CN105084921A - Preparation process for anticorrosion saggar for calcination of lithium battery cathode material - Google Patents

Preparation process for anticorrosion saggar for calcination of lithium battery cathode material Download PDF

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CN105084921A
CN105084921A CN201510607356.6A CN201510607356A CN105084921A CN 105084921 A CN105084921 A CN 105084921A CN 201510607356 A CN201510607356 A CN 201510607356A CN 105084921 A CN105084921 A CN 105084921A
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preparation
saggar
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powder
slurry
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韦国文
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Suzhou Rui Bang Ceramic New Material Co Ltd
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Suzhou Rui Bang Ceramic New Material Co Ltd
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Abstract

The invention discloses a preparation process for an anticorrosion saggar for calcination of a lithium battery cathode material. The preparation process includes the steps of primary aggregate preparation, secondary aggregate preparation, matrix material preparation and saggar preparation. The steps of primary aggregate preparation and secondary aggregate preparation sequentially comprise the procedures of powder preparation, ball milling slurry preparation, slurry preparation, slurry storage, blank preparation, blank drying and blank calcination. The step of matrix material preparation sequentially includes the procedures of matrix material burdening, matrix material ball milling and matrix material screening. The step of saggar preparation sequentially includes the procedures of saggar material preparation, bundling pressing, maintenance drying and high-temperature firing. Primary aggregates, secondary aggregates and a matrix material are mixed according to the process ratio to form a saggar material. The anticorrosion saggar has the alkali-resistant and anti-corrosion functions, and pure magnesium hydrate, aluminum oxide and silicon dioxide are calcinated to obtain high-purity cordierite material aggregates; magnesium-aluminum-rich spinel powder is added for preparing the matrix material, and the saggar is small in heat expansion coefficient, high in heat impact resistance and long in service life.

Description

The corrosion-resistant saggar preparation process of a kind of calcining anode material of lithium battery
Technical field
The present invention relates to a kind of fire-resistant corrosion-resistant saggar kiln furnitures technical equipment field, particularly the corrosion-resistant saggar preparation process of one calcining anode material of lithium battery.
Background technology
Along with the development of electronic product is with universal, anode material of lithium battery obtains unprecedented application, anode material of lithium battery powder has to pass through the calcining of high temperature kiln, burn till and must adopt saggar to load, when utilizing saggar to carry material high-temperature calcination, by carrying Quilonum Retard and alkaline metal oxide carries out pyroreaction in saggar, at high temperature in basic oxide and saggar top layer acidic oxide silicon-dioxide, intermediate oxide as mullite (3Al 2o 32SiO 2) there is chemical reaction, produce glassy substances; Saggar is reused through cold and hot, generally uses and will scrap for 3-5 times.
In prior art, saggar has two kinds of structures, and one is be made up of single matrix material, this saggar can by anode material of lithium battery permeating corrosion after using, cause saggar surface to be stained with to cover a small amount of positive electrode material and cannot clear up, can only bury, cause industrial refuse; Once after being embedded in underground, inevitably cause heavy metal contamination; Another kind is then bilayer structure, namely spray on base layer surface, after using certain number of times, sprayed coating and the matrix physicochemical property on saggar surface change, saggar surface starts to peel off, not only pollute positive electrode material, cause yield rate lower, also easily cause the security incident of follow-up lithium cell.
Shortcoming of the prior art is: produce penetrating power and the strong Lithium Oxide 98min of reactive behavior owing to decomposing, corrode, cause saggar to peel off to saggar, pulverizing problem, and the work-ing life of saggar declines; For erosion resistance and the work-ing life of saggar, research and development corrosion resistance is good, and long-life saggar has ten important effects for the production of anode material of lithium battery and technical progress.
Summary of the invention
For solving the problems of the technologies described above, the invention provides the corrosion-resistant saggar preparation process of a kind of calcining anode material of lithium battery, for deficiency of the prior art, the corrosion-resistant saggar of design preparation calcining anode material of lithium battery, adopts magnesium hydroxide, aluminum oxide, silicon-dioxide to prepare aggregate; Add magnesium-rich spinel powder and prepare substrate material, prepare corrosion resistant saggar by aggregate and substrate material; Saggar anti-erosion, not peel off and efflorescence, saggar long service life.
