CN104070172B - A kind of preparation method of spherical chromium powder - Google Patents
A kind of preparation method of spherical chromium powder Download PDFInfo
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- CN104070172B CN104070172B CN201410280629.6A CN201410280629A CN104070172B CN 104070172 B CN104070172 B CN 104070172B CN 201410280629 A CN201410280629 A CN 201410280629A CN 104070172 B CN104070172 B CN 104070172B
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 49
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 46
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052786 argon Inorganic materials 0.000 claims abstract description 23
- 239000011651 chromium Substances 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 14
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 14
- 230000006698 induction Effects 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000007921 spray Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002923 metal particle Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 39
- 239000003708 ampul Substances 0.000 claims description 37
- 239000010453 quartz Substances 0.000 claims description 37
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000010935 stainless steel Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 230000009471 action Effects 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052753 mercury Inorganic materials 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 238000003723 Smelting Methods 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 claims description 4
- 229910010293 ceramic material Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000002955 isolation Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 238000003701 mechanical milling Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 239000000155 melt Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910001021 Ferroalloy Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011195 cermet Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000009646 cryomilling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The preparation method who the invention discloses a kind of spherical chromium powder, it comprises the following steps: 1) select crome metal piece, carry out Mechanical Crushing; 2) utilize the black brittleness of chromium, crome metal particle is immersed in liquid nitrogen, carry out low temperature vibro-grinding simultaneously; 3), by ethanol washing three times for the hafnium metal powfer after low temperature liquid nitrogen grinding, each consumption is 500～600ml, then uses with the vacuum system of filter paper and filters; 4) by step 3) in dried chromium powder particle insert high energy ball mill and carry out ball milling; 5) set up stable argon gas and carbon monoxide hybrid plasma torch; 6) by step 4) in chromium powder powder after ball milling carry through feeding gun and spray into plasma torch with argon gas and Co mixed gas; 7) the chromium powder powder that enters plasma torch melts rapidly, and enters in gas solid separation chamber and be collected after fast cooled and solidified. Plasma torch of the present invention adopts radio-frequency induction coil, and the spherical chromium powder of preparation is with low cost, nodularization rate is high.
Description
Technical field
The invention belongs to powder metallurgy and manufacture field, be specifically related to a kind of preparation method of spherical chromium powder.
Background technology
Crome metal is the hardest metal, and common chromium is all very crisp, because wherein contain the oxide of hydrogen or trace. High-purity chromium is but not crisp, but is rich in malleability. Because the hardness of chromium is larger, in high-purity chromium powder process of the ultra-fine grade of preparation, run into significant problem, be difficult to meet and both ensured that purity ensured the requirement of granularity again, however be exactly process time long higher with processing cost. Size, shape and other component contents of chromium powder chromium grain is the principal element that affects the material properties such as spraying, high temperature alloy, diamond tool, ferroalloy, scolder, cermet, carbide alloy, resistance heating alloy, electrical contact. The chromium powder using in the manufacture of materials such as spraying, high temperature alloy, diamond tool, ferroalloy, scolder, cermet, carbide alloy, resistance heating alloy, electrical contact is at present to adopt common mechanical crushing method to manufacture, grain shape is irregular, size distribution degree of segregation is large, other compositions, particularly oxygen, nitrogen content are high, thereby have caused inhomogeneous that under the higher and microcosmic of oxygen and nitrogen content in object material, the each element of alloy distributes. The chromium powder that electrolysis is manufactured, again because oxygen content is higher too high with processing cost, and not universal use aborning.
And in recent years, the demand of spherical powder grows with each passing day, be widely used in the powder metallurgical techniques such as preparation, thermal spraying and the injection moulding of porous material. In field of thermal spray, spherical powder not only mobility is fine, and the coating obtaining has better wearability. But the technology of the spherical chromium powder of existing preparation is all immature, make the cost of spherical chromium powder higher, and the obvious chap of chromium powder particle after treatment.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, a kind of preparation method of spherical chromium powder with low cost, that nodularization rate is high is provided, and can realizes quantity-produced industrialization.
