CN102445072A - Continuous dynamic sintering kiln - Google Patents
Continuous dynamic sintering kiln Download PDFInfo
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- CN102445072A CN102445072A CN2010105071081A CN201010507108A CN102445072A CN 102445072 A CN102445072 A CN 102445072A CN 2010105071081 A CN2010105071081 A CN 2010105071081A CN 201010507108 A CN201010507108 A CN 201010507108A CN 102445072 A CN102445072 A CN 102445072A
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- continous way
- powder
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Abstract
The invention relates to a kiln manufacture method of a continuous dynamic sintering powder material, which completely overcomes the three serious defects of inhomogeneity in material sintering, leakage at a high-temperature dynamic sealing part during dynamic sintering of a rotary kiln, non-uniform resident time of powder in a rotating furnace pipe, and demixing of a reaction mixture due to an introduced protection airflow. The kiln manufacture method is characterized in that a tunnel type hearth is designed to be of a downward inclination angle, and two ends of a charging tank with a rolling characteristic are erected on a roller path with a downward inclination automatically roll. The charging tank is made of a porous sintering high-temperature-resisting material and is internally provided with a plurality of shoveling plates and filled with grinding mediums, powder is shoveled, turned and ground, thus dynamic sintering and high-temperature online grinding are realized. A discharging-intercepting rod and a feeding cabin door and a discharging cabin door are linked for discharging and intercepting the rolling charging tank. A LiFePO4 cathode material with a uniform topography structure with a grain size of 200nm and an excellent electrochemical performance, a CoO with high activity, a nano compound oxide with high activity and an ultrathin ceramic powder material are obtained through sintering of the kiln.
Description
Technical field
The invention belongs in the kiln manufacturing field kiln manufacturing approach in order to a kind of particular design of continous way dynamic sinter powder body material.
Background technology
Producing used sintering kiln in order to the continuous industrial of powder body material at present has: tunnel cave, pushed bat kiln, roller kilns, meshbeltfurnace and rotary kiln.Wherein tunnel cave normally material load by kiln car, thruster pushes kiln body agglomerating chamber with the kiln car of loaded material, and carries out advancing.Pushed bat kiln, powder material are contained in the magazine, and magazine places in the push pedal, and the propeller horizontal direction promotes push pedal advances magazine, and magazine gets in the burner hearth to come out from the stove tail again.Roller kilns vertically with kiln road direction at the bottom of its kiln are furnished with many rollers free to rotate, and magazine lies on the roller-way, and roller-way is driven together and rotated in the same way by the outer roller-way connector chain of stove, sprocket wheel, magazine translation forward on the roller that is rotating.Meshbeltfurnace is that magazine lies on the mobile guipure, is moved forward by the mobile drive magazine of guipure.More than four types of kilns; Though magazine moves in the burner hearth sintering zone, be static relatively between the powder material particle in the same magazine, the material in the magazine does not stir and fries motion; So the sintering processing of these four kinds of kilns still belongs to static sintering; In the magazine powder of its upper surface of material be heated with magazine bottom, the bed of material in the middle of powder be heated inconsistently, the powder on magazine surface often has burn-off phenomenon, and middle lower floor powder has to give birth to and burns and half-cooked phenomenon.The powder burning will have the particle of growing up unusually, will cause powder product crystallization imperfection and give birth to burning.LiFePO 4 of anode material (LiFePO for power-type lithium ion battery
4), its sintering process requires high, because LiFePO
4Electrical conductivity and lithium ion conduction performance all bad, the LiFePO that grows up unusually
4Li in the particle
+Be difficult to take off fully embedding and come out and embed into, therefore influence the charge-discharge performance of material greatly.Give birth to the LiFePO that burns
4Material, its crystallization is bad, and the cycle performance of battery is very poor.The sintering heterogeneity has burning to burn phenomenon with giving birth to, and this is the critical defect of static sintering method.Simultaneously static sintering method needs longer sintering time, energy consumption height and production efficiency low.
