CN108149047A - A kind of preparation method of trepanning sound-absorbing foam aluminum - Google Patents
A kind of preparation method of trepanning sound-absorbing foam aluminum Download PDFInfo
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- CN108149047A CN108149047A CN201711362707.7A CN201711362707A CN108149047A CN 108149047 A CN108149047 A CN 108149047A CN 201711362707 A CN201711362707 A CN 201711362707A CN 108149047 A CN108149047 A CN 108149047A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
- C22C1/083—Foaming process in molten metal other than by powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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Abstract
The invention discloses a kind of preparation methods of trepanning sound-absorbing foam aluminum, belong to sound-absorbing material technical field.It is of the invention first using graphene oxide and solution of ferrous chloride as raw material, after constant temperature is stirred, filtering, graphene oxide must be pre-processed, graphene oxide and water ultrasonic disperse will be pre-processed again, and add in hydrazine hydrate, after constant temperature is stirred to react, adjust pH, obtain redox graphene dispersion liquid, again dispersant is added in into redox graphene dispersion liquid, aging is stood after ultrasonic disperse, it is dry, obtain modified graphene gel, then by aluminium powder, magnesium powder and calcium powder heating melting, add modified graphene gel, after continuing insulated and stirred mixing, it heats up again, after insulation reaction, injection molding, cooling, obtain foamed aluminium blank, ultrasonic immersing after foamed aluminium blank is mixed with deionized water again, and add in ice cube cooling, it is washed again and dry, foamed aluminium is sacrificed up to trepanning.Trepanning sound-absorbing foam aluminum of the present invention has the characteristics that excellent mechanical property and sound absorbing performance.
Description
Technical field
The invention discloses a kind of preparation methods of trepanning sound-absorbing foam aluminum, belong to sound-absorbing material technical field.
Background technology
It is considered as a kind of fault of construction in traditional engineering material Hole, is formed and expanded because they are often crackle
The center of exhibition has an adverse effect to the performance of material.But after the quantity increase to a certain extent of material Hole, material
Material will have some properties because of the presence of hole, and so as to form a new material class, here it is so-called
Porous or foamed material.There are many porous materials, such as honeycomb, timber, coral in nature.With the development of science and technology
Miscellaneous artificial porous materials are continued to bring out out again, such as foamed plastics, foamed ceramics, foam glass or even foam metal.
Foamed aluminium is exactly a kind of using aluminum or aluminum alloy as matrix, includes the light porous material of a large amount of holes, it is a kind of function and knot
The integrated new engineering material of structure.In recent years, with the gradual ripe of foamed aluminium preparation process and in automobile, building etc.
Application prospect is increasingly had an optimistic view of.Foamed aluminium material is that a kind of be uniform-distribution in aluminum or aluminum alloy matrix largely connects or do not connect
The novel light multifunctional material of via holes.The hole shape of foamed aluminium material has polyhedron-shaped and elliptical shape, according to hole
Foamed aluminium can be divided into two kinds by type：First, the Open-cell Aluminum Foam with continuous unimpeded three-D pore structure；Second is that exist a large amount of only
The closed-cell aluminum foam of vertical hole.Foamed aluminium is bad there are mechanical property as a kind of very promising buffering energy-absorbing material
The shortcomings that, the major influence factors of the mechanical property of foamed aluminium have：1）The structural property parameter of foamed aluminium, such as relative density, born of the same parents
Pore structure type（Trepanning or closed pore）, the geometric properties of hilum etc.；2）Loading environment, such as loading speed, ambient temperature etc..
In addition to this, with the raising of production and living level, the sound absorbing performance to foamed aluminium material is it is also proposed that carry out higher requirement.
Therefore, it is the shortcomings that how improving conventional foam aluminium mechanical property and bad sound absorbing performance, comprehensive to obtain higher
The foamed aluminium of energy is that it is promoted and applies, meets industrial production demand urgent problem to be solved.
