CN104057095A - Production line for low-oxygen-content hard alloy mixture and production technology thereof - Google Patents

Production line for low-oxygen-content hard alloy mixture and production technology thereof Download PDF

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CN104057095A
CN104057095A CN201410291084.9A CN201410291084A CN104057095A CN 104057095 A CN104057095 A CN 104057095A CN 201410291084 A CN201410291084 A CN 201410291084A CN 104057095 A CN104057095 A CN 104057095A
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transition chamber
chamber
glove box
reduction
transition
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CN104057095B (en
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林涛
王志
张深根
邵慧萍
何新波
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The invention relates to a production line for low-oxygen-content hard alloy mixture. The production line is a sealed system formed by a reduction part used for preparing blue tungsten powder, a reduction part used for preparing tungsten powder, a carbonization part and a pelletizing part. According to the production line disclosed by the invention, nanometer tungsten trioxide is still in the sealed production line from the rotary reduction furnace inlet of a starting end to the spraying drying tower of a tail end; the sealed production line is filled with nitrogen or hydrogen, so that nanometer powder is prevented from contacting with external air all the time so as to reduce the size of nanometer WC (wolfram carbide) particles and prevent nanometer WC from being oxidized and auto-ignited; the oxygen content of the hard alloy mixture is lowered; the stability and the controllability of the ultra-fine grain hard alloy quality are improved; the combination property of the alloy is improved.

Description

A kind of production line of low oxygen content carbide alloy mixture and production technology thereof
invention field
The present invention relates to a kind of production line and production technology thereof of low oxygen content nanometer tungsten carbide compound, belong to powder metallurgic method and prepare carbide alloy field.
background of invention
Carbide alloy is to take WC as hard phase, and the Co of take forms through high-temperature liquid-phase sintering as Binder Phase.Carbide alloy has high rigidity, high strength and high wearability, and its appearance makes machining produce revolutionary progress, is described as " tooth of industry ".
Modern industry requires more and more higher to the combination property of hard alloy cutter, tool and mould, wear-resisting spare part, be mainly reflected in: 1) all-round popularization of high-efficiency high-accuracy Digit Control Machine Tool is had higher requirement to cutter life and stock-removing efficiency; 2) machined material performance improves day by day, and traditional hard alloy cutter can not meet the demands; 3) the complicated hard alloy wear resistance parts that need of working condition possess higher intensity hardness combination property.Can say, high-performance rigid material product plays important supporting role to the progress of modern industry, and the progress of modern industry also impels hard alloy cutter towards high efficiency, high accuracy, high reliability, high life future development, ultrafine gain size is exactly to be born in such environment.Ultrafine gain size refers to that WC grain degree is less than the carbide alloy of 0.5 μ m, along with WC grain size reduction, the performances such as the intensity of carbide alloy, hardness increase substantially, the research and development of high-performance superfine crystal grain carbide alloy and goods and to apply be Cemented Carbide Industry development trend in the world always.
The appearance of nanometer technology, has greatly promoted the development of carbide alloy, can produce the carbide alloy that WC grain size reaches 0.2-0.3 μ m at present, and its combination property is improved significantly.This carbide alloy is to use nano level WC powder preparation.At present, the method for preparing nano WC powder has multiple, such as spraying transformation approach, sol-gal process, in-situ carburization method, high-energy ball milling method etc.Majority method is by obtaining nano tungsten trioxide powder, and then becomes the blue tungsten of nanometer and tungsten powder through reduction, then carbonization obtains nano WC powder.Because the activity of nanometer grade powder is high, in preparation process, contact as easy as rolling off a log oxidation, even spontaneous combustion with air.Cause the oxygen content of final WC high, quality is unstable.When for the preparation of carbide alloy, mixed carbon comtent is wayward, causes occurring in final alloy graphite-phase or poor carbon phase, the hydraulic performance decline of carbide alloy.
summary of the invention
The invention provides a kind of production line of low oxygen content nano tungsten carbide compound, for overcoming above the deficiencies in the prior art part.
