CN110092388A - A kind of preparation method of six ytterbium borides alloy nano particle - Google Patents
A kind of preparation method of six ytterbium borides alloy nano particle Download PDFInfo
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- CN110092388A CN110092388A CN201910400720.XA CN201910400720A CN110092388A CN 110092388 A CN110092388 A CN 110092388A CN 201910400720 A CN201910400720 A CN 201910400720A CN 110092388 A CN110092388 A CN 110092388A
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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
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- C01B35/00—Boron; Compounds thereof
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
The invention discloses six ytterbium boride (YbB of one kind6) alloy nano particle preparation method.Pass through ytterbium chloride (YbCl in liqu id plasmas field3) and diborane (B2H6) reaction prepared YbB in irregular shape6Alloy nano particle, average grain diameter 7.3nm, specific surface area 167.8m2·g‑1.It has quick, stable and highly selective response to alcohol vapour under the conditions of 25 DEG C, and detection is limited to 75ppb.The material has good detection performance to alcohol vapor, is mainly due to its unique alloy property and and its catalytic dehydration to ethyl alcohol.The present invention provides not only a kind of sensing material for capableing of efficient detection alcohol vapour at room temperature, while also providing and a kind of catalysis ethanol dehydration can prepare the catalyst of ether at room temperature.
Description
Technical field
The present invention relates to technical field of nano material, more particularly to a kind of preparation side of six ytterbium boride alloy nano-materials
Method.
Background technique
The main reason for drunk driving is traffic accident in the world, alcohol content in blood are greater than or equal to the driving quilt of 200ppm
It is considered to drive when intoxicated.Therefore, alcohol vapour monitoring technology receives attention in terms of prevention is driven when intoxicated.However, existing
Based on ZnO, SnO2、WO3And LaFeO3Equal ethanol sensors also have comparable sensing selectivity to many other gases, this
Affect their sensing capabilities to ethyl alcohol.In addition, current sensor needs higher operating temperature (100-300 DEG C).Cause
This, it is necessary to the novel sensing material of design and synthesis, making it under cryogenic still has efficient ethyl alcohol sensing selectivity.
Six ytterbium boride (YbB6) there is unique conductive surface, it has broad application prospects in engineer application.It is solely
Special property also improves small molecule selective absorption to YbB6A possibility that surface.Therefore, YbB6It is simultaneously also a kind of potential
Sensing material.
YbB6Traditional synthetic method has mechanochemical reaction, high-temperature sintering process, vacuum calcining method and combustion synthesis method etc..So
And these processes require to expend comparable energy and time.Therefore, YbB is synthesized6Need a kind of new method.In recent years, liquid
Bulk plasmon technology (LPT) causes the extensive concern of people as a kind of novel metal boride synthetic method.At me
In previous research work, CuB is successfully synthesized by LPT technology at room temperature23Nanoparticle, and as room temperature item
H under part2Sensor；EuB is successfully prepared by LPT technology6, HCHO steam is shown at room temperature superior
Sensing capabilities.
Summary of the invention
In present invention work, in room temperature under argon gas (Ar) protective condition, we are successfully in liqu id plasmas field
Pass through ytterbium chloride (YbCl3) and diborane (B2H6) reaction prepared YbB in irregular shape6Alloy nano particle is put down
Equal partial size is 7.3nm, specific surface area 167.8m2·g-1.There is quick, stable and Gao Xuan to alcohol vapour under the conditions of 25 DEG C
The response of selecting property, detection are limited to 75ppb.
