries the supply of gas 30, assist gas 9 and working gas 10.
Be below several embodiments of the present invention, it should be noted that, these embodiment are only used to the present invention more clearly to describe, and scope of the present invention is not limited to following examples.
Embodiment 1:
The particle mean size 50 μ m of raw material oxidation molybdenum powder, carry out spheroidising, and technique is as follows: working gas, assist gas, powder carry gas and be hydrogen, and their flow is followed successively by 6m
3/ h, 2m
3/ h, 0.3m
3/ h, powder feed rate 1.0kg/h; Cartridge heater temperature is 1500 ℃, the nodularization input power 20kW of device.Final products obtained therefrom molybdenum powder nodularization rate is 98%, and the molybdenum powder particle size range of collecting in one-level powder collecting tank is 20～35 μ m, and the molybdenum powder particle size range of collecting in secondary powder collecting tank is 0.1～20 μ m.By ASTMB212-99 standard, raw material molybdenum oxide, spherical molybdenum powder are detected, apparent density is from 1.0g/cm
3bring up to 3.9g/cm
3, flow velocity rises to 21s/50g from 50s/50g.
Embodiment 2:
Raw material molybdenum oxide particle mean size 79 μ m, carry out spheroidising, and technique is as follows: working gas, assist gas, powder carry gas and be hydrogen, and their flow is followed successively by 7.5m
3/ h, 2.3m
3/ h, 0.5m
3/ h, powder feed rate 1.5kg/h; Cartridge heater temperature is 1750 ℃, the nodularization power output 50kW of device.Final products obtained therefrom molybdenum powder nodularization rate is 91%, and the molybdenum powder particle size range of collecting in one-level powder collecting tank is 25～50 μ m, and the molybdenum powder particle size range of collecting in secondary powder collecting tank is 0.1～25 μ m.By ASTMB212-99 standard, raw material molybdenum oxide, spherical molybdenum powder are detected, apparent density is from 1.08g/cm
3bring up to 4.2g/cm
3, flow velocity rises to 19s/50g from 46s/50g.
Embodiment 3:
Raw material molybdenum oxide particle mean size 100 μ m, carry out spheroidising, and technique is as follows: working gas, assist gas, powder carry gas and be hydrogen, and their flow is followed successively by 8m
3/ h, 2.5m
3/ h, 0.8m
3/ h, powder feed rate 2kg/h; Cartridge heater temperature is 1850 ℃, the nodularization power output 50kW of device.Final products obtained therefrom molybdenum powder nodularization rate is 93%, and the molybdenum powder particle size range of collecting in one-level powder collecting tank is 25～50 μ m, and the molybdenum powder particle size range of collecting in secondary powder collecting tank is 0.1～25 μ m.By ASTMB212-99 standard, raw material molybdenum oxide, spherical molybdenum powder are detected, apparent density is from 1.1g/cm
3bring up to 5.1g/cm
3, flow velocity rises to 16s/50g from 41s/50g.
Embodiment 4:
Raw material molybdenum oxide particle mean size 156 μ m, carry out spheroidising, and technique is as follows: working gas, assist gas, powder carry gas and be hydrogen, and their flow is followed successively by 8.5m
3/ h, 2.8m
3/ h, 1.2m
3/ h, powder feed rate 2.5kg/h; Cartridge heater temperature is 1950 ℃, the nodularization input power 85kW of device.Final products obtained therefrom molybdenum powder nodularization rate is 93%, and the molybdenum powder particle size range of collecting in one-level powder collecting tank is 25～100 μ m, and the molybdenum powder particle size range of collecting in secondary powder collecting tank is 0.1～25 μ m.By ASTMB212-99 standard, raw material molybdenum oxide, spherical molybdenum powder are detected, apparent density is from 0.9g/cm
3bring up to 4.5g/cm
3, flow velocity rises to 18s/50g from 45s/50g.
Embodiment 5:
Raw material molybdenum oxide particle mean size 200 μ m, carry out spheroidising, and technique is as follows: working gas, assist gas, powder carry gas and be hydrogen, and their flow is followed successively by 9m
3/ h, 3m
3/ h, 1.5m
3/ h, powder feed rate 3kg/h; Cartridge heater temperature is 2000 ℃, the nodularization input power 100kW of device.Final products obtained therefrom molybdenum powder nodularization rate is 95%, and the molybdenum powder particle size range of collecting in one-level powder collecting tank is 25～120 μ m, and the molybdenum powder particle size range of collecting in secondary powder collecting tank is 0.1～25 μ m.By ASTMB212-99 standard, raw material molybdenum oxide, spherical molybdenum powder are detected, apparent density is from 0.8g/cm
3bring up to 3.5g/cm
3, flow velocity rises to 24s/50g from 52s/50g.
Fig. 2 is raw material molybdenum oxide electromicroscopic photograph, and as can be seen from the figure, raw material molybdenum oxide is irregular particle agglomeration block, rough surface.Fig. 3 is the molybdenum powder obtaining after spheroidising, and as can be seen from the figure molybdenum powder is all able to nodularization, because absorb heat in temperature field inconsistent, the spherical molybdenum powder particle of gained density is difference to some extent.