Technical scheme of the present invention is: a kind of production line of low oxygen content carbide alloy mixture, and this production line forms a closed system by the reduction part for the preparation of blue tungsten powder, the reduction part of preparing tungsten powder, carbonization part and the part of granulating;
Wherein, described blue tungsten powder reduction part comprises First Transition chamber, rotary reduction furnace, the second transition chamber, the first glove box, the first closed vat, the 3rd transition chamber and the first ball mill; Described First Transition chamber, rotary reduction furnace, the second transition chamber, the first glove box and the 3rd transition chamber are from left to right tightly connected successively, described the first closed vat is tightly connected by the first connection chamber and described the first glove box, and the first ball mill is provided with the second connection chamber;
Described tungsten powder reduction part comprises the 4th transition chamber, the second glove box, the 5th transition chamber, reduction furnace, the second closed vat, the 3rd glove box, the 6th transition chamber, the 7th transition chamber and the second ball mill; Described the 4th transition chamber, the second glove box, the 5th transition chamber, reduction furnace, the 6th transition chamber, the 3rd glove box and the 7th transition chamber are from left to right tightly connected successively, described the second glove box is provided with the 3rd connection chamber, described the second closed vat is tightly connected by the 4th connection chamber and described the 3rd glove box, and described the second ball mill is provided with the 5th connection chamber;
Described carbonization partly comprises the 4th glove box, the 8th transition chamber, the 9th transition chamber, carbon shirt-circuiting furnace, the 3rd closed vat, the 5th glove box, the tenth transition chamber and the 11 transition chamber; Described the 8th transition chamber, the 4th glove box, the 9th transition chamber, carbon shirt-circuiting furnace, the tenth transition chamber, the 5th glove box and the 11 transition chamber are from left to right tightly connected successively, described the 4th glove box is provided with the 6th connection chamber, and described the 3rd closed vat is tightly connected by the 7th connection chamber and described the 5th glove box;
Described granulation part comprises the 3rd ball mill, the 4th closed vat, spray drying tower and the 5th closed vat, described the 3rd ball mill is provided with the 8th connection chamber, described the 4th closed vat is tightly connected by the feed end of the 9th connection chamber and described spray drying tower, and the discharge end that described the 5th closed vat is crossed the tenth connection chamber and described spray drying tower is tightly connected.
Further, the structure of described First Transition chamber, the second transition chamber, the 3rd transition chamber, the 4th transition chamber, the 5th transition chamber, the 6th transition chamber, the 7th transition chamber, the 8th transition chamber, the 9th transition chamber, the tenth transition chamber and the 11 transition chamber is all identical, the front end of transition chamber is provided with front flashboard, the rear end of transition chamber is provided with rear flashboard, and transition chamber also comprises the gas outlet near the air inlet of front end and close rear end; Described the first connection chamber, the second connection chamber, the 3rd connection chamber, the 4th connection chamber, the 5th connection chamber, the 6th connection chamber, the 7th connection chamber, the 8th connection chamber, the 9th connection chamber, the tenth structure of connection chamber are identical with the structure of above-mentioned transition chamber.
Another object of the present invention is to provide the production technology of the production line of above-mentioned low oxygen content carbide alloy mixture, and concrete steps are as follows:
First, open the front flashboard of First Transition chamber, pack the reduction boat that tungstic acid is housed into First Transition indoor, close front flashboard, then by air inlet to the indoor nitrogen that is filled with of described First Transition, nitrogen is flowed out by gas outlet; After 2-3 minute, open rear flashboard, reduction boat is pushed in rotary reduction furnace, in rotary reduction furnace, pass into hydrogen, for tungstic acid is reduced into blue tungsten oxide, the blue tungsten having reduced is placed in the first glove box by the second transition chamber, is filled with nitrogen protection simultaneously, and the blue tungsten oxide that reduction is obtained packs in the first closed vat by the first connection chamber, the first closed vat is also filled with nitrogen protection, and the boat that will reduce takes out through the 3rd transition chamber; The first closed vat that blue tungsten is housed is installed on the second connection chamber of the first ball mill, blue tungsten is packed in the first ball mill, be filled with nitrogen protection simultaneously and carry out ball milling, the blue tungsten powder of nanometer after ball milling refills in the first closed vat through the second connection chamber, standby;