Invention content
The present invention solves the technical problem of：It is lacked for conventional foam aluminium mechanical property and sound absorbing performance are bad
Point provides a kind of preparation method of trepanning sound-absorbing foam aluminum.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）It is 1 in mass ratio by graphene oxide and solution of ferrous chloride：10~1：After 20 constant temperature are stirred, filtering obtains pre-
Handle graphene oxide；
（2）It is 1 in mass ratio that graphene oxide and water, which will be pre-processed,：100~1：After 120 mixing, ultrasonic disperse adds oxidation
The hydrazine hydrate that 3~5 times of graphene quality, constant temperature are stirred to react, and to the end of reaction, are adjusted pH to 10.5~11.0, are obtained oxygen reduction
Graphite alkene dispersion liquid；
（3）It is 1 in mass ratio：3~1：After 5 mix dispersant and redox graphene dispersion liquid, ultrasonic disperse is stood old
Change, it is dry, obtain modified graphene gel；
（4）It counts in parts by weight, takes 80~100 parts of aluminium powders, 10~15 parts of magnesium powders successively, 4~6 parts of calcium powders protect shape in argon gas
Under state, 900~920 DEG C, after being stirred 1~2h are heated to, adds the modified graphene gel of aluminium powder quality 4~6%, after
After continuation of insurance temperature is stirred, it is warming up to 1100~1150 DEG C, after insulation reaction, injection molding, and it is naturally cold under argon gas guard mode
But to 300~320 DEG C, foamed aluminium blank is obtained；
（5）Foamed aluminium blank is soaked in temperature is in 20~25 DEG C of deionized water, after 45~60min of ultrasonic immersing, to going
The ice cube of the quality such as deionized water is added in ionized water, continues 10~20min of ultrasonic immersing, is discharged, washing, and protected in nitrogen
Drying is to get trepanning sound-absorbing foam aluminum under state.
Step（1）The solution of ferrous chloride mass fraction is 10~12%.
Step（3）The dispersant configuration process is：It is 1 in mass ratio：200~1：500 by 1- naphthoic acids and anhydrous second
After alcohol mixing, constant temperature stirring obtains dispersant.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention is ferrous in adsorbing chlorinated ferrous iron solution first with the good absorption property of graphene oxide
Ion, then using hydrazine hydrate as reducing agent, the ferrous ion of adsorption is made to be reduced simultaneously while being graphene oxide reduction,
So as to effectively improve the compatibility of graphene oxide and the alloying metal liquid of melting, and graphene oxide is can effectively avoid in metal
Reunite in liquid, so as to which graphene be made to be well dispersed in foamed aluminium system as skeleton, play reinforcing effect, improve product
Mechanical property；
（2）Technical solution of the present invention under lower temperature by using magnesium powder, aluminium powder and calcium powder as metal source, sending out three first
Life it is co-melting, reheat heating, most of magnesium is made to be changed into gaseous state from liquid and volatilize, plays foaming effect, so as to get foam
It containing through-hole and closed pore mixed structure in aluminium blank, then is impregnated by using deionized water, makes calcium and water more active in system
Reaction dissolves out after generating calcium hydroxide, hole-closing structure in system is made to change to open-celled structure, in addition, the production with calcium hydroxide
Raw, system is changed into alkalinity by neutrality, so as to generate micro- corruption to aluminium, the through-hole rate of product is further improved, so as to effectively carry
The sound absorbing performance of high product；
（3）Technical solution of the present invention is using magnalium calcium alloy as matrix alloy, and magnalium binary alloy is in process, easily occurs
Decrepitation, with the addition of calcium, alloy grain attenuates, and fire check volume, which reduces, even to disappear, and the addition of calcium, can make crackle
The metal liquid film of position constantly thickens, and so as to form pleated structure on foam aluminium alloy duct, the generation of pleated structure is carrying
While high product mechanical property, be conducive to the further promotion of product sound absorbing performance.
Specific embodiment
It is 1 in mass ratio：10~1：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid,
In under room temperature, 12~20h is stirred to react with 300~500r/min rotating speeds, then three-necked flask is moved into temperature with blender
For in 4~6 DEG C of ice-water baths, under stirring, the Gao Meng of 0.8~1.5 times of crystalline flake graphite quality is added in into three-necked flask
Sour potassium after being stirred to react 10~30min with 300~500r/min rotating speeds, sequentially adds 0.3~0.5 times of concentrated sulfuric acid quality
The mass fraction of 0.4~0.6 times of deionized water and concentrated sulfuric acid quality is 10~20% hydrogen peroxide, continue to be stirred to react 10~
30min, filtering, obtains filter residue, and filter residue is washed with deionized 3~5 times, then the filter residue after washing is transferred in baking oven, Yu Wen
Spend be 105~110 DEG C under the conditions of dry to constant weight, obtain graphene oxide；It is 1 in mass ratio again：10~1：20 by graphite oxide
The solution of ferrous chloride that alkene and mass fraction are 10~12% is added in beaker, and the beaker immigration digital display constant temperature magnetic force that tests the speed is stirred
Device is mixed, is 45~55 DEG C in temperature, under the conditions of rotating speed is 400~600r/min, constant temperature is stirred 45~60min, and filtering obtains
Filter cake as pre-processes graphene oxide；It is 1 in mass ratio that graphene oxide and water, which will then be pre-processed,：100~1：200 is mixed
Reaction kettle is poured into conjunction, in supersonic frequency under the conditions of 45~50kHz, 2~4h of ultrasonic disperse, to the end of ultrasonic disperse, then to anti-
Answer the hydrazine hydrate that 3~5 times of graphene oxide quality is added in kettle, to the end of hydrazine hydrate adds in, in temperature be 88~90 DEG C, rotating speed