For achieving the above object, technical scheme of the present invention is as follows: the corrosion-resistant saggar preparation process of one calcining anode material of lithium battery, comprises the preparation of one-level aggregate, the preparation of secondary aggregate and substrate material preparation, saggar and prepares, it is characterized in that:
Described one-level aggregate preparation and secondary aggregate are prepared and are comprised powder preparation, the preparation of ball milling slurry, slurry preparation successively, slurry stores, prepared by idiosome, idiosome is dry, idiosome calcining; Described substrate material preparation comprises substrate material batching, the screening of substrate material ball milling, substrate material successively; Described casket body is prepared and is comprised sagger preparation successively, tie up compacting, maintenance is dry, high temperature burns till; Described one-level aggregate, secondary aggregate and substrate material carry out mixing obtained casket body material according to processing compound.
Described calcining anode material of lithium battery corrosion-resistant saggar preparation process flow process is:
One, aggregate preparation:
1.1, powder preparation, select molecular weight to be 65-67, purity is the Mg (OH) of 99.8-99.9% 2, mean particle size is 3 microns, and add-on is 18-22%; Select α-aluminum oxide, granularity 2000 order, purity 99.5-99.8%, add-on is 34-36%; Select silicon-dioxide, granularity 5-10 microns, purity 99-99.5%, add-on is 48-52%; Premixing machine is adopted to be mixed by powder for subsequent use;
1.2, ball milling slurry preparation, use Ball-stirring mill, in Ball-stirring mill, first add water, add-on is 30 of powder---40%; Add the aluminum oxide ball milling pearl of diameter 5 millimeters again, be situated between as mill, consumption is 2 times of powder consumption; Be uniformly mixed, obtain ball milling slurry;
1.3, slurry preparation, in the ball milling slurry in step 1.2, add dispersion agent D134, add-on is 0.55% of powder; Add defoamer F-102, add-on is 0.02% of powder; Be uniformly mixed; Add the mixed powder in step 1, add powder by the amount dropping into powder 10-15%; After adding mixed powder, open and stir, ball milling is until after powder becomes solution, again add mixed powder, and amounting to and throwing add-on is the powder of 35-40%; After powder has all added, start rapid stirring, ball milling, after 4-6 hours, detects and confirms to stop stirring after slurry viscosity declines;
1.4, slurry stores, and the slurry in Ball-stirring mill is put into agitated pool, and the stir shaft in described agitated pool should keep not stopping low rate mixing, prevents slurry from occurring precipitation;
1.5, idiosome preparation, by the slurry in step 1.4, be transported in pressure filter, carry out pressure filtration, leach the moisture content in slurry, obtain moisture content about 8-10% idiosome;
1.6, idiosome is dry, and by the idiosome in step 1.5, be placed in baking room, set temperature is 60-80 DEG C, dries, obtains dry idiosome;
1.7, idiosome calcining, by the dry idiosome in step 1.6, load in calcining furnace, arrange calcining temperature and be 1370-1390 DEG C, the sintering soak time is 6-8 hours, obtains the ripe cordierite material of highly purified bulk;
1.8, one-level aggregate preparation, by ripe for the bulk in step 1.7 cordierite material, is pulverized by pulverizer, further, sieves through vibratory screening apparatus, choose the particle that powder granularity is 0.3-1.2mm; After obtaining granularity material, this granularity trichroite, as primary granule aggregate;
1.9, secondary aggregate preparation, the one-level aggregate in selecting step 1.8, ratio is 25%-35%, then adds the magnesium-aluminium spinel 20-30% that mean particle size is 0.135mm; As secondary coarse particles aggregate; Two, substrate material preparation:
2.1, substrate material batching, chooses magnesium hydroxide, mean particle size 3 microns, consumption 8-10%, α-aluminum oxide, 2000 orders, consumption 13-15%; Silica 1 8-22%, granularity 0.15 micron; Magnesium-rich spinel micro mist, granularity 0.040mm-0.050mm; Described rich magnesium-aluminium spinel uses as strong corrosion inhibitor;
2.2, substrate material ball milling, by kind of the batching of 4 in step 2.1, put into rhombus ball mill, put into the metallic bead that diameter 10-30mm surface coating has urethane, add-on is 2 times of powder, and open rhombus ball mill and start ball milling, the time of ball milling is 2h;
2.3, substrate material screening, by the powder obtained in step 2.2, by vibratory screening apparatus, uses 60 eye mesh screens to sieve, and obtaining minus sieve body is substrate material;
Three, casket body preparation:
3.1, sagger preparation, according to processing compound, takes the one-level aggregate in step 1.8, takes the secondary aggregate in step 1.9, add in mixing pan, carry out the premix of 3-5min by two kinds of granulated aggregates; Add PVA binding agent again, expect during add-on 6%; Add releasing agent again, add-on is 0.5% of doses; Open premixing machine and proceed premix 5min, till confirming that dry granules material surface is all wetted; Take the substrate material in step 2.3; Substrate material is added mixing pan mix, mixing time is 30min; Turn off mixing pan, detect the material that mixes and whether reach standard, to exert oneself Zhua Niecheng group shape tack-free for qualified with hand;
3.2, tie up compacting, the material body in step 3.1 is taken out, puts into Plastic film Bag and tie up, then press the object being about 100kg, suppress; The time of tying up is 36 hours, starts shaping and obtains a saggar, and the pressure of compacting is 500kg/cm 2, obtain saggar green compact;
3.3, maintenance is dry, and by the saggar green compact in step 3.2, be placed in maintenance drying in drying shed, design temperature is 40-60 DEG C, and the maintenance carrying out 24 hours in described drying shed is dry;
3.4, high temperature burns till, and is positioned in calcining furnace by the saggar green compact in step 3.3, in sintering process, is warming up to 250 DEG C, starts to be incubated 2 hours, to remove the crystal water in substrate material; Then be warming up to 300 DEG C with 20 DEG C/h speed, carry out insulation 1-2 hours at this temperature; At 300 DEG C-800 DEG C, heat up, in order to get rid of organism with 60 DEG C of speed per hour; Then be warmed up to 1370 DEG C-1390 DEG C with the speed of 80 DEG C-100 DEG C per hour, and be incubated 4-6 hours; Naturally cooling kiln discharge, obtains corrosion-resistant saggar finished product.
By technique scheme, the beneficial effect of technical solution of the present invention is: the corrosion-resistant saggar of design preparation calcining anode material of lithium battery, adopts magnesium hydroxide, aluminum oxide, silicon-dioxide to prepare aggregate; Add magnesium-rich spinel powder and prepare substrate material, prepare corrosion resistant saggar by aggregate and substrate material; Saggar anti-erosion, not peel off and efflorescence, saggar long service life.Its concrete beneficial effect is:
1, the corrosion-resistant saggar of preparation has the corrosion-resistant function of alkali-resistivity, and anode material of lithium battery pH value is up to 13-14, belongs to basic material, there is very strong corrosive nature, if saggar kiln furnitures are corroded, will anode material of lithium battery be polluted, have a strong impact on the quality of positive electrode material.
2, in prior art, all adopt kaolin under normal circumstances, talcum powder is as the main raw material(s) of synthesis of dichroite, because of in these mineral products materials containing much impurity as potassium, sodium, iron etc., these impurity are easy to be corroded, and therefore the present invention manufactures the higher alkaline cordierite material of purity; Control kaolin, the impurity that talcum powder brings, selects high-purity magnesium oxide, aluminum oxide, silicon-dioxide three kinds of materials to carry out synthesis of dichroite material, obtains the few purity of a kind of impurity high by wet-mixed, the synthesis of dichroite material mixed, obtains highly purified cordierite material by calcining.
3, formulating of recipe of the present invention selects basic material, spinel basic material, and trichroite basic material also guarantees that material purity controls impurity, and such Material selec-tion guarantees that the alkalescence of saggar and basic material chemical reaction can not occur, and can not be corroded.
4, described aggregate, what trichroite grog and substrate material adopted is that same kind raw material and proportioning are made, by same technique and same firing temperature calcining synthesis, therebetween it is basically identical that thermal expansivity can obtain coupling, it is strong that such guarantee saggar can have very little thermal expansivity thermal shock resistance, be subject to can not producing tiny crack under thermal shock conditions, reaching resistance to erosion function and the good product of thermal shock resistance.
5, the present invention introduces the large Spinel micropowder of specific surface area in substrate material, makes these strong basicity spinels to be evenly distributed like this, more promotes the corrosion resistance of finished product saggar.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the one calcining anode material of lithium battery corrosion-resistant saggar preparation process schematic flow sheet disclosed in the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
According to Fig. 1, the invention provides the corrosion-resistant saggar preparation process of one calcining anode material of lithium battery, comprise the preparation of one-level aggregate, the preparation of secondary aggregate and substrate material preparation, saggar and prepare.