Then, reduction boat packs in the second glove box through the 4th transition chamber, the blue tungsten powder of the nanometer that in the first closed vat, ball milling is crossed is installed in reduction boat through the 3rd connection chamber, by the 5th transition chamber, push reduction furnace and carry out reduction reaction, to passing into hydrogen in reduction furnace, play reduction and protective effect, the reduction boat that nano-tungsten powder after reduction is housed is entered in the 3rd glove box of nitrogen protection through the 6th transition chamber, through the 7th transition chamber, pack the required carbon black of carbonization nano-tungsten powder into the 3rd glove box simultaneously, in the 3rd glove box, required carbon black and the nano-tungsten powder of carbonization nano-tungsten powder packed in the second closed vat through the 4th connection chamber, reduction boat takes out by the 7th transition chamber, the second closed vat that nano-tungsten powder and carbon black are housed is installed on the 5th connection chamber and through the 5th connection chamber and packs the second ball mill into, be filled with nitrogen protection simultaneously and carry out ball milling, after ball milling is even, through the 5th connection chamber, under nitrogen protection, pack the second closed vat into again,
Secondly, the second closed vat that nano-tungsten powder and carbon black are housed is installed on the 4th glove box through the 6th connection chamber, carbonization boat is put into the 4th glove box that protective atmosphere is nitrogen by the 8th transition chamber, tungsten powder and carbon black compound are installed to carbonization boat, by the 9th transition chamber, enter carbon shirt-circuiting furnace, carbonization under hydrogen shield becomes tungsten carbide to tungsten powder with carbon black, then via the tenth transition chamber, enter in the 5th glove box that protective atmosphere is nitrogen, cobalt powder after weighing according to the ratio in carbide alloy composition is put into the 5th glove box that protective atmosphere is nitrogen by the 11 transition chamber, nanometer tungsten carbide and cobalt powder are poured in the 3rd closed vat that protective atmosphere is nitrogen through the 7th connection chamber, carbonization boat takes out by the 11 transition chamber,
Finally, in the 3rd ball mill, add appropriate alcohol and paraffin, pass into nitrogen protection, the 3rd closed vat that tungsten carbide and cobalt powder are housed is contained on the 8th connection chamber of the 3rd ball mill, tungsten carbide and cobalt powder are packed in the 3rd ball mill that protective atmosphere is nitrogen through the 8th connection chamber, carry out ball milling, the evenly rear slip of ball milling is put into the 4th closed vat, the 4th closed vat that mixed slurry is housed is installed on the 9th connection chamber of spray drying tower, slip is put into spray drying tower, pass into nitrogen, utilize nitrogen atomization and be dried to thicker carbide alloy mixture particle, after dry, the carbide alloy mixture that this granulation is processed packs in the 5th closed vat that protective atmosphere is nitrogen through the tenth connection chamber, the 6th closed vat that compound is housed can directly be delivered to suppression process and be configured as required cemented carbide parts, or delivering to transfer house preserves.
Production line of the present invention can make nano tungsten trioxide from the rotary reduction furnace entrance of initiating terminal, until the outlet of the spray drying tower of end, all in the production line in described sealing.In described sealing production line, be filled with nitrogen or hydrogen, make nanometer powder can not contact outside air all the time, thereby avoided being oxidized in nanometer powder preparation process, by the Control for Oxygen Content of nano hard alloy compound at minimum level.Thereby easily control the carbon content of final alloy and the performance of alloy, improve stability and the controllability of ultra-fine cemented carbide quality.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of nano hard alloy compound production line of the present invention;
Fig. 2 is transition chamber structural representation.
The specific embodiment
WC grain size is less than the carbide alloy of 0.2 micron and has very high intensity and toughness.Due to growing up of WC in sintering process, so the granularity of WC powder need to be less than 100 nanometers.First this just need to obtain nano level WO by nanometer technology 3.Then through reduction and carbonization, obtain nano level WC.
Nanoscale WC activity is very high, can spontaneous combustion in air.If not spontaneous combustion, its oxygen content is high.The performance of this control for carbon content and final alloy has a significant impact.
