CN106124594B - A kind of preparation method based on lanthanum molybdate nano material air-sensitive testing element - Google Patents
A kind of preparation method based on lanthanum molybdate nano material air-sensitive testing element Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods based on lanthanum molybdate nano material air-sensitive testing element, the preparation method based on lanthanum molybdate nano material air-sensitive testing element weighs a certain amount of La (NO using lanthanum nitrate and ammonium molybdate as raw material, according to LMO stoicheiometries3)3(NH4)6Mo7O24, using distilled water as solvent, citric acid is added in, the molar ratio of citric acid and metal cation is 2:1‑1:1；Lanthanum molybdate nano material is prepared for, and based on this material preparation air-sensitive testing element using Microwave Assisted Process.The present invention is by optimizing LMO synthesis technologies, so that LMO materials have nanoscale, and have many advantages, such as that material morphology is uniform, reproducible, chemism is high, it has excellent air-sensitive response characteristic in medium temperature temperature section, 260 DEG C of sensitivity to 200ppm alcohol gas has good response recovery capability up to 31.
Description
Technical field
The invention belongs to electronic functional material technical fields more particularly to a kind of lanthanum molybdate nano material air-sensitive that is based on to test
The preparation method of element.
Background technology
Lacorre etc. reports a kind of novel oxygen ion conductor material lanthanum molybdate La2Mo2O9(LMO), in 800 DEG C of oxygen
Ionic conductivity has reached 0.06S cm-1More than, " P.Lacorre, F.Goutenoire, O.Bohnke, R.Retoux,
NATURE, 2000,404,856 ".Pass through O18Isotope measures pure and doping LMO samples
(0.5~3) × 10-6cm2s-1, high oxygen ionic conductivity and high oxonium ion diffusion coefficient are corresponding, higher than traditional oxygen
Change zirconium oxide (YSZ) and the doped lanthanum gallate material that yttrium is stablized.Since preparation process is simple and the prices of raw materials are cheap, make molybdenum
Sour lanthanum has larger competitive advantage as the electrolyte of intermediate temperature SOFC and the candidate material of electrode.In addition to fuel cell and oxygen pass
Except sensor, oxygen ion conductor can also be used as active catalyst material.In this case, gas reaction mixture (such as C2H4With
O2) in catalytic electrode surfaces.In view of being an oxygen-ion conductive material, increase a catalysis electrode and the gesture to electrode
The migration of oxygen can be induced by building (± 2V), and oxygen is supplied or remove in real time in interface in the experiment of catalysis.It is surprising
Be that this " oxygen pump " may operate in a very wide temperature range (220-550 DEG C), cause to show very much in catalytic process
The faradic currents modification (this variation and current value are disproportionate) without reversion write, in the selective intermediate frequency of product
It is numerous along with important variation, and with very high sensitivity, " P.Vernoux, L.Lizarraga, M.N.Tsampas,
F.M.Sapountzi, A.De Lucas-Consuegra, J.L.Valverde, S.Souentie, C.G.Vayenas,
D.Tsiplakides, S.Balomenou, E.A.Baranova, CHEM.REV., 2013,113,8192 ".In addition, for not mixing
Miscellaneous lanthanum molybdate material, interface impedance have very sensitive variation under different atmosphere, minor change present in lanthanum molybdate
Stoicheiometry lead to the acute variation of conductivity, therefore applied in terms of sensor there is larger advantage.But lanthanum molybdate
As gas sensing application, not yet have been reported that at present.
Both at home and abroad using solid sintering technology, sol-gal process, freeze-drying, Via Polymeric Precursor Method, hydro-thermal method, original position
A variety of methods such as polymerization are prepared for different-shape and the lanthanum molybdate material of size, achieve certain development of scientific research, but deposit
Pattern is inhomogenous, stability is poor, synthesis technology is complicated, the period is long, high expensive the shortcomings of.And for gas sensing material and
Speech, Semiconductor gas sensors material is short there are service life, and stability is poor, prepares the shortcomings of stringent, and conventional ion conductor base YSZ materials
Material needs higher temperature in use, and activity is relatively low.
