CN106596651A - Molybdenum disulfide/magnesium hydroxide nano composite material as well as preparation method and application thereof - Google Patents
Molybdenum disulfide/magnesium hydroxide nano composite material as well as preparation method and application thereof Download PDFInfo
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- CN106596651A CN106596651A CN201611103265.XA CN201611103265A CN106596651A CN 106596651 A CN106596651 A CN 106596651A CN 201611103265 A CN201611103265 A CN 201611103265A CN 106596651 A CN106596651 A CN 106596651A
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- molybdenum bisuphide
- nanoparticle composite
- molybdenum
- hydroxide nanoparticle
- molybdenum disulfide
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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
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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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
Abstract
The invention discloses a molybdenum disulfide/magnesium hydroxide nano composite material as well as a preparation method and application thereof, relates to a molybdenum disulfide/magnesium hydroxide material as well as preparation and application thereof, and aims to solve the problems of low sensitivity and low response speed of a conventional oxynitride detection sensitive material at a room temperature. The composite material is prepared from molybdenum disulfide, magnesium nitrate, a surfactant and thiourea. The method comprises the following steps: weighing ammonium molybdate, thiourea and polyethylene glycol, and carrying out hydrothermal reaction to obtain a molybdenum disulfide coarse product; washing and drying the molybdenum disulfide coarse product; grinding the molybdenum disulfide coarse product into powder; carrying out hydrothermal reaction to prepare a coarse product; washing and drying the coarse product to obtain the molybdenum disulfide/magnesium hydroxide nano composite material. The molybdenum disulfide/magnesium hydroxide nano composite material is applied to the preparation of a gas sensitive element for detecting NOx. The composite material has a quick sensitive membrane response and a quick recovery response, and is relatively high in selectivity for oxynitride gas, and the method is simple in process. The preparation method is applicable to preparation and application of the molybdenum disulfide/magnesium hydroxide nano composite material.
Description
Technical field
The present invention relates to a kind of molybdenum bisuphide/hydroxide nanoparticle composite and its preparation method and application.
Background technology
With NO and NO2Based on NOx(nitrogen oxides) are the major reasons to form photochemical fog and acid rain.Automobile
NO in tail gasxThe react toxic smog to be formed, referred to as photochemical fog are irradiated with Hydrocarbon Jing ultraviolet, it is photochemical
Learn smog and there is special odor, stimulate eyes, injure plant, and reduce atmospheric visibility；In addition, NOxIn air
Nitric acid and nitrous acid that water reaction is generated are the compositions of acid rain；NO in airxIt is mostly derived from burning and the plant of Fossil fuel
The conversion of nitrogen-containing compound in the burning of body, and agricultural land soil and animal excrements.Therefore, research and development are to NOxIt is high sensitivity, fast
The gas sensor of speed response is of great significance to daily life and commercial production tool.
Molybdenum bisuphide as new nano material, in catalyst, kollag, lithium battery, hydrogen storage, liberation of hydrogen, sensing
The aspects such as device, photoelectricity have huge application prospect, are widely studied by people.In molybdenum bisuphide structure, each molybdenum is former
There are six sulphur atom parcels around sub, represent triangular prism column, especially many Mo-S faceted pebbles are exposed, due to Mo-S faceted pebbles ratio
Surface area is big, and surface activity is very high, so have very high apparent activation energy, therefore, molybdenum bisuphide/hydroxide nanoparticle is combined
Material will more be of practical significance in fields such as gas sensing techniques.There is document report MoS2/ Graphene mixing aeroge is examined
Survey NO2, the sensor is to NO2The testing result of gas is displayed in more sensitive, MoS when operating temperature is 200 DEG C2/ Graphene is mixed
Close aeroge senor operating temperature higher, cannot detect at room temperature, be unfavorable for practical application.And MoS2/ Graphene is mixed
Closing aeroge needs in 450 DEG C of calcinings, and sensor preparation temperature is high, is unfavorable for industrialized production.Document report ZnO modifications
MoS2Nanosheet composite material detects ethanol, and the sensor is displayed in operating temperature to the testing result of alcohol gas for 240 DEG C
When it is more sensitive, but ZnO modification MoS2Nanosheet composite material senor operating temperature is higher, cannot detect at room temperature, also
It is unfavorable for practical application.SnO2Modification molybdenum disulfide nano sheet composite detection NO2, detect 0.5ppm NO2Sensitivity is about
0.6%, sensitivity is relatively low, and actual application value is not high.
