CN109400213A - A kind of preparation method of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion - Google Patents

A kind of preparation method of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion Download PDF

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Publication number
CN109400213A
CN109400213A CN201811386145.4A CN201811386145A CN109400213A CN 109400213 A CN109400213 A CN 109400213A CN 201811386145 A CN201811386145 A CN 201811386145A CN 109400213 A CN109400213 A CN 109400213A
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coating
preparation
powder
calcium hexaluminate
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顾峰
史天石
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JIANGSU ZHONGZHENG CERAMIC SCIENCE & TECHNOLOGY Co Ltd
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JIANGSU ZHONGZHENG CERAMIC SCIENCE & TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5031Alumina
    • C04B41/5032Aluminates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a kind of preparation methods of compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion, include the following steps: the preparation of coated powder, the synthesis of coated powder, the processing of coated powder with compound, coating paste preparation, the preparation of coating and the firing of coating material, the melting temperature for crossing the compound calcium hexaluminate coating material of method preparation of the invention is very high, up to 1875 DEG C, the stability of reduction resistant to high temperatures is good, and resistance to corrosion is strong in alkaline environment;Compound calcium hexaluminate coating material prepared by the method for the present invention has laminar structured, Volumetric expansion when absorbable high temperature, keep the coefficient of expansion of crucible low, be not easy to crack and flake off, impurity in use can be effectively prevent to be mixed into anode material of lithium battery.

Description

A kind of compound calcium hexaluminate with high adhesion force, high temperature resistant reduction and alkaline erosion The preparation method of coating material
Technical field
The present invention relates to the fabricating technology fields of refractory material, in particular to a kind of to have high adhesion force, high temperature resistant The preparation method of the compound calcium hexaluminate coating material of reduction and alkaline erosion.
Background technique
With the continuous development of the industries such as new energy, environment-friendly engineering, research and manufacture to related ancillary equipment and material Requirement be also continuously improved.Attention of the preparation of anode material of lithium battery more and more more by each side in recent years, lithium battery Positive electrode mainly has cobalt acid lithium, LiMn2O4, nickel manganese cobalt ternary material and LiFePO4 etc., the uniformity of these positive electrodes, The indexs such as purity constrain the performance of material, and the impurity content of positive electrode is controlled in production an important factor for influencing its quality Being mixed into for impurity processed is the key that improve quality.The preparation of anode material of lithium battery is generally all anti-through high temperature solid-state by basic material Should synthesize, reactor therein is made of the refractory material of tool property, generally use at present cordierite-type, mullite, The crucibles such as corundum, but due to the positive electrode category strong basicity containing lithium, have very strong corrosivity, it directly results in violet blueness and is easily invaded Erosion makes positive electrode quality decline since objectionable impurities is mixed into crucible;Silicone content is high in mullite, and alkali resistance is poor, for a long time Positive electrode is mixed into using the spall that crucible internal walls will be made to generate and declines the performance of product;The heat of alumina crucible is swollen Swollen coefficient is larger, and crucible in use easily cracks, and influences service life, increase manufacturer's production cost.These problems begin The development of industry is limited eventually.The crucible material for studying, developing novel guarantee anode material of lithium battery performance becomes quite heavy The work wanted.With the development of the society, life kind, industrial class product are more and more abundant;Meanwhile the rise of big industry also makes the mankind Living environment become increasingly severe, requirement of the mankind to environmental protection is growing day by day, and countries in the world government is to environmental protection industry Investment is also increasing, and the industries such as coal gasification, waste incineration are flourishing, and this kind of industry is to high temperature kiln fire proofed wood Material proposes new demand.