Invention content
The technical problem to be solved in the present invention provides a kind of in nano level more to overcome shortcoming of the prior art
The preparation method of brilliant lanthanum molybdate material.Another technical problem is to provide a kind of air-sensitive testing element based on lanthanum molybdate nano material
Preparation method.Relative to traditional gas sensing material, which has good cycling stability, long lifespan, is suitble to high temperature
Using and with wide use temperature range.
The invention is realized in this way a kind of preparation method based on lanthanum molybdate nano material air-sensitive testing element, described
Preparation method based on lanthanum molybdate nano material air-sensitive testing element is matched using lanthanum nitrate and ammonium molybdate as raw material according to LMO chemistry
Than the La (NO for weighing corresponding amount3)3(NH4)6Mo7O24, using distilled water as solvent, add in citric acid, citric acid and metal sun from
The molar ratio of son is 2:1-1:1；It is prepared using Microwave Assisted Process based on lanthanum molybdate nano material air-sensitive testing element.
Further, the preparation method based on lanthanum molybdate nano material air-sensitive testing element includes the following steps：
Step 1 weighs 0.866g La (NO according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And it is dissolved in
In 20mL deionized waters；
The molar ratio of step 2, addition citric acid, citric acid and metal cation is 2:1-1:1, it is stirred 1h shapes
Into uniform solution；
Step 3 is poured into the jar of PTEE sealings, in 140 DEG C of -160 DEG C of progress microwave heating 50-60min, is taken out
Room temperature is naturally cooled to, is centrifuged out the sediment of brown；
Then step 4 rinses for several times sediment in deionized water and in absolute alcohol, then be dried at 80 DEG C,
Obtain prefabricated powder；
Step 5 calcines 2h at 550-700 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis
Body；
Step 6 adds in the nano-powder of preparation in agate mortar, instills a little terpinol after grinding uniformly, is tuned into paste
The ceramic tube coated is placed on after being dried under infrared lamp, to aluminium oxide ceramics tube outside 600 in Muffle furnace by even application after shape
DEG C calcining 2h, it is spare after binder natural cooling used in material to remove；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, then by Ni- by step 7
Cr heater strips pass through from ceramic tube and its both ends are also welded on pedestal, and gas sensor is made, by the element welded 300
DEG C aging 10 days.
Further, the preparation method based on lanthanum molybdate nano material air-sensitive testing element includes the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And be dissolved in 20mL go from
In sub- water；
The molar ratio of addition citric acid, citric acid and metal cation is 2:1；Be stirred 1h formed it is uniform molten
Liquid；
It pours into and carries out microwave heating 50min in the jar of PTEE sealings at 160 DEG C, taking-up naturally cools to room temperature, centrifuges
The out sediment of brown；
Sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtains prefabricated powder；
2h is calcined at 700 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis；
Prepared nano-powder is added in agate mortar, a little terpinol is instilled after grinding uniformly, after being tuned into paste
The ceramic tube coated is placed on after being dried under infrared lamp, is forged for 600 DEG C in Muffle furnace to aluminium oxide ceramics tube outside by even application
2h is burnt, it is spare after binder natural cooling used in material to remove；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, are then heated Ni-Cr
Silk passes through from ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings
10 days.
Further, the preparation method based on lanthanum molybdate nano material air-sensitive testing element includes the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And be dissolved in 20mL go from
In sub- water；
The molar ratio of addition citric acid, citric acid and metal cation is 1.5:1；Be stirred 1h formed it is uniform molten
Liquid；
It pours into and carries out microwave heating 50min in the jar of PTEE sealings at 160 DEG C, taking-up naturally cools to room temperature, centrifuges
The out sediment of brown；
Sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtains prefabricated powder；
2h is calcined at 700 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis；It is ground in agate
The nano-powder of preparation is added in alms bowl, a little terpinol is instilled after grinding uniformly, even application is made pottery to aluminium oxide after being tuned into paste
Outside porcelain tube, the ceramic tube coated is placed on after being dried under infrared lamp, 600 DEG C of calcining 2h in Muffle furnace, to remove in material
It is spare after binder natural cooling used；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, are then heated Ni-Cr
Silk passes through from ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings
10 days.
