CN104046407B - A kind of lubricating oil（Fat）Use antiwear and antifriction compound additive - Google Patents
A kind of lubricating oil（Fat）Use antiwear and antifriction compound additive Download PDFInfo
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Abstract
The invention discloses a kind of lubricating oil（Fat）With antiwear and antifriction composite granule and preparation method thereof, it is related to one kind and can be used for lubricating oil, the oxide nano rare earth Coated muscovite composite granule in the fields such as lubricating grease, it is characterized in that with muscovite powder, rare-earth salts and its part are raw material, using the shearing force produced in mechanical milling process, impulsive force crushes solid-phase reaction system, increase the specific surface area of reactant, improve reaction rate, so as to improve the ratio of nucleation rate and growth rate, prepare fine, uniform predecessor, it is washed out, it is dried, control heat decomposition temperature and time, so as to the oxide nano rare earth Coated muscovite composite granule of different-grain diameter and cladding system can be obtained, the ultra-fine muscovite composite granule surface that oxide nano rare earth is coated is modified in varing proportions（0.5%‑3%）In adding base oil or lubricating grease, coefficient of friction can be reduced in four ball wears, reduce friction pair wear scar diameter.
Description
Technical field
The patent of invention belongs to " antiwear and antifriction composite granule and its technology of preparing ", is related to one kind and can be used for lubricating oil, profit
The oxide nano rare earth Coated muscovite composite granule in the fields such as consistent lubricant and preparation method thereof.
Background technology
With the development of modern industry, mechanized equipment is constantly to directions such as high speed, heavily loaded, integrated, high accuracy, long-lives
Development, friction, wear out failure become one of restriction equipment safety, reliability, technical bottleneck of service life.In order to reduce
The abrasion of equipment component of machine, extends the service life of equipment, and countries in the world all can be provided simultaneously with antiwear and antifriction in searching
With the lubricant or lube oil additive of repair function so as to new by being formed with self-repair function or in wear process
Layer of compensation making up abrasion, so as to realize equipping the dynamic selfreparing that parts wear is damaged, while by improving lubrication realization
Energy-saving and emission-reduction.Since the nineties in 20th century, nanometer technology is day by day ripe, and the research of nano material and range of application are also constantly expanding
Greatly, small-size effect, interface and skin effect, dimensional effect and the macro quanta tunnel effect having due to itself, gives
Which is different from the various special performances of traditional material so as to obtain in the research and application of emerging lubrication oil antiwear anti-friction agent
It is fast-developing.The nano-particle for being currently used as lube oil additive mainly has nano simple substance metal-powder, nano-oxide, receives
Rice hydroxide, nanometer sulfide, nano boric acid salt, polymer nano-microspheres and nano rare earth compound etc..Xia Yanqiu,
The antiwear and antifriction effect of copper nanoparticle, nickel powder, bismuth meal, molybdenum powder, zinc powder in base oil is have studied respectively after brightness, Chen Guoxu etc.,
The carbon series effect of micro Nano material, rare earth compound in lubricating oil simultaneously also quickly grows.02149209.3 disclosure of patent
A kind of antiwear and antifriction type lube oil additive and preparation method thereof, its component is：Aluminium, titanium, alundum (Al2O3) and titanium dioxide
Particle, particle diameter yardstick are 10-200nm, and content is 1-5%；Patent 03139679.8 be related to nano material prepare wear-resistant, antifriction,
Repairing type lubricant additive：With several nano ore micro mists and nanometer metal micropowder and surfactant, dispersant, suspension
Agent, coupling cosolvent and other lubricating oil preparations etc. are according to a certain percentage and technological operation code is formulated.Patent
200810053349.6 a kind of non-sulphur and phosphorus antiwear and friction reducing multifunctional additive agent and preparation method are provided.Patent 200910050138.1
A kind of nano-copper type lubricating oil additive is disclosed, the additive is mainly received by oil soluble reacting nano copper or oil soluble reactivity
Rice copper is constituted with oil solubility nanometer titanium dioxide.Patent 201010569467.X is by nano rare earth, metal, metal oxide and carbon
The nano material with wear-resistant, antifriction, extreme pressure activity such as serial nano material is used as lube oil additive.Patent
200410097197.1 disclose a kind of nano carbon lubricating additive for belonging to lubriation material technology of preparing.Patent
201010292980.9 a kind of spherical oxide nano rare earth lube oil additive and preparation method thereof is disclosed, using precipitation
Method prepares oxide nano rare earth, surface is carried out to nano-particle using organic carboxyl acid and is modified, formed the surface of nano-particle
One layer of organic coating layer, nano yttrium oxide surface is changed into lipophile from hydrophily.Patent 200710075247.X provides one kind
The additive of lubricating oil, its component is：Metallic nano-particle 2%-50%；Metallic compound nano particulate 1%-50%；Base oil or
Lubricating oil 0%-80%；Antioxidant 0%-20%；Detergent-dispersant additive 0%-25%.The disclosed mixing nanometer of patent 201110415955.X
Grease additive is made up of following component：Al2O3Powder：50%~80%；Cu powder：5%~15%；Al powder：15%~35%.Patent
201310494047.3 disclose a kind of preparation method of graft polymeric modification nano yttrium oxide lubriation material.
