CN108503362A - A kind of preparation method of nano-graphite base grinding-material - Google Patents
A kind of preparation method of nano-graphite base grinding-material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of nano-graphite base grinding-material, belong to inolrganic chemicals technical field.The present invention after nano-graphite and absolute ethyl alcohol ultrasonic disperse, will add polyvinylpyrrolidone first, after ultrasonic disperse, constant temperature stirs, nano-graphite dispersion liquid is made, then nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder ultrasonic mixing is uniform, then presoma dilution is added dropwise, ethanol solution is then added dropwise, it is stirred to react, stands through constant temperature again, filtering, it is dry, obtain dried feed；It is cooling after heating pyroreaction by dried feed under argon gas guard mode; blank is obtained, then by after blank hydrofluoric acid wash, is washed; it is dry; abrasive grain is obtained, casting after finally mixing abrasive grain, vitrified bonding and water is dry; demoulding; sintering, it is cooling to get nano-graphite base grinding-material.
Description
Technical field
The invention discloses a kind of preparation methods of nano-graphite base grinding-material, belong to inolrganic chemicals technology neck
Domain.
Background technology
Since new century, with the rapid development of high-tech and the network information, aerospace, integrated circuit and national defence troops
The fields such as work instrument, Surface-micromachining process necessarily develop to superfinishing densification direction.Therefore, Ultraprecision Machining
Development, not only represent the development level of a national high-end technology, but also come into people's lives and national economy
Numerous areas has extremely important research significance.In order to make the instrument applied to hard-core technology field adapt to the swift and violent of science and technology
The directions such as its suface processing quality, production efficiency and cost are proposed severe challenge, especially suface processing quality by development,
It is required that reaching free of surface defects smooth with residual stress minute surface grade.However, for the multiple and complicated manufacturing technology of tradition, such as milling
Mill, polishing and polishing etc., material caused by being ground and corroded due to free abrasive grain remove uncertain and sub-surface damage layer
In the presence of, it is difficult to ensure the higher surface accuracy of instrument, and increase the difficulty of follow-up polishing treatment, it is polynary that component occurs in material composition
The trend of change, and the factors such as the control of the granularity of Multicomponent Powderies and chemical composition largely influence the microstructure of material
And macro property, existing synthesis method are difficult to meet requirement that is quick, largely synthesizing high-purity uniform Multicomponent Powderies.
Therefore, powder new technique for synthesizing and technical research increasingly receive significant attention.Existing powder synthetic technology includes mainly solid
Xiang Fa, vapor phase method and liquid phase method.Wherein, solid phase method process is easy and is easy to produce in enormous quantities, but severe reaction conditions, gained
Powder uniformity is poor；Although made powder purity is higher for vapor phase method, favorable dispersibility, but it is generally used to prepare liquid phase method
It is difficult to the non-oxidized substances superfine powder such as the metal prepared, nitride and carbide；Liquid phase method is prepared in powder process, reaction condition
Easy to control, product is uniform, but its Organic Ingredients cost is higher, is not easy industrialized production.Ultraprecision Machining integrated application
Computer, microelectronics and the advanced technologies such as automatically control, target is the current macroscopic view manufacture of improve and perfect, suitable to realize
The microcosmic manufacture for answering futurity industry to develop.There are coefficient of thermal expansion height, grinding performances to be difficult into one for traditional nano-milled material
The shortcomings that step improves, to influence using effect.
Therefore, how to improve Conventional nano grinding-material there are coefficient of thermal expansion height, grinding performance is difficult to further increase
The shortcomings that, it is the problem of it need to be researched and solved to obtain more high combination property.