The present invention adopts the following technical scheme that:
Specific step is as follows for the preparation method of six ytterbium boride alloy nano particles of the invention:
(1) in room temperature under argon gas (Ar) protective condition, by 0.558g ytterbium chloride (YbCl3) it is added to 20ml [BMIM] BF4
In, and be stirred continuously；
(2) diborane is then passed to, and reacts 45min in plasma field；
(3) sample obtained is washed with ultrapure water and dehydrated alcohol；It is finally that sample is dry at 60 DEG C, it remains standby
With；
The flow velocity of diborane in step (2) is 3mLmin-1；
Step (2) plasma field electric field strength size is 450Vcm-1。
The positive effect of the present invention is as follows:
1) pass through ytterbium chloride (YbCl in liqu id plasmas field3) and diborane (B2H6) reaction prepared shape
Irregular YbB6Alloy nano particle, average grain diameter 7.3nm, specific surface area 167.8m2·g-1；
2) there is quick, stable and highly selective response to alcohol vapour under the conditions of 25 DEG C, detection is limited to 75ppb；
3) present invention provides not only a kind of sensing material for capableing of efficient detection alcohol vapour at room temperature, while also mentioning
It has supplied a kind of catalysis ethanol dehydration to prepare the catalyst of ether at room temperature.
Detailed description of the invention
Fig. 1 is YbB prepared by embodiment 16XRD diagram of the alloy nano-material under different sintering temperatures.
Fig. 2 is YbB prepared by embodiment 16The TEM photo of alloy nano-material；Illustration is SAED picture in photo.
Fig. 3 is YbB prepared by embodiment 16The B1s xps energy spectrum figure of alloy nano-material.
Fig. 4 is YbB prepared by embodiment 16The Yb4p xps energy spectrum figure of alloy nano-material.
Fig. 5 is YbB prepared by embodiment 16Alloy nano-material is at room temperature to the response diagram of 200ppm gas with various.
Fig. 6 is YbB prepared by embodiment 16Alloy nano-material and other difference YbB6Nano material is to 200ppm ethyl alcohol
Response diagram.
Fig. 7 is YbB prepared by embodiment 16The response diagram of alloy nano-material 5-500ppm ethyl alcohol.
Fig. 8 is YbB prepared by embodiment 16Alloy nano-material 5-500ppm ethyl alcohol linear response relationship figure.
Fig. 9 is YbB prepared by embodiment 16Alloy nano-material to the alcohol gas of 200ppm respond 25 weeks it is long-term surely
Determine performance map.
Figure 10 is YbB prepared by embodiment 16The humidity influence diagram that alloy nano-material responds 200ppm alcohol gas.
Figure 11 is YbB prepared by embodiment 16Alloy nano-material and Yb and B different mol ratio YbBxAlloy nano-material pair
The detection performance figure of alcohol gas.
Figure 12 is YbB prepared by embodiment 16Alloy nano-material Yb4p In situ XPS energy during testing 200ppm ethyl alcohol
Spectrogram.
Figure 13 is YbB prepared by embodiment 16Alloy nano-material Yb4d XPS electronics knot during testing 200ppm ethyl alcohol
Closing can variation diagram.
Figure 14 is YbB prepared by embodiment 16The variation of alloy nano-material conductivity under 5-500ppm concentration of alcohol
Figure.
Figure 15 is YbB prepared by embodiment 16The catalysis response diagram of alloy nano-material ethanol dehydration ether.
Table 1 be response parameter (electric field strength, the ionic liquid scale of construction, reaction time and diborane flow velocity) to embodiment 1
The influence table of the composition of prepared nano material, specific surface area and average grain diameter.
Table 2 is different YbB6The contrast table of the specific surface area of alloy nano-material.
Table 3 is YbB prepared by embodiment 16Other sensing materials of alloy nano-material and recent report sense ethyl alcohol
The contrast table of performance.