For achieving the above object, the present invention completes by following technical solution, a kind of preparation method of spherical chromium powder, and it comprises the following steps:
1) select crome metal piece, remove surperficial flaw-piece, oxide-film and nitrogen film; Then utilize, with the hydraulic pressure boulder crusher of water-circulating cooling device, chromium piece is carried out to Mechanical Crushing, make it be broken into the particle below 3mm;
2) utilize the black brittleness of chromium, crome metal particle is immersed in liquid nitrogen, carry out low temperature vibro-grinding simultaneously, this low temperature vibro-grinding is to utilize nanometer AL2O3With ZrO2The vibromill Shell Lining that the high tenacity ceramic material that mixing makes makes and abrasive body carry out, and the time is 3～5 hours;
3) by ethanol washing three times for the hafnium metal powfer after low temperature liquid nitrogen grinding, each consumption is 500～600ml, then use with the vacuum system of filter paper and filter, then in vacuum drying oven, be under 94.5～96.5kPa, to carry out low temperature drying 5 hours at 80 DEG C, vacuum, until moisture content is down to below 1%;
4) by step 3) in dried chromium powder particle insert high energy ball mill and carry out ball milling, ratio of grinding media to material 20: 1, abrasive media is sintered carbide ball, liner is zirconia material, passes into argon shield in mechanical milling process, gas flow is 10～15m3/ h, rotating speed is 450～550r/min, Ball-milling Time is 45～50 hours;
5) set up stable argon gas and carbon monoxide hybrid plasma torch, both volume ratios are 1: 1; The input flow rate of setting up the needed reacting gas argon gas of this plasma torch and carbon monoxide is 55slpm～60slpm, and the high voltage loading on induction coil is 6kV～8kV; Reacting gas input flow rate when described argon gas and the stable operation of carbon monoxide hybrid plasma is 35slpm～45slpm, protective gas 30slpm～50slpm, and system negative pressure is 150mm mercury column～200mm mercury column;
6) by step 4) in chromium powder powder after ball milling carry through feeding gun and spray into plasma torch with argon gas and Co mixed gas; Chromium powder powder average grain diameter after ball milling is 5～10 μ m, and carrying gas control flow is 4slpm～6slpm, and the control flow of chromium powder powder is 40g/min～50g/min;
7) the chromium powder powder that enters plasma torch absorbs a large amount of heat and fusing rapidly in the extremely short time, and enters fast after heat-exchanging chamber cooled and solidified, then enters in gas solid separation chamber and be collected.
Preferably, step 3) in filter paper used be the graceful 50# filter paper of water.
In above-mentioned arbitrary scheme preferably, step 4) in abrasive media be zirconia or agate; The rotating speed of high energy ball mill is 500r/min, and Ball-milling Time is 48 hours.
In above-mentioned arbitrary scheme preferably, step 5) in plasma torch adopt radio-frequency induction coil, it is on the quartz ampoule of ventilation, there is Wilson sealing the upper end of quartz ampoule, in sealing, have telescopic hollow pipe be connected to atmospheric isolation for powder chamber; Under the incentive action of radio-frequency induction coil, the gas in quartz ampoule is transformed into the plasma of high temperature, and the powder smelting of sending here for powder chamber is become to drop the afterbody ejection from quartz ampoule.
In above-mentioned arbitrary scheme preferably, step 7) in heat-exchanging chamber be double-layer stainless steel sleeve pipe, in sleeve pipe, reverse water flowing is cooling, sleeve pipe top dress inlet flange tangential admission, by regulating inflow temperature and air inflow regulation and control cooling effect, cold in-water temperature 10-20 DEG C, cold gas adopts inert gas Ar, and flow is 3-6m3/h。
Beneficial effect of the present invention:
1. technique of the present invention is simple, and cost is lower, can accomplish scale production.
2. by setting up stable argon gas and carbon monoxide plasma, regulate plasma parameter, thereby chromium powder raw material is heated, after cooling curing, separate and obtain fine globular chromium powder, the chromium powder obtaining has than the better mobility of the former powder of chromium, higher density, purity and particle surface fineness, and powder particle porosity is low; The shape that can change chromium powder particle by the method that the present invention proposes, nodularization rate is high, and has increased the apparent density of powder, has increased chromium powder mobility, has improved the physical property of chromium powder, and with low cost.
3. not only product is spherical chromium powder, does not need in addition the processing through calcining and other middle process, and technological process is short, has shortened the production cycle, and operation continous-stable, has improved production efficiency.
