CN105880629B - A kind of preparation method of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet - Google Patents
A kind of preparation method of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet Download PDFInfo
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- CN105880629B CN105880629B CN201610346691.XA CN201610346691A CN105880629B CN 105880629 B CN105880629 B CN 105880629B CN 201610346691 A CN201610346691 A CN 201610346691A CN 105880629 B CN105880629 B CN 105880629B
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract
The invention belongs to technical field of nano material, are related to a kind of preparation method of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet.The metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet is made using metal nitrate, glycine and boric acid as raw material, by one-step treatment process in the present invention.The synthetic method synthesis technology of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet provided by the invention is simple, required raw material is cheap and easily-available in the market raw material, the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet obtained is bulk porous, has extraordinary application prospect in application fields such as capacitor, hydrogen storage carrier and bio-sensings.
Description
Technical field
The invention belongs to technical field of nano material more particularly to a kind of boron carbon nitrogen nanometer sheet are metal nanoparticles loaded miscellaneous
Change the preparation method of material.
Background technology
Carbon is a kind of element that nature is widely present, and has the characteristics that diversity, specificity and popularity.Carbon can
With with sp, sp2、sp3Three kinds of hybrid forms form solid simple substance, can form harder diamond, can also form softer stone
Ink, therefore, in the past 20 years, carbon nanomaterial is always the Disciplinary Frontiers of scientific and technical innovation.Various novel carbon materials emerge one after another,
The fullerene of such as zero dimension, one-dimensional nanotube, two-dimensional graphene.Graphene (Graphene) is a kind of newly discovered tool
There is the carbon nanomaterial of two-dimension plane structure, its special monoatomic layer structure makes it have many unique physical chemistry
Matter, such as larger specific surface area and excellent electronic conduction ability, cause researcher and widely pay close attention to.In recent years, a kind of
Class graphite material boron carbon nitrogen, due to its higher chemical stability, oxidation resistance, thermal stability, excellent machinery and electricity
Performance becomes new research hotspot, has caused " carbon " research boom of scientific and technological circle's new round.
Metal nano catalyst has in application fields such as fuel cell, biosensor, vehicle maintenance services all the time
Irreplaceable role.Wherein, noble metal nano particles (such as gold, silver, platinum) have many excellent physicochemical properties,
The application in the fields such as catalysis, electronics and sensor achieves huge progress.But the at high price of noble metal limits its
It uses.Therefore, the usage amount for how reducing noble metal and the service efficiency for how improving noble metal are current nano science works
One of emphasis of author investigation.On the one hand, (such as by common metal：Iron, cobalt, nickel, copper, bismuth etc.) as an alternative, it is that one kind can
With the means of consideration；On the other hand, it is compound with suitable carrier material, the hybrid material of Development of Novel can not only obtain
Performance more outstanding than metal nanoparticle itself, more the fields such as catalysis, magnetism, photoelectric material provide one it is novel
Material, and the consumption of metal is also greatly reduced, present prodigious economic value.
People are also seldom to the research report of boron carbon nitrogen load common metal particle hybrid material at present, therefore, to solve
It is very significant to study a kind of method preparing the metal nanoparticles loaded hybrid material of boron carbon nitrogen for the deficiencies in the prior art.
Invention content
In response to the deficiencies in the existing technology, boron carbon nitrogen nanometer sheet carried metal nanoparticle is prepared the present invention provides a kind of
The method of sub- hybrid material, this method have low raw-material cost, and preparation process is simple, is held high without synthesizing presoma and not being related to
The advantages that expensive, accurate instrument.
A kind of preparation method of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet provided by the invention, according to
Lower step carries out：
（1）In proportion by glycine, metal nitrate and boric acid mixing, gained mixture disperses in deionized water, point
Solute is dissipated, mixed solution is obtained, is transferred in aluminium oxide porcelain boat after the mixed solution ultrasound of gained；
（2）Above-mentioned aluminium oxide porcelain boat is placed in tube furnace, under argon atmosphere, is warming up to heat preservation one after predetermined temperature
It fixes time, then natural cooling, obtains the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet.
