CN108265191A - The preparation method of oil solubility nanometer copper metallic composite - Google Patents
The preparation method of oil solubility nanometer copper metallic composite Download PDFInfo
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- CN108265191A CN108265191A CN201810064079.2A CN201810064079A CN108265191A CN 108265191 A CN108265191 A CN 108265191A CN 201810064079 A CN201810064079 A CN 201810064079A CN 108265191 A CN108265191 A CN 108265191A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
- C22C32/001—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 with only oxides
- C22C32/0015—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 with only oxides with only single oxides as main non-metallic constituents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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Abstract
The invention discloses the preparation methods of oil solubility nanometer copper metallic composite, SiO 2 powder, copper nanoparticle, organic solvent, silane coupling agent are carried out pyroreaction by the technique, then magnetic force reaction is carried out using the characteristic of acetone, further by adding dipivaloylmethane cerium, nano-sized carbon, silicon nitride, methyl acrylate, parachloroanilinum, oil solubility nanometer copper metallic composite is prepared in the components calcination such as mineral oil, paraffin, last mold, sub-cooled molding.The oil solubility nanometer copper metallic composite being prepared, oil-soluble stability is good, average grain diameter is small, centrifugal sedimentation stability is high, has preferable application prospect.
Description
Technical field
The present invention relates to this technical fields of material, are related specifically to the preparation side of oil solubility nanometer copper metallic composite
Method.
Background technology
For size, the size of fine particles of physicochemical properties significant changes is generally produced at 0.1 micron
(1 meter=1000 millimeters, 1 millimeter=1000 microns, 1 micron=1000 nanometers, 1 nanometer=10 angstroms of note) below, i.e., 100 nanometers with
Under.Therefore, particle size is known as ultra micron material and a kind of nano material in 1~100 nanometer of particle.Nano metal material
Material be the 1980s mid-term succeed in developing, that came out one after another later has Nanometer Semiconductor Films, nano ceramics, Nano ceramic
Property material and nano biological medical material etc..Nanoscale structures material is referred to as nano material (nanometer material),
Refer to the size of its structural unit between 1 nanometer~100 nanometer ranges.Since its size is already close to the relevant of electronics
Length, great changes will take place because strong relevant caused self-organizing causes property for its property.Also, its scale is close to light
Wavelength, in addition its special effects with large surface, therefore its characteristic for being showed, for example, fusing point, magnetism, optics, heat conduction,
Conductive characteristic etc., the property often showed different from the substance in integrality.Nano-particle material is also known as ultra micro
Granular materials is made of nano-particle (nano particle).Nano-particle is also ultramicro powder, generally refer to size 1~
Particle between 100nm is to be in the transitional region that cluster and macro object have a common boundary, from common about microcosmic and macroscopical sight
From the point of view of, such system both atypical microscopic system also atypical macrosystem, is a kind of typical Mesoscopic structure, it has
There are skin effect, small-size effect and macro quanta tunnel effect.When macro object is subdivided into ultramicro powder (nanometer by people
Grade) after, it would indicate that the property of many unusual characteristics, i.e. its optics, calorifics, electricity, magnetics, mechanics and chemistry aspect
Significant difference will be had by being compared when matter is with bulk solid.This research is dedicated to studying oil solubility nanometer copper metallic composite
Preparation process is matched by optimizing raw material, simplifies production technology so that the nanocomposite being prepared has preferable oil
Dissolubility stability, has broad application prospects.