Brief description of the drawings
Fig. 1 is the SEM shape appearance figure before the Cr sphere of powder;
Fig. 2 is the Laser particle-size distribution figure before the Cr sphere of powder;
Fig. 3 is the SEM shape appearance figure after the Cr sphere of powder;
Fig. 4 is the Laser particle-size distribution figure after the Cr sphere of powder;
Fig. 5 is the Laser particle-size distribution curve map after the Cr sphere of powder.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
A preparation method for spherical chromium powder, it comprises the following steps:
1) select crome metal piece, remove surperficial flaw-piece, oxide-film and nitrogen film; Then utilize, with the hydraulic pressure boulder crusher of water-circulating cooling device, chromium piece is carried out to Mechanical Crushing, make it be broken into the particle below 3mm;
2) utilize the black brittleness of chromium, crome metal particle is immersed in liquid nitrogen, carry out low temperature vibro-grinding simultaneously, this low temperature vibro-grinding is to utilize nanometer AL2O3With ZrO2The vibromill Shell Lining that the high tenacity ceramic material that mixing makes makes and abrasive body carry out, and the time is 3 hours;
3) by ethanol washing three times for the hafnium metal powfer after low temperature liquid nitrogen grinding, each consumption is 600ml, then use with the vacuum system of the graceful 50# filter paper of water and filter, then in vacuum drying oven, be under 94.5kPa, to carry out low temperature drying 5 hours at 80 DEG C, vacuum, until moisture content is down to below 1%;
4) by step 3) in dried chromium powder particle insert high energy ball mill and carry out ball milling, ratio of grinding media to material 20: 1, abrasive media is sintered carbide ball, liner is zirconia material, passes into argon shield in mechanical milling process, gas flow is 15m3/ h, rotating speed is 500r/min, Ball-milling Time is 48 hours;
5) set up stable argon gas and carbon monoxide hybrid plasma torch, both volume ratios are 1: 1; This mist can form the magnetic coupling of gas, and the input flow rate of setting up the needed reacting gas argon gas of this plasma torch and carbon monoxide is 55slpm, and the high voltage loading on induction coil is 8kV; Reacting gas input flow rate when described argon gas and the stable operation of carbon monoxide hybrid plasma is 35slpm, protective gas 50slpm, and system negative pressure is 150mm mercury column; Plasma torch adopts radio-frequency induction coil, and it is on the quartz ampoule of ventilation, and there is Wilson sealing the upper end of quartz ampoule, in sealing, have telescopic hollow pipe be connected to atmospheric isolation for powder chamber; Under the incentive action of radio-frequency induction coil, the gas in quartz ampoule is transformed into the plasma of high temperature, and the powder smelting of sending here for powder chamber is become to drop the afterbody ejection from quartz ampoule;
6) by step 4) in chromium powder powder after ball milling carry through feeding gun and spray into plasma torch with argon gas and Co mixed gas; Chromium powder powder average grain diameter after ball milling is 10 μ m, and carrying gas control flow is 4slpm, and the control flow of chromium powder powder is 50g/min;
7) the chromium powder powder that enters plasma torch absorbs a large amount of heat and fusing rapidly in the extremely short time, and enters fast after heat-exchanging chamber cooled and solidified, then enters in gas solid separation chamber and be collected. Heat-exchanging chamber is double-layer stainless steel sleeve pipe, and the interior reverse water flowing of sleeve pipe is cooling, sleeve pipe top dress inlet flange tangential admission, and by regulating inflow temperature and air inflow regulation and control cooling effect, 10 DEG C of cold in-water temperatures, cold gas adopts inert gas Ar, and flow is 6m3/h。
Embodiment 2
A preparation method for spherical chromium powder, it comprises the following steps:
1) select crome metal piece, remove surperficial flaw-piece, oxide-film and nitrogen film; Then utilize, with the hydraulic pressure boulder crusher of water-circulating cooling device, chromium piece is carried out to Mechanical Crushing, make it be broken into the particle below 3mm;
