CN109207778A - A kind of modified graphene enhancing composite material and preparation method thereof - Google Patents
A kind of modified graphene enhancing composite material and preparation method thereof Download PDFInfo
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- CN109207778A CN109207778A CN201811045333.0A CN201811045333A CN109207778A CN 109207778 A CN109207778 A CN 109207778A CN 201811045333 A CN201811045333 A CN 201811045333A CN 109207778 A CN109207778 A CN 109207778A
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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Abstract
The invention discloses a kind of modified graphenes to enhance composite material and preparation method thereof, comprising the following steps: (1) takes humic acid, be added in ethanol solution, dispersion is sufficiently stirred, filter, filter residue is dried for standby；(2) graphene is put into the first solvent, is dispersed with stirring, and is ultrasonically treated, and addition has pre-processed humic acid material, continues to stir, and synchronizing ultrasound is handled；Feed liquid evaporation drying obtains the first middle material；(3) by the first middle material and brass powder ball milling 1-12 hours；(4) under nitrogen protection, 10 DEG C -50 DEG C of brass melting temperature or more are heated to, keeps the temperature 10-30 minutes, furnace cooling after the completion of sintering obtains modified graphene enhancing composite material.Preparation method of the present invention uses ultrasonic wave added, ultrasonic shear acts on so that the dispersion fiting effect of graphene and humic acid is more preferable, when most brass carries out ball milling finally, the compounding that can reach Nano grade mutually mixes enhancing, and it is more preferably significant that final composite material inherits graphene reinforcing effect.
Description
Technical field
The present invention relates to a kind of enhancing composite material and preparation method thereof, especially a kind of modified graphene enhances brass composite wood
Material, belongs to technical field of composite preparation.
Background technique
Graphene (graphene) is the plane state carbon material separated from graphite, and graphene has hexagonal lattice, is put down
Each carbon atom is mutually connected on face with sp2 hybridized orbit.Graphene film thickness only has 0.335 nanometer, the carbon in plane
Atom mutually forms space electronic cloud before with big pi bond, and this structure of graphene, which makes it have, breaks through common graphite alkene material
Special performance performance.
The unique advantage performance of graphene is mainly manifested in graphene planes sp2 hybridized orbit connected structure, in graphene
On the direction that plane extends, graphene stability with super strength, while big pi bond makes graphene extending direction have super-hot
Conduction, electronic conductivity energy.If the formation of graphene can be made full use of, it can play and surmount performance, so that conventional
The performance of material is significantly promoted.
But generally require to be stacked between single-layer graphene molecule in the application process of graphene, it is changed into stone
The state of black property, interlayer misplaces, slides the superpower performance so that inside graphene single layer structure after multi-layer graphene stacks
It is difficult to give full play to.
In the prior art, graphene modification mostly uses greatly strong acid or alkali corrosion to handle, and is formed on the surface of graphene
A certain amount of functional group, improves the dispersibility of graphene, and then plays graphene molecules enhancing characteristic.But graphene molecules
Sp2 hybridized orbit space plane structure perfection characteristic itself makes modification grafted functional group for graphene molecules itself
Structural damage is very big, and modified later graphene cannot keep original advantageous property advantage substantially.
Also it has been proposed that handling later graphene to strong acid or highly basic by the way of chemical bonding carries out cross-linking reaction,
As the reparation of graphene surface, but due to the chemical bond functional group of graphene formation after strong acid or alkali corrosion processing
Complex, chemically reacting reparation, the effect is unsatisfactory.The graphene molecules for eventually passing through modification are often difficult to play
Optimal humidification out.
The present inventor attempts to be modified using humic acid (also referred to as humic acid, humic acid) in research before
Processing, but the dispersion effect of graphene itself is bad, needs to can be only achieved certain modified effect using strong stir process
Fruit.Industrial mass production is processed, intensively stirred controllability is poor, so also needing a kind of modification of optimization
Method.
Summary of the invention
It is an object of the invention to overcome the graphene method of modifying in the presence of the prior art to destroy graphene-structured
Deficiency provides a kind of modified graphene enhancing composite material and preparation method thereof.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes:
A kind of modified graphene enhancing composite material and preparation method thereof, comprising the following steps:
(1) humic acid is taken, is added in ethanol solution, dispersion is sufficiently stirred, is filtered, filter residue is dried for standby.