The continous way rotary kiln is a dynamic sinter, and it has overcome the defective of static sintering, and material is joined by feeding screw in the boiler tube of a rotation from burner, and boiler tube is around its central symmetry axis rotation.Along with the rotation of boiler tube, material rotates in boiler tube and stirs to stove tail direction and advances.But there are three fatal defectives in the rotary kiln sintered manufacturing lithium iron phosphate positive material of atmosphere protection in actual production is used:
1. high temperature dynamic seal (packing) place between the boiler tube of rotation and static burner, the static stove tail is difficult to solve the gas leakage problem; The air of outside tends to suck-back and gets in the boiler tube that rotates; Air during the black furnace blow-on in its boiler tube can not be discharged totally; Oxygen content in the boiler tube is difficult to be controlled at below the 10ppm LiFePO that sintering goes out
4Product often contains more ferric iron dephasign, has a strong impact on product quality.
2. the powder in the rotation boiler tube exists the serious asynchrony phenomenon that advances; The particle of powder is serious disunity of holdup time in the boiler tube high-temperature region; Powder particle as 80% enters into from burner that to come out from the stove tail be in 4-6 hour, and some powder particle holdup times in boiler tube of 20% are 6-10 hour, occurs serious inconsistent of powder granule actual sintered time like this; The serious particle sintering time that lags behind is long, particle is grown up unusually, and properties of product are had a strong impact on.
3. the air-flow that the protective atmosphere that feeds from the stove tail forms will make the mixed powder material particle tinyly blow afloat with the little component particles of density, blow and melt down head even be blown along stove tail flue; Cause reacting the phenomenon that is divided into of mixed powder like this, have a strong impact on product quality.
For lithium iron phosphate positive material, because LiFePO
4Electric conductivity very poor, primary particle need be the particle of nano-scale, solid phase reaction must be fully, the particle crystallization is perfect, simultaneously the bulky grain of growing up unusually can not be arranged.Present existing continous way kiln technology all can not satisfy these harsh sintering conditions of LiFePO 4 material well.
Summary of the invention
The object of the present invention is to provide a kind of novel continuous dynamic sinter kiln, it has overcome the inhomogenous defective of material sintering that the static sintering technology of existing kiln exists fully, also overcome high temperature dynamic seal (packing) place gas leakage, the powder that existing rotary kiln dynamic sinter exists simultaneously makes the reactant mixture material be divided into this three major defects at the boiler tube holdup time disunity of rotation, the protective atmosphere air-flow of feeding.Use kiln dynamic sinter LiFePO4 (LiFePO of the present invention
4) positive electrode, carrying out the online ball milling of sintering and high temperature simultaneously, the material powder is heated evenly, product particle is the appearance structure of homogeneous and outstanding chemical property.Use kiln of the present invention to make highly active cobalt protoxide (CoO) material, the material powder is heated evenly, product particle is the appearance structure of homogeneous sub-micron and outstanding chemical property.Use kiln reduced form of the present invention, direct aerating oxygen can the highly active nano composite oxide SnO of sintering
2-In
2O
3, WO
3-La
2O
3, TiO
2-Cr
2O
3Deng the gas sensor powder body material, sensitivity raises significantly; Sintering superfine ceramic powder material ZrO
2, Al
2O
3, Bi
2O
3, Fe
2O
3, ZnO, and ultra-fine ferrite powder material.
A kind of continous way dynamic sinter kiln of the present invention comprises: have the tunnel type burner hearth 1 at downward inclination angle, and the raceway 2 at two parallel downward inclination angles about being provided with in the burner hearth, the charge can 3 two ends framves with rolling characteristic are on raceway 2; Burner charging aperture hatch door 4 and 5, stove tail water cooling section 6, clearance- interception bar 7 and 8; Protective atmosphere inlet port 9,10,11,12 and 13; Vacuum pumping opening 14 and 15, tail gas outlet 16, discharging hatch door 17,18 and 19.