By nanometer WO 3be prepared into nanometer WC, need through reduction and carbonation stage, these two hot stages all can make nano particle grow up.In order to suppress to grow up, first by nanometer WO 3be reduced into the blue tungsten of nanometer, restore into nano-tungsten powder, then join carbon, last carbonization obtains nanometer tungsten carbide.Next be to prepare carbide alloy mixture, by nanometer tungsten carbide, cobalt powder, binder paraffin and solvent alcohol ball milling, spray-dried granulation obtains the compound for being shaped.Follow-up by being shaped and sintering obtains ultra-fine cemented carbide.
Below in conjunction with accompanying drawing, describe production line of the present invention in detail.Fig. 1 is the schematic diagram of nano hard alloy compound production line of the present invention.
As shown in Figure 1-2, this law is invented a kind of production line of low oxygen content carbide alloy mixture, and this production line forms a closed system by the reduction part for the preparation of blue tungsten powder, the reduction part of preparing tungsten powder, carbonization part and the part of granulating;
Wherein, described blue tungsten powder reduction part comprises First Transition chamber 1, rotary reduction furnace 2, the second transition chamber 3, the first glove box 4, the first closed vat 6, the 3rd transition chamber 5 and the first ball mill 7; Described First Transition chamber 1, rotary reduction furnace 2, the second transition chamber 3, the first glove box 4 and the 3rd transition chamber 5 are from left to right tightly connected successively, described the first closed vat 6 is tightly connected with described the first glove box 4 by the first connection chamber 7, and the first ball mill 8 is provided with the second connection chamber 36;
Described tungsten powder reduction part comprises the 4th transition chamber 9, the second glove box 10, the 5th transition chamber 11, reduction furnace 12, the 6th transition chamber 15, the second closed vat 13, the 3rd glove box 14, the 7th transition chamber 19 and the second ball mill 16; Described the 4th transition chamber 9, the second glove box 10, the 5th transition chamber 11, reduction furnace 12, the 6th transition chamber 15, the 3rd glove box 14 and the 7th transition chamber 19 are from left to right tightly connected successively, described the second glove box 10 is provided with the 3rd connection chamber 17, described the second closed vat 13 is tightly connected with described the 3rd glove box 14 by the 4th connection chamber 18, and described the second ball mill 16 is provided with the 5th connection chamber 38;
Described carbonization partly comprises the 4th glove box 20, the 8th transition chamber 21, carbon shirt-circuiting furnace 22, the 3rd closed vat 23, the 5th glove box 24, the 9th transition chamber 26, the tenth transition chamber 37 and the 11 transition chamber 25; Described the 8th transition chamber 21, the 4th glove box 20, the 9th transition chamber 26, carbon shirt-circuiting furnace 22, the tenth transition chamber 37, the 5th glove box 24 and the 11 transition chamber 25 are from left to right tightly connected successively, described the 4th glove box 20 is provided with the 6th connection chamber 27, and described the 3rd closed vat 23 is tightly connected with described the 5th glove box 24 by the 7th connection chamber 28;
Described granulation part comprises the 3rd ball mill 29, the 4th closed vat 30, spray drying tower 31 and the 5th closed vat 32, described the 3rd ball mill 29 is provided with the 8th connection chamber 33, described the 4th closed vat 30 is tightly connected by the 9th connection chamber 34 and the feed end of described spray drying tower 31, and described the 5th closed vat 32 is tightly connected by the tenth connection chamber 35 and the discharge end of described spray drying tower 31.
Wherein, the structure of described First Transition chamber 1, the second transition chamber 3, the 3rd transition chamber 5, the 4th transition chamber 8, the 5th transition chamber 10, the 6th transition chamber 15, the 7th transition chamber 19, the 8th transition chamber 21, the 9th transition chamber 26, the tenth transition chamber 37 and the 11 transition chamber 25 is all identical, the front end of transition chamber is provided with front flashboard 101, the rear end of transition chamber is provided with rear flashboard 102, and transition chamber also comprises the gas outlet 104 near the air inlet 103 of front end and close rear end; The structure of the first to the tenth connection chamber 7,26,17,18,38,27,28,33,34,35 is identical with the structure of described transition chamber.