Further, the preparation method based on lanthanum molybdate nano material air-sensitive testing element includes the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And be dissolved in 20mL go from
In sub- water；
The molar ratio of addition citric acid, citric acid and metal cation is 2:1；Be stirred 1h formed it is uniform molten
Liquid；
It pours into and carries out microwave heating 50min in the jar of PTEE sealings at 160 DEG C, taking-up naturally cools to room temperature, centrifuges
The out sediment of brown；
Then sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtained pre-
Powder processed；
The white lanthanum molybdate nano powder of Microwave-assisted synthesis can be obtained by calcining 2h at 600 DEG C to prefabricated powder；In agate
It adds in the nano-powder of preparation in Nao mortars, a little terpinol is instilled after grinding uniformly, be tuned into after paste even application to aoxidizing
Outside aluminium ceramic tube, the ceramic tube coated is placed on after being dried under infrared lamp, 600 DEG C of calcining 2h in Muffle furnace, to remove de-material
It is spare after binder natural cooling used in material；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, are then heated Ni-Cr
Silk passes through from ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings
10 days.
Further, the preparation method based on lanthanum molybdate nano material air-sensitive testing element includes the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And be dissolved in 20mL go from
In sub- water；
Citric acid is added in, citric acid and cationic molar ratio are 2:1；It is stirred 1h and forms uniform solution；
It pours into the jar of PTEE sealings and carries out microwave heating 50min at 160 DEG C, then take out to naturally cool to room
Temperature is centrifuged out the sediment of brown；
Sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtains prefabricated powder；
2h is calcined at 550 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis；
The nano-powder of preparation is added in agate mortar, a little binder is instilled after grinding uniformly, is tuned into after paste
It is even to be coated to aluminium oxide ceramics tube outside, the ceramic tube coated is placed on after being dried under infrared lamp, 600 DEG C of calcinings in Muffle furnace
2h, it is spare after binder natural cooling used in material to remove；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, are then heated Ni-Cr
Silk passes through from ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings
10 days.
Preparation method provided by the invention based on lanthanum molybdate nano material air-sensitive testing element, the present invention provides one kind
It prepares the MATERIALS METHODS of nanometer lanthanum molybdate and has manufactured experimently air-sensitive testing element, material preparation method reaction heating is rapid, the period is short,
It is easy to operate, yield is high.By optimizing LMO synthesis technologies so that LMO materials have nanoscale, while have material morphology
The advantages that uniform, reproducible, chemism is high.Air-sensitive testing element based on the material preparation has excellent in medium temperature temperature section
Different air-sensitive response characteristic, 260 DEG C of sensitivity to 200ppm alcohol gas have good response recovery capability up to 31,
It is studied in terms of sensor for this novel oxygen ion conductor and provides new approaches and frontier.
Description of the drawings
Fig. 1 is the preparation method flow provided in an embodiment of the present invention based on lanthanum molybdate nano material air-sensitive testing element
Figure.
Fig. 2 is the LMO nano-powders that the prefabricated powder of Microwave-assisted synthesis provided in an embodiment of the present invention calcines 2h at 700 DEG C
Scanning electron microscopy (SEM) and corresponding power spectrum (EDS).
Fig. 3 is the LMO nano-powders that the prefabricated powder of Microwave-assisted synthesis provided in an embodiment of the present invention calcines 2h at 700 DEG C
X-ray diffraction spectrum (XRD).