In terms of rare earth compound, research earlier finds, CeF3Deng rare earth inorganic compound have excellent high temperature and
Solid lubrication performance, but due to being insoluble in mineral oil, it is impossible to it is directly used as lube oil additive.Nearest relevant research shows,
It is modified by preparing to become nano-particle and carry out lipophilic surface, relevant rare earth inorganic compound can be made to have in mineral oil
There is good dispersiveness, show excellent extreme-pressure anti-wear antifriction performance.
Additionally, having introduced a kind of layer silicate mineral micro mist self-repair material from generation in 20 centurial years Russia, Ukraine
Since, layer silicate mineral particle makes the weight that research of the additive to Tribological Characteristics of Lubricating Oil causes domestic scholars
Depending on poplar Convicting, Li Huafeng, Chen Guoxu have studied laminar silicic acid calcium as the antiwear and friction reduction property of lubricating additive, α-laminar silicic acid
Antiwear and friction reduction property of the sodium as lubricating additive, Yu Helong, Xu Yi, Shi Peijing etc. have studied serpentine superfine powder and make to moisten
The tribological property of oil additive, Cao Juan, Zhang Zhenzhong, Zhao Fangxia have studied the kind lubrication oil drag mill of ultra-fine serpentine powders structural reform
Performance is damaged, Yang Qiming, Bai Zhimin have studied the material behavior of ultra-fine serpentine powders body, tribology intervening act and its industry should
With research finds：Phyllosilicate powder has unique metastable state layer structure, a large amount of unsaturations present on its plane of disruption
Key make its powder have very high characterization of adsorption, not only can adsorbing metal ions, can be with adsorpting anion（Group）With it is organic
Thing.There is eliminating hydroxide reaction under heating condition, layer structure is destroyed, and specific surface area is increased dramatically, and drastically increases
The ability of its adsorbing metal ions.Formation of the metastable state layered crystal structure feature of phyllosilicate powder powder for repair layer
There is provided prerequisite, and the mutual extrusion shearing in friction process between surface of friction pair micro-bulge is acted on and produced moment
Flash temperature, the formation for repair layer provide extrinsic motive.
Mica is a kind of conventional layer silicate mineral, and the antiwear and antifriction Effect study to mica in lubricating oil is very at present
It is few.Only find Yuan Ke, Wang Chengbiao, Yue Wen, Huanghai Sea roc, Wen Qingfeng, Liu Jiajun and have studied muscovite mineral lubricant oil additive
Tribological property, by the granularity to muscovite, addition, crystal formation control, the frictional behaviour of lubricating oil can be improved.
Make appropriate intercalation and surface modification to muscovite, preferably can dissolve in lubricating oil, these process do not interfere with additive
Tribological property.Qian Linmao, Luo Jianbin, Wen Shizhu, Xiao Xudong AFM/FFM measures the microcosmic of reference sample mica and rubs
Performance is wiped, shows that the change of length of the frictional behavior by its cleavage time, humidity and test needle point of mica sample etc. is various
The impact of factor, its surface friction property are unstable.
In sum：In order to improve friction and wear behavior and running status in mechanized equipment running, improving which makes
With the life-span, studying New Kind of Anti-Abrasion antifriction additive has become inevitable development trend, in addition, in existing wear-resistant friction reducer body
On the basis of system, new wear-resistant friction reducer system is produced by function and service, be also expected to obtain special-effect.