Under the conditions of 300~400r/min, constant temperature is stirred to react 2~4h, is 10~20% hydroxides with mass fraction to the end of reaction
Sodium solution adjusts material in reactor pH to 10.5~11.0, obtains redox graphene dispersion liquid；It is 1 in mass ratio again：3~
1：5 mix dispersant and redox graphene dispersion liquid, and under the conditions of supersonic frequency is 50~60kHz, ultrasonic disperse 2
~4h to the end of ultrasonic disperse, in standing aging 12~for 24 hours under room temperature, obtains Ageing solution, and gained Ageing solution vacuum is cold
It is lyophilized dry, obtains modified graphene gel；It counts in parts by weight, takes 80~100 parts of aluminium powders successively, 10~15 parts of magnesium powders, 4~6 parts
Calcium powder, mixing pour into graphite crucible, with after under argon gas guard mode, are heated to 900~920 DEG C, make graphite crucible
Middle material melts completely, and after being stirred 1~2h, then the modified graphene of addition aluminium powder quality 4~6% coagulates into graphite crucible
Glue continues at temperature as under 900~920 DEG C and argon gas guard mode, after insulated and stirred mixes 20~30min, with 8~10 DEG C/
Min rate programs are warming up to 1100~1150 DEG C, and after 10~15min of insulation reaction, material in graphite crucible is poured into mold,
And 300~320 DEG C are naturally cooled under argon gas guard mode, it demoulds, obtains foamed aluminium blank, then gained foamed aluminium blank is taken advantage of
Heat, which is poured into, to be filled in sink of the temperature for 20~25 DEG C of deionized waters, under the conditions of supersonic frequency is 55~60kHz, ultrasonic immersing
After 45~60min, then the ice cube of the quality such as deionized water is added in into sink, continue at supersonic frequency as 60~70kHz conditions
Under, 10~20min of ultrasonic immersing, discharging obtains impregnated stock, and gained impregnated stock is washed with deionized 4~6 times, then will
Drying to constant weight under nitrogen guard mode to get trepanning sound-absorbing foam aluminum for impregnated stock after washing.The dispersant configuration
Process is：It is 1 in mass ratio：200~1：After 500 mix 1- naphthoic acids and absolute ethyl alcohol, constant temperature stirring obtains dispersant.
Example 1
It is 1 in mass ratio：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid, in room temperature condition
Under, 20h is stirred to react with 500r/min rotating speeds with blender, then three-necked flask is moved into the ice-water bath that temperature is 6 DEG C, in stirring
It mixes under state, the potassium permanganate of 1.5 times of crystalline flake graphite quality is added in into three-necked flask, is stirred to react with 500r/min rotating speeds
After 30min, the mass fraction of 0.6 times of deionized water and concentrated sulfuric acid quality for sequentially adding 0.5 times of concentrated sulfuric acid quality is 20%
Hydrogen peroxide continues to be stirred to react 30min, and filtering obtains filter residue, and filter residue is washed with deionized 5 times, then by the filter residue after washing
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain graphene oxide；It is 1 in mass ratio again：20 will oxidation
The solution of ferrous chloride that graphene and mass fraction are 12% is added in beaker, and the beaker immigration digital display constant temperature magnetic force that tests the speed is stirred
Device is mixed, is 55 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred 60min, and filtering obtains filter cake, as pre- place
Manage graphene oxide；It is 1 in mass ratio that graphene oxide and water, which will then be pre-processed,：Reaction kettle is poured into 200 mixing, in supersonic frequency
Under the conditions of rate is 50kHz, ultrasonic disperse 4h to the end of ultrasonic disperse, then adds in 5 times of graphene oxide quality into reaction kettle
Hydrazine hydrate is 90 DEG C in temperature to the end of hydrazine hydrate adds in, and under the conditions of rotating speed is 400r/min, constant temperature is stirred to react 4h, treats anti-
It should terminate, adjust material in reactor pH to 11.0 for 20% sodium hydroxide solution with mass fraction, obtain redox graphene point
Dispersion liquid；It is 1 in mass ratio again：5 mix dispersant and redox graphene dispersion liquid, and in supersonic frequency be 60kHz items
Under part, ultrasonic disperse 4h to the end of ultrasonic disperse, in standing aging for 24 hours under room temperature, obtains Ageing solution, and by gained aging
Liquid vacuum freeze drying obtains modified graphene gel；It counts in parts by weight, takes 100 parts of aluminium powders, 15 parts of magnesium powders, 6 parts of calcium successively
Powder, mixing pour into graphite crucible, with after under argon gas guard mode, are heated to 920 DEG C, make material in graphite crucible complete
Full-fusing after being stirred 2h, then adds in into graphite crucible the modified graphene gel of aluminium powder quality 6%, and continuing at temperature is
920 DEG C, under argon gas guard mode, after insulated and stirred mixing 30min, are warming up to 1150 DEG C, heat preservation with 10 DEG C/min rate programs
After reacting 15min, material in graphite crucible is poured into mold, and 320 DEG C are naturally cooled under argon gas guard mode, taken off
Mould obtains foamed aluminium blank, then gained foamed aluminium blank is poured into while hot and is filled in sink of the temperature for 25 DEG C of deionized waters, Yu Chao
Under the conditions of acoustic frequency is 60kHz, after ultrasonic immersing 60min, then the ice cube of the quality such as deionized water is added in into sink, continued at
Under the conditions of supersonic frequency is 70kHz, ultrasonic immersing 20min, discharging obtains impregnated stock, and gained is washed with deionized and impregnates
Blank 6 times, then drying to constant weight under nitrogen guard mode to get trepanning sound-absorbing foam aluminum by the impregnated stock after washing.Institute
Stating dispersant configuration process is：It is 1 in mass ratio：After 500 mix 1- naphthoic acids and absolute ethyl alcohol, constant temperature stirring must disperse
Agent.