2) utilize the black brittleness of chromium, crome metal particle is immersed in liquid nitrogen, carry out low temperature vibro-grinding simultaneously, this low temperature vibro-grinding is to utilize nanometer AL2O3With ZrO2The vibromill Shell Lining that the high tenacity ceramic material that mixing makes makes and abrasive body carry out, and the time is 5 hours;
3) by ethanol washing three times for the hafnium metal powfer after low temperature liquid nitrogen grinding, each consumption is 500ml, then use with the vacuum system of the graceful 50# filter paper of water and filter, then in vacuum drying oven, be under 96.5kPa, to carry out low temperature drying 5 hours at 80 DEG C, vacuum, until moisture content is down to below 1%;
4) by step 3) in dried chromium powder particle insert high energy ball mill and carry out ball milling, ratio of grinding media to material 20: 1, abrasive media is sintered carbide ball, liner is zirconia material, passes into argon shield in mechanical milling process, gas flow is 10m3/ h, rotating speed is 450～550r/min, Ball-milling Time is 45～50 hours;
5) set up stable argon gas and carbon monoxide hybrid plasma torch, both volume ratios are 1: 1; This mist can form the magnetic coupling of gas, and the input flow rate of setting up the needed reacting gas argon gas of this plasma torch and carbon monoxide is 60slpm, and the high voltage loading on induction coil is 6kV; Reacting gas input flow rate when described argon gas and the stable operation of carbon monoxide hybrid plasma is 45slpm, protective gas 30slpm, and system negative pressure is 200mm mercury column; Plasma torch adopts radio-frequency induction coil, and it is on the quartz ampoule of ventilation, and there is Wilson sealing the upper end of quartz ampoule, in sealing, have telescopic hollow pipe be connected to atmospheric isolation for powder chamber; Under the incentive action of radio-frequency induction coil, the gas in quartz ampoule is transformed into the plasma of high temperature, and the powder smelting of sending here for powder chamber is become to drop the afterbody ejection from quartz ampoule;
6) by step 4) in chromium powder powder after ball milling carry through feeding gun and spray into plasma torch with argon gas and Co mixed gas; Chromium powder powder average grain diameter after ball milling is 5 μ m, and carrying gas control flow is 6slpm, and the control flow of chromium powder powder is 40g/min;
7) the chromium powder powder that enters plasma torch absorbs a large amount of heat and fusing rapidly in the extremely short time, and enters fast after heat-exchanging chamber cooled and solidified, then enters in gas solid separation chamber and be collected. Heat-exchanging chamber is double-layer stainless steel sleeve pipe, and the interior reverse water flowing of sleeve pipe is cooling, sleeve pipe top dress inlet flange tangential admission, and by regulating inflow temperature and air inflow regulation and control cooling effect, 20 DEG C of cold in-water temperatures, cold gas adopts inert gas Ar, and flow is 3m3/h。
In addition, described quartz ampoule in the present invention is by interior quartz ampoule, middle quartz ampoule and outer quartz ampoule is coaxially arranged forms, outer quartz ampoule is connected with interior quartz ampoule lower end, between the lower end of middle quartz ampoule and outer quartz ampoule and the bottom of interior quartz ampoule, leave circulation gap, make between interior quartz ampoule and middle quartz ampoule, the cooling duct that forms quartz ampoule external member between middle quartz ampoule and outer quartz ampoule is provided with cooling water import and export on fixture, and they communicate with the cooling duct of quartz ampoule.
Described plasma in the present invention excite and maintain be to outer quartz ampoule external spiral shape around air core coil pass into radio-frequency current, from being built in, quartz ampoule coaxial interior quartz ampoule pass into ignition gas, with the exciting of the sparker of outer quartz ampoule outer wall vertical under, radio-frequency current is the inner induced field that forms of quartz ampoule outside, excites ionization to form radio frequency glow discharge inductively coupled plasma ignition gas.
