CN108862299A - A kind of amorphous state EuB6The preparation method of nano material - Google Patents
A kind of amorphous state EuB6The preparation method of nano material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of amorphous state EuB6The preparation method of nano material.The present invention restores anhydrous Europium chloride by diborane gas, successfully synthesizes amorphous state EuB at room temperature under liquid phase plasma body technique auxiliary6Nano material.The amorphous state EuB synthesized by this method6Nano material not only large specific surface area, but also there is excellent formaldehyde adsorption desorption responding ability at room temperature.The material has broad application prospects in terms of formaldehyde room temperature monitoring technical field.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of amorphous state EuB6The preparation side of nano material
Method.
Background technique
Influence of the formaldehyde to people's health is mainly manifested in allotriosmia, stimulation, allergy.The aerial concentration of formaldehyde reaches
0.06-0.07mg/m3When, children will occur slightly to pant；When formaldehyde content in indoor air is 0.1 mg/m3When, it will pierce
The eyes for swashing people are shed tears；Reach 0.6mg/m3When, throat discomfort or pain can be caused；When concentration is higher, nausea and vomiting can be caused,
It coughs uncomfortable in chest, asthma even pulmonary edema.Direct skin contact formaldehyde can cause dermatitis, color spot, cutaneous necrosis.Long-term sucking is few
Amount formaldehyde can cause slow poisoning, mucous hyperemia, skin irritatin disease, allergic dermatitis, nail angling etc. occur.Constitutional symptom has
Headache, out of strength, palpitaition, insomnia, weight loss, paramenia etc., it is more serious to cause nasopharyngeal carcinoma, colon cancer, brain tumor, cell
The gene mutation of core causes neonatal chromosome abnormality, leukaemia, and teenager's memory and intelligence is caused to decline.All
In contactee, children and pregnant woman's PARA FORMALDEHYDE PRILLS(91,95) are most sensitive.
With the development of industry, formaldehyde is widely used, so that the content of formaldehyde in certain work and living environment is significantly
More than safe range, very big threat is caused to human health.Therefore, it is necessary to often detect the content of formaldehyde in environment.About first
Oneself becomes a hot spot of Research of Environmental Sciences in recent years for the research of the monitoring method of aldehyde and apparatus.In order to greatly increase
The analysis speed of formaldehyde mitigates the workload of frequently detection formaldehyde, meets that capital's inhabitants are growing to want healthy and safe
It asks, new principle, new method, the new technology of research and development formaldehyde rapid field detection are a highly important job, it will right
The improvement of global habitat environment, the guarantee of food safety play a significant role.
In recent years, europium boride（EuB6）It is such as steady because of the special physical property of some as one of rare-earth boride
Fixed resistivity and low-expansion coefficient, compares the sensor for being suitable as high-resolution detector, so as to cause scientific and technical research
The research interest of person.However, EuB6Generally by 1650 DEG C of vacuum carbothermal reduction europium oxides（Eu2O3）And boron carbide
（B4C）, or prepare in 1400 DEG C of vacuum reduction EuO and B.Since temperature is very high, energy consumption is increased, is unfavorable for cleaning life
It produces.Therefore developing a new preparation method that low energy consumption has crucial work to the reduction of material cost in the industrial production
With.The present invention restores anhydrous Europium chloride by diborane gas, successfully closes at room temperature under liquid phase plasma body technique auxiliary
At amorphous state EuB6Nano material reduces energy consumption, so that its commercialization is advantageously.
Summary of the invention
The present invention uses liquid phase plasma body technique（LPT）, anti-using liquid phase plasma with independent intellectual property rights
Answer device（Utility model patent：201420301030.1）, anhydrous Europium chloride is restored by diborane gas at room temperature, is successfully closed
At amorphous state EuB6Nano material.Amorphous state EuB prepared by the present invention6PARA FORMALDEHYDE PRILLS(91,95) gas is shown nano material at room temperature
Out quickly, stable and highly selective response.
The present invention adopts the following technical scheme that：
（1）In 298K, under protection of argon gas by anhydrous Europium chloride（EuCl3）It is dissolved in chlorination 1- butyl -3- methylimidazole liquid
（[BMIM]Cl）In ionic liquid in, be transferred in liquid phase plasma reactor according;
（2）By diborane under 298K（B2H6）It is passed into（1）Solution in and be stirred continuously；
（3）It carries out liquid phase plasma precursor reactant 40 minutes, stirs simultaneously；Electricity between two electrodes of liquid phase plasma reactor according
Field is 500Vcm-1;
（4）Products therefrom is with after being washed with deionized, then three times with ethanol washing；
（5）Drying at 60 DEG C by it.