The content of the invention
The present invention for less to muscovite own layer shape characteristic research situation in existing antiwear and antifriction system, using room
Warm ball milling solid state reaction method realizes cladding same on surface in muscovite substrate deposit or Coated rare earth oxide
The fine of Shi Jinhang powders, using the layer structure of muscovite, the chemical redemption of generation of appraising at the current rate with reference to rare earth element, Jin Erti
Can be used as lubricating oil for one kind（Fat）The composite granule of anti wear and friction reducing additives.The present invention mechanism be：Produce in mechanical milling process
Shearing force, impulsive force can crush solid-phase reactant, increase the specific surface area of reactant, improve reactant contact surface and reaction speed
Rate, therefore the ratio of nucleation rate and growth rate is improve, fine, uniform predecessor can be prepared, heat point is then controlled
Solution temperature and time, so as to the ultra-fine muscovite composite granule of different-grain diameter can be obtained, while realizing Surface coating.
, with muscovite powder, rare-earth salts and its part as raw material, processing step is as follows successively for the method that the present invention is provided：
1st, dispensing
A certain amount of muscovite powder, rare-earth salts and part are weighed, rare-earth salts is 1: 2-6 with the mol ratio of part, rare earth
It is 1 ~ 10% that oxide accounts for the molar percentage of composite granule；
2nd, batch mixing
Muscovite powder, the rare-earth salts and its part that meet ratio are mixed, till uniform；
3rd, room-temperature ball-milling solid state reaction method prepares predecessor
The reaction system being well mixed is carried out into ball milling so as to the mechanical shear stress that produces in mechanical milling process, impulsive force
The lower refinement muscovite of effect, while rare-earth salts occurs chemical reaction with its part generates rare earth predecessor, until generationization completely
Till learning reaction, lubricant during ball milling, is added, the addition of lubricant is being kept dispersion to be limited by ball milling system；
4th, predecessor removal of impurities
Predecessor removal of impurities adopts washing and filtering method；
5th, predecessor is dried
Predecessor is dried using natural air drying or dries at 30-80 DEG C；
6th, predecessor thermal decomposition
At 400-900 DEG C, the time is 2-4 hours to the control of predecessor heat decomposition temperature, and Surface coating rare earth oxygen is obtained
The ultra-fine muscovite composite granule of compound；
In said method, rare-earth salts is one or more in lanthanum nitrate, cerous nitrate, lanthanum chloride or cerium chloride, and part is
Oxalic acid, ammonium carbonate or ammonium hydrogen carbonate；The lubricant added during ball milling is ethanol or acetone.
The present invention has advantages below and beneficial effect：
1st, react in the presence of the shearing force that produced in mechanical milling process due to reaction system, impulsive force, can increase
The surface area of reactant, the diffusion velocity of solid phase particles in the contact surface and system of raising reactant, thus chemical reaction velocity
Accelerate, chemical time shortens；
2nd, in reacting, the presence of solid phase particles, can keep reactant concentration constant, cause nucleation rate to be far longer than core long
Big speed, thus the predecessor of fine particles is easily formed, it is to obtain nano-powder to create condition；
3rd, the predecessor for being obtained can obtain different content from different rare earths through decomposing by adjusting thermal decomposition process
The ultra-fine muscovite composite granule of cladding system.
Description of the drawings
Fig. 1 is to prepare method according to the room-temperature ball-milling solid state reaction of ultra-fine muscovite composite granule provided by the present invention
Process chart.
Fig. 2 is+10% nano Ce O of muscovite prepared using said method2Composite granule shape appearance figure.