Another object of the present invention is the production technology of the production line of above-mentioned low oxygen content carbide alloy mixture, and concrete steps are as follows:
First, open the front flashboard 101 of First Transition chamber 1, pack reduction boat into First Transition chamber 1, close front flashboard 101.Then by entrance 103, be filled with nitrogen, nitrogen is by exporting 104 outflows.After 2-3 minute, open rear flashboard 102, by boat pushing mechanism, reduction boat is pushed to the pipeline of blue tungsten reduction furnace 2.In blue tungsten reduction furnace 2, pass into hydrogen, tungstic acid is reduced into blue tungsten oxide, the blue tungsten having reduced is placed in the first glove box 4 by the second transition chamber 3, simultaneously, be filled with nitrogen protection, the blue tungsten oxide that reduction is obtained packs in the first closed vat 6 by the first connection chamber 7, the first closed vat 6 is also filled with nitrogen protection, and the front flashboard by reduction boat through the 3rd transition chamber 5 takes out; The first closed vat 6 that blue tungsten is housed is installed on the second connection chamber 37 of the first ball mill 8, blue tungsten is packed in the first ball mill 8, be filled with nitrogen protection simultaneously, through row ball milling, nano-tungsten powder after ball milling refills in the first closed vat 6 through the second connection chamber 7 equally, standby;
Then, reduction boat packs in the second glove box 10 through the 4th transition chamber 9, the nano-tungsten powder that in the first closed vat 6, ball milling is crossed is installed in reduction boat through the 3rd connection chamber 17, by the 5th transition chamber 11, push reduction furnace 12 and carry out reduction reaction, to passing into hydrogen in reduction furnace 12, play reduction and protective effect, after reaction, reduction boat is entered in the 3rd glove box 14 of nitrogen protection through the 6th transition chamber 15, through the 7th transition chamber 19, pack the required carbon black of carbonization nano-tungsten powder into the 3rd glove box 14 simultaneously, in the 3rd glove box 14, required carbon black and the nano-tungsten powder of carbonization nano-tungsten powder packed in the second closed vat 13 through the 4th connection chamber 18, reduction boat takes out by the rear flashboard of the 7th transition chamber 19, the second closed vat 12 that nano-tungsten powder and carbon black are housed is installed on the 5th connection chamber 38 and through the 5th connection chamber 38 and packs the second ball mill 16 into, be filled with nitrogen protection simultaneously, through row ball milling, after ball milling is even, through the 5th connection chamber 39, under nitrogen protection, pack the second closed vat 13 into again,
First nano tungsten trioxide is reduced into the blue tungsten of nanometer, then after ball milling, is reduced into nano-tungsten powder, can suppress growing up of nano particle.
Secondly, the second closed vat 13 that nano-tungsten powder and carbon black are housed is installed on the 4th glove box 20 through the 4th connection chamber 27, carbonization boat is put into the 4th glove box 20 that protective atmosphere is nitrogen by the 8th transition chamber 21, tungsten powder and carbon black compound are installed to carbonization boat, by the 9th transition chamber 26, enter carbon shirt-circuiting furnace 22, carbonization under hydrogen shield becomes tungsten carbide to tungsten powder with carbon black, then via the tenth transition chamber 37, enter in the 5th glove box 24 that protective atmosphere is nitrogen, cobalt powder after weighing according to the ratio in carbide alloy composition is put into the 5th glove box 24 that protective atmosphere is nitrogen by the 11 transition chamber 25, nanometer tungsten carbide and cobalt powder are poured in the 3rd closed vat 23 that protective atmosphere is nitrogen through the 5th connection chamber 28, carbonization boat takes out by the 11 transition chamber 27,
Finally, in the 3rd ball mill 29, add appropriate alcohol and paraffin, pass into nitrogen protection, the 3rd closed vat 23 that tungsten carbide and cobalt powder are housed is contained on the 6th connection chamber 33 of the 3rd ball mill 29, tungsten carbide and cobalt powder are packed in the 3rd ball mill 29 that protective atmosphere is nitrogen through the 6th connection chamber 33, carry out ball milling, the evenly rear slip of ball milling is put into the 5th closed vat 30, the 5th closed vat 30 that mixed slurry is housed is installed on the 7th connection chamber 34 of spray drying tower 31, slip is put into spray drying tower 31, pass into nitrogen, utilize nitrogen atomization and be dried to thicker carbide alloy mixture particle, after dry, the carbide alloy mixture that this granulation is processed packs in the 6th closed vat 32 that protective atmosphere is nitrogen through the 8th connection chamber 35, the 6th closed vat 32 that compound is housed can directly be delivered to suppression process and be configured as required cemented carbide parts, or delivering to transfer house preserves.