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, the preparation step of specific six ytterbium borides alloy nano-material are as follows:
1) in room temperature under argon gas (Ar) protective condition, by 0.558g ytterbium chloride (YbCl3) it is added to 20mL [BMIM] BF4
In, and be stirred continuously；
2) diborane is then passed to, and reacts 45min in plasma field；
3) sample obtained is washed with ultrapure water and dehydrated alcohol；It is finally that sample is dry at 60 DEG C, it remains standby
With；
The flow velocity of diborane in step (2) is 3mLmin-1；
Step (2) plasma field electric field strength size is 450Vcm-1。
YbB of the invention6The performance of alloy nano-material:
At 25 DEG C, the XRD diagram of sample has a broad peak (Fig. 1) in 2 θ=30.5 °, shows YbB6Crystallinity is very poor or is
Non crystalline structure obtains crystalline material (JCPDS-25-1343, Fig. 1) after heat treated.Grain shape is irregular (Fig. 2), average ruler
Very little 7.3nm.Selective electron diffraction result (Fig. 2 illustration) also demonstrates the YbB of preparation6Amorphous structure.Measure sample in B and
The mass percent of Yb is respectively 27.27% and 72.73%, this and YbB6Calculated value it is consistent.The specific surface area of sample is
167.8m2·g-1.As shown in Figure 3 and Figure 4, can be seen that the valence state of Yb and B from Yb4d, Yb4p, B1s XPS spectrum figure is zero.Yb
Combination can (Yb4d3/2And Yb4d5/2) distinguish negative offset 1.3eV (187.7vs.190.0eV) and 0.9eV
(178.9vs.179.8eV).In addition, Yb4p1/2And Yb4p3/2Signal distinguish negative offset 1.9eV (398.9vs.397.0eV) and
1.1eV(344.4vs.345.4eV).The peak B1s shows the positive offset (187.7vs.187.1eV) of 0.6eV.Therefore, Yi Xie electricity
Son is transferred to Yb from B, forms Yb-B alloy.In other words, Yb is rich in electronics, this is previously with regards to amorphous metal boron compound
Report it is consistent.After crystallization, forward migration can occur for the combination of Yb4d and Yb4p, and negative offset can occur for the combination of B1s XPS.
Yb4d3/2、Yb4d5/2、Yb4p1/2、Yb4p3/2, combination of the B1s signal in 1123k can be respectively 189.5,180.4,400.1,
348.2 (349.7), 185.8eV, it is consistent with previous report.
In order to prepare YbB6Nanoparticle, plasma field must be adjusted to a suitable value, use in this experiment
It is 450Vcm-1.YbB in order to prevent6The oxidation of alloy, experiment need to carry out under Ar atmosphere.YbB6The shape of alloy nano particle
At can be indicated with equation (1):
2YbCl3+2B2H6+ plasma → 2YbB6+6HCl+3H2 (1)
Prepare that size is small, YbB of large specific surface area6The optimum synthesis condition (table 1) of nanoparticle is as follows: the reaction time is
45min；Electric field is 450Vcm-1；[BMIM]BF4Amount be 20mL；The charge velocity of diborane is 3mLmin-1。
By measurement capacity (C) variation, amorphous state YbB is had studied6The sensing capabilities of alloy nanoparticle in the sensor.
The device has response to 100ppm ethyl alcohol, but to hydrogen sulfide, methanol, isopropanol, formaldehyde, methane, nitrogen dioxide, 92# gasoline, first
Benzene, acetone, ammonia, hydrogen and carbon monoxide do not respond to (Fig. 5), and ethyl alcohol/methanol response ratio is 9.8.Therefore, our material can
To carry out selective sensing to ethyl alcohol.YbB of the ethyl alcohol sensing capabilities better than other sintering in our work6Sample and commercialization
YbB6Sample (Fig. 6), this is because biggish specific surface area (Tables 1 and 2) helps to increase ethanol molecule and YbB6Surface
Contact.In addition, our sample shows linear response (Fig. 7 and Fig. 8) to alcohol vapour between 5-500ppm, detection is limited to
75ppb。
Sample is respectively less than 30s (Fig. 7) to response/recovery time of 5-500ppm alcohol vapour, and slightly below ZnO nanorod exists
Response/recovery time of 6s/31s at 300 DEG C and ZnO/SnO2To the 2s/38s of 100ppm alcohol vapour at 275 DEG C
Response/recovery time.But our sensor performance at low temperature with Ag/SWCNT (at 25 DEG C to 200ppm ethyl alcohol steam
The sensing capabilities of vapour are 116s/38s), Ag/Zn/LaFeO3It (is 100s/ to the sensing capabilities of 100ppm ethyl alcohol at 55 DEG C
20s)、TiO2(being 50s/1s to the sensing capabilities of ethyl alcohol at 25 DEG C) suitable (table 3).