The content of the invention
At room temperature sensitivity is low, response speed for the sensitive material that solves existing detection oxynitride for the present invention
Slow problem, and a kind of molybdenum bisuphide/hydroxide nanoparticle composite and its preparation method and application is provided.
Molybdenum bisuphide of the present invention/hydroxide nanoparticle composite is by molybdenum bisuphide, magnesium nitrate, surfactant and thiourea
It is prepared from；The surfactant is sodium lauryl sulphate；
In the molybdenum bisuphide/hydroxide nanoparticle composite：The mass fraction of molybdenum bisuphide is 10～14%, nitric acid
The mass fraction of magnesium is 26～30%, and the mass fraction of surfactant is 18～22%, balance of thiourea；The magnesium nitrate is
Crystal magnesium nitrate；
The preparation method of the molybdenum bisuphide/hydroxide nanoparticle composite is carried out according to the following steps：
First, it is in molar ratio 25：150：1 weighs ammonium molybdate, thiourea and Polyethylene Glycol as raw material, by material dissolution in 6
In the distilled water of times raw material volume, 25～35 minutes are stirred, then supersound process 25～35 minutes, then will be molten in 10 minutes
The pH value of liquid is adjusted to 1.5～2.5, finally solution is moved in the water heating kettle that liner is politef, at 180～220 DEG C
At a temperature of carry out 18～26h of hydro-thermal reaction, naturally cool to room temperature and obtain molybdenum bisuphide crude product；
The molecular weight of the Polyethylene Glycol is 1000～10000；The stir speed (S.S.) is 400～500r/min；The tune
The reagent of the pH of section solution is the sulfuric acid solution of 6～12mol/kg or the hydrochloric acid solution of 6～12mol/kg；
2nd, molybdenum bisuphide crude product three times is washed with deionized, is then again finally washed ethanol with washing with alcohol three times
Molybdenum bisuphide crude product after washing is placed in 55～65 DEG C of dry casees and is dried 10～14h, obtains molybdenum disulfide nano sheet；
3rd, the molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, grind to into particle diameter be 200～500 purposes
Powder；
4th, molybdenum disulfide powder that the step of weighing 10～14% by mass fraction three obtains, 26～30% magnesium nitrate,
18～22% surfactant and the thiourea of surplus；In molybdenum disulfide powder quality and distilled water volume ratio for (0.3～
0.5g)：40ml is scattered in the molybdenum disulfide powder for weighing in distilled water, and ultrasound adds the nitric acid for weighing after 15～25 minutes
Magnesium, surfactant and thiourea, then magnetic agitation obtain mixed solution within 30 minutes, it is poly- finally mixed solution to be moved to into liner
In the water heating kettle of tetrafluoroethene, 1.5～2.5h of hydro-thermal reaction is carried out at a temperature of 140～160 DEG C, after the completion of naturally cool to room
Temperature, obtains molybdenum bisuphide/hydroxide nanoparticle composite crude product；The surfactant is sodium lauryl sulphate；Institute
Magnesium nitrate is stated for crystal magnesium nitrate；
5th, first deionized water carries out three washings to molybdenum bisuphide/hydroxide nanoparticle composite crude product, so
Carry out three times with ethanol again afterwards to wash, the product obtained after washing is placed in 55～65 DEG C of dry casees and is dried 10～14h, obtain two
Molybdenum sulfide/hydroxide nanoparticle composite；
The application of the molybdenum bisuphide/hydroxide nanoparticle composite is molybdenum bisuphide/hydroxide nanoparticle composite wood
Expect for detecting NOx, specifically carry out according to the following steps：
Molybdenum bisuphide/hydroxide nanoparticle composite is placed in mortar the powder for being ground to that particle diameter is 200～500 mesh
End, during then powder to be added the dehydrated alcohol of 6 times of volumes, supersound process obtains molybdenum bisuphide/hydroxide nanoparticle composite wood
Material solution；Finally molybdenum bisuphide/hydroxide nanoparticle composite solution is coated in golden interdigital electrode, is dried in the air at room temperature
It is dry, gas sensor is obtained, it is under conditions of 25%～35% that the gas sensor of preparation is placed in into temperature for 15 DEG C～30 DEG C, humidity
To NOxDetected.The ratio of the powder and dehydrated alcohol is 1:10；The time of supersound process is 5min.