(2) graphene is put into the first solvent, is dispersed with stirring, and is ultrasonically treated, and the drying humic that step 1 has pre-processed is added
Acid starting material continues to stir, and synchronizing ultrasound is handled；After the completion, by feed liquid evaporation of solvent, dried powder is obtained, in first
Between expect.
(3) the first middle material and brass powder are added in ball mill together, ball milling 1-12 hours, ethyl alcohol or acetone conduct
Medium.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 10 DEG C of brass melting temperature or more-
50 DEG C, 10-30 minutes are kept the temperature, furnace cooling after the completion of sintering obtains modified graphene enhancing composite material.
Modified graphene enhancing composite material of the present invention is clean using humic acid progress ethanol washing, removes in humic acid
Small molecule ingredient, then with carry out composite modified under graphene ultrasound state, graphene is filled using the shear action of ultrasonic wave
It scatter, cooperation stirring action makes humic acid and graphene, and sufficiently effect reaches modified between each other.Finally, by modified
Graphene and brass ball mill mixing, nitrogen protective sintering obtain modified graphene enhancing composite material.
Further, step 1, the ethyl alcohol is the ethanol solution of 60v% or more, and the higher ethyl alcohol dissolution of purity is selected to remove
The effect of impurity is more preferable, and less moisture is smaller for the influence of humic acid overall quality, it is easier to which drying removes solution, makes
It is more outstanding to obtain the compound quality of humic acid and graphene in successive modified treatment process.
Further, step 1, ethanol solution dosage is 5-10 times of humic acid weight to be processed.Excess ethyl alcohol sufficiently dissolves
Impurity component in humic acid is removed, humic acid material is preferably purified.
Further, step 1, the humic acid material is the humic acid by milling processing.Preferably, corruption more than 80 mesh
Grow acid starting material.
Further, step 1, be dispersed with stirring is using mechanical stirring, speed of agitator 100r/min or more, mixing time 2-
30min。
Preferably, speed of agitator is greater than 600r/min, mixing time 5-15min.Be sufficiently stirred so that ethanol solution for
The better dispersing and dissolving impurity component of humic acid.
Further, it is 1:2-10 that humic acid and the weight ratio of graphene, which is added, in step 2.
Further, step 2, first solvent be water, low mass molecule alcohol, acetone etc. any one or a few.
Preferably, step 2, first solvent is water.Solvent is more environmentally-friendly, and graphene and humic acid are compound later dry
Dry processing is also easier and safe.
Further, step 2, the dosage of the first solvent is 5-20 times of the sum of humic acid and graphene weight.It is fully dispersed
Graphene and humic acid so that the two preferably mutually disperse it is compound.Preferably, dosage is 10-20 times.
Further, step 2, mixing speed 60-600r/min.
Further, step 2, sonification power 100-500w.
Further, step 2, sonication treatment time 10-40min.
Further, step 3, the material mixing ratio relationship of ball-milling treatment is as follows: the first middle material and brass powder parts by weight
Proportion is 7-16:93-84.Inventor is attempted by repetition test, is optimized and revised the first middle material and brass distribution ratio relationship, is reached
Enhance composite property effect to more outstanding collaboration.
Further, step 4, it is heated to above 10-20 DEG C of brass melting temperature.
Further, the brass is H62, H65, H70, H75, H80, H85, H90, H96 brass.
Preferably, the brass is the brass that copper content is 80-96wt%.It is highly preferred that copper content is 92- in brass
96wt%.
Preferably, 934 degree of brass melting temperature brass H62, H68 fusing point, brass H80 fusing point are 967.
Compared with prior art, beneficial effects of the present invention:
1, modified graphene enhancing composite material and preparation method thereof of the present invention pre-processes humic acid, cleaner, and
Cooperation stirring and the mode of ultrasonic wave added combine graphene and humic acid sufficiently in solution, finally with brass powder ball milling
Mixing, sintering obtain modified graphene enhancing composite material.