In use, can in air, open the 6th closed vat 32 that compound is housed, the nano hard alloy compound after granulation, can be not oxidized owing to there being paraffin parcel.The compacting of follow-up process again and sintering obtain ultra-fine cemented carbide goods.
Transition chamber and connection chamber are for forming an isolation ward at production line, and its effect is that glove box, blue tungsten reduction furnace, tungsten powder reducing furnace, ball mill, carbon shirt-circuiting furnace and spray drying tower are kept apart, or they and outside air are isolated.On the one hand the hydrogen in blue tungsten reduction furnace, tungsten powder reducing furnace and carbon shirt-circuiting furnace is kept apart, guarantee safety.While making material or other operation tool pass in and out whole closed system by it on the other hand, prevent that outside air from entering.
Production line of the present invention can make nano tungsten trioxide from the blue tungsten reduction furnace entrance of initiating terminal, until the outlet of the spray drying tower of end, all in the production line in described sealing.In described sealing production line, be filled with nitrogen or hydrogen, make nanometer powder can not contact outside air all the time, thereby avoided in nanometer powder preparation process oxidation and spontaneous combustion, can be by the Control for Oxygen Content of nano hard alloy compound at minimum level in refinement tungsten carbide particle as far as possible.Thereby easily control the carbon content of final alloy, improve stability and the controllability of ultra-fine cemented carbide quality, and can reduce to greatest extent the WC particle size of carbide alloy, improve the combination property of carbide alloy.

Claims (3)

1. a production line for low oxygen content carbide alloy mixture, is characterized in that, this production line forms a closed system by the reduction part for the preparation of blue tungsten powder, the reduction part of preparing tungsten powder, carbonization part and the part of granulating;
Wherein, described blue tungsten powder reduction part comprises First Transition chamber (1), rotary reduction furnace (2), the second transition chamber (3), the first glove box (4), the first closed vat (6), the 3rd transition chamber (5) and the first ball mill (7); Described First Transition chamber (1), rotary reduction furnace (2), the second transition chamber (3), the first glove box (4) and the 3rd transition chamber (5) are from left to right tightly connected successively, described the first closed vat (6) is tightly connected by the first connection chamber (7) and described the first glove box (4), and the first ball mill (8) is provided with the second connection chamber (36);
Described tungsten powder reduction part comprises the 4th transition chamber (9), the second glove box (10), the 5th transition chamber (11), reduction furnace (12), the 6th transition chamber (15), the second closed vat (13), the 3rd glove box (14), the 7th transition chamber (19) and the second ball mill (16); Described the 4th transition chamber (9), the second glove box (10), the 5th transition chamber (11), reduction furnace (12), the 6th transition chamber (15), the 3rd glove box (14) and the 7th transition chamber (19) are from left to right tightly connected successively, described the second glove box (10) is provided with the 3rd connection chamber (17), described the second closed vat (13) is tightly connected by the 4th connection chamber (18) and described the 3rd glove box (14), and described the second ball mill (16) is provided with the 5th connection chamber (38);
Described carbonization partly comprises the 4th glove box (20), the 8th transition chamber (21), carbon shirt-circuiting furnace (22), the 3rd closed vat (23), the 5th glove box (24), the 4th closed vat (25) and the 9th transition chamber (26), the tenth transition chamber (37) and the 11 transition chamber (25); Described the 8th transition chamber (21), the 4th glove box (20), the 9th transition chamber (26), carbon shirt-circuiting furnace (22), the tenth transition chamber (37), the 5th glove box (24) and the 11 transition chamber (25) are from left to right tightly connected successively, described the 4th glove box (20) is provided with the 6th connection chamber (27), and described the 3rd closed vat (23) is tightly connected by the 7th connection chamber (28) and described the 5th glove box (24);
Described granulation part comprises the 3rd ball mill (29), the 4th closed vat (30), spray drying tower (31) and the 5th closed vat (32), described the 3rd ball mill (29) is provided with the 8th connection chamber (33), described the 4th closed vat (30) is tightly connected by the 9th connection chamber (34) and the feed end of described spray drying tower (31), and described the 5th closed vat (32) is tightly connected by the tenth connection chamber (35) and the discharge end of described spray drying tower (31).