Fig. 4 is response recovery curve and sensitivity schematic diagram provided in an embodiment of the present invention；
In figure：(a) 260 DEG C when, nanometer LMO micro-structures sensing element restores bent in the response of different ethanol gas concentrations
Line；(b) LMO gas-sensitive element structures and schematic diagram；(c) 260 DEG C when, nanometer LMO micro-structures sensing element is in different alcohol gas
Sensitivity under concentration.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The present invention prepares the nanometer lanthanum molybdate material with certain dispersibility using Microwave Assisted Process, is received for lanthanum molybdate
The efficient controlledly synthesis of rice material and medium temperature temperature section air-sensitive performance provide necessary theoretical foundation and practical experience.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
As shown in Figure 1, the preparation method based on lanthanum molybdate nano material air-sensitive testing element of the embodiment of the present invention includes
Following steps：
S101：A certain amount of La (NO are weighed according to LMO stoicheiometries3)3(NH4)6Mo7O24And be dissolved in 20mL go from
In sub- water；
S102：A certain amount of citric acid is added in, citric acid and cationic molar ratio are 2:1-1:1.It is stirred one
It fixes time to form uniform solution；
S103：It pours into the jar of PTEE sealings in 140 DEG C of -160 DEG C of progress microwave heating 50-60min, then takes out and
Room temperature is naturally cooled to, is centrifuged out the sediment of brown；
S104：Then sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtained
To prefabricated powder；
S105：The white lanthanum molybdate nano of Microwave-assisted synthesis can be obtained by calcining 2h at 550-700 DEG C to prefabricated powder
Powder；
S106：A small amount of nano-powder is added in agate mortar, a little binder (terpinol) is instilled after grinding uniformly, adjusts
The ceramic tube coated is placed on after being dried under infrared lamp, to aluminium oxide ceramics tube outside in Muffle furnace by even application after into paste
In 600 DEG C of calcining 2h, it is spare after binder natural cooling used in material to remove；
S107：4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, then by Ni-Cr
Heater strip passes through from ceramic tube and its both ends is also welded on pedestal, and gas sensor is made, by the element welded at 300 DEG C
Aging 10 days.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1 weighs the La (NO of corresponding amount according to LMO stoicheiometries3)3(NH4)6Mo7O24And it is dissolved in 20mL and goes
In ionized water.Add in a certain amount of citric acid, the molar ratio of citric acid and metal cation is 2:1.It is stirred a timing
Between form uniform solution；It pours into the jar of PTEE sealings and carries out microwave heating 50min at 160 DEG C, then take out and carry out nature
Room temperature is cooled to, is centrifuged out the sediment of brown；Then sediment is rinsed for several times in deionized water and in absolute alcohol, then
It is dried at 80 DEG C, obtains prefabricated powder；The white of Microwave-assisted synthesis can be obtained by calcining 2h at 700 DEG C to prefabricated powder
Lanthanum molybdate nano powder；A small amount of nano-powder is added in agate mortar, a little binder (terpinol) is instilled after grinding uniformly,
The ceramic tube coated is placed on after being dried under infrared lamp, to aluminium oxide ceramics tube outside in Muffle by even application after being tuned into paste
600 DEG C of calcining 2h in stove, it is spare after binder natural cooling used in material to remove；LMO base nano-powders will be coated with
4 Pt wire electrodes of ceramic tube are welded on pedestal, and then Ni-Cr heater strips are passed through from ceramic tube and also weld at its both ends
It is connected on pedestal, gas sensor is made.In order to improve the stability of element and repeatability, by the element welded in 300 DEG C of agings
10 days.LMO nano-powders scanning electron microscopy that be the prefabricated powder of Microwave-assisted synthesis in Fig. 2 calcine 2h at 700 DEG C and right
It should be able to compose.Fig. 3 is its XRD spectrum.It can be seen from the figure that prepared material is LMO pure phases, and with certain dispersibility and
Uniform nanostructured composition.Response recovery curve of the air-sensitive testing element based on the making of such material under different ethanol concentration
With sensitivity as shown in figure 4, it can be seen from the figure that at 260 DEG C, to the sensitivity of 200ppm alcohol gas up to 31, and have
There is preferable response recovery capability.Fig. 4 (b) is structural representation and the schematic diagram of its gas sensor.