Invention content
The present invention solves the technical problem of：For Conventional nano grinding-material, there are coefficient of thermal expansion height, grindings
Performance is difficult to the shortcomings that further increasing, and provides that the invention discloses a kind of preparation methods of nano-graphite base grinding-material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of nano-graphite base grinding-material, specific preparation process are：
（1）It is 1 in mass ratio by nano-graphite and absolute ethyl alcohol：10~1：After 15 ultrasonic disperses, nano-graphite quality is added
0.2~0.4 times of polyvinylpyrrolidone, after ultrasonic disperse, constant temperature stirring obtains nano-graphite dispersion liquid；
（2）It is 1 by volume：5~1：7, by presoma and absolute ethyl alcohol ultrasonic mixing, obtain presoma dilution；
（3）It counts in parts by weight, takes 60~80 parts of nano-graphite dispersion liquids successively, 80~100 parts of presoma dilutions, 10~20
Part ethanol solution, 4~5 parts of sodium fluorides, 2~5 parts of nanometer iron powders first surpass nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder
Sound is uniformly mixed, then presoma dilution is added dropwise, and after adjusting pH to 7.6 ~ 7.8, then ethanol solution is added dropwise, then is stirred instead through constant temperature
It answers, stands, filter, it is dry, obtain dried feed；
（4）By gained dried feed as in tube furnace, under argon gas guard mode, 1500~1600 DEG C are heated to, heat preservation
After reacting 3~5h, cools to room temperature with the furnace, obtain blank；
（5）It after gained blank hydrofluoric acid wash, then is washed with deionized, is then dried to constant weight, obtains abrasive grain；
（6）It counts in parts by weight, takes 30~60 parts of abrasive grains, 40~80 parts of vitrified bonds, 8~10 parts of carboxymethyl fibres successively
The plain sodium of dimension, 10~20 parts of water, after being uniformly mixed, injection molding is dry, demoulds, and sintering is cooling to be ground to get nano-graphite base
Material.
Step（2）The presoma is any one in methyl orthosilicate or ethyl orthosilicate.
Step（6）The vitrified bond is compounded by the raw material of following parts by weight：4~6 parts of boron oxides, 4~6
Part aluminium oxide, 2~4 parts of zirconium oxides, 50~60 parts of sodium metasilicate, 10~20 parts of calcium silicates.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention, as matrix abrasive particle, first, is situated between using absolute ethyl alcohol as dispersion using nano-graphite
Matter is opened mutual soft-agglomerated of nano-graphite, is added polyvinylpyrrolidone, it is made well to inhale using supersound process
Invest nano-graphite surface, the nano-graphite in subsequent processes avoided to reunite again, then by nano-graphite dispersion liquid and
Presoma dilution mixes, and the silica generated using presoma hydrolysis is wrapped up in nano-graphite adsorption, on the one hand, two
Silica can be catalyzed it and chemically reacted with the carbon in graphite under the catalysis of sodium fluoride and nanometer iron powder, in graphite
Si-C keys are formed with silicon dioxide interface junction, make to form chemical bonding between nano-graphite and silica, the two reaction
The coefficient of thermal expansion of the silicon carbide of formation and the coefficient of thermal expansion of graphite are closer to, to can effectively avoid follow-up sintering process
In and product in use, because caused by coefficient of thermal expansion difference is larger cracking, to make product service life obtain
Effectively to extend, while in use, lower coefficient of thermal expansion can ensure higher machining accuracy；On the other hand, two
Silica can be filled the surface defect and micro-crack generated in nano-graphite thinning process, and during subsequent reactions
It is transformed into silicon carbide, since silicon carbide coefficient of thermal expansion and graphite are close, the silicon carbide being filled in micro-crack is using
The micro-crack that can effectively avoid in the process in graphite surface further expands, and so that the grinding performance of product is positively maintained same
When, service life is effectively extended；
（2）Technical solution of the present invention washs blank by using hydrofluoric acid, and silica extra in blank is enable to remove,
After pore structure and vitrified bond sinter molding to make to be formed connection inside blank, pore structure therein can be advantageous
In vitrified bond, diffusion enters inside blank in sintering process, is effectively bonded both to make, avoids being ground
Abrasive grain peels off and causes to block in journey, meanwhile, the presence of the hole of connection has the chip removal being conducive in grinding process and dissipates
Heat avoids blocking and burning workpiece, improves the grinding efficiency of product.