The present invention possesses following beneficial effect：
Molybdenum bisuphide of the present invention/hydroxide nanoparticle composite sensitive membrane response and recovery response are fast, and to nitrogen oxygen
The selectivity of chemical compound gas is preferable.This method process is simple, environmental friendliness, low cost, favorable repeatability, it is easy to apply.
Molybdenum bisuphide of the present invention/hydroxide nanoparticle composite can as sensitive material, for temperature be 15 DEG C～
30 DEG C, humidity be 25%～35% under conditions of to NOxThe detection of gas, works as NOxWhen gas concentration is 100ppm, the composite wood
Material is to NOxThe sensitivity of gas is up to 72%, response time 3.3s；And minimum mole of the gas that composite can detect that
Concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Description of the drawings：
Fig. 1 is 40000 times of scanning electron microscope (SEM) photographs of molybdenum bisuphide/hydroxide nanoparticle composite prepared by embodiment 1；
Fig. 2 is gas sensor detection NO prepared by testing example 1xSensitivity curve；
Fig. 3 be embodiment 1 prepare molybdenum bisuphide/hydroxide nanoparticle composite as gas sensor to NOxSpirit
Sensitivity and NOxRelation curve between concentration；
Fig. 4 is molybdenum bisuphide/NO of the hydroxide nanoparticle composite to 100ppm prepared by embodiment 1xGas-sensitive
Degree stability test curve；
Fig. 5 is the molybdenum bisuphide/hydroxide nanoparticle composite of the preparation of embodiment 1 to N2Adsorption-desorption curve；
Fig. 6 is 15000 times of transmission electron microscope pictures of molybdenum bisuphide/hydroxide nanoparticle composite prepared by embodiment 1；
Fig. 7 is 400000 times of transmission electron microscope pictures of molybdenum bisuphide/hydroxide nanoparticle composite prepared by embodiment 1；
Fig. 8 is the SEAD figure of molybdenum bisuphide/hydroxide nanoparticle composite prepared by embodiment 1.
Specific embodiment：
Technical solution of the present invention is not limited to act specific embodiment set forth below, also including between each specific embodiment
Any reasonable combination.
Specific embodiment one：Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite, the composite is by two
Molybdenum sulfide, magnesium nitrate, surfactant and thiourea are prepared from；
In the molybdenum bisuphide/hydroxide nanoparticle composite：The mass fraction of molybdenum bisuphide is 10～14%, nitric acid
The mass fraction of magnesium is 26～30%, and the mass fraction of surfactant is 18～22%, balance of thiourea.
Present embodiment possesses following beneficial effect：
Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite sensitive membrane response and recovery response are fast and right
The selectivity of oxynitride gas is preferable.This method process is simple, environmental friendliness, low cost, favorable repeatability, it is easy to should
With.
Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite can be 15 for temperature as sensitive material
DEG C～30 DEG C, humidity be 25%～35% under conditions of to NOxThe detection of gas, works as NOxWhen gas concentration is 100ppm, this is answered
Condensation material is to NOxThe sensitivity of gas is up to 72%, response time 3.3s；And the gas that composite can detect that is minimum
Molar concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Specific embodiment two：Present embodiment from unlike specific embodiment one：The magnesium nitrate is crystal nitre
Sour magnesium.Other steps and parameter are identical with specific embodiment one.
Specific embodiment three：Present embodiment from unlike specific embodiment one or two：The surfactant
For sodium lauryl sulphate.Other steps and parameter are identical with specific embodiment one or two.