Claims (10)
1. a method of preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder, is characterized in that, specifically comprises the steps:
1) preparation facilities is carried out to gas displacement, original gas in it is discharged completely;
2) through working gas entrance (12) and auxiliary gas entry (14), in heating cylindrical shell (15), send into working gas (10) and assist gas (9); Working gas (10) and assist gas (9) all adopt hydrogen;
3) open electrical system and make to heat the induction coil energising on cylindrical shell (15), in the inner gradient temperature field (8) that forms of heating cylindrical shell (15);
4) to one-level powder collecting tank (7), pass into recirculated water, to packing auger (3), add molybdenum oxide powder, open the first motor (5) and drive packing auger (3) operation simultaneously; From tracheae (2), pass into powder and carry gas (30), powder carries gas (30) and adopts hydrogen; Powder carries gas (30) and carries the molybdenum oxide powder by packing auger (3) output, successively through powder uniforming device (1) and powder feeding flue (11), be transported in heating cylindrical shell (15), molybdenum oxide powder, in heating cylindrical shell (15) reaction, obtains spherical molybdenum micro mist or Ultramicro-powder and is collected successively by one-level powder collecting tank (7) and secondary powder collecting tank (19);
5) while preparing task amount and complete, first close the first motor (5) to stop carrying oxidation molybdenum powder, then close the electrical system being connected with the induction coil that heats cylindrical shell (15), final cutting powder carries the supply of gas, assist gas and working gas.
2. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 1, it is characterized in that, described step 1) concrete operations: utilize aspiration pump (20) to make to form negative pressure in it by vacuumizing in preparation facilities, then pass into hydrogen from tracheae (2), auxiliary gas entry (14) and working gas entrance (12) simultaneously and realize gas displacement.
3. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 1, is characterized in that, described step 2) in, the flow of described working gas (10) is 6～9m
3/ h; The flow of described assist gas (9) is 2～3m
3/ h.
4. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 1, is characterized in that, described step 3) in, the high-tension electricity loading on described induction coil is 6kV～9kV, electrical system input power is 20～100kW.
5. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 1, is characterized in that, described step 4) in, the particle diameter of described molybdenum oxide powder is 50～200 μ m, it is 1.0～3kg/h that molybdenum oxide powder adds speed.
6. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 1, is characterized in that, described step 4) in, it is 0.3～1.5m that described powder carries gas (30) flow
3/ h.
7. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 1, is characterized in that, described step 4) in, described in the spherical molybdenum micro mist that obtains or the particle size range of Ultramicro-powder be 0.1～100 μ m.
8. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 1, it is characterized in that, described preparation facilities comprises powder uniforming device (1), tracheae (2), packing auger (3), feed bin (4), the first motor (5), one-level powder collecting tank (7), powder feeding flue (11), insulated end cover (13), heating cylindrical shell (15), cartridge heater body support frame (16), secondary powder collecting tank (19), aspiration pump (20) and the second motor (22), wherein:
Described the first motor (5) connects packing auger (3) provides driving force for it; Feed bin (4) connects the feed end of packing auger (3), and packing auger (3) connects heating cylindrical shell (15) by powder feeding flue (11); Between described packing auger (3) and powder feeding flue (11), powder uniforming device (1) is installed, this powder uniforming device (1) is with two tracheaes (2); Powder uniforming device (1) adopts a caliber than the large cylinder of powder feeding pipe caliber of packing auger (3);
On the outer wall of described heating cylindrical shell (15), uniform winding has the induction coil being connected with electrical system; The upper end of heating cylindrical shell (15) is removably provided with insulated end cover (13); The middle part that described powder feeding flue (11) enters insulated end cover (13) and extends to heating cylindrical shell (15) enters the top of gradient temperature field (8); The outside suit of heating cylindrical shell (15) cartridge heater body support frame (16), and be arranged on one-level tank powder collection (7) top by cartridge heater body support frame (16); Heating cylindrical shell (15) lower end is communicated with one-level powder collecting tank (7);
The outlet of one-level powder collecting tank (7) is connected with the entrance of secondary powder collecting tank (19) by tube connector (18), and tube connector (18) is along the powder direction of motion certain angle that is inclined upwardly; The exit of secondary powder collecting tank (19) is provided with Waste gas outlet (21), and this outlet connects with the second motor (aspiration pump of 22 (20).
9. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 8, is characterized in that, described insulated end cover (13) comprises upper cover (24) and lower cover (25) two parts; Wherein, described upper cover (24) is circular and there is discoid projection (26) at its middle part, and the bottom of projection (26) is cylindrical cavity, and the center of projection (26) is provided with central through hole (27); Described lower cover (25) is a disk with mesopore, and lower cover (25) below is provided with a cylinder (29); This cylinder (29) internal diameter with the internal diameter of lower cover (25), the internal diameter of upper cover (24) is all identical; Upper cover (24) forms a working gas transport tube between the two after fastening with lower cover (25); On the sustained height of the sidewall of upper cover (24), be arranged with two working gas entrances (12), by these two working gas entrances, (12 is starting point, along the inwall of above-mentioned working gas transport tube, is provided with two helical grooves that parallel as working gas transfer passage (28); On the sustained height of the sidewall of lower cover (25) the latter half, be arranged with two auxiliary gas entries (14); The central spot of the lower end of described cylinder (29) and heating cylindrical shell (15) is in sustained height; Between the outer wall of cylinder (29) and heating cylindrical shell (15) inwall, form a toroidal cavity; This toroidal cavity can make the assist gas (9) that is entered heating cylindrical shell (15) by auxiliary gas entry (14) form gas curtain on heating cylindrical shell (15) inwall, in case metal powder sticks on the inwall of heating cylindrical shell (15).
10. the method for preparing metal molybdenum ball-shaped micro powder or Ultramicro-powder as claimed in claim 8, it is characterized in that, described one-level powder collecting tank (7) is a cylinder, its sidewall is double-layer stainless steel structure, between this double-decker, form the cavity of even thickness, this cavity is connected with cooling water inlet (6) on the sidewall of one-level powder collecting tank (7) lower end and the coolant outlet (17) of its opposite side wall upper end, and this cavity is used for passing into recirculated water to the high temperature powder rapid condensation nodularization in one-level powder collecting tank (7).
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