2. production line according to claim 1, it is characterized in that, described First Transition chamber (1), the second transition chamber (3), the 3rd transition chamber (5), the 4th transition chamber (8), the 5th transition chamber (10), the 6th transition chamber (15), the 7th transition chamber (19), the 8th transition chamber (21), the 9th transition chamber (26), the structure of the tenth transition chamber (37) and the 11 transition chamber (25) is all identical, the front end of transition chamber is provided with front flashboard (101), the rear end of transition chamber is provided with rear flashboard (102), transition chamber also comprises the gas outlet (104) near the air inlet (103) of front end and close rear end, the structure of the first to the tenth connection chamber (7,26,17,18,38,27,28,33,34,35) is identical with the structure of described transition chamber.
3. a production technology for the production line of low oxygen content carbide alloy mixture as claimed in claim 1 or 2, is characterized in that, concrete steps are as follows:
First, the front flashboard (101) of opening First Transition chamber (1), packs the reduction boat that tungstic acid is housed in First Transition chamber (1) into, closes front flashboard (101), then by air inlet (103), in described First Transition chamber (1), be filled with nitrogen, nitrogen is flowed out by gas outlet (104); After 2-3 minute, open rear flashboard (102), reduction boat is pushed in rotary reduction furnace (2), in rotary reduction furnace (2), pass into hydrogen, for tungstic acid is reduced into blue tungsten oxide, the blue tungsten having reduced is placed in the first glove box (4) by the second transition chamber (3), be filled with nitrogen protection simultaneously, the blue tungsten oxide that reduction is obtained packs in the first closed vat (6) by the first connection chamber (7), the first closed vat (6) is also filled with nitrogen protection, and the boat that will reduce takes out through the 3rd transition chamber (5); The first closed vat (6) that blue tungsten is housed is installed on second connection chamber (37) of the first ball mill (8), blue tungsten is packed in the first ball mill (8), be filled with nitrogen protection simultaneously and carry out ball milling, the blue tungsten powder of nanometer after ball milling refills in the first closed vat (6) through the second connection chamber (37), standby;
Then, reduction boat packs in the second glove box (10) through the 4th transition chamber (9), the blue tungsten powder of nanometer that ball milling in the first closed vat (6) is crossed installs in reduction boat through the 3rd connection chamber (17), by the 5th transition chamber (11), push reduction furnace (12) and carry out reduction reaction, to passing into hydrogen in reduction furnace (12), play reduction and protective effect, the reduction boat that nano-tungsten powder after reduction is housed is entered in the 3rd glove box (14) of nitrogen protection through the 6th transition chamber (15), through the 7th transition chamber (19), pack the required carbon black of carbonization nano-tungsten powder into the 3rd glove box (14) simultaneously, in the 3rd glove box (14), by carbonization nano-tungsten powder, required carbon black and nano-tungsten powder packs in the second closed vat (13) through the 4th connection chamber (18), reduction boat takes out by the 7th transition chamber (19), the second closed vat (13) that nano-tungsten powder and carbon black are housed is installed to the 5th connection chamber (38) above and packs the second ball mill (16) into through the 5th connection chamber (38), be filled with nitrogen protection simultaneously and carry out ball milling, after ball milling is even, through the 5th connection chamber (39), under nitrogen protection, pack the second closed vat (13) into again,