Calcium hexaluminate is CaO-Al2O3Most important compound in this binary system, fusing point are up to 1875 DEG C, anti-height Temperature reduction stability it is good, resistance to corrosion is strong in alkaline environment, it is low to the wetability of molten metal and slag and its Have many advantages, such as low-solubility in slag containing iron oxide, is a kind of promising high-temperature flame-proof inner lining of furnace material, by extensive Concern and application.Common manufacturing method calcium hexaluminate density obtained is not high, and bulk density is only 2.5g/cm3Hereinafter, Have by calcium hexaluminate prepared by specific modification technology it is special laminar structured, since the presence of piece interlayer spacings makes Material can absorb certain volume change effect in temperature change, so that the material be made to have the lower coefficient of expansion;Simultaneously Since the laminar structured thermal conductivity for making material is lower, preferable insulation effect is made it have, calcium hexaluminate adds by appropriate Add modified realization part distortion of lattice, can be made into tool compared with the refractory material and reactor that high density, low bulk, anti-highly basic corrode (crucible).Spray etc. technique in existing refractory surface according to special technological means to be coated and form one Fixed thickness, then be sintered and be formed by curing composite material, fire proofed wood can be effectively promoted under the premise of cost is not significantly increased The performance of material is applicable at the high temperature in fields such as the increased quality to anode material of lithium battery synthesis crucible, environmental protection industry It is modified to manage inner lining of kiln refractory material.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind under the premise of cost is not significantly increased, and has high attachment Power, high temperature resistant reduction and compound calcium hexaluminate coating material of alkaline erosion and preparation method thereof.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
A kind of preparation side of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion Method includes the following steps:
A. the preparation of coated powder:
(1) by calcium carbonate, 1:6-1:8 ingredient is stand-by in molar ratio with alumina powder;
(2) it is put into grinding drum by the material being prepared in step (1), by material: water: mill ball quality is 1:1:1-1:1:2 Proportion ball milling 10-20 hours after discharge, 115-120 DEG C is dried for standby;
B. the synthesis of coated powder:
(3) mixture dried in step (2) is rolled into crushing, be fitted into crucible, it is small in 1460-1500 DEG C of heat preservation 3-5 When solid phase reaction, obtain that have laminar structured calcium hexaluminate powder spare;
C. the processing of coated powder with it is compound:
(4) by the calcium hexaluminate powder synthesized in step (3) is broken and mass fraction 0.8-1.2% rare earth oxide It is uniformly mixed stand-by;
(5) mixture in step (4) is packed into ball milling bucket, by material: water: ball mass ratio is the proportion of 1:1:1-1:1:2, It discharges within ball milling 8-12 hours, it is spare that 110-120 DEG C of drying obtains powder;
D. the preparation of coating paste:
(6) powder by step (5) drying crushes, and crosses 40 meshes, is placed in ball grinder, is separately added into triethanolamine examination Agent, PVA (polyvinyl alcohol), water and alumina balls, are in mass ratio powder: triethanolamine: PVA: water: alumina balls 1: The proportion of 0.001:0.0025:0.40:1.5 ball milling mixing 1-7 hours, exports slurry and crosses 40 mesh standard sieves, it is suitable to obtain viscosity Middle and high solid concentration, high dispersive, stable coating paste;
E. the preparation of coating:
(7) coating paste obtained in step (6) is put into rotation watering can, substrate table is sprayed at using rotation spray coating Face is controlled coating layer thickness in 0.5-2.0mm by the control rotary spraying time;
(8) spray piece after spraying is still in clean, ventilation environment after 1-2 hours, it is dry through 60-100 DEG C of baking oven Dry processing 3-5 hours, the moisture content of part to be sprayed less than 1% after can enter coating material the firing stage;
F. the firing of coating material:
(9) spray piece after being dried in step (8) is placed in high-temperature electric resistance furnace, temperature setting are as follows: room temperature to 400 DEG C, 0.8-1.2 DEG C/min;400-800 DEG C, 1.0-1.4/ minutes, keep the temperature 0.5-1.5 hours;800-1100 DEG C, 1-2 DEG C/minute Clock keeps the temperature 3-5 hours and is burnt into, and natural cooling is come out of the stove, that is, obtaining has answering for high adhesion force, high temperature resistant reduction and alkaline erosion Close calcium hexaluminate coating material.
Preferably, the purity of the calcium carbonate in the step (1) is greater than 98.5%, and granularity is less than 3 μm;The alumina powder Body is r-Al2O3, purity is greater than 99%.
Preferably, the rare earth oxide granularity in the step (4) is less than 2 μm.