Example 2
It is 1 in mass ratio：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid, in room temperature condition
Under, 20h is stirred to react with 500r/min rotating speeds with blender, then three-necked flask is moved into the ice-water bath that temperature is 6 DEG C, in stirring
It mixes under state, the potassium permanganate of 1.5 times of crystalline flake graphite quality is added in into three-necked flask, is stirred to react with 500r/min rotating speeds
After 30min, the mass fraction of 0.6 times of deionized water and concentrated sulfuric acid quality for sequentially adding 0.5 times of concentrated sulfuric acid quality is 20%
Hydrogen peroxide continues to be stirred to react 30min, and filtering obtains filter residue, and filter residue is washed with deionized 5 times, then by the filter residue after washing
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain graphene oxide；It counts in parts by weight, takes 100 successively
Part aluminium powder, 15 parts of magnesium powders, 6 parts of calcium powders, mixing are poured into graphite crucible, with after under argon gas guard mode, are heated to 920
DEG C, material in graphite crucible is made to melt completely, after being stirred 2h, then adds in into graphite crucible the graphene of aluminium powder quality 6%
Gel, it is under 920 DEG C and argon gas guard mode, after insulated and stirred mixing 30min, with 10 DEG C/min rate programs to continue at temperature
Be warming up to 1150 DEG C, after insulation reaction 15min, material in graphite crucible poured into mold, and under argon gas guard mode from
So be cooled to 320 DEG C, demoulding obtains foamed aluminium blank, then gained foamed aluminium blank poured into while hot fill temperature for 25 DEG C go from
In the sink of sub- water, in supersonic frequency under the conditions of 60kHz, after ultrasonic immersing 60min, then to add in deionized water etc. into sink
The ice cube of quality continues at supersonic frequency as under the conditions of 70kHz, ultrasonic immersing 20min, discharging obtains impregnated stock, and spend from
Impregnated stock 6 times obtained by sub- water washing, then drying to constant weight under nitrogen guard mode to get opening by the impregnated stock after washing
Hole sound-absorbing foam aluminum.