2, preparation method of the present invention uses ultrasonic wave added, and ultrasonic shear acts on so that the dispersion of graphene and humic acid cooperates
Effect is more preferable, and when most brass carries out ball milling finally, the compounding that can reach Nano grade mutually mixes enhancing, final composite material
It is more preferably significant to inherit graphene reinforcing effect.
3, it is auxiliary to combine ultrasound compared to the method for conventional strong stirring admixed graphite alkene and humic acid for the method for the present invention
After helping, multi-layer graphene is fully stripped dispersion, and the reinforcing effect in final composite material is more significant.
Specific embodiment
Below with reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
It is all that this is belonged to based on the technology that the content of present invention is realized for the scope of the above subject matter of the present invention is limited to the following embodiments
The range of invention.
Humic acid, also known as humic acid, humic acid, humic acid are the larger molecular organics being widely present in a kind of nature
Matter.Humic acid is that animals and plants remains are caused and accumulated by microorganism decomposition and conversion and a series of geochemical processes
A kind of organic substance to get up.The basic structure of humic acid macromolecular is aromatic ring, alicyclic ring, be connected on ring carboxyl, hydroxyl, carbonyl,
The functional groups such as quinonyl, methoxyl group.
Embodiment 1
Modified graphene enhances composite material preparation
(1) humic acid 2g is taken, is added in 85v% ethyl alcohol 20mL solution, magnetic agitation 20min dispersion, filtering, filter residue drying
It is spare.
(2) graphene 10g is put into 10v% ethanol water, and stirring 5min is uniformly dispersed.Open 300w ultrasonic instrument pair
Solution ultrasonic treatment, while the drying humic acid material that step 1 has pre-processed is added, continue stirring and synchronizing ultrasound processing
15min；After the completion, drying is evaporated under reduced pressure in feed liquid, obtains dried powder, the first middle material.
(3) the first middle material and H95 brass powder 88g are added in ball mill together, ball milling 6 hours, acetone is as Jie
Matter.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1040 DEG C and keeps the temperature 20 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Embodiment 2
Modified graphene enhances composite material preparation
(1) humic acid 3g is taken, is added in 85v% ethyl alcohol 20mL solution, magnetic agitation 20min dispersion, filtering, filter residue drying
It is spare.
(2) graphene 12g is put into 30mL aqueous solution, and stirring 10min is uniformly dispersed.300w ultrasonic instrument is opened to solution
Ultrasonic treatment, while the drying humic acid material that step 1 has pre-processed is added, continue stirring and synchronizing ultrasound processing 15min；It is complete
Drying is evaporated under reduced pressure in feed liquid by Cheng Hou, obtains dried powder, the first middle material.
(3) the first middle material and H90 brass powder 85g are added in ball mill together, ball milling 8 hours, acetone is as Jie
Matter.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1040 DEG C and keeps the temperature 15 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Embodiment 3
Modified graphene enhances composite material preparation
(1) humic acid 3g is taken, is added in 90v% ethyl alcohol 30mL solution, 200r/min mechanical stirring 20min dispersion, filtering,
Filter residue is dried for standby.
(2) graphene 12g is put into 30mL aqueous solution, and 300r/min stirring 15min is uniformly dispersed.Open 300w Ultrasound Instrument
Device is ultrasonically treated solution, while the drying humic acid material that step 1 has pre-processed is added, and continues stirring and synchronizing ultrasound processing
15min；After the completion, drying is evaporated under reduced pressure in feed liquid, obtains dried powder, the first middle material.
(3) the first middle material and H90 brass powder 85g are added in ball mill together, ball milling 8 hours, acetone is as Jie
Matter.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1040 DEG C and keeps the temperature 15 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Embodiment 4
Modified graphene enhances composite material preparation
(1) humic acid 4g is taken, is added in 90v% ethyl alcohol 20mL solution, 200r/min mechanical stirring 20min dispersion, filtering,
Filter residue is dried for standby.
(2) graphene 15g is put into 50mL aqueous solution, and 300r/min stirring 15min is uniformly dispersed.Open 300w Ultrasound Instrument
Device is ultrasonically treated solution, while the drying humic acid material that step 1 has pre-processed is added, and continues stirring and synchronizing ultrasound processing
15min；After the completion, drying is evaporated under reduced pressure in feed liquid, obtains dried powder, the first middle material.