Preferably, the rotation spray coating in the step (7) is constant speed spraying.
Preferably, the substrate in the step (7) is cordierite, mullite or corundum crucible.
By adopting the above technical scheme, the melting of (1) compound calcium hexaluminate coating material prepared by the method for the present invention Temperature is very high, and up to 1875 DEG C, the stability of reduction resistant to high temperatures is good, and resistance to corrosion is strong in alkaline environment;(2) by this hair The compound calcium hexaluminate coating material of bright method preparation has laminar structured, can absorb Volumetric expansion when high temperature, Keep the coefficient of expansion of crucible low, be not easy to crack and flake off, impurity in use can be effectively prevent to be mixed into anode material of lithium battery; (3) compound calcium hexaluminate coating material is prepared by means of the present invention, it is important to which powder table is improved by addition triethanolamine The current potential in face improves the solid concentration of slurry and reduces viscosity, the adhesion of slurry is improved by the way that PVA (polyvinyl alcohol) is added Can, obtain effective coating on substrate refractory material;(4) of the invention that there is high adhesion force, high temperature resistant reduction and alkaline erosion The preparation method of compound calcium hexaluminate coating material be a kind of by addition rare earth oxide La2O3Calcium hexaluminate is repaired Modified material is adornd, the purpose is to make to mix La3+The Al in tetrahedral interstice and octahedral interstice can partially be replaced3+, cause Synthetic product calcium hexaluminate phase cell parameter becomes larger, and distortion of lattice is formed by the ion exchange in fault of construction meeting accelerating structure It is gradually increased therewith with the agglutinating property of the fast growth of crystal grain, the calcium hexaluminate material of synthesis, and six aluminic acids of synthesis can be improved Calcium material thermal shock resistance plays the role of promoting the sintering of calcium hexaluminate material, is conducive to coating material and realizes cause in firing Densification improves intensity, while increasing the adhesive force with base material, prevents from falling off, adjustable by the incorporation for changing silicon powder The density of resulting coating is saved, to adapt to different needs, with the increase of incorporation, density improves Adhesion enhancement.
Detailed description of the invention
Fig. 1 is compound six with high adhesion force, high temperature resistant reduction and alkaline erosion prepared using method of the invention The SEM micro-structure diagram of calcium aluminate coating material.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing.It should be noted that for The explanation of these embodiments is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, disclosed below The each embodiment of the present invention involved in technical characteristic can be combined with each other as long as they do not conflict with each other.
Embodiment 1
A kind of preparation side of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion Method includes the following steps:
A. the preparation of coated powder:
(1) by calcium carbonate, 1:7 ingredient is stand-by in molar ratio with alumina powder;
(2) it is put into grinding drum by the material being prepared in step (1), by material: water: mill ball quality is matching for 1:1:1.5 It discharges after than ball milling 15 hours, 115 DEG C are dried for standby;
B. the synthesis of coated powder:
(3) mixture dried in step (2) is rolled into crushing, be fitted into crucible, it is anti-in 1480 DEG C of heat preservations, 4 hours solid phases It answers, it is spare to obtain the laminar structured calcium hexaluminate powder of tool;
C. the processing of coated powder with it is compound:
(4) the calcium hexaluminate powder synthesized in step (3) is crushed and 1.0% rare earth oxide of mass fraction mixes It is uniformly stand-by;
(5) mixture in step (4) is packed into ball milling bucket, by material: water: ball mass ratio is the proportion of 1:1:1.5, ball milling It discharges within 10 hours, it is spare that 115 DEG C of drying obtain powder;
D. the preparation of coating paste:
(6) powder by step (5) drying crushes, and crosses 40 meshes, is placed in ball grinder, is separately added into triethanolamine examination Agent, PVA (polyvinyl alcohol), water and alumina balls, are in mass ratio powder: triethanolamine: PVA: water: alumina balls 1: The proportion of 0.001:0.0025:0.40:1.5 ball milling mixing 4 hours, exports slurry and crosses 40 mesh standard sieves, it is suitable to obtain viscosity Middle and high solid concentration, high dispersive, stable coating paste;
E. the preparation of coating:
(7) coating paste obtained in step (6) is put into rotation watering can, substrate table is sprayed at using rotation spray coating Face is controlled coating layer thickness in 1.0mm by the control rotary spraying time;
(8) spray piece after spraying is still in clean, ventilation environment after 1.5 hours, at 80 DEG C of oven dryings Reason 4 hours, the moisture content of part to be sprayed less than 1% after can enter coating material the firing stage;
F. the firing of coating material:
(9) spray piece after being dried in step (8) is placed in high-temperature electric resistance furnace, temperature setting are as follows: room temperature to 400 DEG C, 1.0 DEG C/min;600 DEG C, 1.2/ minute, keep the temperature 1.0 hours;It 1000 DEG C, 1.5 DEG C/min, keeps the temperature 4 hours and is burnt into, it is natural It is cooling, it comes out of the stove, that is, obtains the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion.