Embodiment 2 weighs the La (NO of corresponding amount according to LMO stoicheiometries3)3(NH4)6Mo7O24And it is dissolved in 20mL and goes
In ionized water.Add in a certain amount of citric acid, the molar ratio of citric acid and metal cation is 1.5:1.It is stirred certain
Time forms uniform solution；It pours into the jar of PTEE sealings and carries out microwave heating 50min at 160 DEG C, then take out and come from
Room temperature so is cooled to, is centrifuged out the sediment of brown；Then sediment is rinsed for several times in deionized water and in absolute alcohol,
It is dried at 80 DEG C again, obtains prefabricated powder；The white of Microwave-assisted synthesis can be obtained by calcining 2h at 700 DEG C to prefabricated powder
Color lanthanum molybdate nano powder；A small amount of nano-powder is added in agate mortar, a little terpinol is instilled after grinding uniformly, is tuned into paste
The ceramic tube coated is placed on after being dried under infrared lamp, to aluminium oxide ceramics tube outside 600 in Muffle furnace by even application after shape
DEG C calcining 2h, it is spare after binder natural cooling used in material to remove；The ceramic tube of LMO base nano-powders will be coated with
4 Pt wire electrodes are welded on pedestal, and then Ni-Cr heater strips are passed through from ceramic tube and its both ends is also welded to pedestal
On, gas sensor is made.In order to improve the stability of element and repeatability, by the element welded in 300 DEG C of agings 10 days.
Embodiment 3 weighs the La (NO of corresponding amount according to LMO stoicheiometries3)3(NH4)6Mo7O24And it is dissolved in 20mL and goes
In ionized water.Add in a certain amount of citric acid, the molar ratio of citric acid and metal cation is 2:1.It is stirred a timing
Between form uniform solution；It pours into the jar of PTEE sealings and carries out microwave heating 50min at 160 DEG C, then take out and carry out nature
Room temperature is cooled to, is centrifuged out the sediment of brown；Then sediment is rinsed for several times in deionized water and in absolute alcohol, then
It is dried at 80 DEG C, obtains prefabricated powder；The white of Microwave-assisted synthesis can be obtained by calcining 2h at 600 DEG C to prefabricated powder
Lanthanum molybdate nano powder；A small amount of nano-powder is added in agate mortar, a little terpinol is instilled after grinding uniformly, is tuned into paste
The ceramic tube coated is placed on after being dried under infrared lamp, to aluminium oxide ceramics tube outside 600 DEG C in Muffle furnace by even application afterwards
2h is calcined, it is spare after binder natural cooling used in material to remove；The 4 of the ceramic tube of LMO base nano-powders will be coated with
A Pt wire electrodes are welded on pedestal, and then Ni-Cr heater strips are passed through from ceramic tube and its both ends is also welded to pedestal
On, gas sensor is made.In order to improve the stability of element and repeatability, by the element welded in 300 DEG C of agings 10 days.
Embodiment 4 weighs the La (NO of corresponding amount according to LMO stoicheiometries3)3(NH4)6Mo7O24And it is dissolved in 20mL and goes
In ionized water.Add in a certain amount of citric acid, the molar ratio of citric acid and metal cation is 2:1.It is stirred a timing
Between form uniform solution；It pours into the jar of PTEE sealings and carries out microwave heating 50min at 160 DEG C, then take out and carry out nature
Room temperature is cooled to, is centrifuged out the sediment of brown；Then sediment is rinsed for several times in deionized water and in absolute alcohol, then
It is dried at 80 DEG C, obtains prefabricated powder；The white of Microwave-assisted synthesis can be obtained by calcining 2h at 550 DEG C to prefabricated powder
Lanthanum molybdate nano powder；A small amount of nano-powder is added in agate mortar, a little binder (terpinol) is instilled after grinding uniformly,
The ceramic tube coated is placed on after being dried under infrared lamp, to aluminium oxide ceramics tube outside in Muffle by even application after being tuned into paste
600 DEG C of calcining 2h in stove, it is spare after binder natural cooling used in material to remove；LMO base nano-powders will be coated with
4 Pt wire electrodes of ceramic tube are welded on pedestal, and then Ni-Cr heater strips are passed through from ceramic tube and also weld at its both ends
It is connected on pedestal, gas sensor is made.In order to improve the stability of element and repeatability, by the element welded in 300 DEG C of agings
10 days.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of preparation method based on lanthanum molybdate nano material air-sensitive testing element, which is characterized in that described to be based on lanthanum molybdate