(3) the first middle material and H90 brass powder 81g are added in ball mill together, ball milling 8 hours, acetone is as Jie
Matter.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1040 DEG C and keeps the temperature 15 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Embodiment 5
Modified graphene enhances composite material preparation
(1) humic acid 1.5g is taken, is added in 70v% ethyl alcohol 25mL solution, 200r/min mechanical stirring 20min dispersion, mistake
Filter, filter residue are dried for standby.
(2) graphene 10g is put into 50mL aqueous solution, and 300r/min stirring 15min is uniformly dispersed.Open 300w Ultrasound Instrument
Device is ultrasonically treated solution, while the drying humic acid material that step 1 has pre-processed is added, and continues stirring and synchronizing ultrasound processing
30min；After the completion, drying is evaporated under reduced pressure in feed liquid, obtains dried powder, the first middle material.
(3) the first middle material and H90 brass powder 88.5g are added in ball mill together, ball milling 6 hours, acetone conduct
Medium.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1080 DEG C and keeps the temperature 12 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Embodiment 6
Modified graphene enhances composite material preparation
(1) humic acid 2g is taken, is added in 70v% ethyl alcohol 25mL solution, 200r/min mechanical stirring 20min dispersion, filtering,
Filter residue is dried for standby.
(2) graphene 8g is put into 50mL aqueous solution, and 300r/min stirring 15min is uniformly dispersed.Open 300w Ultrasound Instrument
Device is ultrasonically treated solution, while the drying humic acid material that step 1 has pre-processed is added, and continues stirring and synchronizing ultrasound processing
30min；After the completion, drying is evaporated under reduced pressure in feed liquid, obtains dried powder, the first middle material.
(3) the first middle material and H90 brass powder 90g are added in ball mill together, ball milling 6 hours, acetone is as Jie
Matter.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1080 DEG C and keeps the temperature 12 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Embodiment 7
Modified graphene enhances composite material preparation
(1) humic acid 2.2g is taken, is added in 70v% ethyl alcohol 25mL solution, 200r/min mechanical stirring 20min dispersion, mistake
Filter, filter residue are dried for standby.
(2) graphene 8g is put into 50mL aqueous solution, and 300r/min stirring 15min is uniformly dispersed.Open 200w Ultrasound Instrument
Device is ultrasonically treated solution, while the drying humic acid material that step 1 has pre-processed is added, and continues stirring and synchronizing ultrasound processing
20min；After the completion, drying is evaporated under reduced pressure in feed liquid, obtains dried powder, the first middle material.
(3) the first middle material and H90 brass powder 89.8g are added in ball mill together, ball milling 6 hours, acetone conduct
Medium.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1080 DEG C and keeps the temperature 12 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Embodiment 8
Modified graphene enhances composite material preparation
(1) humic acid 2g is taken, is added in 70v% ethyl alcohol 25mL solution, 200r/min mechanical stirring 20min dispersion, filtering,
Filter residue is dried for standby.
(2) graphene 8g is put into 50mL aqueous solution, and 300r/min stirring 15min is uniformly dispersed.Open 300w Ultrasound Instrument
Device is ultrasonically treated solution, while the drying humic acid material that step 1 has pre-processed is added, and continues stirring and synchronizing ultrasound processing
40min；After the completion, drying is evaporated under reduced pressure in feed liquid, obtains dried powder, the first middle material.
(3) the first middle material and H90 brass powder 90g are added in ball mill together, ball milling 6 hours, acetone is as Jie
Matter.
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, it is heated to 1010 DEG C and keeps the temperature 12 minutes, sintering
Furnace cooling after the completion obtains modified graphene enhancing composite material.
Comparative example 1
Graphene enhances brass composite material, by the graphene 8% and H95 brass powder 92% of weight percent, mixing
Uniformly, under nitrogen protection, with being heated to 1100 DEG C, 10min is kept the temperature, sinter molding obtains graphene composite material.