Concrete steps of the present invention are: tunnel type chamber design is the corner structure that dips down; Wherein the burner feed end is higher than stove tail discharge end; Charge can two ends frame with rolling characteristic have downward inclination angle about on two raceways, charge can rolls to the stove tail along raceway voluntarily under the effect of sliding force.Powder is contained in the charge can with rolling characteristic, and charge can is provided with the butt joint of cover or two halves, and charge can is porous sintered high temperature resistant material, and the gas that its internal-response produces can freely overflow and powder material can not spill.Be provided with the flight of several and axially parallel in the charge can, when charge can rolled, flight was taken up powder, stir.Put into the unloaded charge can of full stove in the burner hearth in advance; Fire box temperature and atmosphere reach set require after; Clearance-interception action is implemented in clearance-interception bar and the interlock of discharging hatch door at the stove tail, quantitatively emits the top several charge cans of stove tail, and these several charge cans roll out at the downslide active force automatically; Meanwhile in burner clearance-interception bar and the also clearance-interception of the interlock enforcement simultaneously action of charging hatch door, the same number of charge can that is mounted with powder material rolls in the burner hearth voluntarily.After accomplishing quantitatively regularly charging-discharging action, charging hatch door, discharging hatch door are closed, and vacuumize and recharge the action of protective atmosphere.Two joint discharging cabin and three road discharging hatch doors, alternately opening and closing of three road discharging hatch doors vacuumizes and the protective gas that backwashes, and guarantees that the outer air of stove does not get in the burner hearth, guarantees that oxygen content is below 5ppm in the burner hearth.When roll-fed-discharging was moved so at regular time and quantity, all charge cans in the burner hearth rolled to stove tail direction with speed simultaneously.Charge can along the charging cabin, burner hearth, panel, discharging cabin one and discharging cabin two roll.
Above-described charge can; Its material is sintering 310S or 321 high temperature resistant stainless steels of porous/microcellular structure, the sintrered nickel based high-temp-resistant alloy or the sintered titanium based high-temp-resistant alloy of porous/microcellular structure; Its porosity 15%-65%; Aperture 0.2um-80um, the gas that jar internal reaction produces can overflow easily, and a jar interior powder granule can not spill.
Above-mentioned charge can inwall is provided with the 1-8 root flight parallel with central symmetry axis to copy a jar interior material, and the flight height is the 1/9-2/5 of charge can interior diameter.Charge can is when rolling, and powder stir-fry owing to flight in jar is moved with stirring and frying, and powder is heated more even.
In above-mentioned charge can, optionally put into the stainless steel ball or the alloying pellet of resistant to elevated temperatures zirconium dioxide mill ball, alumina lap ball or high temperature resistant inertia, when charge can rolled like this, mill ball carried out the high temperature on-line grinding to powder in tank body.The high temperature on-line grinding makes powder further homogenize and ultra-fineization.
The above-mentioned charge can with rolling characteristic, its structure are simple cylindrical structure, composite cylindrical-frustum cone structure or composite cylindrical-column structure (see figure 2)s, and two halves dock in the centre or at one end add a cover.The charge can shown in Fig. 2 b and Fig. 2 c wherein; Because the column type perimeter of section at rolling position, two ends is little; Same burner hearth length and same sintering time, then the charge can of this structure in burner hearth, rotate upset circumference number will be much larger than the column type charge can of single structure.The circumference number that material rotates upset increases, and the effect of on-line grinding is more obvious, and it is more favourable with ultra-fineization to homogenize.
Description of drawings
Fig. 1 is the sketch map of continous way dynamic sinter kiln.
Fig. 2 is the structural representation of charge can.
Fig. 3 is the stereoscan photograph of the nano lithium iron phosphate material that makes among the embodiment.