Step（1）Middle reaction protective gas is argon gas;
Step（1）In [BMIM] Cl liquid amount be 20mL;
Step（1）Middle EuCl3Amount be 2mmol;
Step（2）Middle B2H6Flow velocity be 5mL/min;
Step（3）Middle reaction temperature is 298K;
Step（3）Electric field between two electrodes of middle liquid phase plasma reactor according is 500Vcm-1;
Step（3）The middle reaction time is 40min.
The positive effect of the present invention is as follows：
1）The present invention synthesizes EuB using fluid plasma body technique at room temperature6Nano material, with the preparation EuB reported at present6
The method of material is compared, and low energy consumption for this method, to be more conducive to its industrialization.
2) amorphous state EuB prepared by the present invention6Nano material is compared other reported formaldehyde sensor materials, is had
PARA FORMALDEHYDE PRILLS(91,95) sensing sensitivity is higher at room temperature and senses the better advantage of selectivity.
Detailed description of the invention
Fig. 1 is amorphous state EuB prepared by embodiment 16XRD diagram of the nano material under different sintering temperatures.
Fig. 2 is amorphous state EuB prepared by embodiment 16The TEM photo of nano material；Illustration is SAED figure in photo
Piece.
Fig. 3 is amorphous state EuB prepared by embodiment 16The Eu3d xps energy spectrum figure of nano material.
Fig. 4 is amorphous state EuB prepared by embodiment 16The B1sXPS energy spectrum diagram of nano material.
Fig. 5 is amorphous state EuB prepared by embodiment 16Nano material is at room temperature to 10ppm gas with various（H2S, ethyl alcohol,
Isopropanol, CH4, NO2, 92#Gasoline, toluene, acetone, NH3, H2And CO）Response diagram.
Fig. 6 is amorphous state EuB prepared by embodiment 16Nano material and different EuB6Sound of the sample to 10 ppm HCHO
Ying Tu.
Fig. 7 is amorphous state EuB prepared by embodiment 16Response of the nano material in different formaldehyde gas concentration is sensitive
Degree, response time and recovery time.
Fig. 8 is amorphous state EuB prepared by embodiment 16Linear response of the nano material under different formaldehyde gas concentration
Figure.
Fig. 9 is amorphous state EuB prepared by embodiment 16Cycle performance figure of the nano material in 10ppm formaldehyde gas.
Figure 10 is amorphous state EuB prepared by embodiment 16Nano material influences the humidity that 10ppm formaldehyde gas responds
Figure.
Figure 11 is amorphous state EuB prepared by embodiment 16During absorption and desorption of the nano material in formaldehyde gas
Eu3dXPS spectrogram in situ.
Figure 12 is amorphous state EuB prepared by embodiment 16During absorption and desorption of the nano material in formaldehyde gas
DRIFTS spectrogram in situ.
Figure 13 is amorphous state EuB prepared by embodiment 16Conductivity of the nano material under different formaldehyde gas concentration becomes
Change figure.
Specific embodiment
The following examples are a further detailed description of the invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
To achieve the above object, amorphous state EuB6The preparation step of nano material is：
（1）In 298K, under protection of argon gas by anhydrous Europium chloride（EuCl3）It is dissolved in chlorination 1- butyl -3- methylimidazole liquid
（[BMIM]Cl）In ionic liquid in, be transferred in liquid phase plasma reactor according;
（2）By diborane under 298K（B2H6）It is passed into（1）Solution in and be stirred continuously；
（3）It carries out liquid phase plasma precursor reactant 40 minutes, stirs simultaneously；Electricity between two electrodes of liquid phase plasma reactor according
Field is 500Vcm-1;
（4）Products therefrom is with after being washed with deionized, then three times with ethanol washing；
（5）Drying at 60 DEG C by it.
Amorphous state EuB prepared by embodiment 16The XRD spectrum of nano material is shown in Figure 1.Its at room temperature, 2 θ=
Only one broad peak near 30.1 ° shows EuB prepared by embodiment 16Nano material is amorphous.However, in such as 973K
After annealing 2 hours in the high temperature argon atmosphere of 1173K, crystalline state EuB is obtained6Nano material（Fig. 1）.
TEM image in Fig. 2 shows that sample has irregular form, and the average diameter of particle is about 6nm.Selected area
Domain electronic diffraction（SAED）Haloing in pattern（Illustration in Fig. 2）Further demonstrate its amorphous structure.