Example 3
It is 1 in mass ratio：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid, in room temperature condition
Under, 20h is stirred to react with 500r/min rotating speeds with blender, then three-necked flask is moved into the ice-water bath that temperature is 6 DEG C, in stirring
It mixes under state, the potassium permanganate of 1.5 times of crystalline flake graphite quality is added in into three-necked flask, is stirred to react with 500r/min rotating speeds
After 30min, the mass fraction of 0.6 times of deionized water and concentrated sulfuric acid quality for sequentially adding 0.5 times of concentrated sulfuric acid quality is 20%
Hydrogen peroxide continues to be stirred to react 30min, and filtering obtains filter residue, and filter residue is washed with deionized 5 times, then by the filter residue after washing
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain graphene oxide；Then graphene oxide and water are pressed
Mass ratio is 1：Reaction kettle is poured into 200 mixing, in supersonic frequency under the conditions of 50kHz, ultrasonic disperse 4h treats ultrasonic disperse knot
Beam, then the hydrazine hydrate of 5 times of graphene oxide quality is added in into reaction kettle, to the end of hydrazine hydrate adds in, it is 90 DEG C in temperature, turns
Under the conditions of speed is 400r/min, constant temperature is stirred to react 4h, is that 20% sodium hydroxide solution is adjusted with mass fraction to the end of reaction
Material in reactor pH to 11.0 obtains redox graphene dispersion liquid；It is 1 in mass ratio again：5 by dispersant and reduction-oxidation
Graphene dispersing solution mixes, and under the conditions of supersonic frequency is 60kHz, ultrasonic disperse 4h, to the end of ultrasonic disperse, in room temperature item
Aging is stood under part for 24 hours, obtains Ageing solution, and by gained Ageing solution vacuum freeze drying, obtains modified graphene gel；By weight
Number meter takes 100 parts of aluminium powders successively, and 15 parts of magnesium powders, 6 parts of calcium powders, mixing is poured into graphite crucible, with after argon gas guard mode
Under, 920 DEG C are heated to, material in graphite crucible is made to melt completely, after being stirred 2h, then aluminium is added in into graphite crucible
The modified graphene gel of silty amount 6% continues at temperature as under 920 DEG C and argon gas guard mode, insulated and stirred mixes 30min
Afterwards, 1150 DEG C are warming up to 10 DEG C/min rate programs, after insulation reaction 15min, material in graphite crucible are poured into mold,
And 320 DEG C are naturally cooled under argon gas guard mode, it demoulds, obtains foamed aluminium blank, then gained foamed aluminium blank is fallen while hot
Enter to fill in sink of the temperature for 25 DEG C of deionized waters, under the conditions of supersonic frequency is 60kHz, after ultrasonic immersing 60min, then to
The ice cube of the quality such as deionized water is added in sink, continues at supersonic frequency as under the conditions of 70kHz, ultrasonic immersing 20min goes out
Material, obtains impregnated stock, and gained impregnated stock is washed with deionized 6 times, then the impregnated stock after washing is protected in nitrogen
Drying to constant weight under state to get trepanning sound-absorbing foam aluminum.The dispersant configuration process is：It is 1 in mass ratio：500 by 1-
After naphthoic acid and absolute ethyl alcohol mixing, constant temperature stirring obtains dispersant.
Example 4
It is 1 in mass ratio：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid, in room temperature condition
Under, 20h is stirred to react with 500r/min rotating speeds with blender, then three-necked flask is moved into the ice-water bath that temperature is 6 DEG C, in stirring
It mixes under state, the potassium permanganate of 1.5 times of crystalline flake graphite quality is added in into three-necked flask, is stirred to react with 500r/min rotating speeds
After 30min, the mass fraction of 0.6 times of deionized water and concentrated sulfuric acid quality for sequentially adding 0.5 times of concentrated sulfuric acid quality is 20%
Hydrogen peroxide continues to be stirred to react 30min, and filtering obtains filter residue, and filter residue is washed with deionized 5 times, then by the filter residue after washing
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain graphene oxide；It is 1 in mass ratio again：20 will oxidation
The solution of ferrous chloride that graphene and mass fraction are 12% is added in beaker, and the beaker immigration digital display constant temperature magnetic force that tests the speed is stirred
Device is mixed, is 55 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred 60min, and filtering obtains filter cake, as pre- place
Manage graphene oxide；It is 1 in mass ratio that graphene oxide and water, which will then be pre-processed,：Reaction kettle is poured into 200 mixing, in supersonic frequency
Under the conditions of rate is 50kHz, ultrasonic disperse 4h to the end of ultrasonic disperse, then adds in 5 times of graphene oxide quality into reaction kettle
Hydrazine hydrate is 90 DEG C in temperature to the end of hydrazine hydrate adds in, and under the conditions of rotating speed is 400r/min, constant temperature is stirred to react 4h, treats anti-
It should terminate, adjust material in reactor pH to 11.0 for 20% sodium hydroxide solution with mass fraction, obtain redox graphene point
Dispersion liquid；It is 1 in mass ratio again：5 mix dispersant and redox graphene dispersion liquid, and in supersonic frequency be 60kHz items
Under part, ultrasonic disperse 4h to the end of ultrasonic disperse, in standing aging for 24 hours under room temperature, obtains Ageing solution, and by gained aging
Liquid vacuum freeze drying obtains modified graphene gel；It counts in parts by weight, takes 100 parts of aluminium powders, 6 parts of calcium powders successively, mixing is poured into
In graphite crucible, with after under argon gas guard mode, 920 DEG C are heated to, material in graphite crucible is made to melt completely, stirred
After mixing 2h, then the modified graphene gel of aluminium powder quality 6% is added in into graphite crucible, continue at temperature as 920 DEG C and argon gas
Under guard mode, after insulated and stirred mixing 30min, 1150 DEG C are warming up to 10 DEG C/min rate programs, insulation reaction 15min
Afterwards, material in graphite crucible is poured into mold, and 320 DEG C is naturally cooled under argon gas guard mode, demoulded, obtain foamed aluminium
Blank, then gained foamed aluminium blank is poured into while hot and is filled in sink of the temperature for 25 DEG C of deionized waters, it is in supersonic frequency
Under the conditions of 60kHz, after ultrasonic immersing 60min, then the ice cube of the quality such as deionized water is added in into sink, continue at supersonic frequency
Under the conditions of 70kHz, ultrasonic immersing 20min, discharging obtains impregnated stock, and gained impregnated stock is washed with deionized 6 times,
By the impregnated stock after washing, drying to constant weight under nitrogen guard mode to get trepanning sound-absorbing foam aluminum again.The dispersant
Configuration process is：It is 1 in mass ratio：After 500 mix 1- naphthoic acids and absolute ethyl alcohol, constant temperature stirring obtains dispersant.