Secondly, the second closed vat (13) that nano-tungsten powder and carbon black are housed is installed on the 4th glove box (20) through the 6th connection chamber (27), carbonization boat is put into the 4th glove box (20) that protective atmosphere is nitrogen by the 8th transition chamber (21), tungsten powder and carbon black compound are installed to carbonization boat, by the 9th transition chamber (26), enter carbon shirt-circuiting furnace (22), carbonization under hydrogen shield becomes tungsten carbide to tungsten powder with carbon black, then via the tenth transition chamber (37), enter in the 5th glove box (24) that protective atmosphere is nitrogen, cobalt powder after weighing according to the ratio in carbide alloy composition is put into the 5th glove box (24) that protective atmosphere is nitrogen by the 11 transition chamber (25), nanometer tungsten carbide and cobalt powder are poured in the 3rd closed vat (23) that protective atmosphere is nitrogen through the 7th connection chamber (28), carbonization boat takes out by the 11 transition chamber (25),
Finally, in the 3rd ball mill (29), add appropriate alcohol and paraffin, pass into nitrogen protection, the 3rd closed vat (23) that tungsten carbide and cobalt powder are housed is contained on the 8th connection chamber (33) of the 3rd ball mill (29), tungsten carbide and cobalt powder are packed in the 3rd ball mill (29) that protective atmosphere is nitrogen through the 8th connection chamber (33), carry out ball milling, the evenly rear slip of ball milling is put into the 4th closed vat (30), the 4th closed vat (30) that mixed slurry is housed is installed on the 9th connection chamber (34) of spray drying tower (31), slip is put into spray drying tower (31), pass into nitrogen, utilize nitrogen atomization and be dried to thicker carbide alloy mixture particle, after dry, the carbide alloy mixture that this granulation is processed packs in the 5th closed vat (32) that protective atmosphere is nitrogen through the tenth connection chamber (35), the 6th closed vat (32) that compound is housed can directly be delivered to suppression process and be configured as required cemented carbide parts, or delivering to transfer house preserves.
CN201410291084.9A 2014-06-25 2014-06-25 A kind of production line of low oxygen content carbide alloy mixture and production technology thereof Expired - Fee Related CN104057095B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105217078A (en) * 2015-11-10 2016-01-06 西安欧中材料科技有限公司 A kind of packaging facilities of oxidizable powder
CN106216696A (en) * 2016-08-31 2016-12-14 有研粉末新材料(北京)有限公司 A kind of titaniferous copper base diamond matrix composite materials prepare pipelining equipment
CN114015954A (en) * 2021-09-08 2022-02-08 先导薄膜材料有限公司 Device and method for reducing oxygen content in aluminum alloy

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1096003A (en) * 1996-07-30 1998-04-14 Toho Titanium Co Ltd Titanium-based powder and its production
CN1328889A (en) * 2001-06-26 2002-01-02 中国科学院长春应用化学研究所 Tungsten aluminium carbide hard alloy nanometer powder preparation method
CN101195901A (en) * 2007-12-06 2008-06-11 上海交通大学 Reaction spray coating metal ceramic composite powder and method for producing the same
CN101352756A (en) * 2008-09-02 2009-01-28 金堆城钼业股份有限公司 Method for preparing molybdenum powder with high-apparent density and low-oxygen content
CN103817335A (en) * 2013-09-12 2014-05-28 厦门钨业股份有限公司 Alloy powder for rare-earth magnet, methods for manufacturing alloy powder and rare-earth magnet and powder manufacturing device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1096003A (en) * 1996-07-30 1998-04-14 Toho Titanium Co Ltd Titanium-based powder and its production
CN1328889A (en) * 2001-06-26 2002-01-02 中国科学院长春应用化学研究所 Tungsten aluminium carbide hard alloy nanometer powder preparation method
CN101195901A (en) * 2007-12-06 2008-06-11 上海交通大学 Reaction spray coating metal ceramic composite powder and method for producing the same
CN101352756A (en) * 2008-09-02 2009-01-28 金堆城钼业股份有限公司 Method for preparing molybdenum powder with high-apparent density and low-oxygen content
CN103817335A (en) * 2013-09-12 2014-05-28 厦门钨业股份有限公司 Alloy powder for rare-earth magnet, methods for manufacturing alloy powder and rare-earth magnet and powder manufacturing device

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105217078A (en) * 2015-11-10 2016-01-06 西安欧中材料科技有限公司 A kind of packaging facilities of oxidizable powder
CN106216696A (en) * 2016-08-31 2016-12-14 有研粉末新材料(北京)有限公司 A kind of titaniferous copper base diamond matrix composite materials prepare pipelining equipment
CN114015954A (en) * 2021-09-08 2022-02-08 先导薄膜材料有限公司 Device and method for reducing oxygen content in aluminum alloy
CN114015954B (en) * 2021-09-08 2022-07-01 先导薄膜材料有限公司 Method for reducing oxygen content in aluminum alloy

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