The collection of described spherical chromium powder is the negative blast stainless steel pipes transmission of spherical chromium powder, refers under the negative Action of Wind pressure of air exhauster, enters in powder catcher by the transmission of " Z " font double layer hollow stainless steel pipes; Stainless steel tube hollow sandwich leads to circulating water, " Z " font design balance of double layer hollow stainless steel transmission pipeline the negative Action of Wind pressure of air exhauster, maintain the stable of radio frequency plasma flame in large quartz ampoule and reduce reaction end gas in the lip-deep absorption of dusty material. Described powder catcher is to adopt impulse electromagnetic valve to coordinate glass fiber filter cloth bag and air exhauster to carry out work, " z " type length of the power of air exhauster and stainless steel transmission pipeline, the surface area of powder collection filter bag are positively related, in powder catcher nano-powder material by under the effect of glass fiber filter cloth bag and electromagnetic impulse valve with reaction end gas surface desorption, reaction end gas enters vertical spray tower under the negative Action of Wind pressure of air exhauster. In the vertical spray tower of described reaction end gas and absorb process refer to plasma chemical reaction produce tail gas in powder catcher with nano-powder material surface desorption after, enter vertical spray tower under the negative Action of Wind pressure of air exhauster in and absorption plant, during reaction end gas and neutralization solution system occur and chemical reaction, eliminate reaction end gas, reach environment protection emission requirement.
Following table is the testing result contrast of plasma spheroidization Cr powder and original chromium powder.
Table 1
(1) chemical composition
(2) physical property
| Material | State | Apparent density g/cm3 | Tap density g/cm3 | Flow velocity s/50g |
| Original Cr powder | Cryomilling | 3.26 | 4.01 | 22.23 |
| Spherical Cr powder | Nodularization rate >=95% | 4.27 | 4.65 | 12.91 |
As can be seen here, adopt spherical chromium powder density and the purity making of the present invention higher, mobility is better, and nodularization rate is high. Show thus, the parameters in the inventive method is all optimal selections, can realize the optimal effectiveness of the inventive method.
The above, be only preferred embodiment of the present invention, is not the restriction of the present invention being made to other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations. But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (5)
1. a preparation method for spherical chromium powder, is characterized in that comprising the following steps:
1) select crome metal piece, remove surperficial flaw-piece, oxide-film and nitrogen film; Then utilize, with the hydraulic pressure boulder crusher of water-circulating cooling device, chromium piece is carried out to Mechanical Crushing, make it be broken into the particle below 3mm;
2) utilize the black brittleness of chromium, crome metal particle is immersed in liquid nitrogen, carry out low temperature vibro-grinding simultaneously, this low temperature vibro-grinding is to utilize nanometer Al2O3With ZrO2The vibromill Shell Lining that the high tenacity ceramic material that mixing makes makes and abrasive body carry out, and the time is 3～5 hours;
3) by ethanol washing three times for the hafnium metal powfer after low temperature liquid nitrogen grinding, each consumption is 500～600ml, then use with the vacuum system of filter paper and filter, then in vacuum drying oven, be under 94.5～96.5kPa, to carry out low temperature drying 5 hours at 80 DEG C, vacuum, until moisture content is down to below 1%;
4) by step 3) in dried chromium powder particle insert high energy ball mill and carry out ball milling, ratio of grinding media to material 20: 1, abrasive media is sintered carbide ball, liner is zirconia material, passes into argon shield in mechanical milling process, gas flow is 10～15m3/ h, rotating speed is 450～550r/min, Ball-milling Time is 45～50 hours;
5) set up stable argon gas and carbon monoxide hybrid plasma torch, both volume ratios are 1: 1; The input flow rate of setting up the needed reacting gas argon gas of this plasma torch and carbon monoxide is 55slpm～60slpm, and the high voltage loading on induction coil is 6kV～8kV; Reacting gas input flow rate when described argon gas and the stable operation of carbon monoxide hybrid plasma is 35slpm～45slpm, protective gas 30slpm～50slpm, and system negative pressure is 150mm mercury column～200mm mercury column;
6) by step 4) in chromium powder powder after ball milling carry through feeding gun and spray into plasma torch with argon gas and Co mixed gas; Chromium powder powder average grain diameter after ball milling is 5～10 μ m, and carrying gas control flow is 4slpm～6slpm, and the control flow of chromium powder powder is 40g/min～50g/min;
7) the chromium powder powder that enters plasma torch absorbs a large amount of heat and fusing rapidly in the extremely short time, and enters fast after heat-exchanging chamber cooled and solidified, then enters in gas solid separation chamber and be collected.
2. the preparation method of spherical chromium powder according to claim 1, is characterized in that step 3) in filter paper used be the graceful 50# filter paper of water.