Comparative example 2
A kind of modified graphene brass composite material, is prepared by following material: graphene 8%, and humic acid 2% is remaining
Amount is H90 brass.The method for preparing the modified graphene composite material is as follows:
(1) graphene and humic acid are mixed, is put into the 80v% ethyl alcohol of 3 times of weight, 3000r/min is stirred
30min is concentrated to dryness, and obtains graphene and humic acid mixture.
(2) brass raw material is taken, 1100 DEG C is heated to and melts, under nitrogen protection, by step 1 gained graphene and humic acid-mixed
It closes material to be added in the brass raw material of thawing, be uniformly mixed, continue melting 12min, it is compound to obtain modified graphene brass
Material.
Test
Above-described embodiment 2-10 and comparative example 1-2 composite material prepared is tested, the tensile strength of material is detected
MPa, thermal coefficient/W (mK)-1, result it is as follows:
1 test result of table
| Tensile strength/MPa | Thermal coefficient/W (mK)-1 | |
| Brass H85 | 312 | 152 |
| Brass H90 | 322 | 188 |
| Embodiment 2 | 336 | 236 |
| Embodiment 3 | 345 | 245 |
| Embodiment 4 | 342 | 253 |
| Embodiment 5 | 339 | 258 |
| Embodiment 6 | 348 | 251 |
| Embodiment 7 | 352 | 263 |
| Embodiment 8 | 353 | 259 |
| Comparative example 1 | 256 | 187 |
| Comparative example 2 | 332 | 245 |
Preparation method of the present invention mixes graphene and humic acid in the solution, assists promoting in conjunction with ultrasonic wave, make
Graphene and humic acid to meet effect more preferable, can achieve more preferable effect 30min more compound than 3000r/min high-speed stirred,
After graphene and humic acid modified later composite material and brass carry out being smelted into composite material, comprehensive tensile strength and
Thermal coefficient all has clear improvement, and shows that graphene is preferably dispersed, for the humidification of composite material brass base
Significantly.
Claims (10)
1. a kind of modified graphene enhances composite material and preparation method thereof, which comprises the following steps:
(1) humic acid is taken, is added in ethanol solution, dispersion is sufficiently stirred, is filtered, filter residue is dried for standby；
(2) graphene is put into the first solvent, is dispersed with stirring, and is ultrasonically treated, and it is former that the drying humic acid that step 1 has pre-processed is added
Material, continues to stir, and synchronizing ultrasound is handled；After the completion, by feed liquid evaporation of solvent, dried powder, the first middle material are obtained；
(3) the first middle material and brass powder are added in ball mill together, ball milling 1-12 hours, ethyl alcohol or acetone are as Jie
Matter；
(4) ball milling material is poured out, is filtered, vacuum drying；Under nitrogen protection, 10 DEG C -50 DEG C of brass melting temperature or more are heated to,
Heat preservation 10-30 minutes, furnace cooling after the completion of sintering obtain modified graphene enhancing composite material.
2. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that step 1, ethyl alcohol is molten
Liquid dosage is 5-10 times of humic acid weight to be processed.
3. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that step 1, the corruption
Growing acid starting material is the humic acid by milling processing.
4. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that step 1, stirring point
Dissipate is using mechanical stirring, speed of agitator 100r/min or more, mixing time 2-30min.
5. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that speed of agitator is greater than
600r/min, mixing time 5-15min.
6. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that corruption is added in step 2
The weight ratio for growing acid and graphene is 1:2-10.
7. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that step 2, described the
One solvent be water, low mass molecule alcohol, acetone etc. any one or a few.
8. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that step 2, at ultrasound
Manage power 100-500w.
9. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that step 2, at ultrasound
Manage time 10-40min.
10. modified graphene enhances composite material and preparation method thereof according to claim 1, which is characterized in that step 3, ball milling
The material mixing ratio relationship of processing is as follows: the first middle material and brass powder weight are 7-16:93-84.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105652A (en) * | 2021-11-19 | 2022-03-01 | 贵州万为金科特种建材有限公司 | Composite ceramic water reducing agent |
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2018
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105652A (en) * | 2021-11-19 | 2022-03-01 | 贵州万为金科特种建材有限公司 | Composite ceramic water reducing agent |
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