In addition, the YbB of preparation6Alloy keeps stable sensing capabilities to 200ppm alcohol vapour in 25 weeks at 25 DEG C
(Fig. 9).Relative humidity (RH) does not find that humidity has a significant impact (Figure 10) to sample detection performance within the scope of 10%-90%.
In addition, influence of the B/Yb ratio to sample detection performance between 5.6~6.5 be not significant.However, and YbB6It compares, business
The YbB of change2And YbB12Sample is poor to the response of alcohol vapour (Figure 11).
In general, material depends on the oxygen of absorption on the surface of the material to ethanol molecule to the selective sensing capability of ethyl alcohol
Oxidation, change so as to cause the conductivity of material.We using isotope labelling ethyl alcohol (13C2H5 16O2H) it is
Incude gas, after then testing and analyzing to the discharge gas after it has incuded, discovery exists2H2 16O and (13C2H5)2 16O, but
It is not detected13C16O2、2H2O、13CO2、13C2H4 16O and2H2.This result shows that, the YbB prepared by us6Alloy is to ethyl alcohol
Selective sensing effect is that ether progress is formed by the intermolecular dehydration of ethyl alcohol, as shown in equation (2):
2CH3CH2OH→(C2H5)2O+H2O (2)
It can (BE) displacement in addition, the combination of Yb in the sample has also been observed dduring test；But there is no form Yb
Oxide (Figure 12 and Figure 13).In addition, Yb2O3, B and B2O3Alcohol vapour is not responded to.Therefore, in the YbB of preparation6Alloy
In nano particle, the Yb of electron rich is the active site of alcohol vapor detection.Obviously, YbB6The 6s track and C of middle Yb2H5O in OH
2p orbital hybridization promote its absorption to alcohol vapor, electronics is from YbB6In rich in electronics Yb be transferred to ethyl alcohol O (figure
12 and Figure 13).To make YbB6The electric conductivity of alloy enhances (Figure 14), this is attributed to the increase of its surface voids concentration.YbB6Table
The ethyl alcohol of face absorption, which further reacts, generates ether and water:
2CH3CH2OH (absorption) → (CH3CH2)2O (gas)+H2O (gas) (3)
Control experiment confirms YbB6Alloy has the catalytic activity (Figure 15) to ethanol dehydration ether in air.This
It is YbB6The reason more preferable to the response ratio of alcohol vapour other gases.
Amorphous state YbB has been prepared under liqu id plasmas auxiliary for the first time6Alloy nano particle.The material is at room temperature
There are quick, stable and highly selective sensing characteristics to alcohol vapor, detection is limited to 75ppb.The material has alcohol vapor
There is good detection performance, is mainly due to its alloy property and and its catalytic dehydration to ethyl alcohol.The present invention not only mentions
A kind of sensing material for capableing of efficient detection alcohol vapour at room temperature has been supplied, while having also provided and a kind of can be catalyzed at room temperature
Ethanol dehydration prepares the catalyst of ether.
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 (3)
1. a kind of preparation method of six ytterbium boride alloy nano particles, it is characterised in that:
Specific step is as follows for made Preparation Method:
1) under room temperature, argon gas (Ar) atmosphere protection, by 0.558g ytterbium chloride (YbCl3) it is added to 20ml [BMIM] BF4In；
2) diborane is then passed to, and reacts 45min in plasma field；
3) sample obtained is washed with ultrapure water and dehydrated alcohol；It is finally that sample is dry at 60 DEG C, it remains spare.
2. the preparation method of six ytterbium borides alloy nano particle as described in claim 1, it is characterised in that: in step (2)
The flow velocity of diborane is 3mLmin-1。
3. the preparation method of six ytterbium borides alloy nano particle as described in claim 1, it is characterised in that: step (2) is medium
Gas ions field electric field strength size is 450Vcm-1。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589846A (en) * | 2019-10-23 | 2019-12-20 | 成都理工大学 | Preparation method of ytterbium hexaboride nanorod crystal |
| 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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Application publication date: 20190806 |