Specific implementation mode
It is 1 in mass ratio：10~1：Nano-graphite and absolute ethyl alcohol are mixed and are poured into No. 1 beaker by 15, and by No. 1 beaker
Ultrasonic disperse instrument is moved into, under the conditions of supersonic frequency is 45~60kHz, after 30~60min of ultrasonic disperse, then into No. 1 beaker
The polyvinylpyrrolidone of 0.2~0.4 times of nano-graphite quality is added, continues with the supersonic frequency ultrasonic disperse of 55~60kHz
After 20~40min, No. 1 beaker is moved into digital display and is tested the speed in constant temperature blender with magnetic force, in temperature be 65~70 DEG C, rotating speed 300
Under the conditions of~500r/min, constant temperature is stirred 2~4h, obtains nano-graphene dispersion liquid；It is 1 by volume：5~1：7 will before
Drive body and absolute ethyl alcohol to pour into No. 2 beakers, and No. 2 beakers moved into ultrasonic disperse instrument, in supersonic frequency be 45~50kHz
Under the conditions of, 30~45min of ultrasonic mixing obtains presoma dilution；It counts in parts by weight, takes 60~80 parts of nano-graphites point successively
Dispersion liquid, 80~100 parts of presoma dilutions, the ethanol solution that 10~20 parts of mass fractions are 55~60%, 4~5 parts of sodium fluorides, 2
~5 parts of nanometer iron powders, first pour into nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder in three-necked flask, and by three-necked flask
As in sonic oscillation instrument, under the conditions of supersonic frequency is 40~50kHz, 45~60min of ultrasonic mixing, then three-necked flask is moved
Enter digital display to test the speed in constant temperature blender with magnetic force, in temperature be 40~45 DEG C, under the conditions of rotating speed is 300~500r/min, side constant temperature
Presoma dilution is added dropwise into three-necked flask for stirring side, and control presoma dilution drop rate is 4~8mL/min, before waiting for
It drives body dilution to be added dropwise, material pH is to 7.6~7.8 in adjusting three-necked flask, then ethanol solution is added dropwise, and controls ethanol solution
Drop rate is 6~9nL/min, waits for that ethanol solution is added dropwise, and continues constant temperature and is stirred to react 6~8h, then will be in three-necked flask
Material pours into No. 3 beakers, under room temperature stand 2~4h after, filtering, obtain filter cake, and be washed with deionized filter cake 3~
5 times, then the filter cake after washing is transferred in baking oven, it is dry to constant weight under the conditions of temperature is 105~110 DEG C, obtain dried feed；
Gained dried feed is moved into tube furnace again, argon gas is passed through into stove with 60~80mL/min rates, under argon gas guard mode,
It is warming up to 1500~1600 DEG C with 8~10 DEG C/min rate programs, after 3~5h of insulation reaction, cools to room temperature with the furnace, discharges,
Blank is obtained, after gained blank is washed 45~60min with the hydrofluoric acid dips that mass fraction is 8~10%, then is washed with deionized water
It washs 4~6 times, then the blank after deionized water is cleaned is transferred in baking oven, is dried to perseverance under the conditions of being 105~110 DEG C in temperature
Weight, obtains abrasive grain；It counts in parts by weight, takes 30~60 parts of abrasive grains successively, 40~80 parts of vitrified bonds, 8~10 parts
Sodium carboxymethylcellulose, 10~20 parts of water, is poured into blender, after being stirred 2~4h with 600~800r/min rotating speeds, then
By in material injection mold in blender, after drying and moulding, demould, under the conditions of temperature is 1000~1100 DEG C, sintering 8~
10h, it is cooling to get nano-graphite base grinding-material.The presoma is any one in methyl orthosilicate or ethyl orthosilicate
Kind.The vitrified bond is compounded by the raw material of following parts by weight：4~6 parts of boron oxides, 4~6 parts of aluminium oxide, 2~
4 parts of zirconium oxides, 50~60 parts of sodium metasilicate, 10~20 parts of calcium silicates.
Example 1
It is 1 in mass ratio：15 pour into nano-graphite and absolute ethyl alcohol mixing in No. 1 beaker, and No. 1 beaker is moved into ultrasound point
Instrument is dissipated, under the conditions of supersonic frequency is 60kHz, after ultrasonic disperse 60min, then nano-graphite quality 0.4 is added into No. 1 beaker
No. 1 beaker after continuing with the supersonic frequency ultrasonic disperse 40min of 60kHz, is moved into digital display and tested the speed by polyvinylpyrrolidone again
It it is 70 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred 4h, obtains nano-graphite in constant temperature blender with magnetic force
Alkene dispersion liquid；It is 1 by volume：7 pour into presoma and absolute ethyl alcohol in No. 2 beakers, and No. 2 beakers are moved into ultrasonic disperse
In instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 45min obtains presoma dilution；It counts, takes successively in parts by weight
80 parts of nano-graphite dispersion liquids, 100 parts of presoma dilutions, the ethanol solution that 20 parts of mass fractions are 60%, 5 parts of sodium fluorides, 5
Part nanometer iron powder, first pours into nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder in three-necked flask, and by three-necked flask as
In sonic oscillation instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 60min, then three-necked flask immigration digital display is tested the speed perseverance
In warm magnetic stirring apparatus, it is 45 DEG C in temperature, under the conditions of rotating speed is 500r/min, is added dropwise into three-necked flask when constant temperature is stirred