Invention content
In order to solve the above technical problems, the invention discloses the preparation method of oil solubility nanometer copper metallic composite, it should
SiO 2 powder, copper nanoparticle, organic solvent, silane coupling agent are carried out pyroreaction by technique, then utilize the spy of acetone
Property carry out magnetic force reaction, further by add dipivaloylmethane cerium, nano-sized carbon, silicon nitride, methyl acrylate, to chlorobenzene
The components calcination such as amine, mineral oil, paraffin, last mold, sub-cooled molding are prepared oil solubility nanometer copper metal and answer
Condensation material.The oil solubility nanometer copper metallic composite being prepared, oil-soluble stability is good, average grain diameter is small, centrifugation is heavy
It is high to drop stability, there is preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
The preparation method of oil solubility nanometer copper metallic composite, includes the following steps：
(1) by 12-15 parts of SiO 2 powder, 15-20 parts of copper nanoparticle, 10-12 parts of organic solvent, silane coupling agent 3-
6 parts are positioned in tube furnace, and stove is first evacuated to air pressure as 5Pa, then be passed through 50 standard cubic centimeters/point 5%H2/ 95%Ar
Mixed carrier gas, while stove is heated up, it is reacted 8 hours at 1000-1300 DEG C, after stove natural cooling, it is compound to obtain silicon
Material；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and is ultrasonically treated
25min removes supernatant liquid, adds acetone, in triplicate, be cooled to room temperature, clean transparent to supernatant, utilizes additional magnetic
Field is detached, dry, obtains Nanometer Copper metallic composite；
(3) by 2-5 parts of 8-13 parts of Nanometer Copper metallic composite, dipivaloylmethane cerium, the nano-sized carbon 3-7 of step (2)
Part, 1-4 parts of silicon nitride, 3-9 parts of methyl acrylate, 2-5 parts of parachloroanilinum, 7-15 parts of mineral oil, 3-5 parts of paraffin inject tubular type
It in stove, is roasted under oxygen-containing atmosphere, temperature range is 780-850 DEG C, and roasting time is 8-12 hours, obtains oxidation nanometer material
Material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, material after molding is direct
It is put into -30 DEG C of cryogenic box and cools down 35 minutes；
(5) molding materials after the sub-cooled in step (4) are put into inert gas storage box, are cooled to room temperature, obtain
To finished product.
Preferably, the silane coupling agent in the step (1) is gamma-aminopropyl-triethoxy-silane, γ-glycidol ether
Oxygen propyl trimethoxy silicane, γ-(2,3 the third oxygen of epoxy) propyl trimethoxy silicane, N- (β-aminoethyl)-γ-aminopropyl three
One kind in methoxy silane.
Preferably, the organic solvent in the step (1) for n,N-Dimethylformamide, methanol, acetonitrile, N, N'- carbonyls
One or more of diimidazole.
Preferably, the externally-applied magnetic field condition in the step (2) is multi-joint magnetic agitation instrument magnetic force under the conditions of 35-45 DEG C
Stir 30-40min.
Preferably, the inert gas in the step (5) is nitrogen.
Compared with prior art, the present invention advantage is：
(1) preparation method of oil solubility nanometer copper metallic composite of the invention by SiO 2 powder, copper nanoparticle,
Organic solvent, silane coupling agent carry out pyroreaction, then carry out magnetic force reaction using the characteristic of acetone, further pass through addition
The components calcination such as dipivaloylmethane cerium, nano-sized carbon, silicon nitride, methyl acrylate, parachloroanilinum, mineral oil, paraffin, most
Oil solubility nanometer copper metallic composite is prepared in mold, sub-cooled molding afterwards.The oil solubility nanometer copper gold being prepared
Belong to composite material, oil-soluble stability is good, average grain diameter is small, centrifugal sedimentation stability is high, has preferable application prospect.
(2) oil solubility nanometer copper metallic composite raw material of the invention is easy to get, is simple for process, suitable for heavy industrialization
With highly practical.
Specific embodiment
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) by 12 parts of SiO 2 powder, 15 parts of copper nanoparticle, 10 parts of n,N-Dimethylformamide, three second of γ-aminopropyl
3 parts of oxysilane is positioned in tube furnace, and stove is first evacuated to air pressure as 5Pa, then be passed through 50 standard cubic centimeters/point 5%
H2/ 95%Ar mixed carrier gas, while stove is heated up, it is reacted 8 hours at 1000 DEG C, after stove natural cooling, obtains silicon
Composite material；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and is ultrasonically treated
25min removes supernatant liquid, adds acetone, in triplicate, be cooled to room temperature, clean transparent to supernatant, utilizes additional magnetic
Field is detached, dry, Nanometer Copper metallic composite is obtained, wherein multi-joint magnetic agitation instrument magnetic agitation under the conditions of 35 DEG C
30min；
(3) by 2 parts of 8 parts of Nanometer Copper metallic composite, the dipivaloylmethane cerium of step (2), 3 parts of nano-sized carbon, nitridation
1 part of silicon, 3 parts of methyl acrylate, 2 parts of parachloroanilinum, 7 parts of mineral oil, 3 parts of paraffin are injected in tube furnace, are roasted under oxygen-containing atmosphere
It burns, temperature range is 780 DEG C, and roasting time is 8 hours, obtains oxidation nanometer material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, material after molding is direct
It is put into -30 DEG C of cryogenic box and cools down 35 minutes；
(5) molding materials after the sub-cooled in step (4) are put into nitrogen storage box, are cooled to room temperature, obtain into
Product.