Specific embodiment
Embodiment 1：
In the present embodiment, with 800 mesh muscovites as raw material, reaction system is cerium chloride, and part is oxalic acid, and technological process is such as
Shown in Fig. 1, there are following steps successively：
1st, dispensing
Weigh 0.95mol muscovites, 0.05mol cerium chlorides, 0.1mol oxalic acid
2nd, batch mixing
The muscovite for weighing, cerium chloride are mixed with oxalic acid, till uniform；
3rd, room-temperature ball-milling chemical reaction method prepares predecessor
The muscovite being well mixed, cerium chloride and oxalic acid are carried out ball milling so as in mechanical milling process under room temperature, normal pressure
Reaction under the mechanical shear stress of generation, impact force action generates predecessor, the rotating speed of ball mill at 300 revs/min, 60 points of ball milling
Clock can make cerium chloride that chemical reaction occur completely with oxalic acid and generate predecessor cerium oxalate, be uniformly distributed in muscovite surface, ball
Add ethanol during mill, the addition of ethanol is being kept dispersion to be limited by ball milling system；
4th, predecessor removal of impurities
The removal of impurities of predecessor cerium oxalate adopts washing and filtering method, and detergent is distilled water, washing and filtering three times；
5th, predecessor is dried
Cerium oxalate after removal of impurities is dried at 40 DEG C with muscovite, and the time is 6 hours；
6th, predecessor thermal decomposition
Cerium oxalate after drying and muscovite are placed in Muffle furnace, heat decomposition temperature is controlled at 400 DEG C, are incubated 4 hours,
The ultra-fine muscovite composite granule of nano-cerium oxide cladding is obtained；
The ultra-fine muscovite composite granule surface that nano-cerium oxide is coated is modified in varing proportions（0.5%-3%）Add
In base oil or lubricating grease, coefficient of friction can be reduced in four ball wears, reduce friction pair wear scar diameter.
Embodiment 2:
In the present embodiment, with 800 mesh muscovites as raw material, reaction system is lanthanum chloride, and part is oxalic acid, and technological process is such as
Shown in Fig. 1, there are following steps successively
1st, dispensing
Weigh 0.98mol muscovites, 0.02mol lanthanum chlorides, 0.06mol oxalic acid
2nd, batch mixing
The muscovite for weighing, lanthanum chloride are mixed with oxalic acid, till uniform；
3rd, room-temperature ball-milling chemical reaction method prepares predecessor
The muscovite being well mixed, lanthanum chloride and oxalic acid are carried out ball milling so as in mechanical milling process under room temperature, normal pressure
Reaction under the mechanical shear stress of generation, impact force action generates predecessor, the rotating speed of ball mill at 400 revs/min, 40 points of ball milling
Clock can make lanthanum chloride that chemical reaction occur completely with oxalic acid and generate predecessor lanthanum oxalate, be uniformly distributed in muscovite surface, ball
Add acetone during mill, the addition of acetone is being kept dispersion to be limited by ball milling system；
4th, predecessor removal of impurities
The removal of impurities of predecessor lanthanum oxalate adopts washing and filtering method, and detergent is distilled water, washing and filtering three times；
5th, predecessor is dried
Lanthanum oxalate after removal of impurities and muscovite natural air drying at room temperature, the time is 10 hours；
6th, predecessor thermal decomposition
Lanthanum oxalate after drying and muscovite are placed in Muffle furnace, heat decomposition temperature is controlled at 800 DEG C, insulation 2.5 is little
When, the ultra-fine muscovite composite granule of nano lanthanum oxide cladding is obtained；
The ultra-fine muscovite composite granule surface that nano lanthanum oxide is coated is modified in varing proportions（0.5%-3%）Add
In base oil or lubricating grease, coefficient of friction can be reduced in four ball wears, reduce friction pair wear scar diameter.
Embodiment 3：
In the present embodiment, with 800 mesh muscovites as raw material, reaction system is cerous nitrate, and part is ammonium hydrogen carbonate, technique stream
Journey is as shown in figure 1, there is following steps successively
1st, dispensing
Weigh 0.90mol muscovites, 0.10mol cerous nitrates, 0.6mol ammonium hydrogen carbonate
2nd, batch mixing
The muscovite for weighing, cerous nitrate are mixed with ammonium hydrogen carbonate, till uniform；
3rd, room-temperature ball-milling chemical reaction method prepares predecessor
The muscovite being well mixed, cerous nitrate and ammonium hydrogen carbonate are carried out ball milling so as in ball milling mistake under room temperature, normal pressure
Reaction under the mechanical shear stress that produces in journey, impact force action generates predecessor, the rotating speed of ball mill at 250 revs/min, ball milling
Can make within 80 minutes cerous nitrate that chemical reaction occur completely with ammonium hydrogen carbonate and generate predecessor cerous carbonate, be uniformly distributed in muscovite
Surface, adds acetone during ball milling, the addition of acetone is being kept dispersion to be limited by ball milling system；
4th, predecessor removal of impurities
The removal of impurities of predecessor cerous carbonate adopts washing and filtering method, and detergent is distilled water, washing and filtering three times；
5th, predecessor is dried
Cerous carbonate after removal of impurities is dried at 60 DEG C with muscovite, and the time is 4 hours；
6th, predecessor thermal decomposition
Cerous carbonate after drying and muscovite are placed in Muffle furnace, heat decomposition temperature is controlled at 500 DEG C, are incubated 3 hours,
The ultra-fine muscovite composite granule of nano-cerium oxide cladding is obtained；
The ultra-fine muscovite composite granule surface that nano-cerium oxide is coated is modified in varing proportions（0.5%-3%）Add
In base oil or lubricating grease, coefficient of friction can be reduced in four ball wears, reduce friction pair wear scar diameter.