Presoma dilution, control presoma dilution drop rate are 8mL/min, wait for that presoma dilution is added dropwise, and adjust three
Material pH is to 7.8 in mouth flask, then ethanol solution is added dropwise, and control ethanol solution drop rate is 9nL/min, waits for that ethanol solution drips
It adds complete, continues constant temperature and be stirred to react 8h, then material in three-necked flask is poured into No. 3 beakers, in standing 4h under room temperature
Afterwards, filter, obtain filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, in temperature be 110
It is dry to constant weight under the conditions of DEG C, obtain dried feed；Gained dried feed is moved into tube furnace again, with 80mL/min rates into stove
It is passed through argon gas, under argon gas guard mode, 1600 DEG C are warming up to 10 DEG C/min rate programs, after insulation reaction 5h, with furnace cooling
But to room temperature, discharging obtains blank, after gained blank is washed 60min with the hydrofluoric acid dips that mass fraction is 10%, then spends
Ion water washing 6 times, then blank after deionized water is cleaned are transferred in baking oven, are dried to perseverance under the conditions of being 110 DEG C in temperature
Weight, obtains abrasive grain；It counts in parts by weight, takes 60 parts of abrasive grains, 80 parts of vitrified bonds, 10 parts of carboxymethyl celluloses successively
Sodium, 20 parts of water, is poured into blender, after being stirred 4h with 800r/min rotating speeds, then by blender material injection mold in,
After drying and moulding, demoulding is sintered 10h under the conditions of temperature is 1100 DEG C, cooling to get nano-graphite base grinding-material.Institute
It is methyl orthosilicate to state presoma.The vitrified bond is compounded by the raw material of following parts by weight：6 parts of boron oxides, 6
Part aluminium oxide, 4 parts of zirconium oxides, 60 parts of sodium metasilicate, 20 parts of calcium silicates.
Example 2
It is 1 in mass ratio：15 pour into Nano diamond powder and absolute ethyl alcohol mixing in No. 1 beaker, and No. 1 beaker is moved into
Ultrasonic disperse instrument after ultrasonic disperse 60min, then nanometer Buddha's warrior attendant is added into No. 1 beaker under the conditions of supersonic frequency is 60kHz
After continuing with the supersonic frequency ultrasonic disperse 40min of 60kHz, No. 1 is burnt for the polyvinylpyrrolidone that 0.4 times of stone powder quality
Cup immigration digital display tests the speed in constant temperature blender with magnetic force, is 70 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred
4h obtains Nano diamond powder alkene dispersion liquid；It is 1 by volume：7 pour into presoma and absolute ethyl alcohol in No. 2 beakers, and will
No. 2 beakers move into ultrasonic disperse instrument, and under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 45min obtains presoma dilution；
It counts in parts by weight, takes the 80 parts of Nano diamond powder dispersion liquids, 100 parts of presoma dilutions, 20 parts of mass fractions to be successively
60% ethanol solution, 5 parts of sodium fluorides, 5 parts of nanometer iron powders, first by Nano diamond powder dispersion liquid and sodium fluoride, nanometer iron powder
It pours into three-necked flask, and by three-necked flask as in sonic oscillation instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing
60min, then three-necked flask immigration digital display is tested the speed in constant temperature blender with magnetic force, it is 45 DEG C in temperature, rotating speed is 500r/min items
Under part, presoma dilution is added dropwise into three-necked flask when constant temperature is stirred, control presoma dilution drop rate is 8mL/
Min waits for that presoma dilution is added dropwise, and material pH is to 7.8 in adjusting three-necked flask, then ethanol solution is added dropwise, and controls ethyl alcohol
Solution drop rate is 9nL/min, waits for that ethanol solution is added dropwise, and continues constant temperature and is stirred to react 8h, then by object in three-necked flask
Material pours into No. 3 beakers, and after standing 4h under room temperature, filtering obtains filter cake, and filter cake is washed with deionized 5 times, then will
Filter cake after washing is transferred in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains dried feed；Again by gained dried feed
It moves into tube furnace, argon gas is passed through into stove with 80mL/min rates, under argon gas guard mode, with 10 DEG C/min rate programs
It is warming up to 1600 DEG C, after insulation reaction 5h, cools to room temperature with the furnace, discharge, obtain blank, be with mass fraction by gained blank
It after 10% hydrofluoric acid dips washing 60min, then is washed with deionized 6 times, then the blank after deionized water is cleaned is transferred to baking
In case, is dried to constant weight under the conditions of being 110 DEG C in temperature, obtain abrasive grain；It counts in parts by weight, takes 60 parts of abrasive materials successively
Grain, 80 parts of vitrified bonds, 10 parts of sodium carboxymethylcelluloses, 20 parts of water pour into blender, mixed with the stirring of 800r/min rotating speeds
After closing 4h, then by material injection mold in blender, after drying and moulding, demoulding is sintered under the conditions of temperature is 1100 DEG C
10h, it is cooling to get Nano diamond powder base grinding-material.The presoma is methyl orthosilicate.The vitrified bond is
It is compounded by the raw material of following parts by weight：6 parts of boron oxides, 6 parts of aluminium oxide, 4 parts of zirconium oxides, 60 parts of sodium metasilicate, 20 parts of silicon
Sour calcium.