Example 5
It is 1 in mass ratio：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid, in room temperature condition
Under, 20h is stirred to react with 500r/min rotating speeds with blender, then three-necked flask is moved into the ice-water bath that temperature is 6 DEG C, in stirring
It mixes under state, the potassium permanganate of 1.5 times of crystalline flake graphite quality is added in into three-necked flask, is stirred to react with 500r/min rotating speeds
After 30min, the mass fraction of 0.6 times of deionized water and concentrated sulfuric acid quality for sequentially adding 0.5 times of concentrated sulfuric acid quality is 20%
Hydrogen peroxide continues to be stirred to react 30min, and filtering obtains filter residue, and filter residue is washed with deionized 5 times, then by the filter residue after washing
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain graphene oxide；It is 1 in mass ratio again：20 will oxidation
The solution of ferrous chloride that graphene and mass fraction are 12% is added in beaker, and the beaker immigration digital display constant temperature magnetic force that tests the speed is stirred
Device is mixed, is 55 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred 60min, and filtering obtains filter cake, as pre- place
Manage graphene oxide；It is 1 in mass ratio that graphene oxide and water, which will then be pre-processed,：Reaction kettle is poured into 200 mixing, in supersonic frequency
Under the conditions of rate is 50kHz, ultrasonic disperse 4h to the end of ultrasonic disperse, then adds in 5 times of graphene oxide quality into reaction kettle
Hydrazine hydrate is 90 DEG C in temperature to the end of hydrazine hydrate adds in, and under the conditions of rotating speed is 400r/min, constant temperature is stirred to react 4h, treats anti-
It should terminate, adjust material in reactor pH to 11.0 for 20% sodium hydroxide solution with mass fraction, obtain redox graphene point
Dispersion liquid；It is 1 in mass ratio again：5 mix dispersant and redox graphene dispersion liquid, and in supersonic frequency be 60kHz items
Under part, ultrasonic disperse 4h to the end of ultrasonic disperse, in standing aging for 24 hours under room temperature, obtains Ageing solution, and by gained aging
Liquid vacuum freeze drying obtains modified graphene gel；It counts in parts by weight, takes 100 parts of aluminium powders, 15 parts of magnesium powders successively, mixing is fallen
Enter in graphite crucible, with after under argon gas guard mode, be heated to 920 DEG C, material in graphite crucible is made to melt completely, is stirred
It mixes after mixing 2h, then the modified graphene gel of aluminium powder quality 6% is added in into graphite crucible, continue at temperature as 920 DEG C and argon
Under gas shielded state, after insulated and stirred mixing 30min, 1150 DEG C are warming up to 10 DEG C/min rate programs, insulation reaction 15min
Afterwards, material in graphite crucible is poured into mold, and 320 DEG C is naturally cooled under argon gas guard mode, demoulded, obtain foamed aluminium
Blank, then gained foamed aluminium blank is poured into while hot and is filled in sink of the temperature for 25 DEG C of deionized waters, it is in supersonic frequency
Under the conditions of 60kHz, after ultrasonic immersing 60min, then the ice cube of the quality such as deionized water is added in into sink, continue at supersonic frequency
Under the conditions of 70kHz, ultrasonic immersing 20min, discharging obtains impregnated stock, and gained impregnated stock is washed with deionized 6 times,
By the impregnated stock after washing, drying to constant weight under nitrogen guard mode to get trepanning sound-absorbing foam aluminum again.The dispersant
Configuration process is：It is 1 in mass ratio：After 500 mix 1- naphthoic acids and absolute ethyl alcohol, constant temperature stirring obtains dispersant.