Wherein, the mass ratio of the glycine and metal nitrate is 0.25 ~ 3:1, the mass ratio of glycine and boric acid
It is 1 ~ 10:1, the mixture ultrasonic time is 0.5 ~ 1 hour；
Described be warming up to after predetermined temperature keeps the temperature concrete operations and is：It is warming up to 400 ~ 800 with the speed of 1 ~ 10 DEG C/min
DEG C, kept for 1 ~ 5 hour of temperature.
The metal of the metal nitrate includes nickel（Ni）, copper（Cu）Or bismuth（Bi）.
Beneficial effects of the present invention are：
（1）The present invention provides one kind preparing the metal nanoparticles loaded hydridization of boron carbon nitrogen nanometer sheet in one-step treatment process
The method of material, synthesis technology is simple, and required raw material is cheap and easily-available in the market raw material, and the period is short, is not related to expensive, essence
Close instrument is suitble to industrialized production；
（2）Boron carbon nitrogen nanometer sheet prepared by the present invention is metal nanoparticles loaded, is a kind of bulk porous material, can be with
Look forward to it has extraordinary application prospect in application fields such as double layer capacitor, hydrogen storage carrier and bio-sensings.
Description of the drawings
Fig. 1 is the optics picture of boron carbon nitrogen nanometer sheet carried metal copper nano-particle prepared by the embodiment of the present invention 2；
Fig. 2 is the X-ray of boron carbon nitrogen nanometer sheet carried metal copper nano-particle hybrid material prepared by the embodiment of the present invention 2
Diffracting spectrum（XRD）.
Specific implementation mode
Below in conjunction with the accompanying drawings and specific embodiment the present invention is further illustrated, but protection scope of the present invention is simultaneously
It is without being limited thereto.
Embodiment 1
The preparation of boron carbon nitrogen nanometer sheet carried metal nickel nano particle hybrid material：
200 mg nickel nitrates, 200 mg glycine and 50 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters
In, the mixture ultrasound of gained is transferred to after 0.5 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace
Heat preservation 1 hour after being warming up to 400 DEG C, then natural cooling, obtains boron carbon nitrogen nanometer sheet carried metal nickel nano particle hydridization
Material.
Embodiment 2
The preparation of boron carbon nitrogen nanometer sheet carried metal nickel nano particle hybrid material：
200 mg nickel nitrates, 50 mg glycine and 50 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters,
The mixture ultrasound of gained is transferred to after 0.6 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace and is heated up
Heat preservation 3 hours after to 500 DEG C, then natural cooling, obtains boron carbon nitrogen nanometer sheet carried metal nickel nano particle hydridization material
Material.
Embodiment 3
The preparation of boron carbon nitrogen nanometer sheet carried metal nickel nano particle hybrid material：
200 mg nickel nitrates, 600 mg glycine and 60 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters
In, the mixture ultrasound of gained is transferred to after 1 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace and is heated up
Heat preservation 5 hours after to 800 DEG C, then natural cooling, obtains boron carbon nitrogen nanometer sheet carried metal nickel nano particle hydridization material
Material.
Embodiment 4
The preparation of boron carbon nitrogen nanometer sheet carried metal copper nano-particle hybrid material：
200 mg copper nitrates, 200 mg glycine and 50 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters
In, the mixture ultrasound of gained is transferred to after 0.5 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace
Heat preservation 1 hour after being warming up to 400 DEG C, then natural cooling, obtains boron carbon nitrogen nanometer sheet carried metal copper nano-particle hydridization
Material.
Embodiment 5
The preparation of boron carbon nitrogen nanometer sheet carried metal copper nano-particle hybrid material：
200 mg copper nitrates, 50 mg glycine and 50 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters,
The mixture ultrasound of gained is transferred to after 0.6 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace and is heated up
Heat preservation 3 hours after to 500 DEG C, then natural cooling, obtains boron carbon nitrogen nanometer sheet carried metal copper nano-particle hydridization material
Material.
Fig. 1 is the boron carbon nitrogen nanometer sheet carried metal copper nano-particle hybrid material that the present embodiment obtains, as shown in Figure 1,
The boron carbon nitrogen nanometer sheet carried metal copper nano-particle powder of preparation is bulk, and specific surface is larger；
Fig. 2 is the X diffracting spectrums of boron carbon nitrogen nanometer sheet carried metal copper nano-particle made from the present embodiment, the mark with copper
Quasi- card matches, it was confirmed that the successful preparation of boron carbon nitrogen nanometer sheet carried metal copper nano-particle.
