CN105798287B - The process for dispersing that a kind of nickel nanowire surface covalent modification is modified - Google Patents

The process for dispersing that a kind of nickel nanowire surface covalent modification is modified Download PDF

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Publication number
CN105798287B
CN105798287B CN201610280443.XA CN201610280443A CN105798287B CN 105798287 B CN105798287 B CN 105798287B CN 201610280443 A CN201610280443 A CN 201610280443A CN 105798287 B CN105798287 B CN 105798287B
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nickel
nano wire
nickel nano
modified
dispersing
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CN105798287A (en
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徐金霞
曹亚龙
张长宽
蒋林华
宋迎宾
冯伟
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Hohai University HHU
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Hohai University HHU
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0547—Nanofibres or nanotubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • B22F1/147—Making a dispersion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38—Fibrous materials; Whiskers
    • C04B14/48—Metal

Abstract

The invention discloses the process for dispersing that a kind of nickel nanowire surface covalent modification is modified, the process for dispersing comprises the steps：(1) nickel nanowire surface processing solution and modifying agent are configured；(2) nickel nano wire is added in surface processing solution, after constant temperature stirring, is rinsed to neutrality and be dried in vacuo repeatedly with deionized water；(3) the nickel nano wire after processing is added in modifying agent, after constant temperature stirring, is rinsed well and be dried in vacuo repeatedly with ethanol solution with deionized water；(4) some obtained Modified Nickel nano wires are weighed to be added in the aqueous solution, after at the uniform velocity stirring, the nickel nano wire aqueous solution is made.Compared with prior art, the process for dispersing solves the problems, such as that nickel nano wire is easy to reunite or wind in aqueous, make it that nickel nano wire is fully dispersed in aqueous using relatively low cost, simple to operate, cost is low, efficiency high, has broad application prospects.