Example 3
It is 1 in mass ratio：15 pour into nano-graphite and absolute ethyl alcohol mixing in No. 1 beaker, and No. 1 beaker is moved into ultrasound point
Instrument is dissipated, under the conditions of supersonic frequency is 60kHz, after ultrasonic disperse 60min, then nano-graphite quality 0.4 is added into No. 1 beaker
No. 1 beaker after continuing with the supersonic frequency ultrasonic disperse 40min of 60kHz, is moved into digital display and tested the speed by polyvinylpyrrolidone again
It it is 70 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred 4h, obtains nano-graphite in constant temperature blender with magnetic force
Alkene dispersion liquid；It is 1 by volume：7 pour into butyl titanate and absolute ethyl alcohol in No. 2 beakers, and No. 2 beakers are moved into ultrasound
In separating apparatus, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 45min obtains butyl titanate dilution；In parts by weight
Meter, takes 80 parts of nano-graphite dispersion liquids successively, 100 parts of butyl titanate dilutions, and the ethyl alcohol that 20 parts of mass fractions are 60% is molten
Liquid, 5 parts of sodium fluorides, 5 parts of nanometer iron powders first pour into nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder in three-necked flask, and
By three-necked flask as in sonic oscillation instrument, under the conditions of supersonic frequency 50kHz, ultrasonic mixing 60min, then three-necked flask is moved
Enter digital display to test the speed in constant temperature blender with magnetic force, in temperature be 45 DEG C, under the conditions of rotating speed is 500r/min, when constant temperature is stirred to three
Butyl titanate dilution is added dropwise in mouth flask, control butyl titanate dilution drop rate is 8mL/min, waits for four fourth of metatitanic acid
Ester dilution is added dropwise, and material pH is to 7.8 in adjusting three-necked flask, then ethanol solution is added dropwise, and speed is added dropwise in control ethanol solution
Rate is 9nL/min, waits for that ethanol solution is added dropwise, and continues constant temperature and is stirred to react 8h, then material in three-necked flask is poured into No. 3 burnings
In cup, after standing 4h under room temperature, filtering obtains filter cake, and filter cake is washed with deionized 5 times, then by the filter after washing
Cake is transferred in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains dried feed；Gained dried feed is moved into tube furnace again
In, argon gas is passed through into stove with 80mL/min rates, under argon gas guard mode, 1600 are warming up to 10 DEG C/min rate programs
DEG C, it after insulation reaction 5h, cools to room temperature with the furnace, discharges, obtain blank, the hydrofluoric acid for being 10% by gained blank mass fraction
It after washing by soaking 60min, then is washed with deionized 6 times, then the blank after deionized water is cleaned is transferred in baking oven, in temperature
It is dried to constant weight under the conditions of being 110 DEG C, obtains abrasive grain；It counts in parts by weight, takes 60 parts of abrasive grains, 80 parts of ceramic junctions successively
Mixture, 10 parts of sodium carboxymethylcelluloses, 20 parts of water pour into blender, after being stirred 4h with 800r/min rotating speeds, then will stir
Mix in machine in material injection mold, after drying and moulding, demoulding is sintered 10h under the conditions of temperature is 1100 DEG C, it is cooling to get
Nano-graphite base grinding-material.The butyl titanate is methyl orthosilicate.The vitrified bond is by following parts by weight
Raw material compound：6 parts of boron oxides, 6 parts of aluminium oxide, 4 parts of zirconium oxides, 60 parts of sodium metasilicate, 20 parts of calcium silicates.