Preferably, the purity of the calcium carbonate in the step (1) is greater than 98.5%, and granularity is less than 3 μm;The alumina powder Body is r-Al2O3, purity is greater than 99%.
Preferably, the rare earth oxide granularity in the step (4) is less than 2 μm.
Preferably, the rotation spray coating in the step (7) is constant speed spraying.
Preferably, the substrate in the step (7) is cordierite, mullite or corundum crucible.
Embodiment 2
A kind of preparation side of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion Method includes the following steps:
A. the preparation of coated powder:
(1) by calcium carbonate, 1:6 ingredient is stand-by in molar ratio with alumina powder;
(2) it is put into grinding drum by the material being prepared in step (1), by material: water: mill ball quality is the proportion of 1:1:1 Ball milling discharges after 10 hours, and 115 DEG C are dried for standby;
B. the synthesis of coated powder:
(3) mixture dried in step (2) is rolled into crushing, be fitted into crucible, it is anti-in 1460 DEG C of heat preservations, 3 hours solid phases It answers, it is spare to obtain the laminar structured calcium hexaluminate powder of tool;
C. the processing of coated powder with it is compound:
(4) the calcium hexaluminate powder synthesized in step (3) is crushed and 0.8% rare earth oxide of mass fraction mixes It is uniformly stand-by;
(5) mixture in step (4) is packed into ball milling bucket, by material: water: ball mass ratio is the proportion of 1:1:1, ball milling 8 Hour discharging, it is spare that 110 DEG C of drying obtain powder;
D. the preparation of coating paste:
(6) powder by step (5) drying crushes, and crosses 40 meshes, is placed in ball grinder, is separately added into triethanolamine examination Agent, PVA (polyvinyl alcohol), water and alumina balls, are in mass ratio powder: triethanolamine: PVA: water: alumina balls 1: The proportion of 0.001:0.0025:0.40:1.5 ball milling mixing 1 hour, exports slurry and crosses 40 mesh standard sieves, it is suitable to obtain viscosity Middle and high solid concentration, high dispersive, stable coating paste;
E. the preparation of coating:
(7) coating paste obtained in step (6) is put into rotation watering can, substrate table is sprayed at using rotation spray coating Face is controlled coating layer thickness in 0.5mm by the control rotary spraying time;
(8) spray piece after spraying is still in clean, ventilation environment after 1 hour, through 60 DEG C of oven drying processing 3 Hour, the moisture content of part to be sprayed less than 1% after can enter coating material the firing stage;
F. the firing of coating material:
(9) spray piece after being dried in step (8) is placed in high-temperature electric resistance furnace, temperature setting are as follows: room temperature to 400 DEG C, 0.8 DEG C/min;400 DEG C, 1.0/ minute, keep the temperature 0.5 hour;It 800 DEG C, 1 DEG C/min, keeps the temperature 3 hours and is burnt into, it is naturally cold But, it comes out of the stove, that is, obtains the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion.
Preferably, the purity of the calcium carbonate in the step (1) is greater than 98.5%, and granularity is less than 3 μm;The alumina powder Body is r-Al2O3, purity is greater than 99%.
Preferably, the rare earth oxide granularity in the step (4) is less than 2 μm.
Preferably, the rotation spray coating in the step (7) is constant speed spraying.