Description

The process for dispersing that a kind of nickel nanowire surface covalent modification is modified
Technical field
The present invention relates to a kind of preparation method of nano material, and in particular to what a kind of nickel nanowire surface covalent modification was modified Process for dispersing.
Technical background
For building or built great concrete structure engineering and infrastructure (such as high-rise building, bridge spanning the sea, big Type production platform and nuclear power station etc.), there is an urgent need to take effective monitoring means to evaluate its health status, to repair in time Damaged with control, it is ensured that reliability, security and the durability of engineering.Build great concrete structure engineering and infrastructure Health monitoring systems are, it is necessary to high-performance, long-life and stable smart sensor.It can pass through from cement-base composite material is perceived Macroscopical electric property change efficient diagnosis is suitable for sensing element with monitoring stress, strain or the damage of concrete structure. Compared with existing other sensing elements, there is natural compatibility from cement-base composite material and concrete structure is perceived, use There is unique advantage with monitoring in the Gernral Check-up of concrete structure, at the same time, it also has high sensitivity, good endurance etc. many Advantage.
Nevertheless, due to preparing the self-defect from the conductive filler for perceiving cement-base composite material, such as easily it is passivated, leads It is electrically bad, be difficult to it is scattered etc. so that it is existing from perceive cement-base composite material generally face uniformity and repeatability it is poor, The defects of combination property (including mechanical property, electric conductivity and self-sensing properties etc.) is not high, the presence of these defects limit now Development and application of some from perception cement-base composite material.Therefore, there is an urgent need to research and develop other new high quality fillers and its From the preparation method for perceiving cement-base composite material.
Nickel nano wire has good alkali resistance corrosive power, and has fabulous electric conductivity and excellent mechanical property, is One prepares from the potential high quality filler for perceiving cement-base composite material, has development and application prospect well.But nickel is received Rice noodles specific surface area is big, and surface energy is high, and non-thermodynamics stable state is between nano wire, easily occurs to reunite or winds.It is based on This, needs first solve scattering problem by the use of it as filler, but being currently available that ultrasonic disperse, high-power machinery are scattered easily makes nickel receive Rice noodles fracture, and can destroy nickel nano thread structure with reducing nano wire performance, so, still make at present without good method Nickel nano wire is fully dispersed in aqueous.
The content of the invention
Goal of the invention：It is an object of the invention to provide a kind of nickel nanowire surface covalent modification be modified process for dispersing, with Solve nickel nano wire easily to occur to reunite in aqueous or winding, can not be fully dispersed the problem of.
Technical scheme：The process for dispersing that a kind of nickel nanowire surface covalent modification of the present invention is modified, including following steps Suddenly：
(1) nickel nanowire surface processing solution and modifying agent are configured；Described surface processing solution be 0.20mol/L~ 0.30mol/L sulfuric acid solution；Described modifying agent is the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:15 ~1:10.
(2) nickel nano wire is added in the surface processing solution of step (1) configuration, after constant temperature stirring, uses deionized water Nickel nano wire is rinsed repeatedly to neutrality and to be dried in vacuo；
Wherein, the whipping temp of described constant temperature stirring is 50 DEG C~70 DEG C, and mixing time is 4min~5min, stirring speed Rate is 400rpm~800rpm；Described vacuum drying drying temperature is 40 DEG C~50 DEG C.
(3) the nickel nano wire after step (2) processing is added in the modifying agent of step (1) configuration, after constant temperature stirring, used Deionized water is rinsed well and is dried in vacuo repeatedly with ethanol solution, and Modified Nickel nano wire is made；
Wherein, the quality of described nickel nano wire is 5%~15% of oleic acid quality in modifying agent；Described constant temperature stirring Whipping temp be 60 DEG C~70 DEG C, mixing time is 90min~120min, and stir speed (S.S.) is 400rpm~800rpm；It is described Vacuum drying drying temperature be 40 DEG C~50 DEG C.
(4) Modified Nickel nano wire made from some steps (3) of weighing is added in the aqueous solution, and after at the uniform velocity stirring, nickel is made The nano wire aqueous solution；
Wherein, the mass concentration of the described nickel nano wire aqueous solution is less than 0.08%；During the described stirring at the uniform velocity stirred Between be 10min~15min, stir speed (S.S.) is 400rpm~800rpm.
Beneficial effect：Compared with prior art, the present invention is using oleic acid as modifying agent, and oleic acid is a kind of organic acid, by table Ni existing for nickel nano wire after the processing of face2+With OH-, oleic acid molecular and these Ni2+With OH-Combined in the form of chemical bonding, Reduce the surface energy of nickel nano wire so that nickel nano wire in aqueous can be relatively stable dispersed, thus solves The problem of nickel nano wire is easy to reunite or wind in aqueous.