The preparation method of nano material air-sensitive testing element weighs certain using lanthanum nitrate and ammonium molybdate as raw material according to LMO stoicheiometries
La (the NO of amount3)3(NH4)6Mo7O24, using distilled water as solvent, add in the molar ratio of citric acid, citric acid and metal cation
Example is 2:1-1:1；It is prepared using Microwave Assisted Process based on lanthanum molybdate nano material air-sensitive testing element；
The preparation method based on lanthanum molybdate nano material air-sensitive testing element includes the following steps：
Step 1 weighs 0.866g La (NO according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And it is dissolved in 20mL and goes
In ionized water；
The molar ratio of step 2, addition citric acid, citric acid and metal cation is 2:1-1:1, it is stirred 1h and is formed
One solution；
Step 3 is poured into the jar of PTEE sealings, in 140 DEG C of -160 DEG C of progress microwave heating 50-60min, takes out nature
Room temperature is cooled to, is centrifuged out the sediment of brown；
Then step 4 rinses for several times sediment in deionized water and in absolute alcohol, then be dried at 80 DEG C, obtains
Prefabricated powder；
Step 5 calcines 2h at 550-700 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis；
Step 6 adds in the nano-powder of preparation in agate mortar, a little terpinol is instilled after grinding uniformly, after being tuned into paste
The ceramic tube coated is placed on after being dried under infrared lamp, is forged for 600 DEG C in Muffle furnace to aluminium oxide ceramics tube outside by even application
2h is burnt, it is spare after binder natural cooling used in material to remove；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, then add Ni-Cr by step 7
Heated filament passes through from ceramic tube and its both ends is also welded on pedestal, and gas sensor is made, and the element welded is old at 300 DEG C
Change 10 days.
2. the preparation method as described in claim 1 based on lanthanum molybdate nano material air-sensitive testing element, which is characterized in that institute
The preparation method based on lanthanum molybdate nano material air-sensitive testing element is stated to include the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And it is dissolved in 20mL deionized waters
In；
The molar ratio of addition citric acid, citric acid and metal cation is 2:1；It is stirred 1h and forms uniform solution；
It pours into and carries out microwave heating 50min in the jar of PTEE sealings at 160 DEG C, taking-up naturally cools to room temperature, is centrifuged out
The sediment of brown；
Sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtains prefabricated powder；
2h is calcined at 700 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis；
Prepared nano-powder is added in agate mortar, a little terpinol is instilled after grinding uniformly, is tuned into after paste uniformly
Aluminium oxide ceramics tube outside is coated to, the ceramic tube coated is placed on after being dried under infrared lamp, 600 DEG C of calcinings in Muffle furnace
2h, it is spare after binder natural cooling used in material to remove；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, then by Ni-Cr heater strips from
It is passed through in ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings 10
My god.
3. the preparation method as described in claim 1 based on lanthanum molybdate nano material air-sensitive testing element, which is characterized in that institute
The preparation method based on lanthanum molybdate nano material air-sensitive testing element is stated to include the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And it is dissolved in 20mL deionized waters
In；
The molar ratio of addition citric acid, citric acid and metal cation is 1.5:1；It is stirred 1h and forms uniform solution；
It pours into and carries out microwave heating 50min in the jar of PTEE sealings at 160 DEG C, taking-up naturally cools to room temperature, is centrifuged out
The sediment of brown；
Sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtains prefabricated powder；
2h is calcined at 700 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis；In agate mortar
The nano-powder prepared is added in, a little terpinol is instilled after grinding uniformly, is tuned into after paste even application to alumina ceramic tube
The ceramic tube coated is placed on after being dried under infrared lamp by outside, 600 DEG C of calcining 2h in Muffle furnace, used in material to remove
Binder natural cooling after it is spare；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, then by Ni-Cr heater strips from
It is passed through in ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings 10
My god.