Preferably, the substrate in the step (7) is cordierite, mullite or corundum crucible.
Embodiment 3
A kind of preparation side of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion Method includes the following steps:
A. the preparation of coated powder:
(1) by calcium carbonate, 1:8 ingredient is stand-by in molar ratio with alumina powder;
(2) it is put into grinding drum by the material being prepared in step (1), by material: water: mill ball quality is the proportion of 1:1:2 Ball milling discharges after 20 hours, and 120 DEG C are dried for standby;
B. the synthesis of coated powder:
(3) mixture dried in step (2) is rolled into crushing, be fitted into crucible, it is anti-in 1500 DEG C of heat preservations, 5 hours solid phases It answers, it is spare to obtain the laminar structured calcium hexaluminate powder of tool;
C. the processing of coated powder with it is compound:
(4) the calcium hexaluminate powder synthesized in step (3) is crushed and 1.2% rare earth oxide of mass fraction mixes It is uniformly stand-by;
(5) mixture in step (4) is packed into ball milling bucket, by material: water: ball mass ratio is the proportion of 1:1:2, ball milling 12 Hour discharging, it is spare that 120 DEG C of drying obtain powder;
D. the preparation of coating paste:
(6) powder by step (5) drying crushes, and crosses 40 meshes, is placed in ball grinder, is separately added into triethanolamine examination Agent, PVA (polyvinyl alcohol), water and alumina balls, are in mass ratio powder: triethanolamine: PVA: water: alumina balls 1: The proportion of 0.001:0.0025:0.40:1.5 ball milling mixing 7 hours, exports slurry and crosses 40 mesh standard sieves, it is suitable to obtain viscosity Middle and high solid concentration, high dispersive, stable coating paste;
E. the preparation of coating:
(7) coating paste obtained in step (6) is put into rotation watering can, substrate table is sprayed at using rotation spray coating Face is controlled coating layer thickness in 2.0mm by the control rotary spraying time;
(8) spray piece after spraying was still in clean, ventilation environment after 2 hours, is handled through 100 DEG C of oven dryings 5 hours, the moisture content of part to be sprayed less than 1% after can enter coating material the firing stage;
F. the firing of coating material:
(9) spray piece after being dried in step (8) is placed in high-temperature electric resistance furnace, temperature setting are as follows: room temperature to 400 DEG C, 1.2 DEG C/min;800 DEG C, 1.4/ minute, keep the temperature 1.5 hours;It 1100 DEG C, 2 DEG C/min, keeps the temperature 5 hours and is burnt into, it is naturally cold But, it comes out of the stove, that is, obtains the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion.
Preferably, the purity of the calcium carbonate in the step (1) is greater than 98.5%, and granularity is less than 3 μm;The alumina powder Body is r-Al2O3, purity is greater than 99%.
Preferably, the rare earth oxide granularity in the step (4) is less than 2 μm.
Preferably, the rotation spray coating in the step (7) is constant speed spraying.
Preferably, the substrate in the step (7) is cordierite, mullite or corundum crucible.
As shown in Figure 1, the answering with high adhesion force, high temperature resistant reduction and alkaline erosion prepared using method of the invention The SEM micro-structure diagram of calcium hexaluminate coating material is closed, under a scanning electron microscope, the shape of particle is in the six of rule mostly Side shape, layer structure is obvious, even particle distribution, and the structure between particle and particle is more close, and the porosity is low, the hair of crystal Educate also more complete, the average-size of crystal grain is about 2 μm, with a thickness of 0.3 μm.
In conjunction with attached drawing, the embodiments of the present invention are described in detail above, but the present invention is not limited to described implementations Mode.For a person skilled in the art, in the case where not departing from the principle of the invention and spirit, to these embodiments A variety of change, modification, replacement and modification are carried out, are still fallen in protection scope of the present invention.