Example 4
It is 1 in mass ratio：15 pour into nano-graphite and absolute ethyl alcohol mixing in No. 1 beaker, and No. 1 beaker is moved into ultrasound point
Instrument is dissipated, under the conditions of supersonic frequency is 60kHz, after ultrasonic disperse 60min, then nano-graphite quality 0.4 is added into No. 1 beaker
No. 1 beaker after continuing with the supersonic frequency ultrasonic disperse 40min of 60kHz, is moved into digital display and tested the speed by polyvinylpyrrolidone again
It it is 70 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred 4h, obtains nano-graphite in constant temperature blender with magnetic force
Alkene dispersion liquid；It is 1 by volume：7 pour into presoma and absolute ethyl alcohol in No. 2 beakers, and No. 2 beakers are moved into ultrasonic disperse
In instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 45min obtains presoma dilution；It counts, takes successively in parts by weight
80 parts of nano-graphite dispersion liquids, 100 parts of presoma dilutions, the ethanol solution that 20 parts of mass fractions are 60%, first by nano-graphite
Dispersion liquid pours into three-necked flask, and three-necked flask under the conditions of supersonic frequency is 50kHz, is surpassed as in sonic oscillation instrument
Sound mixing 60min, then three-necked flask immigration digital display is tested the speed in constant temperature blender with magnetic force, in temperature be 45 DEG C, rotating speed 500r/
Under the conditions of min, presoma dilution is added dropwise into three-necked flask when constant temperature is stirred, control presoma dilution drop rate is
8mL/min waits for that presoma dilution is added dropwise, and material pH is to 7.8 in adjusting three-necked flask, then ethanol solution is added dropwise, and controls
Ethanol solution drop rate is 9nL/min, waits for that ethanol solution is added dropwise, and continues constant temperature and is stirred to react 8h, then by three-necked flask
Middle material pours into No. 3 beakers, and after standing 4h under room temperature, filtering obtains filter cake, and filter cake is washed with deionized 5 times,
The filter cake after washing is transferred in baking oven again, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain dried feed；Gained is done again
Dry material moves into tube furnace, argon gas is passed through into stove with 80mL/min rates, under argon gas guard mode, with 10 DEG C/min rates
Temperature programming after insulation reaction 5h, cools to room temperature with the furnace to 1600 DEG C, discharges, blank is obtained, by gained blank mass fraction
For 10% hydrofluoric acid dips wash 60min after, then be washed with deionized 6 times, then the blank after deionized water is cleaned is transferred to
In baking oven, is dried to constant weight under the conditions of being 110 DEG C in temperature, obtain abrasive grain；It counts in parts by weight, takes 60 parts of abrasive materials successively
Grain, 80 parts of vitrified bonds, 10 parts of sodium carboxymethylcelluloses, 20 parts of water pour into blender, mixed with the stirring of 800r/min rotating speeds
After closing 4h, then by material injection mold in blender, after drying and moulding, demoulding is sintered under the conditions of temperature is 1100 DEG C
10h, it is cooling to get nano-graphite base grinding-material.The presoma is methyl orthosilicate.The vitrified bond is by following
The raw material of parts by weight compounds：6 parts of boron oxides, 6 parts of aluminium oxide, 4 parts of zirconium oxides, 60 parts of sodium metasilicate, 20 parts of calcium silicates.
Example 5
It is 1 in mass ratio：15 pour into nano-graphite and absolute ethyl alcohol mixing in No. 1 beaker, and No. 1 beaker is moved into ultrasound point
Instrument is dissipated, under the conditions of supersonic frequency is 60kHz, after ultrasonic disperse 60min, then nano-graphite quality 0.4 is added into No. 1 beaker
No. 1 beaker after continuing with the supersonic frequency ultrasonic disperse 40min of 60kHz, is moved into digital display and tested the speed by polyvinylpyrrolidone again
It it is 70 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred 4h, obtains nano-graphite in constant temperature blender with magnetic force
Alkene dispersion liquid；It is 1 by volume：7 pour into presoma and absolute ethyl alcohol in No. 2 beakers, and No. 2 beakers are moved into ultrasonic disperse
In instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 45min obtains presoma dilution；It counts, takes successively in parts by weight
80 parts of nano-graphite dispersion liquids, 100 parts of presoma dilutions, the ethanol solution that 20 parts of mass fractions are 60%, 5 parts of sodium fluorides, 5
Part nanometer iron powder, first pours into nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder in three-necked flask, and by three-necked flask as
In sonic oscillation instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 60min, then three-necked flask immigration digital display is tested the speed perseverance
In warm magnetic stirring apparatus, it is 45 DEG C in temperature, under the conditions of rotating speed is 500r/min, is added dropwise into three-necked flask when constant temperature is stirred
Presoma dilution, control presoma dilution drop rate are 8mL/min, wait for that presoma dilution is added dropwise, and adjust three