Embodiment 4
In the present embodiment, with 800 mesh muscovites as raw material, reaction system is lanthanum nitrate, and part is ammonium carbonate, technological process
As shown in figure 1, there is following steps successively
1st, dispensing
Weigh 0.97mol muscovites, 0.03mol lanthanum nitrates, 0.09mol ammonium carbonates
2nd, batch mixing
The muscovite for weighing, lanthanum nitrate are mixed with ammonium carbonate, till uniform；
3rd, room-temperature ball-milling chemical reaction method prepares predecessor
The muscovite being well mixed, lanthanum nitrate and ammonium carbonate are carried out ball milling so as in mechanical milling process under room temperature, normal pressure
Reaction under the mechanical shear stress of middle generation, impact force action generates predecessor, the rotating speed of ball mill at 350 revs/min, ball milling 50
Make lanthanum nitrate that chemical reaction occur completely with ammonium carbonate by minute and generate predecessor lanthanum carbonate, be uniformly distributed in white clouds matrix
Face, adds ethanol during ball milling, the addition of ethanol is being kept dispersion to be limited by ball milling system；
4th, predecessor removal of impurities
The removal of impurities of predecessor lanthanum carbonate adopts washing and filtering method, and detergent is distilled water, washing and filtering three times；
5th, predecessor is dried
Lanthanum carbonate after removal of impurities is dried at 80 DEG C with muscovite, and the time is 3 hours；
6th, predecessor thermal decomposition
Lanthanum carbonate after drying and muscovite are placed in Muffle furnace, heat decomposition temperature is controlled at 850 DEG C, are incubated 2 hours,
The ultra-fine muscovite composite granule of nano lanthanum oxide cladding is obtained；
The ultra-fine muscovite composite granule surface that nano lanthanum oxide is coated is modified in varing proportions（0.5%-3%）Add
In base oil or lubricating grease, coefficient of friction can be reduced in four ball wears, reduce friction pair wear scar diameter.
Embodiment 5：
In the present embodiment, with 800 mesh muscovites as raw material, reaction system is lanthanum nitrate, and cerous nitrate, part are ammonium carbonate,
Technological process is as shown in figure 1, there is following steps successively
1st, dispensing
Weigh 0.94mol muscovites, 0.03mol lanthanum nitrates, 0.03mol cerous nitrates, 0.18mol ammonium carbonates
2nd, batch mixing
The muscovite for weighing, lanthanum nitrate, cerous nitrate are mixed with ammonium carbonate, till uniform；
3rd, room-temperature ball-milling chemical reaction method prepares predecessor
The muscovite being well mixed, lanthanum nitrate, cerous nitrate are carried out into ball milling under room temperature, normal pressure with ammonium carbonate so as to
Reaction under the mechanical shear stress that produces in mechanical milling process, impact force action generates predecessor, and the rotating speed of ball mill is at 450 revs/min
Clock, ball milling can make lanthanum nitrate, cerous nitrate chemical reaction occur completely with ammonium carbonate and generate predecessor lanthanum carbonate and carbon for 30 minutes
Sour cerium, is uniformly distributed in muscovite surface, adds ethanol during ball milling, and the addition of ethanol is being kept being separated into by ball milling system
Limit；
4th, predecessor removal of impurities
Predecessor lanthanum carbonate and cerous carbonate removal of impurities adopt washing and filtering method, and detergent is distilled water, washing and filtering three times；
5th, predecessor is dried
Lanthanum carbonate and cerous carbonate after removal of impurities is dried at 50 DEG C with muscovite, and the time is 5 hours；
6th, predecessor thermal decomposition
Lanthanum carbonate and cerous carbonate after drying and muscovite are placed in Muffle furnace, heat decomposition temperature is controlled at 750 DEG C, are protected
Temperature 3 hours, is obtained nano lanthanum oxide, the ultra-fine muscovite composite granule of cerium oxide cladding；
The ultra-fine muscovite composite granule surface that nano lanthanum oxide, cerium oxide are coated is modified in varing proportions（0.5%-
3%）In adding base oil or lubricating grease, coefficient of friction can be reduced in four ball wears, reduce friction pair wear scar diameter.