Claims (5)

1. a kind of preparation method of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion, It is characterized by comprising following steps:
A. the preparation of coated powder:
(1) by calcium carbonate, 1:6-1:8 ingredient is stand-by in molar ratio with alumina powder;
(2) it is put into grinding drum by the material being prepared in step (1), by material: water: mill ball quality is matching for 1:1:1-1:1:2 It discharges after than ball milling 10-20 hours, 115-120 DEG C is dried for standby;
B. the synthesis of coated powder:
(3) mixture dried in step (2) is rolled into crushing, be fitted into crucible, consolidated within heat preservation 3-5 hours in 1460-1500 DEG C It is spare to obtain the laminar structured calcium hexaluminate powder of tool for phase reaction;
C. the processing of coated powder with it is compound:
(4) the calcium hexaluminate powder synthesized in step (3) is crushed and mass fraction 0.8-1.2% rare earth oxide mixes It is uniformly stand-by;
(5) mixture in step (4) is packed into ball milling bucket, by material: water: ball mass ratio is the proportion of 1:1:1-1:1:2, ball milling It discharges within 8-12 hours, it is spare that 110-120 DEG C of drying obtains powder;
D. the preparation of coating paste:
(6) powder by step (5) drying crushes, and crosses 40 meshes, is placed in ball grinder, is separately added into triethanolamine reagent, PVA (polyvinyl alcohol), water and alumina balls are in mass ratio powder: triethanolamine: PVA: water: alumina balls 1:0.001: The proportion of 0.0025:0.40:1.5 ball milling mixing 1-7 hours, exports slurry and crosses 40 mesh standard sieves, obtain moderate viscosity, height Solid concentration, high dispersive, stable coating paste;
E. the preparation of coating:
(7) coating paste obtained in step (6) is put into rotation watering can, substrate surface is sprayed at using rotation spray coating, Coating layer thickness is controlled in 0.5-2.0mm by the control rotary spraying time;
(8) spray piece after spraying is still in clean, ventilation environment after 1-2 hours, at 60-100 DEG C of oven drying Reason 3-5 hour, the moisture content of part to be sprayed less than 1% after can into coating material the firing stage;
F. the firing of coating material:
(9) spray piece after being dried in step (8) is placed in high-temperature electric resistance furnace, temperature setting are as follows: room temperature to 400 DEG C, 0.8-1.2 DEG C/min;400-800 DEG C, 1.0-1.4/ minutes, keep the temperature 0.5-1.5 hours;800-1100 DEG C, 1-2 DEG C/min, It is burnt within heat preservation 3-5 hours, natural cooling is come out of the stove, that is, obtaining has compound the six of high adhesion force, high temperature resistant reduction and alkaline erosion Calcium aluminate coating material.
2. the compound calcium hexaluminate coating according to claim 1 with high adhesion force, high temperature resistant reduction and alkaline erosion The preparation method of material, it is characterised in that: the purity of the calcium carbonate in the step (1) is greater than 98.5%, and granularity is less than 3 μm; The alumina powder is r-Al2O3, purity is greater than 99%.
3. the compound calcium hexaluminate coating according to claim 1 with high adhesion force, high temperature resistant reduction and alkaline erosion The preparation method of material, it is characterised in that: the rare earth oxide granularity in the step (4) is less than 2 μm.
4. the compound calcium hexaluminate coating according to claim 1 with high adhesion force, high temperature resistant reduction and alkaline erosion The preparation method of material, it is characterised in that: the rotation spray coating in the step (7) is constant speed spraying.
5. the compound calcium hexaluminate coating according to claim 1 with high adhesion force, high temperature resistant reduction and alkaline erosion The preparation method of material, it is characterised in that: the substrate in the step (7) is cordierite, mullite or corundum crucible.
CN201811386145.4A 2018-11-20 2018-11-20 A kind of preparation method of the compound calcium hexaluminate coating material with high adhesion force, high temperature resistant reduction and alkaline erosion Pending CN109400213A (en)

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* Cited by examiner, † Cited by third party
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CN113860918A (en) * 2021-11-15 2021-12-31 北京中科海钠科技有限责任公司 Alkali-resistant coating slurry, crucible with alkali-resistant coating and preparation method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113860918A (en) * 2021-11-15 2021-12-31 北京中科海钠科技有限责任公司 Alkali-resistant coating slurry, crucible with alkali-resistant coating and preparation method

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