4. the preparation method as described in claim 1 based on lanthanum molybdate nano material air-sensitive testing element, which is characterized in that institute
The preparation method based on lanthanum molybdate nano material air-sensitive testing element is stated to include the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And it is dissolved in 20mL deionized waters
In；
The molar ratio of addition citric acid, citric acid and metal cation is 2:1；It is stirred 1h and forms uniform solution；
It pours into and carries out microwave heating 50min in the jar of PTEE sealings at 160 DEG C, taking-up naturally cools to room temperature, is centrifuged out
The sediment of brown；
Then sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtain prefabricated powder；
The white lanthanum molybdate nano powder of Microwave-assisted synthesis can be obtained by calcining 2h at 600 DEG C to prefabricated powder；It is ground in agate
The nano-powder of preparation is added in alms bowl, a little terpinol is instilled after grinding uniformly, even application is made pottery to aluminium oxide after being tuned into paste
Outside porcelain tube, the ceramic tube coated is placed on after being dried under infrared lamp, 600 DEG C of calcining 2h in Muffle furnace, to remove in material
It is spare after binder natural cooling used；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, then by Ni-Cr heater strips from
It is passed through in ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings 10
My god.
5. the preparation method as described in claim 1 based on lanthanum molybdate nano material air-sensitive testing element, which is characterized in that institute
The preparation method based on lanthanum molybdate nano material air-sensitive testing element is stated to include the following steps：
0.866g La (NO are weighed according to LMO stoicheiometries3)3With 0.332g (NH4)6Mo7O24And it is dissolved in 20mL deionized waters
In；
Citric acid is added in, citric acid and cationic molar ratio are 2:1；It is stirred 1h and forms uniform solution；
It pours into the jar of PTEE sealings and carries out microwave heating 50min at 160 DEG C, then take out to naturally cool to room temperature, from
The heart comes out the sediment of brown；
Sediment in deionized water and in absolute alcohol is rinsed for several times, then is dried at 80 DEG C, obtains prefabricated powder；
2h is calcined at 550 DEG C to prefabricated powder and obtains the white lanthanum molybdate nano powder of Microwave-assisted synthesis；
The nano-powder of preparation is added in agate mortar, a little binder is instilled after grinding uniformly, is uniformly applied after being tuned into paste
Aluminium oxide ceramics tube outside is applied to, the ceramic tube coated is placed on after being dried under infrared lamp, 600 DEG C of calcining 2h in Muffle furnace,
It is spare after binder natural cooling used in material to remove；
4 Pt wire electrodes of the ceramic tube for being coated with LMO base nano-powders are welded on pedestal, then by Ni-Cr heater strips from
It is passed through in ceramic tube and its both ends is also welded on pedestal, gas sensor is made, by the element welded in 300 DEG C of agings 10
My god.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101363134A (en) * | 2007-08-07 | 2009-02-11 | 中国科学院合肥物质科学研究院 | Lanthanum molybdate base porous membrane material and preparation method thereof |
| CN102079655A (en) * | 2011-02-24 | 2011-06-01 | 西北工业大学 | Preparation method of strontium-doped lanthanum molybdate ceramic |
| CN102502843A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing lanthanum molybdate nanotube material by microwave radiation method |
| CN104819999A (en) * | 2015-05-05 | 2015-08-05 | 太原理工大学 | Preparation method of ethanol gas sensor component having ultrafast response recovery property |
-
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- 2016-06-12 CN CN201610408714.5A patent/CN106124594B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101363134A (en) * | 2007-08-07 | 2009-02-11 | 中国科学院合肥物质科学研究院 | Lanthanum molybdate base porous membrane material and preparation method thereof |
| CN102079655A (en) * | 2011-02-24 | 2011-06-01 | 西北工业大学 | Preparation method of strontium-doped lanthanum molybdate ceramic |
| CN102502843A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing lanthanum molybdate nanotube material by microwave radiation method |
| CN104819999A (en) * | 2015-05-05 | 2015-08-05 | 太原理工大学 | Preparation method of ethanol gas sensor component having ultrafast response recovery property |
Non-Patent Citations (2)
| Title |
|---|
| Microwave-assisted combustion synthesis of nanocrystalline La2Mo2O9 oxide-ion conductor and its characterization;T.Saradha S 等;《JOURNAL OF SOLID STATE ELECTROCHEMISTRY》;20070707;第12卷(第2期);全文 * |
| Monoclinic Distortion Shrinkage and Enhanced Properties of La2Mo2O9 Oxide Ion Conductors Synthesized by an Isobaric-Microwave Assisted Method;Xiao Liu 等;《ECS SOLID STATE LETTERS》;20130605;第2卷(第9期);第N27页 * |
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