Specific embodiment four：The preparation method of present embodiment molybdenum bisuphide/hydroxide nanoparticle composite press with
Lower step is carried out：
First, it is in molar ratio 25：150：1 weighs ammonium molybdate, thiourea and Polyethylene Glycol as raw material, by material dissolution in 6
In the distilled water of times raw material volume, 25～35 minutes are stirred, then supersound process 25～35 minutes, then will be molten in 10 minutes
The pH value of liquid is adjusted to 1.5～2.5, finally solution is moved in the water heating kettle that liner is politef, at 180～220 DEG C
At a temperature of carry out 18～26h of hydro-thermal reaction, naturally cool to room temperature and obtain molybdenum bisuphide crude product；
2nd, molybdenum bisuphide crude product three times is washed with deionized, is then again finally washed ethanol with washing with alcohol three times
Molybdenum bisuphide crude product after washing is placed in 55～65 DEG C of dry casees and is dried 10～14h, obtains molybdenum disulfide nano sheet；
3rd, the molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, grind to into particle diameter be 200～500 purposes
Powder；
4th, molybdenum disulfide powder that the step of weighing 10～14% by mass fraction three obtains, 26～30% magnesium nitrate,
18～22% surfactant and the thiourea of surplus；In molybdenum disulfide powder quality and distilled water volume ratio for (0.3～
0.5g)：40ml is scattered in the molybdenum disulfide powder for weighing in distilled water, and ultrasound adds the nitric acid for weighing after 15～25 minutes
Magnesium, surfactant and thiourea, then magnetic agitation obtain mixed solution within 30 minutes, it is poly- finally mixed solution to be moved to into liner
In the water heating kettle of tetrafluoroethene, 1.5～2.5h of hydro-thermal reaction is carried out at a temperature of 140～160 DEG C, after the completion of naturally cool to room
Temperature, obtains molybdenum bisuphide/hydroxide nanoparticle composite crude product；The surfactant is sodium lauryl sulphate；Institute
Magnesium nitrate is stated for crystal magnesium nitrate；
5th, first deionized water carries out three washings to molybdenum bisuphide/hydroxide nanoparticle composite crude product, so
Carry out three times with ethanol again afterwards to wash, the product obtained after washing is placed in 55～65 DEG C of dry casees and is dried 10～14h, obtain two
Molybdenum sulfide/hydroxide nanoparticle composite.
Present embodiment possesses following beneficial effect：
Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite sensitive membrane response and recovery response are fast and right
The selectivity of oxynitride gas is preferable.This method process is simple, environmental friendliness, low cost, favorable repeatability, it is easy to should
With.
Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite can be 15 for temperature as sensitive material
DEG C～30 DEG C, humidity be 25%～35% under conditions of to NOxThe detection of gas, works as NOxWhen gas concentration is 100ppm, this is answered
Condensation material is to NOxThe sensitivity of gas is up to 72%, response time 3.3s；And the gas that composite can detect that is minimum
Molar concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Specific embodiment five：Present embodiment from unlike specific embodiment four：Polyethylene Glycol described in step one
Molecular weight be 1000～10000.Other steps and parameter are identical with specific embodiment four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Described in step
Stir speed (S.S.) is 400～500r/min.Other steps and parameter are identical with one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Described in step
The reagent for adjusting the pH of solution is the sulfuric acid solution of 6～12mol/kg or the hydrochloric acid solution of 6～12mol/kg.Other steps and ginseng
Number is identical with one of specific embodiment one to six.
Specific embodiment eight：The application of one molybdenum bisuphide of present embodiment/hydroxide nanoparticle composite is two sulfur
Changing molybdenum/hydroxide nanoparticle composite is used to detect NOx, specifically carry out according to the following steps：
Molybdenum bisuphide/hydroxide nanoparticle composite is placed in mortar the powder for being ground to that particle diameter is 200～500 mesh
End, during then powder to be added the dehydrated alcohol of 6 times of volumes, supersound process obtains molybdenum bisuphide/hydroxide nanoparticle composite wood
Material solution；Finally molybdenum bisuphide/hydroxide nanoparticle composite solution is coated in golden interdigital electrode, is dried in the air at room temperature
It is dry, gas sensor is obtained, it is under conditions of 25%～35% that the gas sensor of preparation is placed in into temperature for 15 DEG C～30 DEG C, humidity
To NOxDetected；The ratio of the powder and dehydrated alcohol is 1:10.
Present embodiment possesses following beneficial effect：
Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite sensitive membrane response and recovery response are fast and right
The selectivity of oxynitride gas is preferable.This method process is simple, environmental friendliness, low cost, favorable repeatability, it is easy to should
With.
Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite can be 15 for temperature as sensitive material
DEG C～30 DEG C, humidity be 25%～35% under conditions of to NOxThe detection of gas, works as NOxWhen gas concentration is 100ppm, this is answered
Condensation material is to NOxThe sensitivity of gas is up to 72%, response time 3.3s；And the gas that composite can detect that is minimum
Molar concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Specific embodiment nine：Present embodiment from unlike specific embodiment eight：The time of the supersound process
For 5min.Other steps and parameter are identical with specific embodiment eight.