In addition, the process for dispersing to nickel nano wire almost without destructiveness, avoid generally use now ultrasonic disperse, High-power machinery is scattered easily to make nickel nano wire fracture, and can destroy nickel nano thread structure with reducing lacking for nano wire performance Fall into.The process for dispersing does not need expensive reagent or equipment, it is not required that and especially the professional talent carries out high-precision operation, Can solve the scattering problem of nickel nano wire in aqueous using relatively low cost, nickel nano wire is fully divided in aqueous Dissipate, simple to operate, cost is low, efficiency high, has broad application prospects.
Embodiment
Technical scheme is described further with reference to specific embodiment, it should be understood that these embodiments are only used In the explanation present invention rather than limitation the scope of the present invention.
It should be noted that in the examples below that, the dispersion effect of nickel nano wire is with the standing sedimentation time and by ultraviolet It can be seen that the luminosity measurement obtained absorbance of examination characterizes.Wherein, the standing sedimentation time is longer, the more high then dispersion effect of absorbance Better.
Embodiment 1：
(1) nickel nanowire surface processing solution and modifying agent are configured, surface processing solution is 0.2mol/L sulfuric acid solution, Modifying agent is the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:10；
(2) nickel nano wire is placed in surface processing solution, constant temperature stirring, whipping temp is 50 DEG C, and mixing time is 4min, stir speed (S.S.) 400rpm, then nickel nano wire is rinsed to neutrality repeatedly with deionized water, be put into vacuum drying chamber baking Dry, drying temperature is 40 DEG C；
(3) the nickel nano wire of oleic acid quality 5% is added in modifying agent, constant temperature stirring, whipping temp is 60 DEG C, during stirring Between be 90min, stir speed (S.S.) 400rpm；Nickel nano wire, 1500rpm speed are rinsed repeatedly with deionized water and ethanol solution It is dried in vacuo after centrifugal sedimentation, drying temperature is 40 DEG C, and Modified Nickel nano wire is made；
(4) 0.012g Modified Nickel nano wires are weighed, 15ml deionized water is added, at the uniform velocity stirs, whipping temp is 20 DEG C, Mixing time is 10min, stir speed (S.S.) 400rpm, and the nickel nano wire aqueous solution is made.
At room temperature, the nickel being dispersed through nanowire suspended liquid sedimentation time and 1h absorbance are tested, its value is respectively The nanowire suspended liquid phase ratio of nickel of non-modified processing, its sedimentation time extend under 13min and 0.723, with equal conditions 30%, absorbance improves 12.79%, and in other words dispersion effect is improved.
Embodiment 2：
(1) nickel nanowire surface processing solution and modifying agent are configured, surface processing solution is that 0.25mol/L sulfuric acid is molten Liquid, modifying agent are the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:15；
(2) nickel nano wire is placed in surface processing solution, constant temperature stirring, whipping temp is 60 DEG C, and mixing time is 4min, stir speed (S.S.) 500rpm, then nickel nano wire is rinsed to neutrality repeatedly with deionized water, be put into vacuum drying chamber baking Dry, drying temperature is 50 DEG C；
(3) the nickel nano wire of oleic acid quality 10% is added in modifying agent, constant temperature stirring, whipping temp is 60 DEG C, stirring Time is 90min, stir speed (S.S.) 400rpm；Nickel nano wire, 2000rpm speed are rinsed repeatedly with deionized water and ethanol solution It is dried in vacuo after rate centrifugal sedimentation, drying temperature is 40 DEG C, and Modified Nickel nano wire is made；
(4) 0.01g Modified Nickel nano wires are weighed, 15ml deionized water is added, at the uniform velocity stirs, whipping temp is 20 DEG C, Mixing time is 15min, stir speed (S.S.) 600rpm, and the nickel nano wire aqueous solution is made.
At room temperature, the nickel being dispersed through nanowire suspended liquid sedimentation time and 1h absorbance are tested, its value is respectively The nanowire suspended liquid phase ratio of nickel of non-modified processing, its sedimentation time extend under 12min and 0.714, with equal conditions 20%, absorbance improves 11.38%, and in other words dispersion effect is improved.
Embodiment 3：
(1) nickel nanowire surface processing solution and modifying agent are configured, surface processing solution is 0.3mol/L sulfuric acid solution, Modifying agent is the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:15；
(2) nickel nano wire is placed in surface processing solution, constant temperature stirring, whipping temp is 70 DEG C, and mixing time is 5min, stir speed (S.S.) 600rpm, then nickel nano wire is rinsed to neutrality repeatedly with deionized water, be put into vacuum drying chamber baking Dry, drying temperature is 45 DEG C；
(3) the nickel nano wire of oleic acid quality 15% is added in modifying agent, constant temperature stirring, whipping temp is 60 DEG C, stirring Time is 100min, stir speed (S.S.) 500rpm；Nickel nano wire is rinsed repeatedly with deionized water and ethanol solution, 2500rpm's It is dried in vacuo after speed centrifugal sedimentation, drying temperature is 40 DEG C, and Modified Nickel nano wire is made；