The performance test results of oil solubility nanometer copper metallic composite obtained are as shown in table 1.
Embodiment 2
(1) by 13 parts of SiO 2 powder, 17 parts of copper nanoparticle, 10 parts of methanol, γ-glycidyl ether oxygen propyl trimethoxy
4 parts of base silane is positioned in tube furnace, and stove is first evacuated to air pressure as 5Pa, then be passed through 50 standard cubic centimeters/point 5%H2/
95%Ar mixed carrier gas, while stove is heated up, it is reacted 8 hours at 1100 DEG C, after stove natural cooling, it is compound to obtain silicon
Material；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and is ultrasonically treated
25min removes supernatant liquid, adds acetone, in triplicate, be cooled to room temperature, clean transparent to supernatant, utilizes additional magnetic
Field is detached, dry, Nanometer Copper metallic composite is obtained, wherein multi-joint magnetic agitation instrument magnetic agitation under the conditions of 38 DEG C
33min；
(3) by 3 parts of 10 parts of Nanometer Copper metallic composite, the dipivaloylmethane cerium of step (2), 4 parts of nano-sized carbon, nitridation
2 parts of silicon, 5 parts of methyl acrylate, 3 parts of parachloroanilinum, 9 parts of mineral oil, 4 parts of paraffin are injected in tube furnace, are roasted under oxygen-containing atmosphere
It burns, temperature range is 800 DEG C, and roasting time is 9 hours, obtains oxidation nanometer material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, material after molding is direct
It is put into -30 DEG C of cryogenic box and cools down 35 minutes；
(5) molding materials after the sub-cooled in step (4) are put into nitrogen storage box, are cooled to room temperature, obtain into
Product.
The performance test results of oil solubility nanometer copper metallic composite obtained are as shown in table 1.
Embodiment 3
(1) by 14 parts of SiO 2 powder, 18 parts of copper nanoparticle, 11 parts of acetonitrile, γ-(2,3 the third oxygen of epoxy) propyl front three
5 parts of oxysilane is positioned in tube furnace, and stove is first evacuated to air pressure as 5Pa, then be passed through 50 standard cubic centimeters/point 5%
H2/ 95%Ar mixed carrier gas, while stove is heated up, it is reacted 8 hours at 1200 DEG C, after stove natural cooling, obtains silicon
Composite material；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and is ultrasonically treated
25min removes supernatant liquid, adds acetone, in triplicate, be cooled to room temperature, clean transparent to supernatant, utilizes additional magnetic
Field is detached, dry, Nanometer Copper metallic composite is obtained, wherein multi-joint magnetic agitation instrument magnetic agitation under the conditions of 42 DEG C
37min；
(3) by 4 parts of 11 parts of Nanometer Copper metallic composite, the dipivaloylmethane cerium of step (2), 6 parts of nano-sized carbon, nitridation
3 parts of silicon, 8 parts of methyl acrylate, 4 parts of parachloroanilinum, 12 parts of mineral oil, 4 parts of paraffin are injected in tube furnace, under oxygen-containing atmosphere
Roasting, temperature range are 820 DEG C, and roasting time is 11 hours, obtains oxidation nanometer material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, material after molding is direct
It is put into -30 DEG C of cryogenic box and cools down 35 minutes；
(5) molding materials after the sub-cooled in step (4) are put into nitrogen storage box, are cooled to room temperature, obtain into
Product.
The performance test results of oil solubility nanometer copper metallic composite obtained are as shown in table 1.