Example 6
It is 1 in mass ratio：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid, in room temperature condition
Under, 20h is stirred to react with 500r/min rotating speeds with blender, then three-necked flask is moved into the ice-water bath that temperature is 6 DEG C, in stirring
It mixes under state, the potassium permanganate of 1.5 times of crystalline flake graphite quality is added in into three-necked flask, is stirred to react with 500r/min rotating speeds
After 30min, the mass fraction of 0.6 times of deionized water and concentrated sulfuric acid quality for sequentially adding 0.5 times of concentrated sulfuric acid quality is 20%
Hydrogen peroxide continues to be stirred to react 30min, and filtering obtains filter residue, and filter residue is washed with deionized 5 times, then by the filter residue after washing
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain graphene oxide；It is 1 in mass ratio again：20 will oxidation
The solution of ferrous chloride that graphene and mass fraction are 12% is added in beaker, and the beaker immigration digital display constant temperature magnetic force that tests the speed is stirred
Device is mixed, is 55 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred 60min, and filtering obtains filter cake, as pre- place
Manage graphene oxide；It is 1 in mass ratio that graphene oxide and water, which will then be pre-processed,：Reaction kettle is poured into 200 mixing, in supersonic frequency
Under the conditions of rate is 50kHz, ultrasonic disperse 4h to the end of ultrasonic disperse, then adds in 5 times of graphene oxide quality into reaction kettle
Hydrazine hydrate is 90 DEG C in temperature to the end of hydrazine hydrate adds in, and under the conditions of rotating speed is 400r/min, constant temperature is stirred to react 4h, treats anti-
It should terminate, adjust material in reactor pH to 11.0 for 20% sodium hydroxide solution with mass fraction, obtain redox graphene point
Dispersion liquid；It is 1 in mass ratio again：5 mix dispersant and redox graphene dispersion liquid, and in supersonic frequency be 60kHz items
Under part, ultrasonic disperse 4h to the end of ultrasonic disperse, in standing aging for 24 hours under room temperature, obtains Ageing solution, and by gained aging
Liquid vacuum freeze drying obtains modified graphene gel；It counts in parts by weight, takes 100 parts of aluminium powders, 15 parts of magnesium powders, 6 parts of calcium successively
Powder, mixing pour into graphite crucible, with after under argon gas guard mode, are heated to 920 DEG C, make material in graphite crucible complete
Full-fusing after being stirred 2h, then adds in into graphite crucible the modified graphene gel of aluminium powder quality 6%, and continuing at temperature is
920 DEG C, under argon gas guard mode, after insulated and stirred mixing 30min, are warming up to 1150 DEG C, heat preservation with 10 DEG C/min rate programs
After reacting 15min, material in graphite crucible is poured into mold, and 320 DEG C are naturally cooled under argon gas guard mode, taken off
Mould is to get trepanning sound-absorbing foam aluminum.The dispersant configuration process is：It is 1 in mass ratio：500 by 1- naphthoic acids and anhydrous second
After alcohol mixing, constant temperature stirring obtains dispersant.
Example 7
It is 1 in mass ratio：Crystalline flake graphite and mass fraction are poured into three-necked flask by 20 for the mixing of 98% concentrated sulfuric acid, in room temperature condition
Under, 20h is stirred to react with 500r/min rotating speeds with blender, then three-necked flask is moved into the ice-water bath that temperature is 6 DEG C, in stirring
It mixes under state, the potassium permanganate of 1.5 times of crystalline flake graphite quality is added in into three-necked flask, is stirred to react with 500r/min rotating speeds
After 30min, the mass fraction of 0.6 times of deionized water and concentrated sulfuric acid quality for sequentially adding 0.5 times of concentrated sulfuric acid quality is 20%
Hydrogen peroxide continues to be stirred to react 30min, and filtering obtains filter residue, and filter residue is washed with deionized 5 times, then by the filter residue after washing
It is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight, obtain graphene oxide；It is 1 in mass ratio again：20 will oxidation
The solution of ferrous chloride that graphene and mass fraction are 12% is added in beaker, and the beaker immigration digital display constant temperature magnetic force that tests the speed is stirred
Device is mixed, is 55 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature is stirred 60min, and filtering obtains filter cake, as pre- place
Manage graphene oxide；It is 1 in mass ratio that graphene oxide and water, which will then be pre-processed,：Reaction kettle is poured into 200 mixing, in supersonic frequency
Under the conditions of rate is 50kHz, ultrasonic disperse 4h to the end of ultrasonic disperse, then adds in 5 times of graphene oxide quality into reaction kettle
Hydrazine hydrate is 90 DEG C in temperature to the end of hydrazine hydrate adds in, and under the conditions of rotating speed is 400r/min, constant temperature is stirred to react 4h, treats anti-
It should terminate, adjust material in reactor pH to 11.0 for 20% sodium hydroxide solution with mass fraction, obtain redox graphene point