(4) 0.008g Modified Nickel nano wires are weighed, 15ml deionized water is added, at the uniform velocity stirs, whipping temp is 20 DEG C, Mixing time is 12min, stir speed (S.S.) 500rpm, and the nickel nano wire aqueous solution is made.
At room temperature, the nickel being dispersed through nanowire suspended liquid sedimentation time and 1h absorbance are tested, its value is respectively The nanowire suspended liquid phase ratio of nickel of non-modified processing, its sedimentation time extend under 14min and 0.734, with equal conditions 40%, absorbance improves 14.5%, and in other words dispersion effect is improved.
Embodiment 4：
(1) nickel nanowire surface processing solution and modifying agent are configured, surface processing solution is that 0.25mol/L sulfuric acid is molten Liquid, modifying agent are the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:12；
(2) nickel nano wire is placed in surface processing solution, constant temperature stirring, whipping temp is 65 DEG C, and mixing time is 5min, stir speed (S.S.) 800rpm, then nickel nano wire is rinsed to neutrality repeatedly with deionized water, be put into vacuum drying chamber baking Dry, drying temperature is 45 DEG C；
(3) the nickel nano wire of oleic acid quality 10% is added in modifying agent, constant temperature stirring, whipping temp is 60 DEG C, stirring Time is 120min, stir speed (S.S.) 600rpm；Nickel nano wire is rinsed repeatedly with deionized water and ethanol solution, 2000rpm's It is dried in vacuo after speed centrifugal sedimentation, drying temperature is 40 DEG C, and Modified Nickel nano wire is made；
(4) 0.006g Modified Nickel nano wires are weighed, 15ml deionized water is added, at the uniform velocity stirs, whipping temp is 20 DEG C, Mixing time is 13min, stir speed (S.S.) 600rpm, and the nickel nano wire aqueous solution is made.
At room temperature, the nickel being dispersed through nanowire suspended liquid sedimentation time and 1h absorbance are tested, its value is respectively The nanowire suspended liquid phase ratio of nickel of non-modified processing, its sedimentation time extend under 13min and 0.731, with equal conditions 30%, absorbance improves 14.0%, and in other words dispersion effect is improved.
Embodiment 5：
(1) nickel nanowire surface processing solution and modifying agent are configured, surface processing solution is that 0.25mol/L sulfuric acid is molten Liquid, modifying agent are the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:13；
(2) nickel nano wire is placed in surface processing solution, constant temperature stirring, whipping temp is 60 DEG C, and mixing time is 5min, stir speed (S.S.) 700rpm, then nickel nano wire is rinsed to neutrality repeatedly with deionized water, be put into vacuum drying chamber baking Dry, drying temperature is 40 DEG C；
(3) the nickel nano wire of oleic acid quality 12% is added in modifying agent, constant temperature stirring, whipping temp is 70 DEG C, stirring Time is 120min, stir speed (S.S.) 800rpm；Nickel nano wire is rinsed repeatedly with deionized water and ethanol solution, 1500rpm's It is dried in vacuo after speed centrifugal sedimentation, drying temperature is 45 DEG C, and Modified Nickel nano wire is made；
(4) 0.01g Modified Nickel nano wires are weighed, 15ml deionized water is added, at the uniform velocity stirs, whipping temp is 20 DEG C, Mixing time is 14min, stir speed (S.S.) 700rpm, and the nickel nano wire aqueous solution is made.
At room temperature, the nickel being dispersed through nanowire suspended liquid sedimentation time and 1h absorbance are tested, its value is respectively The nanowire suspended liquid phase ratio of nickel of non-modified processing, its sedimentation time extend under 14.5min and 0.763, with equal conditions 45%, absorbance improves 19.0%, and in other words dispersion effect is improved.
Embodiment 6：
(1) nickel nanowire surface processing solution and modifying agent are configured, surface processing solution is that 0.20mol/L sulfuric acid is molten Liquid, modifying agent are the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:10；
(2) nickel nano wire is placed in surface processing solution, constant temperature stirring, whipping temp is 65 DEG C, and mixing time is 4min, stir speed (S.S.) 800rpm, then nickel nano wire is rinsed to neutrality repeatedly with deionized water, be put into vacuum drying chamber baking Dry, drying temperature is 40 DEG C；
(3) the nickel nano wire of oleic acid quality 15% is added in modifying agent, constant temperature stirring, whipping temp is 70 DEG C, stirring Time is 120min, stir speed (S.S.) 600rpm；Nickel nano wire is rinsed repeatedly with deionized water and ethanol solution, 2000rpm's It is dried in vacuo after speed centrifugal sedimentation, drying temperature is 45 DEG C, and Modified Nickel nano wire is made；
(4) 0.008g Modified Nickel nano wires are weighed, 15ml deionized water is added, at the uniform velocity stirs, whipping temp is 20 DEG C, Mixing time is 15min, stir speed (S.S.) 800rpm, and the nickel nano wire aqueous solution is made.
At room temperature, the nickel being dispersed through nanowire suspended liquid sedimentation time and 1h absorbance are tested, its value is respectively The nanowire suspended liquid phase ratio of nickel of non-modified processing, its sedimentation time extend under 14min and 0.745, with equal conditions 40%, absorbance improves 16.2%, and in other words dispersion effect is improved.