3. the preparation method of spherical chromium powder according to claim 1 and 2, is characterized in that step 4) in abrasive media be zirconia or agate; The rotating speed of high energy ball mill is 500r/min, and Ball-milling Time is 48 hours.
4. the preparation method of spherical chromium powder according to claim 3, it is characterized in that step 5) in plasma torch adopt radio-frequency induction coil, it is on the quartz ampoule of ventilation, there is Wilson sealing the upper end of quartz ampoule, in sealing, have telescopic hollow pipe be connected to atmospheric isolation for powder chamber; Under the incentive action of radio-frequency induction coil, the gas in quartz ampoule is transformed into the plasma of high temperature, and the powder smelting of sending here for powder chamber is become to drop the afterbody ejection from quartz ampoule.
5. the preparation method of spherical chromium powder according to claim 3, it is characterized in that step 7) in heat-exchanging chamber be double-layer stainless steel sleeve pipe, in sleeve pipe, reverse water flowing is cooling, sleeve pipe top dress inlet flange tangential admission, by regulating inflow temperature and air inflow regulation and control cooling effect, cold in-water temperature 10-20 DEG C, cold gas adopts inert gas Ar, and flow is 3-6m3/h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410280629.6A CN104070172B (en) | 2014-06-23 | 2014-06-23 | A kind of preparation method of spherical chromium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410280629.6A CN104070172B (en) | 2014-06-23 | 2014-06-23 | A kind of preparation method of spherical chromium powder |
Publications (2)
| Publication Number | Publication Date |
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| RU2623608C1 (en) * | 2016-02-09 | 2017-06-28 | Владимир Никитович Анциферов | Method of milling the powder from plastic material |
| CN107267787A (en) * | 2017-07-10 | 2017-10-20 | 铜山县丰华工贸有限公司 | A kind of chromium agent and preparation method thereof of aluminum alloy smelting |
| CN107584132A (en) * | 2017-09-08 | 2018-01-16 | 张家港创博金属科技有限公司 | A kind of preparation method of spherical micro-particle |
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| CN109182833B (en) * | 2018-08-28 | 2020-11-06 | 合肥工业大学 | Copper-based powder metallurgy pantograph pan material taking spherical chromium powder as strengthening phase and preparation method thereof |
| CN110014158A (en) * | 2019-04-22 | 2019-07-16 | 西安斯瑞先进铜合金科技有限公司 | A kind of method that aerosolization prepares spherical chromium powder |
| CN111531164B (en) * | 2020-04-15 | 2022-03-04 | 河南中钻新材料有限公司 | Method for reducing oxygen and nitrogen contents in chromium powder particles at low cost |
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| CN111922350B (en) * | 2020-09-22 | 2021-01-01 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of low-hydrochloric-acid-insoluble metal chromium powder |
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| CN1004637B (en) * | 1987-08-05 | 1989-06-28 | 北京有色金属研究总院 | Method for producing low-oxygen chromium powder |
| CN1259147C (en) * | 2003-07-04 | 2006-06-14 | 中山大学 | Superfine grinding apparatus of nanometer material for making high toughness ceramic parts |
| CN1555949A (en) * | 2004-01-08 | 2004-12-22 | 北京科技大学 | Method of preparing nano powderusing liquid nitrogen low temperature ball mill |
| CN101161347B (en) * | 2006-10-13 | 2010-05-12 | 南京理工大学 | Bidirectional tosh grinding ultra-fine crashing objects and its method |
| US8268237B2 (en) * | 2009-01-08 | 2012-09-18 | General Electric Company | Method of coating with cryo-milled nano-grained particles |
| CN102060296A (en) * | 2010-10-26 | 2011-05-18 | 锦州市金属材料研究所 | Production method of chrome carbide powder |
| US9145296B2 (en) * | 2011-03-02 | 2015-09-29 | GM Global Technology Operations LLC | Mitigating diborane release from borohydride-based hydrogen storage materials |
| CN102350503A (en) * | 2011-10-21 | 2012-02-15 | 株洲硬质合金集团有限公司 | Method for producing spherical thermal-spraying powder |
| CN102825257A (en) * | 2012-08-21 | 2012-12-19 | 苏州晶纯新材料有限公司 | Method for preparing ultrafine chromium powder |
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