Dispersion liquid；It is 1 in mass ratio again：5 mix dispersant and redox graphene dispersion liquid, and in supersonic frequency be 60kHz items
Under part, ultrasonic disperse 4h to the end of ultrasonic disperse, in standing aging for 24 hours under room temperature, obtains Ageing solution, and by gained aging
Liquid vacuum freeze drying obtains modified graphene gel；It counts in parts by weight, takes 100 parts of aluminium powders, 15 parts of magnesium powders, 6 parts of calcium successively
Powder, mixing pour into graphite crucible, with after under argon gas guard mode, are heated to 920 DEG C, make material in graphite crucible complete
Full-fusing after being stirred 2h, then adds in into graphite crucible the modified graphene gel of aluminium powder quality 6%, and continuing at temperature is
920 DEG C, under argon gas guard mode, after insulated and stirred mixing 30min, are warming up to 1150 DEG C, heat preservation with 10 DEG C/min rate programs
After reacting 15min, material in graphite crucible is poured into mold, and 320 DEG C are naturally cooled under argon gas guard mode, taken off
Mould obtains foamed aluminium blank, then gained foamed aluminium blank is poured into while hot and is filled in sink of the temperature for 25 DEG C of deionized waters, Yu Chao
Under the conditions of acoustic frequency is 60kHz, after ultrasonic immersing 60min, discharging obtains impregnated stock, and gained is washed with deionized and impregnates
Blank 6 times, then drying to constant weight under nitrogen guard mode to get trepanning sound-absorbing foam aluminum by the impregnated stock after washing.Institute
Stating dispersant configuration process is：It is 1 in mass ratio：After 500 mix 1- naphthoic acids and absolute ethyl alcohol, constant temperature stirring must disperse
Agent.
Comparative example：The foamed aluminium of Liaoning new material Science and Technology Ltd. production.
The trepanning sound-absorbing foam aluminum of 1 to 7 gained of example and comparative example product are subjected to performance detection, specific detection method is such as
Under：
1. mechanical property：Test specimen compression strength is detected with reference to JG/T 359；
2. sound absorbing performance：Test specimen acoustic absorptivity is detected with reference to JG/T 359.
Specific testing result is as shown in table 1：
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Comparative example |
| Compression strength/MPa | 15.1 | 11.3 | 9.7 | 9.5 | 8.4 | 7.3 | 7.7 | 5.3 |
| Acoustic absorptivity | 0.99 | 0.91 | 0.87 | 0.86 | 0.73 | 0.69 | 0.66 | 0.51 |
By 1 testing result of table it is found that trepanning sound-absorbing foam aluminum prepared by technical solution of the present invention have excellent mechanical property and
The characteristics of sound absorbing performance, has broad prospects in the development of sound-absorbing material industry.
Claims (3)
1. a kind of preparation method of trepanning sound-absorbing foam aluminum, it is characterised in that specifically preparation process is：
（1）It is 1 in mass ratio by graphene oxide and solution of ferrous chloride：10~1：After 20 constant temperature are stirred, filtering obtains pre-
Handle graphene oxide；
（2）It is 1 in mass ratio that graphene oxide and water, which will be pre-processed,：100~1：After 120 mixing, ultrasonic disperse adds oxidation
The hydrazine hydrate that 3~5 times of graphene quality, constant temperature are stirred to react, and to the end of reaction, are adjusted pH to 10.5~11.0, are obtained oxygen reduction
Graphite alkene dispersion liquid；
（3）It is 1 in mass ratio：3~1：After 5 mix dispersant and redox graphene dispersion liquid, ultrasonic disperse is stood old
Change, it is dry, obtain modified graphene gel；
（4）It counts in parts by weight, takes 80~100 parts of aluminium powders, 10~15 parts of magnesium powders successively, 4~6 parts of calcium powders protect shape in argon gas
Under state, 900~920 DEG C, after being stirred 1~2h are heated to, adds the modified graphene gel of aluminium powder quality 4~6%, after
After continuation of insurance temperature is stirred, it is warming up to 1100~1150 DEG C, after insulation reaction, injection molding, and it is naturally cold under argon gas guard mode
But to 300~320 DEG C, foamed aluminium blank is obtained；
（5）Foamed aluminium blank is soaked in temperature is in 20~25 DEG C of deionized water, after 45~60min of ultrasonic immersing, to going
The ice cube of the quality such as deionized water is added in ionized water, continues 10~20min of ultrasonic immersing, is discharged, washing, and protected in nitrogen
Drying is to get trepanning sound-absorbing foam aluminum under state.
2. a kind of preparation method of trepanning sound-absorbing foam aluminum according to claim 1, it is characterised in that：Step（1）It is described
Solution of ferrous chloride mass fraction is 10~12%.
3. a kind of preparation method of trepanning sound-absorbing foam aluminum according to claim 1, it is characterised in that：Step（3）It is described
Dispersant configuration process is：It is 1 in mass ratio：200~1：After 500 mix 1- naphthoic acids and absolute ethyl alcohol, constant temperature stirring obtains
Dispersant.
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