Described one-level aggregate preparation and secondary aggregate are prepared and are comprised powder preparation, the preparation of ball milling slurry, slurry preparation successively, slurry stores, prepared by idiosome, idiosome is dry, idiosome calcining; Described substrate material preparation comprises substrate material batching, the screening of substrate material ball milling, substrate material successively; Described casket body is prepared and is comprised sagger preparation successively, tie up compacting, maintenance is dry, high temperature burns till; Described one-level aggregate, secondary aggregate and substrate material carry out mixing obtained casket body material according to processing compound.
Described calcining anode material of lithium battery corrosion-resistant saggar preparation process flow process is:
One, aggregate preparation:
1.1, powder preparation, select molecular weight to be 65---67, purity is the Mg (OH) of 99.8-99.9% 2, mean particle size is 3 microns, and add-on is 20%; Select α-aluminum oxide, granularity 2000 order, purity 99.5-99.8%, add-on is 35%; Select silicon-dioxide, granularity 5-10 microns, purity 99-99.5%, add-on is 50%; Premixing machine is adopted to be mixed by powder for subsequent use;
1.2, ball milling slurry preparation, use Ball-stirring mill, in Ball-stirring mill, first add water, add-on is 35% of powder; Add the aluminum oxide ball milling pearl of diameter 5 millimeters again, be situated between as mill, consumption is 2 times of powder consumption; Be uniformly mixed, obtain ball milling slurry;
1.3, slurry preparation, in the ball milling slurry in step 1.2, add dispersion agent D134, add-on is 0.55% of powder; Add defoamer F-102, add-on is 0.02% of powder; Be uniformly mixed; Add the mixed powder in step 1, add powder by the amount dropping into powder 10-15%; After adding mixed powder, open and stir, ball milling is until after powder becomes solution, again add mixed powder, and amounting to and throwing add-on is the powder of 40%; After powder has all added, start rapid stirring, ball milling, after 5 hours, detects and confirms to stop stirring after slurry viscosity declines;
1.4, slurry stores, and the slurry in Ball-stirring mill is put into agitated pool, and the stir shaft in described agitated pool should keep not stopping low rate mixing, prevents slurry from occurring precipitation;
1.5, idiosome preparation, by the slurry in step 1.4, be transported in pressure filter, carry out pressure filtration, leach the moisture content in slurry, obtain moisture content about 8-10% idiosome;
1.6, idiosome is dry, and by the idiosome in step 1.5, be placed in baking room, set temperature is 780 DEG C, dries, obtains dry idiosome;
1.7, idiosome calcining, by the dry idiosome in step 1.6, load in calcining furnace, arrange calcining temperature and be 1380-1400 DEG C, the sintering soak time is 6-8 hours, obtains the ripe cordierite material of highly purified bulk;
1.8, one-level aggregate preparation, by ripe for the bulk in step 1.7 cordierite material, is pulverized by pulverizer, further, sieves through vibratory screening apparatus, choose the particle that powder granularity is 0.3-1.0mm; After obtaining granularity material, this granularity high purity trichroite, as primary granule aggregate;
1.9, secondary aggregate preparation, the one-level aggregate in selecting step 1.8, ratio is 30%, then adds the magnesium-aluminium spinel 25% that mean particle size is 0.135mm; As secondary coarse particles aggregate;
Two, substrate material preparation:
2.1, substrate material batching, chooses magnesium hydroxide, mean particle size 3 microns, consumption 9%, α-aluminum oxide, 2000 orders, consumption 15%; Silicon-dioxide 20%, granularity 0.15 micron; Magnesium-rich spinel micro mist, granularity 0.045mm; Described rich magnesium-aluminium spinel uses as corrosion inhibitor;
2.2, substrate material ball milling, by kind of the batching of 4 in step 2.1, put into rhombus ball mill, put into the metallic bead that diameter 10-30mm surface coating has urethane, add-on is 2 times of powder, and open rhombus ball mill and start ball milling, the time of ball milling is 2h;
2.3, substrate material screening, by the powder obtained in step 2.2, by vibratory screening apparatus, uses 50 eye mesh screens to sieve, and obtaining minus sieve body is substrate material;
Three, casket body preparation:
3.1, sagger preparation, according to processing compound, takes the one-level aggregate in step 1.8, takes the secondary aggregate in step 1.9, add in mixing pan, carry out the premix of 3-5min by two kinds of granulated aggregates; Add PVA binding agent again, expect during add-on 6%; Add releasing agent again, add-on is 0.5% of doses; Open premixing machine and proceed premix 5min, till confirming that dry granules material surface is all wetted; Take the substrate material in step 2.3; Substrate material is added mixing pan mix, mixing time is 30min; Turn off mixing pan, detect the material mixed and whether reach standard, firmly pinch with hand tack-free for qualified;
3.2, tie up compacting, the material body in step 3.1 is taken out, puts into Plastic film Bag and tie up, then press the object being about 100kg, suppress; The time of tying up is 36 hours, starts shaping and obtains a saggar, and the pressure of compacting is 500kg/cm 2, obtain saggar green compact;
3.3, maintenance is dry, and by the saggar green compact in step 3.2, be placed in maintenance drying in drying shed, design temperature is 40-60 DEG C, and the maintenance carrying out 24 hours in described drying shed is dry;
3.4, high temperature burns till, and is positioned in calcining furnace by the saggar green compact in step 3.3, and in sintering process, temperature is 250 DEG C, starts to be incubated 2 hours, to remove the crystal water in substrate material; Then be warming up to 300 DEG C with 20 DEG C/h speed, be incubated at this temperature; At 300 DEG C-800 DEG C, heat up, in order to get rid of organism with 60 DEG C of speed per hour; Then be warmed up to 1370 DEG C-1390 DEG C with the speed of 100 DEG C per hour, and be incubated 6 hours; Cooling kiln discharge, obtains corrosion-resistant saggar finished product.
By above-mentioned specific embodiment, the invention has the beneficial effects as follows: the corrosion-resistant saggar of design preparation calcining anode material of lithium battery, adopts magnesium hydroxide, aluminum oxide, silicon-dioxide to prepare high purity trichroite aggregate; Add rich magnesium aluminium spinel powder and prepare substrate material, prepare corrosion resistant saggar by aggregate and substrate material; Saggar anti-erosion, not peel off and efflorescence, saggar long service life.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.

Claims (2)

1. calcine the corrosion-resistant saggar preparation process of anode material of lithium battery, it is characterized in that, comprise the preparation of one-level aggregate, the preparation of secondary aggregate and substrate material preparation, saggar and prepare; Described one-level aggregate preparation and secondary aggregate are prepared and are comprised powder preparation, the preparation of ball milling slurry, slurry preparation successively, slurry stores, prepared by idiosome, idiosome is dry, idiosome calcining; Described substrate material preparation comprises substrate material batching, the screening of substrate material ball milling, substrate material successively; Described casket body is prepared and is comprised sagger preparation successively, tie up compacting, maintenance is dry, high temperature burns till; Described one-level aggregate, secondary aggregate and substrate material carry out mixing obtained casket body material according to processing compound.
2. the corrosion-resistant saggar preparation process of one calcining anode material of lithium battery according to claim 1, it is characterized in that, described calcining anode material of lithium battery corrosion-resistant saggar preparation process flow process is:
2.1 aggregate preparations:
2.1.1, powder preparation, select molecular weight to be 65-67, purity is the Mg (OH) of 99.8-99.9% 2, mean particle size is 3 microns, and add-on is 18-22%; Select α-aluminum oxide, granularity 2000 order, purity 99.5-99.8%, add-on is 34-36%; Select silicon-dioxide, granularity 5-10 microns, purity 99-99.5%, add-on is 48-52%; Premixing machine is adopted to be mixed by powder for subsequent use;
2.1.2, ball milling slurry preparation, use Ball-stirring mill, in Ball-stirring mill, first add water, add-on is 30-40% of powder; Add the aluminum oxide ball milling pearl of diameter 5 millimeters again, be situated between as mill, consumption is 2 times of powder consumption; Be uniformly mixed, obtain ball milling slurry;