Embodiment 6
The preparation of boron carbon nitrogen nanometer sheet carried metal copper nano-particle hybrid material：
200 mg copper nitrates, 600 mg glycine and 60 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters
In, the mixture ultrasound of gained is transferred to after 1 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace and is risen
Temperature was to heat preservation after 800 DEG C 5 hours, and then natural cooling, obtains boron carbon nitrogen nanometer sheet carried metal copper nano-particle hydridization material
Material.
Embodiment 7
The preparation of the sub- hybrid material of boron carbon nitrogen nanometer sheet carried metal bismuth nanoparticle：
200 mg bismuth nitrates, 200 mg glycine and 50 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters
In, the mixture ultrasound of gained is transferred to after 0.5 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace
Heat preservation 1 hour after being warming up to 400 DEG C, then natural cooling, obtains boron carbon nitrogen nanometer sheet carried metal copper nano-particle hydridization
Material.
Embodiment 8
The preparation of the sub- hybrid material of boron carbon nitrogen nanometer sheet carried metal bismuth nanoparticle：
200 mg bismuth nitrates, 50 mg glycine and 50 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters,
The mixture ultrasound of gained is transferred to after 0.6 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace and is heated up
Heat preservation 3 hours after to 500 DEG C, then natural cooling, obtains the sub- hydridization material of boron carbon nitrogen nanometer sheet carried metal bismuth nanoparticle
Material.
Embodiment 9
The preparation of the sub- hybrid material of boron carbon nitrogen nanometer sheet carried metal bismuth nanoparticle：
200 mg copper nitrates, 600 mg glycine and 60 mg boric acid are added in beaker, are dispersed in 5 mL deionized waters
In, the mixture ultrasound of gained is transferred to after 1 hour in aluminium oxide porcelain boat；Above-mentioned aluminium oxide porcelain boat is placed in tube furnace and is risen
Temperature was to heat preservation after 800 DEG C 5 hours, and then natural cooling, obtains the sub- hydridization material of boron carbon nitrogen nanometer sheet carried metal bismuth nanoparticle
Material.
Claims (3)
1. a kind of preparation method of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet, which is characterized in that including as follows
Step：
（1）In proportion by glycine, metal nitrate and boric acid mixing, gained mixture disperses in deionized water, and dispersion is molten
Matter obtains mixed solution, is transferred in aluminium oxide porcelain boat after the mixed solution ultrasound of gained；The glycine and metal nitre
The mass ratio of hydrochlorate is 0.25 ~ 3:1, the mass ratio of glycine and boric acid is 1 ~ 10:1；
（2）Above-mentioned aluminium oxide porcelain boat is placed in tube furnace, under argon atmosphere, pre- constant temperature is warming up to the speed of 1 ~ 10 DEG C/min
1 ~ 5 hour is kept the temperature after 400 ~ 800 DEG C of degree, then natural cooling, it is metal nanoparticles loaded miscellaneous to obtain boron carbon nitrogen nanometer sheet
Change material.
2. a kind of preparation method of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet according to claim 1,
It is characterized in that, step（1）In, the mixed solution ultrasonic time is 0.5 ~ 1 hour.
3. a kind of preparation method of the metal nanoparticles loaded hybrid material of boron carbon nitrogen nanometer sheet according to claim 1,
It is characterized in that, the metal of the metal nitrate includes nickel, copper or bismuth.
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| CN107117589B (en) * | 2017-05-25 | 2019-03-12 | 华侨大学 | A kind of high specific capacitance (BC) xNyOz material and its synthetic method |
| CN107215852A (en) * | 2017-06-22 | 2017-09-29 | 山东大学 | The method that a kind of utilization graphene and boron nitride nanosheet prepare boron carbon nitrogen nanometer sheet |
| CN108439345A (en) * | 2018-03-15 | 2018-08-24 | 山东理工大学 | A method of preparing two-dimensional metallic oxide material on a large scale |
| CN110639592B (en) * | 2019-10-12 | 2022-09-23 | 浙江工业大学 | Boron and nitrogen doped carbon porous nanosheet supported transition metal nanoparticle material catalyst and preparation method and application thereof |
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