Elemental analysis the result shows that, the B/Eu ratio of sample is 6.In addition, the specific surface area of sample is 221.3m2g-1, long-range
In business EuB6（14.6m2g-1）.At 1156.5 and 1128.8eV（Fig. 3）The peak Eu 3d XPS correspond respectively to Eu0 3d3/2
And Eu0 3d5/2, show that Eu element belongs to atomic state in the material.In addition, B also exists with state of atom, in conjunction with can be
188.3eV（Fig. 4）.The combination energy excursion of Eu3d（Eu 3d3/2Negative offset 0.5eV, Eu3d5/2Negative offset 0.8eV）And B1s（Just
Deviate 1.2eV）Show that some electronics are transferred to Eu from B.This shows EuB6It is Eu electron rich material, is similar to most of reports
Amorphous metal-the boron alloy in road.
With to other gases（Hydrogen sulfide, ethyl alcohol, isopropanol, methane, nitrogen dioxide, 92#Gasoline, toluene, acetone, ammonia,
Hydrogen and carbon monoxide）Response compare, our amorphous state EuB6Sensor is more preferable to the response of 10ppm formaldehyde gas（Figure
5）.In addition, carbon monoxide has certain volume change（ΔC/C）.But methane, hydrogen and toluene only have the signal of very little.
Business EuB is compared in Fig. 66With amorphous state EuB6Response to 10ppm formaldehyde gas.It was found that amorphous state EuB6Compare crystalline state
EuB6With better formaldehyde gas response performance, it is attributed to amorphous state EuB6Amorphous structure and biggish surface area（Quotient
Industry EuB6Specific surface is 221.3m2g-1, business EuB6For 14.6m2g-1）, increase the adsorption site of formaldehyde gas.In addition, amorphous
State EuB6Response time of the response of PARA FORMALDEHYDE PRILLS(91,95) gas within the scope of 2 to 20ppm and recovery response time are respectively less than 35 seconds（Figure
7）, and the response of PARA FORMALDEHYDE PRILLS(91,95) gas and formaldehyde gas concentration are in a linear relationship（Fig. 8）.
Meanwhile amorphous state EuB6Stable cycle performance is shown in test in 30 days by a definite date（Fig. 9）.In addition, in 10-
60% relative humidity（RH）Under, humidity is to amorphous state EuB6Sensing capabilities influence it is very small or negligible.But when
When relative humidity is further increased to 80%RH from 60%RH, humidity is to amorphous state EuB6Sensing capabilities influence increase（Figure
10）.
In general, the sensing characteristics of material PARA FORMALDEHYDE PRILLS(91,95) gas, because of the oxygen of formaldehyde gas molecule and its Adsorption on Surface
Chemical reaction between substance forms carbon dioxide and water so as to cause the variation of material electric conductivity.To amorphous state EuB6Come
It says, in the response process of formaldehyde gas, does not observe the oxidation or decomposition of formaldehyde gas molecule.Because adopting in an experiment
With with2H and13When the formaldehyde gas of C isotope labelling, do not observe2H2,2H2O and13CO2.Meanwhile during the experiment, exist
EuB6Surface does not find the oxidation of Eu（Figure 11）.In addition, B or B2O3PARA FORMALDEHYDE PRILLS(91,95) gas is without any response.This illustrates metal Eu
It is amorphous state EuB6PARA FORMALDEHYDE PRILLS(91,95) gas generates the sole active site of response.Therefore, amorphous state EuB6The good biography of PARA FORMALDEHYDE PRILLS(91,95) gas
Perception can be attributable to the interaction between formaldehyde gas molecule and its site Eu rich in electronics, this can pass through amorphous state
EuB6The Eu 3d XPS in situ observed during PARA FORMALDEHYDE PRILLS(91,95) gas molecule adsorbs and desorbs combines the variation of energy to be confirmed
（Figure 11）.
In addition, formaldehyde gas molecule and amorphous state EuB6Between this interaction can pass through diffusing reflection in situ simultaneously
Fourier transform infrared spectroscopy（DRIFTS）In the wave number at the part peak of formaldehyde molecule observed be displaced and further confirmed
（Figure 12）.It can be recognized from fig. 12 that peak is not observed before formaldehyde absorbing.After introducing formaldehyde, occur 2960,2915,
2864,2753,1780,1729,1543,1428,1350,1300,1246cm-1The new absorption peak at place.2960,2915,2864 Hes
2753cm-1The bands of a spectrum at place be C-H in formaldehyde molecule it is flexible caused by absorption peak, 1780,1729,1543,1428,1350,
1300 and 1246cm-1Place is absorbed as EuB6Generated peak after upper formaldehyde adsorption molecule.