2.1.3, slurry preparation, in the ball milling slurry in step 2.1.2, add dispersion agent D134, add-on is 0.55% of powder; Add defoamer F-102, add-on is 0.02% of powder; Be uniformly mixed; Add the mixed powder in step 1, add powder by the amount dropping into powder 10-15%; After adding mixed powder, open and stir, ball milling is until after powder becomes solution, again add mixed powder, and amounting to and throwing add-on is the powder of 35-40%; After powder has all added, start rapid stirring, ball milling, after 4-6 hours, detects and confirms to stop stirring after slurry viscosity declines;
2.1.4, slurry store, the slurry in Ball-stirring mill is put into agitated pool, and the stir shaft in described agitated pool should keep not stopping low rate mixing, prevent slurry occur precipitation;
2.1.5, idiosome preparation, by the slurry in step 2.1.4, be transported in pressure filter, carry out pressure filtration, leach the moisture content in slurry, obtain moisture content about 8-10% idiosome;
2.1.6, idiosome is dry, and by the idiosome in step 2.1.5, be placed in baking room, set temperature is 60-80 DEG C, dries, obtains dry idiosome;
2.1.7, idiosome calcining, by the dry idiosome in step 2.1.6, load in calcining furnace, arrange calcining temperature and be 1370-1390 DEG C, the sintering soak time is 6-8 hours, obtains the ripe cordierite material of highly purified bulk;
2.1.8, one-level aggregate preparation, by ripe for the bulk in step 2.1.7 cordierite material, pulverized by pulverizer, further, sieve through vibratory screening apparatus, choose the particle that powder granularity is 0.3-1.2mm; After obtaining granularity material, this granularity trichroite, as primary granule aggregate;
2.1.9, secondary aggregate preparation, the one-level aggregate in selecting step 2.1.8, ratio is 25%-35%, then adds the magnesium-aluminium spinel 20-30% that mean particle size is 0.135mm; As secondary coarse particles aggregate;
2.2 substrate material preparations:
2.2.1, substrate material batching, choose magnesium hydroxide, mean particle size 3 microns, consumption 8-10%, α-aluminum oxide, 2000 orders, consumption 13-15%; Silica 1 8-22%, granularity 0.15 micron; Magnesium-rich spinel micro mist, granularity 0.040-0.050mm; Described rich magnesium-aluminium spinel uses as strong corrosion inhibitor;
2.2.2, substrate material ball milling, by 4 in step 2.2.1 kind batching, put into rhombus ball mill, put into the metallic bead that diameter 10-30mm surface coating has urethane, add-on is 2 times of powder, and open rhombus ball mill and start ball milling, the time of ball milling is 2h;
2.2.3, substrate material screening, by the powder obtained in step 2.2.2, by vibratory screening apparatus, use 60 eye mesh screens to sieve, obtaining minus sieve body is substrate material;
2.3 casket body preparations:
2.3.1, sagger preparation, according to processing compound, take the one-level aggregate in step 2.1.8, take the secondary aggregate in step 2.1.9, two kinds of granulated aggregates are added in mixing pan, carries out the premix of 3-5min; Add PVA binding agent again, expect during add-on 6%; Add releasing agent again, add-on is 0.5% of doses; Open premixing machine and proceed premix 5min, till confirming that dry granules material surface is all wetted; Take the substrate material in step 2.2.3; Substrate material is added mixing pan mix, mixing time is 30min; Turn off mixing pan, detect the material that mixes and whether reach standard, tack-free for qualified with hand Zhua Niecheng group shape of exerting oneself;
2.3.2, tie up compacting, the material body in step 2.3.1 is taken out, puts into Plastic film Bag and tie up, then press the object being about 100kg, suppress; The time of tying up is 36 hours, starts shaping and obtains a saggar, and the pressure of compacting is 500kg/cm 2, obtain saggar green compact;
2.3.3, maintenance is dry, and by the saggar green compact in step 2.3.2, it is dry to be placed in maintenance in drying shed, and design temperature is 40-60 DEG C, and the maintenance carrying out 24 hours in described drying shed is dry;
2.3.4, high temperature burns till, and is positioned in calcining furnace, in sintering process, is warming up to 250 DEG C, start to be incubated 2 hours, to remove the crystal water in substrate material by the saggar green compact in step 2.3.3; Then be warming up to 300 DEG C with 20 DEG C/h speed, carry out insulation 1-2 hours at this temperature; At 300 DEG C-800 DEG C, heat up, in order to get rid of organism with 60 DEG C of speed per hour; Then be warmed up to 1370 DEG C-1390 DEG C with the speed of 80 DEG C-100 DEG C per hour, and be incubated 4-6 hours; Naturally cooling kiln discharge, obtains corrosion-resistant saggar finished product.