The specific embodiment
Embodiment 1:
Make continous way dynamic sinter kiln as shown in Figure 1, wherein kiln sintering zone length is 25 meters, is divided into 5 warm areas, separately by PID system temperature control.The maximum temperature of sintering zone is controlled at 600-700 ℃.The water cooling zone is jacket structured, and length is 6 meters, feeds 8 ℃ of water at low temperature cooled materials.Burner charging cabin, stove tail discharging cabin one and discharging cabin two are all 0.3 meter.The cross sectional dimensions of burner hearth is 350x200mm
2(wide x is high).Be provided with the inclination angle about in the burner hearth and be two raceways of 1.5 °.Charge can is cylinder-round platform composite construction, porous sintered 310S stainless steel, butt joint (shown in Fig. 2 b) in the middle of the halves, and charge can longitudinal section largest outer diameter is 150mm, two ends are diameter 40mm solid cylinder.The stir-fry plate that to be provided with three height in the charge can be 50mm, the charge can frame about on two raceways.Clearance-interception bar, discharging hatch door and the charging hatch door of stove tail clearance-interception bar, burner are linked by programme-control, and the charging cabin got into 2 charge cans in per 6 minutes, and the cabin of discharging simultaneously emits 2 discharge tanks.Material sintering time in 25 meters heating furnaces is that the material in 500 minutes, charge can overturn for 199 weeks 25 meters long sintering zones, fries moving 597 times.
With Fe
2O
3, LiH
2PO
4With carbon black be primary raw material, with H
2TiO
3, Mg (OH)
2Be doped raw material, according to LiFe
1-xM
xPO
4Form batching, wherein M is Mg or Ti, x=0.01-0.05.Raw material is packed into behind pre-burning, ball milling in the charge can, adds Φ 5 zirconium oxide abrasive balls simultaneously, and the mass ratio of zirconium oxide abrasive ball and raw material is 5: 1.It is 1000Pa that vacuum suction reaches absolute pressure, and recharging purity then is that 99.999% nitrogen to malleation is 1000Pa.Highest temperature district, sintering zone is at 600-700 ℃.Sintering 500 minutes, upset are come out of the stove for 199 times, advance pulverizing again, and packing obtains the LiFePO that the primary particle particle diameter is the excellent performance about 200 nanometers
4Material.
Embodiment 2:
Make continous way dynamic sinter kiln as shown in Figure 1, wherein kiln sintering zone length is 15 meters, is divided into 3 warm areas, separately by PID system temperature control.The maximum temperature of sintering zone is controlled at 550-650 ℃.The water cooling zone is jacket structured, and length is 6 meters, feeds 8 ℃ of water at low temperature cooled materials.Burner charging cabin, stove tail discharging cabin one and discharging cabin two are all 0.3 meter.The cross sectional dimensions of burner hearth is 350x200mm
2(wide x is high).Be provided with the inclination angle about in the burner hearth and be two raceways of 1.5 °.Charge can is composite cylindrical-frustum cone structure, porous sintered 310S stainless steel, butt joint (shown in Fig. 2 b) in the middle of the halves, and charge can longitudinal section largest outer diameter is 150mm, two ends are diameter 40mm solid cylinder.The stir-fry plate that to be provided with three height in the charge can be 50mm, the charge can frame about on two raceways.Clearance-interception bar, discharging hatch door and the charging hatch door of stove tail clearance-interception bar, burner are linked by programme-control, and the charging cabin got into 2 charge cans in per 6 minutes, and the cabin of discharging simultaneously emits 2 discharge tanks.Material sintering time in 15 meters heating furnaces is that the material in 300 minutes, charge can overturn for 119 weeks 15 meters long sintering zones, fries moving 357 times.
With CoC
2O
42H
2O is a raw material, in the charge can of packing into, adds Φ 5 zirconium oxide abrasive balls simultaneously, and the mass ratio of zirconium oxide abrasive ball and raw material is 4: 1.It is 1000Pa that vacuum suction reaches absolute pressure, and recharging purity then is that 99.999% nitrogen to malleation is 1000Pa.Highest temperature district, sintering zone is at 550-650 ℃.Sintering 300 minutes, upset are come out of the stove for 119 times, advance pulverizing again, packing, and obtaining the primary particle particle diameter is the high activity CoO material about 150 nanometers.