Claims (5)

  1. A kind of 1. process for dispersing that nickel nanowire surface covalent modification is modified, it is characterised in that：Comprise the steps：
    (1) nickel nanowire surface processing solution and modifying agent are configured；Described surface processing solution be 0.20mol/L~ 0.30mol/L sulfuric acid solution；Described modifying agent is the mixed liquor of oleic acid and ethanol, and the mass ratio of oleic acid and ethanol is 1:15 ~1:10；
    (2) nickel nano wire is added in the surface processing solution of step (1) configuration, after constant temperature stirring, with deionized water repeatedly Nickel nano wire is rinsed to neutrality and to be dried in vacuo；
    (3) the nickel nano wire after step (2) processing is added in the modifying agent of step (1) configuration, described nickel nano wire Quality is 5%~15% of oleic acid quality in modifying agent, after constant temperature stirring, is rinsed well repeatedly with ethanol solution with deionized water And be dried in vacuo, Modified Nickel nano wire is made；
    (4) Modified Nickel nano wire made from some steps (3) of weighing is added in the aqueous solution, and after at the uniform velocity stirring, nickel nanometer is made The line aqueous solution.
  2. 2. the process for dispersing that nickel nanowire surface covalent modification according to claim 1 is modified, it is characterised in that：Step (2) whipping temp of the constant temperature stirring described in is 50 DEG C~70 DEG C, and mixing time is 4min~5min, and stir speed (S.S.) is 400rpm~800rpm；Vacuum drying drying temperature described in step (2) is 40 DEG C~50 DEG C.
  3. 3. the process for dispersing that nickel nanowire surface covalent modification according to claim 1 is modified, it is characterised in that：Step (3) whipping temp of the constant temperature stirring described in is 60 DEG C~70 DEG C, and mixing time is 90min~120min, and stir speed (S.S.) is 400rpm~800rpm；Vacuum drying drying temperature described in step (3) is 40 DEG C~50 DEG C.
  4. 4. the process for dispersing that nickel nanowire surface covalent modification according to claim 1 is modified, it is characterised in that：Step (4) mass concentration of the nickel nano wire aqueous solution described in is less than 0.08%.
  5. 5. the process for dispersing that nickel nanowire surface covalent modification according to claim 1 is modified, it is characterised in that：Step (4) mixing time at the uniform velocity stirred described in is 10min~15min, and stir speed (S.S.) is 400rpm~800rpm.
CN201610280443.XA 2016-04-29 2016-04-29 The process for dispersing that a kind of nickel nanowire surface covalent modification is modified Expired - Fee Related CN105798287B (en)

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Publication number Priority date Publication date Assignee Title
CN106673532B (en) * 2017-01-20 2019-02-12 河海大学 A kind of perception nickel nanofiber cement-base composite material certainly
CN111434384B (en) * 2019-01-14 2023-07-25 中国石油天然气股份有限公司 Heavy oil aquathermolysis catalyst and preparation method and application thereof

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CN103785826A (en) * 2014-02-19 2014-05-14 南京林业大学 Method for preparing modified nanometer nickel powder
CN103962570A (en) * 2013-02-03 2014-08-06 宇辰新能源材料科技无锡有限公司 Preparation method of nickel nanopowder
CN104371452A (en) * 2014-10-31 2015-02-25 常熟市微尘电器有限公司 Conductive coating for electronic device and preparation method of conductive coating

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Publication number Priority date Publication date Assignee Title
JP2004043892A (en) * 2002-07-11 2004-02-12 Sumitomo Electric Ind Ltd Fine particle of noble metal and manufacturing method therefor
CN102136329A (en) * 2011-04-01 2011-07-27 钢铁研究总院 Iron-based composite soft magnetic material and preparation method thereof
CN103962570A (en) * 2013-02-03 2014-08-06 宇辰新能源材料科技无锡有限公司 Preparation method of nickel nanopowder
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