Material pH is to 7.8 in mouth flask, then ethanol solution is added dropwise, and control ethanol solution drop rate is 9nL/min, waits for that ethanol solution drips
It adds complete, continues constant temperature and be stirred to react 8h, then material in three-necked flask is poured into No. 3 beakers, in standing 4h under room temperature
Afterwards, filter, obtain filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, in temperature be 110
It is dry to constant weight under the conditions of DEG C, obtain dried feed；Gained dried feed is moved into tube furnace again, with 80mL/min rates into stove
It is passed through argon gas, under argon gas guard mode, 1600 DEG C are warming up to 10 DEG C/min rate programs, after insulation reaction 5h, with furnace cooling
But to room temperature, discharging obtains blank, after the hydrochloric acid washing by soaking 60min for being 10% by gained blank mass fraction, then spend from
Sub- water washing 6 times, then blank after deionized water is cleaned are transferred in baking oven, are dried to constant weight under the conditions of being 110 DEG C in temperature,
Obtain abrasive grain；It counts in parts by weight, takes 60 parts of abrasive grains successively, 80 parts of vitrified bonds, 10 parts of sodium carboxymethylcelluloses,
20 parts of water, are poured into blender, after being stirred 4h with 800r/min rotating speeds, then by material injection mold in blender, are done
After dry molding, demoulding is sintered 10h under the conditions of temperature is 1100 DEG C, cooling to get nano-graphite base grinding-material.It is described
Presoma is methyl orthosilicate.The vitrified bond is compounded by the raw material of following parts by weight：6 parts of boron oxides, 6 parts
Aluminium oxide, 4 parts of zirconium oxides, 60 parts of sodium metasilicate, 20 parts of calcium silicates.
Example 6
It is 1 in mass ratio：15 pour into nano-graphite and absolute ethyl alcohol mixing in No. 1 beaker, and No. 1 beaker is moved into ultrasound point
Instrument is dissipated, under the conditions of supersonic frequency is 60kHz, after ultrasonic disperse 60min, then nano-graphite quality 0.4 is added into No. 1 beaker
No. 1 beaker after continuing with the supersonic frequency ultrasonic disperse 40min of 60kHz, is moved into digital display and tested the speed by polyvinylpyrrolidone again
It it is 70 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature is stirred 4h, obtains nano-graphite in constant temperature blender with magnetic force
Alkene dispersion liquid；It is 1 by volume：7 pour into presoma and absolute ethyl alcohol in No. 2 beakers, and No. 2 beakers are moved into ultrasonic disperse
In instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 45min obtains presoma dilution；It counts, takes successively in parts by weight
80 parts of nano-graphite dispersion liquids, 100 parts of presoma dilutions, the ethanol solution that 20 parts of mass fractions are 60%, 5 parts of sodium fluorides, 5
Part nanometer iron powder, first pours into nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder in three-necked flask, and by three-necked flask as
In sonic oscillation instrument, under the conditions of supersonic frequency is 50kHz, ultrasonic mixing 60min, then three-necked flask immigration digital display is tested the speed perseverance
In warm magnetic stirring apparatus, it is 45 DEG C in temperature, under the conditions of rotating speed is 500r/min, is added dropwise into three-necked flask when constant temperature is stirred
Presoma dilution, control presoma dilution drop rate are 8mL/min, wait for that presoma dilution is added dropwise, and adjust three
Material pH is to 7.8 in mouth flask, then ethanol solution is added dropwise, and control ethanol solution drop rate is 9nL/min, waits for that ethanol solution drips
It adds complete, continues constant temperature and be stirred to react 8h, then material in three-necked flask is poured into No. 3 beakers, in standing 4h under room temperature
Afterwards, filter, obtain filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, in temperature be 110
It is dry to constant weight under the conditions of DEG C, obtain dried feed；Gained dried feed is moved into tube furnace again, with 80mL/min rates into stove
It is passed through argon gas, under argon gas guard mode, 1600 DEG C are warming up to 10 DEG C/min rate programs, after insulation reaction 5h, with furnace cooling
But to room temperature, discharging obtains blank, after gained blank is washed 60min with the hydrofluoric acid dips that mass fraction is 10%, then spends
Ion water washing 6 times, then blank after deionized water is cleaned are transferred in baking oven, are dried to perseverance under the conditions of being 110 DEG C in temperature
Weight, obtains abrasive grain；It counts in parts by weight, takes 60 parts of abrasive grains, 80 parts of vitrified bonds, 10 parts of carboxymethyl celluloses successively
Sodium, 20 parts of water, is poured into blender, after being stirred 4h with 800r/min rotating speeds, then by blender material injection mold in,
After drying and moulding, demoulding is sintered 10h under the conditions of temperature is 1100 DEG C, cooling to get nano-graphite base grinding-material.Institute
It is methyl orthosilicate to state presoma.The vitrified bond is compounded by the raw material of following parts by weight：6 parts of boron oxides, 4
Part zirconium oxide, 60 parts of sodium metasilicate, 20 parts of calcium silicates.