CN201510607356.6A 2015-09-22 2015-09-22 Preparation process for anticorrosion saggar for calcination of lithium battery cathode material Pending CN105084921A (en)

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CN110467436A (en) * 2019-08-01 2019-11-19 辽宁科技大学 A kind of method that discarded magnesia-alumina-carbon brick prepares square magnesium stone-spinel matter saggar
CN111792950A (en) * 2020-07-11 2020-10-20 浙江锋锂新能源科技有限公司 Garnet solid electrolyte powder sintering container
CN112028650A (en) * 2020-09-03 2020-12-04 深圳市飞粤新材料科技有限公司 Sagger for lithium ion battery anode material
CN112680037A (en) * 2020-12-24 2021-04-20 湖北华联耐火材料有限公司 Anticorrosive paint and sagger coated with same
US11152603B2 (en) 2016-06-13 2021-10-19 Research Institute Of Industrial Science & Technology Saggar for firing active material of lithium secondary battery, and method for manufacturing active material using same
CN113773067A (en) * 2021-11-11 2021-12-10 长沙中瓷新材料科技有限公司 Sagger based on cordierite and production process thereof
CN114249358A (en) * 2022-03-01 2022-03-29 宜宾锂宝新材料有限公司 Positive electrode material and preparation method thereof

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Cited By (19)

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Publication number Priority date Publication date Assignee Title
US11152603B2 (en) 2016-06-13 2021-10-19 Research Institute Of Industrial Science & Technology Saggar for firing active material of lithium secondary battery, and method for manufacturing active material using same
CN108046792B (en) * 2017-12-12 2020-10-16 浙江大学 Cordierite-spinel sagger, preparation method and application thereof
CN108046792A (en) * 2017-12-12 2018-05-18 浙江大学 Light cordierite-spinel saggar, preparation method and applications
CN108033798A (en) * 2017-12-12 2018-05-15 浙江大学 Light cordierite-spinel hollow ball saggar, preparation method and applications
CN108083823B (en) * 2017-12-25 2021-02-12 浙江大学 Composite sagger, preparation method and application thereof
CN108083823A (en) * 2017-12-25 2018-05-29 浙江大学 Compound saggar, its preparation method and application
CN109467422A (en) * 2018-04-20 2019-03-15 湖南德景源科技有限公司 Dedicated high circulation special cermacis crucible of a kind of lithium electricity and preparation method thereof
CN108610024A (en) * 2018-05-07 2018-10-02 武汉科技大学 A kind of saggar and preparation method thereof for anode material for lithium-ion batteries roasting
CN108610024B (en) * 2018-05-07 2020-11-03 武汉科技大学 Sagger for roasting lithium ion battery anode material and preparation method thereof
CN108484188A (en) * 2018-05-07 2018-09-04 武汉科技大学 A kind of silicon carbide sagger and preparation method thereof for anode material of lithium battery roasting
CN108484188B (en) * 2018-05-07 2021-04-16 武汉科技大学 Silicon carbide sagger for roasting lithium battery anode material and preparation method thereof
CN109053165A (en) * 2018-05-18 2018-12-21 宜兴市东山新型材料有限公司 One kind is for lithium battery anode roasting saggar and preparation method thereof
CN110467436A (en) * 2019-08-01 2019-11-19 辽宁科技大学 A kind of method that discarded magnesia-alumina-carbon brick prepares square magnesium stone-spinel matter saggar
CN111792950A (en) * 2020-07-11 2020-10-20 浙江锋锂新能源科技有限公司 Garnet solid electrolyte powder sintering container
CN112028650A (en) * 2020-09-03 2020-12-04 深圳市飞粤新材料科技有限公司 Sagger for lithium ion battery anode material
CN112680037A (en) * 2020-12-24 2021-04-20 湖北华联耐火材料有限公司 Anticorrosive paint and sagger coated with same
CN113773067A (en) * 2021-11-11 2021-12-10 长沙中瓷新材料科技有限公司 Sagger based on cordierite and production process thereof
CN113773067B (en) * 2021-11-11 2022-01-18 长沙中瓷新材料科技有限公司 Sagger based on cordierite and production process thereof
CN114249358A (en) * 2022-03-01 2022-03-29 宜宾锂宝新材料有限公司 Positive electrode material and preparation method thereof

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Application publication date: 20151125