Reaction is: CoC
2O
42H
2O=====CoO+2CO
2↑+2H
2O ↑
Embodiment 3:
Make continous way dynamic sinter kiln as shown in Figure 1, wherein kiln sintering zone length is 6 meters, is divided into 2 warm areas, separately by PID system temperature control.The maximum temperature of sintering zone is controlled at 650 ℃.The water cooling zone is jacket structured, and length is 2 meters, feeds 8 ℃ of water at low temperature cooled materials.Burner charging cabin, stove tail discharging cabin one and discharging cabin two are all 0.3 meter.The cross sectional dimensions of burner hearth is 350x200mm
2(wide x is high).Be provided with the inclination angle about in the burner hearth and be two raceways of 1.5 °.Charge can is composite cylindrical-frustum cone structure, porous sintered 310S stainless steel, butt joint (shown in Fig. 2 b) in the middle of the halves, and charge can longitudinal section largest outer diameter is 150mm, two ends are diameter 30mm solid cylinder.The stir-fry plate that to be provided with four height in the charge can be 45mm, the charge can frame about on two raceways.Clearance-interception bar, discharging hatch door and the charging hatch door of stove tail clearance-interception bar, burner are linked by programme-control, and the charging cabin got into 2 charge cans in per 6 minutes, and the cabin of discharging simultaneously emits 2 discharge tanks.Material sintering time in 15 meters heating furnaces is that the material in 120 minutes, charge can overturn for 64 weeks 6 meters long sintering zones, fries moving 256 times.
With nano SnO
2And In
2O
3Be raw material, both mass ratioes: SnO
2: In
2O
3=97: 3.The mixed material that ball milling is good is packed in the charge can, adds Φ 5 zirconium oxide abrasive balls simultaneously, and the mass ratio of zirconium oxide abrasive ball and raw material is 4: 1; Aerating oxygen is sintering in oxygen atmosphere; The sintering zone temperature is 650 ℃, and sintering 120 minutes, upset are come out of the stove for 64 times, advance pulverizing again; Packing, obtaining the primary particle particle diameter is about 350 nanometers chlorine to be had highly sensitive air-sensitive SnO
2/ In
2O
3Nano composite material.
Claims (10)
1. continous way dynamic sinter kiln; Comprise in burner hearth heating temperature-controlling system, the burner hearth clearance-intercepting system and the vacuum suction of the charge can that raceway is set, has rolling characteristic, discharging cooling system, feed system, discharge system, charge can and recharge the protective gas system; It is characterized in that: the burner hearth Tunnel Design is the structure that has a down dip; Wherein the feed furnace head end is higher than discharging stove tail end; Two raceways about being provided with in the burner hearth, frame is distinguished on the raceway of the left and right sides in the two ends with charge can of rolling characteristic, and charge can effect owing to sliding force in burner hearth is rolled to the stove tail along raceway; Be designed with flight in the charge can and add abrasive media; Therefore material is stirred, is copied and ball milling in charge can, and the clearance-intercepting system that is arranged at burner and stove tail is regularly implemented to let pass and interception to charge can, realizes continous way dynamic sinter and high temperature on-line grinding.
2. a kind of continous way dynamic sinter kiln according to claim 1; It is characterized in that: the burner hearth Tunnel Design is a horizontal structure; Be provided with raceway in the burner hearth, the raceway in the burner hearth under the impetus of burner push rod of the charge can with rolling characteristic rolls to the stove tail.
3. a kind of continous way dynamic sinter kiln according to claim 1; It is characterized in that: the charge can with rolling characteristic has porous or microcellular structure; Porosity 15%-65%; Aperture 0.2um-80um; The powder sintered material of high temperature resistant stainless steel, powder titanium sintering material, the powder sintered material of Ni-based high-temperature alloy or titanium based high-temp-resistant alloy powder sintering material, the charge can of porous or microcellular structure guarantee that outside the timely drain tank of gas of materials inside reaction generation, the powder in the jar does not leak out simultaneously.
4. a kind of continous way dynamic sinter kiln according to claim 1; It is characterized in that: the charge can with rolling characteristic is designed to cylindrical structure, composite cylindrical type structure or composite cylindrical-circular platform type structure, and it has lateral symmetry axle and vertical plane of symmetry.
5. a kind of continous way dynamic sinter kiln according to claim 1; It is characterized in that: have and be designed with the 1-8 root flight parallel with the charge can central symmetry axis in the charge can of rolling characteristic with the material in copying jar, the flight height is the 1/9-2/5 of charge can interior diameter.