Comparative example：
The nano-graphite base grinding-material and comparative example product of example 1 to 6 gained of example are subjected to performance detection, specific detection side
Method is as follows：
Coefficient of thermal expansion：Using the DIL402C thermodilatometric analysis instrument of German Netzsch companies to the coefficient of thermal expansion of agent testing bar
It is tested.Test condition：Air atmosphere；Heating rate is 5 °C/min；Range of measuring temp is 30~520 °C.
Flexural strength：Flexural strength measurement, span L are carried out to strip by surface and interface for material performance aircraft
For 16mm, load loading speed is 0.5mm/min, and each to be formulated sample testing ten times, final result is averaged.
Apparent porosity is surveyed：Using DXR type apparent porosity unit weight testers, principle is the same as Archimedes's drainage, each sample
It at least tests three times, as a result takes its average value.Testing bar surface requirements to be tested are clean and tidy, no marking is split
Line, and the drying and processing in Muffle furnace, volume are not less than 10cm3, vacuum degree is not less than 0.09MPa.
Specific testing result is as shown in table 1：
The 1 specific testing result of nano-graphite base grinding-material of table
By 1 testing result of table, it is found that nano-graphite base grinding-material prepared by technical solution of the present invention has, coefficient of thermal expansion is high,
The good feature of grinding performance, has broad prospects in the development of inolrganic chemicals industry.
Claims (3)
1. a kind of preparation method of nano-graphite base grinding-material, it is characterised in that specifically preparation process is：
（1）It is 1 in mass ratio by nano-graphite and absolute ethyl alcohol：10~1：After 15 ultrasonic disperses, nano-graphite quality is added
0.2~0.4 times of polyvinylpyrrolidone, after ultrasonic disperse, constant temperature stirring obtains nano-graphite dispersion liquid；
（2）It is 1 by volume：5~1：7, by presoma and absolute ethyl alcohol ultrasonic mixing, obtain presoma dilution；
（3）It counts in parts by weight, takes 60~80 parts of nano-graphite dispersion liquids successively, 80~100 parts of presoma dilutions, 10~20
Part ethanol solution, 4~5 parts of sodium fluorides, 2~5 parts of nanometer iron powders first surpass nano-graphite dispersion liquid and sodium fluoride, nanometer iron powder
Sound is uniformly mixed, then presoma dilution is added dropwise, and after adjusting pH to 7.6 ~ 7.8, then ethanol solution is added dropwise, then is stirred instead through constant temperature
It answers, stands, filter, it is dry, obtain dried feed；
（4）By gained dried feed as in tube furnace, under argon gas guard mode, 1500~1600 DEG C are heated to, heat preservation
After reacting 3~5h, cools to room temperature with the furnace, obtain blank；
（5）It after gained blank hydrofluoric acid wash, then is washed with deionized, is then dried to constant weight, obtains abrasive grain；
（6）It counts in parts by weight, takes 30~60 parts of abrasive grains, 40~80 parts of vitrified bonds, 8~10 parts of carboxymethyl fibres successively
The plain sodium of dimension, 10~20 parts of water, after being uniformly mixed, injection molding is dry, demoulds, and sintering is cooling to be ground to get nano-graphite base
Material.
2. a kind of preparation method of nano-graphite base grinding-material according to claim 1, which is characterized in that step（2）
The presoma is any one in methyl orthosilicate or ethyl orthosilicate.
3. a kind of preparation method of nano-graphite base grinding-material according to claim 1, which is characterized in that step（6）
The vitrified bond is compounded by the raw material of following parts by weight：4~6 parts of boron oxides, 4~6 parts of aluminium oxide, 2~4 parts
Zirconium oxide, 50~60 parts of sodium metasilicate, 10~20 parts of calcium silicates.
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| CN116144270A (en) * | 2023-02-20 | 2023-05-23 | 湖南三安半导体有限责任公司 | Polishing solution and preparation method thereof |
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