Embodiment 4
(1) by 15 parts of SiO 2 powder, 20 parts of copper nanoparticle, N, 12 parts of N'- carbonyl dimidazoles, N- (β-aminoethyl)-
6 parts of γ-aminopropyltrimethoxysilane is positioned in tube furnace, and stove is first evacuated to air pressure as 5Pa, then is passed through 50 standard cubes
The 5%H of centimeters/minute2/ 95%Ar mixed carrier gas, while stove is heated up, it is reacted 8 hours at 1300 DEG C, when stove is naturally cold
But after, silicon composite is obtained；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and is ultrasonically treated
25min removes supernatant liquid, adds acetone, in triplicate, be cooled to room temperature, clean transparent to supernatant, utilizes additional magnetic
Field is detached, dry, Nanometer Copper metallic composite is obtained, wherein multi-joint magnetic agitation instrument magnetic agitation under the conditions of 45 DEG C
40min；
(3) by 5 parts of 13 parts of Nanometer Copper metallic composite, the dipivaloylmethane cerium of step (2), 7 parts of nano-sized carbon, nitridation
4 parts of silicon, 9 parts of methyl acrylate, 5 parts of parachloroanilinum, 15 parts of mineral oil, 5 parts of paraffin are injected in tube furnace, under oxygen-containing atmosphere
Roasting, temperature range are 850 DEG C, and roasting time is 12 hours, obtains oxidation nanometer material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, material after molding is direct
It is put into -30 DEG C of cryogenic box and cools down 35 minutes；
(5) molding materials after the sub-cooled in step (4) are put into nitrogen storage box, are cooled to room temperature, obtain into
Product.
The performance test results of oil solubility nanometer copper metallic composite obtained are as shown in table 1.
Comparative example 1
(1) by 12 parts of SiO 2 powder, 15 parts of copper nanoparticle, 10 parts of n,N-Dimethylformamide, three second of γ-aminopropyl
3 parts of oxysilane is positioned in tube furnace, is reacted 8 hours at 1000 DEG C, after stove natural cooling, is obtained silicon composite wood
Material；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and is ultrasonically treated
25min removes supernatant liquid, adds acetone, in triplicate, be cooled to room temperature, clean transparent to supernatant, utilizes additional magnetic
Field is detached, dry, Nanometer Copper metallic composite is obtained, wherein multi-joint magnetic agitation instrument magnetic agitation under the conditions of 35 DEG C
30min；
(3) by 2 parts of 8 parts of Nanometer Copper metallic composite, the dipivaloylmethane cerium of step (2), 3 parts of nano-sized carbon, nitridation
1 part of silicon, 3 parts of methyl acrylate, 2 parts of parachloroanilinum, 7 parts of mineral oil, 3 parts of paraffin are injected in tube furnace, are roasted under oxygen-containing atmosphere
It burns, temperature range is 780 DEG C, and roasting time is 8 hours, obtains oxidation nanometer material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, material after molding is direct
It is put into -30 DEG C of cryogenic box and cools down 35 minutes；
(5) molding materials after the sub-cooled in step (4) are put into nitrogen storage box, are cooled to room temperature, obtain into
Product.
The performance test results of oil solubility nanometer copper metallic composite obtained are as shown in table 1.
Comparative example 2
(1) by 15 parts of SiO 2 powder, 20 parts of copper nanoparticle, N, 12 parts of N'- carbonyl dimidazoles, N- (β-aminoethyl)-
6 parts of γ-aminopropyltrimethoxysilane is positioned in tube furnace, and stove is first evacuated to air pressure as 5Pa, then is passed through 50 standard cubes
The 5%H of centimeters/minute2/ 95%Ar mixed carrier gas, while stove is heated up, it is reacted 8 hours at 1300 DEG C, when stove is naturally cold
But after, silicon composite is obtained；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and is ultrasonically treated
25min removes supernatant liquid, adds acetone, in triplicate, be cooled to room temperature, clean transparent to supernatant, utilizes additional magnetic
Field is detached, dry, Nanometer Copper metallic composite is obtained, wherein multi-joint magnetic agitation instrument magnetic agitation under the conditions of 45 DEG C
40min；
(3) by 5 parts of 13 parts of Nanometer Copper metallic composite, the dipivaloylmethane cerium of step (2), 7 parts of nano-sized carbon, nitridation
4 parts of silicon, 9 parts of methyl acrylate, 5 parts of parachloroanilinum, 15 parts of mineral oil, 5 parts of paraffin are injected in tube furnace, under oxygen-containing atmosphere
Roasting, temperature range are 850 DEG C, and roasting time is 12 hours, obtains oxidation nanometer material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, natural cooling molding to get
Finished product.