Embodiment 6：
In the present embodiment, with 800 mesh muscovites as raw material, reaction system is lanthanum chloride, cerium chloride, and part is oxalic acid, work
Skill flow process is as shown in figure 1, there is following steps successively
1st, dispensing
Weigh 0.96mol muscovites, 0.02mol lanthanum chlorides, 0.02mol cerium chlorides, 0.16mol oxalic acid
2nd, batch mixing
The muscovite for weighing, lanthanum chloride, cerium chloride are mixed with oxalic acid, till uniform；
3rd, room-temperature ball-milling chemical reaction method prepares predecessor
The muscovite being well mixed, lanthanum chloride, cerium chloride and oxalic acid are carried out ball milling so as in ball under room temperature, normal pressure
Reaction under the mechanical shear stress that produces during mill, impact force action generates predecessor, the rotating speed of ball mill at 400 revs/min,
Ball milling 40 minutes can make muscovite, lanthanum chloride, cerium chloride and oxalic acid occur completely chemical reaction generate predecessor lanthanum oxalate and
Cerium oxalate, is uniformly distributed in muscovite surface, adds acetone during ball milling, and the addition of acetone is being kept being separated into by ball milling system
Limit；
4th, predecessor removal of impurities
Predecessor lanthanum oxalate and cerium oxalate removal of impurities adopt washing and filtering method, and detergent is distilled water, washing and filtering three times；
5th, predecessor is dried
Lanthanum oxalate and cerium oxalate after removal of impurities is dried at 40 DEG C with muscovite, and the time is 6 hours；
6th, predecessor thermal decomposition
Lanthanum oxalate and cerium oxalate after drying and muscovite are placed in Muffle furnace, heat decomposition temperature is controlled at 900 DEG C, are protected
Temperature 2 hours, is obtained nano lanthanum oxide, the ultra-fine muscovite composite granule of cerium oxide cladding；
The ultra-fine muscovite composite granule surface that nano lanthanum oxide, cerium oxide are coated is modified in varing proportions（0.5%-
3%）In adding base oil or lubricating grease, coefficient of friction can be reduced in four ball wears, reduce friction pair wear scar diameter.
Claims (1)
1. a kind of oxide nano rare earth Coated muscovite composite granule that can be used for lubricating oil, lubricating grease field, which is special
Levy is that, with muscovite powder, rare-earth salts and its part as raw material, rare-earth salts is 1: 2-6 with the mol ratio of part, rare-earth oxidation
It is 1 ~ 10% that thing accounts for the molar percentage of composite granule, and processing step is as follows successively：
1）Dispensing
A certain amount of muscovite powder, rare-earth salts and part are weighed, rare-earth salts is 1: 2-6 with the mol ratio of part, rare-earth oxidation
It is 1 ~ 10% that thing accounts for the molar percentage of composite granule；
2）Batch mixing
Muscovite powder, the rare-earth salts and its part that meet ratio are mixed, till uniform；
3）Room-temperature ball-milling solid state reaction method prepares predecessor
The reaction system being well mixed is carried out into ball milling so as to the mechanical shear stress that produces in mechanical milling process, impact force action
Lower refinement muscovite, while rare-earth salts occurs chemical reaction with its part generates rare earth predecessor, until it is anti-that chemistry occurs completely
Should till, add lubricant during ball milling, the addition of lubricant is being kept dispersion to be limited by ball milling system；
4）Predecessor removal of impurities
Predecessor removal of impurities adopts washing and filtering method；
5）Predecessor is dried
Predecessor is dried using natural air drying or dries at 30-80 DEG C；
6）Predecessor is thermally decomposed
At 400-900 DEG C, the time is 2-4 hours to the control of predecessor heat decomposition temperature, and Surface coating rare earth oxide is obtained
Ultra-fine muscovite composite granule；
In said method, rare-earth salts be lanthanum nitrate, cerous nitrate, lanthanum chloride or cerium chloride in one or more, part be oxalic acid,
Ammonium carbonate or ammonium hydrogen carbonate；The lubricant added during ball milling is ethanol or acetone.
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