This interaction may be attributed to formaldehyde molecule/EuB6In system between the 2p track of oxygen and the 6s track of Eu
Hydridization, this and H at room temperature2Report in S sensing system is similar.In adsorption process, some electronics are from EuB6The Eu of middle electron rich
The O being transferred in formaldehyde molecule.Therefore, with the absorption of PARA FORMALDEHYDE PRILLS(91,95) molecule, it can be observed that amorphous state EuB6Conductivity by
It is cumulative to add（Figure 13）.This is attributed to amorphous state EuB6Due to leading to the increase of its hole concentration after electronics transfer on surface.
PARA FORMALDEHYDE PRILLS(91,95) gas is shown quickly sample prepared by embodiment 1 at room temperature, and stable and highly selective response is
Effective formaldehyde gas monitoring system is constructed at room temperature, and the health of people is protected to provide possibility.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of amorphous state EuB6The preparation method of nano material, it is characterised in that：
Specific step is as follows for synthetic method：
In 298K, under protection of argon gas by anhydrous Europium chloride（EuCl3）It is dissolved in chlorination 1- butyl -3- methylimidazole liquid
（[BMIM]Cl）In ionic liquid in, be transferred in liquid phase plasma reactor according;
By diborane under 298K（B2H6）It is passed into（1）Solution in and be stirred continuously；
It carries out liquid phase plasma precursor reactant 40 minutes, stirs simultaneously；Electric field between two electrodes of liquid phase plasma reactor according
For 500Vcm-1;
Products therefrom is with after being washed with deionized, then three times with ethanol washing；
Drying at 60 DEG C by it.
2. a kind of amorphous state EuB as described in claim 16The method of the preparation method of nano material, it is characterised in that：Step
（1）Middle reaction protective gas is argon gas.
3. a kind of amorphous state EuB as described in claim 16The preparation method of nano material, it is characterised in that：Step（1）In
The amount of [BMIM] Cl liquid is 20mL.
4. a kind of amorphous state EuB as described in claim 16The preparation method of nano material, it is characterised in that：Step（1）In
EuCl3Amount be 2mmol.
5. a kind of amorphous state EuB as described in claim 16The preparation method of nano material, it is characterised in that：Step（2）In
B2H6Flow velocity be 5mL/min.
6. a kind of amorphous state EuB as described in claim 16The preparation method of nano material, it is characterised in that：Step（3）In it is anti-
Answering temperature is 298K.
7. a kind of amorphous state EuB as described in claim 16The preparation method of nano material, it is characterised in that：Step（3）Middle liquid
Electric field between two electrodes of phase plasma reactor is 500Vcm-1。
8. a kind of amorphous state EuB as described in claim 16The preparation method of nano material, it is characterised in that：Step（3）In it is anti-
It is 40 minutes between seasonable.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665537A (en) * | 2019-02-22 | 2019-04-23 | 成都理工大学 | A kind of low temperature preparation EuB6The method of nanocube crystal |
| CN110002459A (en) * | 2019-04-12 | 2019-07-12 | 成都理工大学 | A kind of preparation method for mixing nickel europium boride |
| CN110092388A (en) * | 2019-05-15 | 2019-08-06 | 成都理工大学 | A kind of preparation method of six ytterbium borides alloy nano particle |
| CN110745838A (en) * | 2019-10-25 | 2020-02-04 | 成都理工大学 | CuB23Preparation method of nanoflower |
| CN110759350A (en) * | 2019-12-04 | 2020-02-07 | 成都理工大学 | Preparation method of zirconium boride nanoparticles |
| CN110759349A (en) * | 2019-10-30 | 2020-02-07 | 成都理工大学 | Porous CuB23Preparation method of (1) |
| CN110862094A (en) * | 2019-11-27 | 2020-03-06 | 成都理工大学 | CaB6Process for preparing nanoparticles |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665537A (en) * | 2019-02-22 | 2019-04-23 | 成都理工大学 | A kind of low temperature preparation EuB6The method of nanocube crystal |
| CN110002459A (en) * | 2019-04-12 | 2019-07-12 | 成都理工大学 | A kind of preparation method for mixing nickel europium boride |
| CN110092388A (en) * | 2019-05-15 | 2019-08-06 | 成都理工大学 | A kind of preparation method of six ytterbium borides alloy nano particle |
| CN110745838A (en) * | 2019-10-25 | 2020-02-04 | 成都理工大学 | CuB23Preparation method of nanoflower |
| CN110759349A (en) * | 2019-10-30 | 2020-02-07 | 成都理工大学 | Porous CuB23Preparation method of (1) |
| CN110862094A (en) * | 2019-11-27 | 2020-03-06 | 成都理工大学 | CaB6Process for preparing nanoparticles |
| CN110759350A (en) * | 2019-12-04 | 2020-02-07 | 成都理工大学 | Preparation method of zirconium boride nanoparticles |
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