6. a kind of continous way dynamic sinter kiln according to claim 1; It is characterized in that: in having the charge can of rolling characteristic, add abrasive media: the stainless steel ball or the high temperature resistant nickel-base alloy ball of resistant to elevated temperatures zirconium dioxide mill ball, 99 porcelain alumina lap balls, high temperature resistant inertia; Charge can is when rolling; Mill ball carries out the high temperature on-line grinding to powder in tank body, make powder further homogenize and ultra-fineization.
7. a kind of continous way dynamic sinter kiln according to claim 1 is characterized in that: use this continous way dynamic sinter kiln sintering lithium ion battery anode material lithium iron phosphate LiFePO
4With cobalt black CoO, continous way dynamic sinter and high temperature on-line grinding.
8. a kind of continous way dynamic sinter kiln according to claim 1 is characterized in that: the protective gas that recharges after the vacuum suction is that purity is at the nitrogen more than 99.999%, argon gas or carbon dioxide.
9. a kind of continous way dynamic sinter kiln according to claim 1; It is characterized in that: after omitting vacuum suction, omit the protective gas that recharges and omitting two sections discharging cabins, in air atmosphere, carry out continous way dynamic sinter and high temperature on-line grinding and make nano-powder material.
10. a kind of continous way dynamic sinter kiln according to claim 1; It is characterized in that: behind vacuum suction, recharge oxygen, in pure oxygen atmosphere, carry out continous way dynamic sinter and high temperature on-line grinding and make nano-oxide and nano composite oxide powder material.
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|---|---|---|---|
| CN2010105071081A CN102445072A (en) | 2010-10-05 | 2010-10-05 | Continuous dynamic sintering kiln |
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|---|---|---|---|
| CN2010105071081A CN102445072A (en) | 2010-10-05 | 2010-10-05 | Continuous dynamic sintering kiln |
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|---|---|
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Family
ID=46007808
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103456932A (en) * | 2012-05-27 | 2013-12-18 | 湖南省正源储能材料与器件研究所 | Preparation method of energy storage material |
| CN104987075A (en) * | 2015-06-09 | 2015-10-21 | 四川大学 | Rotary dynamic continuous preparation method for (M1, M2) (CxN1-x) powder and rotary dynamic continuous sintering device |
| WO2018223439A1 (en) * | 2017-06-09 | 2018-12-13 | 深圳市星特烁科技有限公司 | Vacuum sintering furnace enabling continuous production |
| CN110937629A (en) * | 2019-12-07 | 2020-03-31 | 西北有色金属研究院 | Method for preparing Bi-2212 precursor powder by inclined rotary sintering method |
| WO2020172784A1 (en) * | 2019-02-26 | 2020-09-03 | Linde Gmbh | Method and apparatus for producing ternary cathode material |
-
2010
- 2010-10-05 CN CN2010105071081A patent/CN102445072A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103456932A (en) * | 2012-05-27 | 2013-12-18 | 湖南省正源储能材料与器件研究所 | Preparation method of energy storage material |
| CN104987075A (en) * | 2015-06-09 | 2015-10-21 | 四川大学 | Rotary dynamic continuous preparation method for (M1, M2) (CxN1-x) powder and rotary dynamic continuous sintering device |
| CN104987075B (en) * | 2015-06-09 | 2019-05-21 | 四川大学 | (M1,M2)(CxN1-x) powder the rotary continuous preparation method of dynamic and rotary dynamic continuous sintering device |
| WO2018223439A1 (en) * | 2017-06-09 | 2018-12-13 | 深圳市星特烁科技有限公司 | Vacuum sintering furnace enabling continuous production |
| WO2020172784A1 (en) * | 2019-02-26 | 2020-09-03 | Linde Gmbh | Method and apparatus for producing ternary cathode material |
| CN110937629A (en) * | 2019-12-07 | 2020-03-31 | 西北有色金属研究院 | Method for preparing Bi-2212 precursor powder by inclined rotary sintering method |
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Application publication date: 20120509 |