The performance test results of oil solubility nanometer copper metallic composite obtained are as shown in table 1.
The oil solubility nanometer copper metallic composite obtained of embodiment 1-4 and comparative example 1-2 is carried out to average grain respectively
Diameter, centrifugal sedimentation stability, oil-soluble evaluate this several performance tests.
Table 1
The present invention oil solubility nanometer copper metallic composite preparation method by SiO 2 powder, copper nanoparticle, have
Solvent, silane coupling agent carry out pyroreaction, then carry out magnetic force reaction using the characteristic of acetone, further pass through addition two
Tertiary valeryl methane cerium, nano-sized carbon, silicon nitride, methyl acrylate, the components calcination such as parachloroanilinum, mineral oil, paraffin, finally
Oil solubility nanometer copper metallic composite is prepared in mold, sub-cooled molding.The oil solubility nanometer copper metal being prepared
Composite material, oil-soluble stability is good, average grain diameter is small, centrifugal sedimentation stability is high, has preferable application prospect.This hair
Bright oil solubility nanometer copper metallic composite raw material is easy to get, is simple for process, is used suitable for heavy industrialization, highly practical.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright description is made directly or indirectly is used in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (5)
1. the preparation method of oil solubility nanometer copper metallic composite, which is characterized in that include the following steps：
(1) by 12-15 parts of SiO 2 powder, 15-20 parts of copper nanoparticle, 10-12 parts of organic solvent, 3-6 parts of silane coupling agent
Be positioned in tube furnace, stove is first evacuated to air pressure as 5Pa, then be passed through 50 standard cubic centimeters/point 5%H2/95%Ar mix
Carrier gas is closed, while stove is heated up, is reacted 8 hours at 1000-1300 DEG C, after stove natural cooling, obtains silicon composite wood
Material；
(2) silicon composite that step (1) obtains is scattered in acetone, is transferred in Ultrasound Instrument and carries out supersound process 25min,
Supernatant liquid is removed, acetone is added, in triplicate, is cooled to room temperature, cleans transparent to supernatant, is carried out using externally-applied magnetic field
Separation, it is dry, obtain Nanometer Copper metallic composite；
(3) by 2-5 parts of 8-13 parts of Nanometer Copper metallic composite, the dipivaloylmethane cerium of step (2), 3-7 parts of nano-sized carbon, nitrogen
1-4 parts of SiClx, 3-9 parts of methyl acrylate, 2-5 parts of parachloroanilinum, 7-15 parts of mineral oil, 3-5 parts of paraffin are injected in tube furnace,
It is roasted under oxygen-containing atmosphere, temperature range is 780-850 DEG C, and roasting time is 8-12 hours, obtains oxidation nanometer material；
(4) the oxidation nanometer material that step (3) obtains is directly injected into mold compression moulding, material after molding is directly put
Enter in -30 DEG C of cryogenic box and cool down 35 minutes；
(5) molding materials after the sub-cooled in step (4) are put into inert gas storage box, are cooled to room temperature, obtain into
Product.
2. the preparation method of oil solubility nanometer copper metallic composite according to claim 1, which is characterized in that the step
Suddenly the silane coupling agent in (1) for gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl trimethoxy silicane,
One kind in γ-(2,3 the third oxygen of epoxy) propyl trimethoxy silicane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane.
3. the preparation method of oil solubility nanometer copper metallic composite according to claim 1, which is characterized in that the step
Suddenly the organic solvent in (1) is n,N-Dimethylformamide, methanol, acetonitrile, one or more of N, N'- carbonyl dimidazoles.
4. the preparation method of oil solubility nanometer copper metallic composite according to claim 1, which is characterized in that the step
Suddenly the externally-applied magnetic field condition in (2) is multi-joint magnetic agitation instrument magnetic agitation 30-40min under the conditions of 35-45 DEG C.
5. the preparation method of oil solubility nanometer copper metallic composite according to claim 1, which is characterized in that the step
Suddenly the inert gas in (5) is nitrogen.
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| CN113416474A (en) * | 2021-05-12 | 2021-09-21 | 宁波格莱美厨具有限公司 | Uniform heat conduction non-stick pan coating and preparation method thereof |
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