Embodiment 1：
The preparation method of molybdenum bisuphide described in the present embodiment/hydroxide nanoparticle composite is carried out according to the following steps：
First, it is in molar ratio 25：150：1 weighs ammonium molybdate, thiourea and Polyethylene Glycol as raw material, by material dissolution in 6
In the distilled water of times raw material volume, 30 minutes are stirred, then supersound process 30 minutes, then by the pH value of solution in 10 minutes
Adjust to 2, finally solution is moved in the water heating kettle that liner is politef, hydro-thermal reaction is carried out at a temperature of 220 DEG C
26h, naturally cools to room temperature and obtains molybdenum bisuphide crude product；
The molecular weight of the Polyethylene Glycol is 1000；The stir speed (S.S.) is 500r/min；The pH's for adjusting solution
Reagent is the sulfuric acid solution of 12mol/kg or the hydrochloric acid solution of 12mol/kg；
2nd, molybdenum bisuphide crude product three times is washed with deionized, is then again finally washed ethanol with washing with alcohol three times
Molybdenum bisuphide crude product after washing is placed in 60 DEG C of dry casees and is dried 12h, obtains molybdenum disulfide nano sheet；
3rd, the molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, is ground to into the powder that particle diameter is 400 mesh；
4th, weigh the molybdenum disulfide powder obtained by 0.5g step 3 to be scattered in 40ml distilled water, ultrasound makes it in 20 minutes
It is uniformly dispersed, is subsequently adding the Mg (NO of 0.35g3)2·6H2The sodium lauryl sulphate of O, 0.2g and the thiourea of 0.3g, then magnetic
Power stirring obtains mixed solution in 30 minutes, finally mixed solution is moved in the water heating kettle that liner is politef, at 150 DEG C
At a temperature of carry out hydro-thermal reaction 2h, after the completion of naturally cool to room temperature, obtain molybdenum bisuphide/hydroxide nanoparticle composite thick
Product；
5th, first deionized water carries out three washings to molybdenum bisuphide/hydroxide nanoparticle composite crude product, so
Carry out with ethanol three washings again afterwards, the product obtained after washing be placed in 60 DEG C of dry casees and be dried 12h, obtain molybdenum bisuphide/
Hydroxide nanoparticle composite；The surfactant is sodium lauryl sulphate；The magnesium nitrate is crystal magnesium nitrate.
The molybdenum bisuphide for obtaining/hydroxide nanoparticle composite is placed in mortar the powder for being ground to that particle diameter is 500 mesh
End, during then powder to be added the dehydrated alcohol of 6 times of volumes, supersound process obtains molybdenum bisuphide/hydroxide nanoparticle composite wood
Material solution；Finally molybdenum bisuphide/hydroxide nanoparticle composite solution is coated in golden interdigital electrode, is dried in the air at room temperature
It is dry, gas sensor is obtained, it is to NO under conditions of 35% that the gas sensor of preparation is placed in into temperature for 25 DEG C, humidityxExamined
Survey；The ratio of the powder and dehydrated alcohol is 1:10.
The present embodiment molybdenum bisuphide/hydroxide nanoparticle composite sensitive membrane response and recovery response are fast, and to nitrogen
The selectivity of oxygen compound gas is preferable.This method process is simple, environmental friendliness, low cost, favorable repeatability, it is easy to apply.
Present embodiment molybdenum bisuphide/hydroxide nanoparticle composite can be 25 for temperature as sensitive material
DEG C, humidity be 35% under conditions of to NOxThe detection of gas, works as NOxWhen gas concentration is 100ppm, the composite is to NOxGas
The sensitivity of body is up to 72%, response time 3.3s；And the minimum molar concentration of the gas that composite can detect that is
0.1ppm, sensitivity is about 28.4%, response time 5.3s.
Fig. 1 is 40000 times of scanning electron microscope (SEM) photographs of molybdenum bisuphide/hydroxide nanoparticle composite prepared by embodiment 1；From
It can be seen that molybdenum bisuphide/hydroxide nanoparticle composite is the petal-like structures of curling in Fig. 1；Fig. 2 is testing example 1
The gas sensor detection NO of preparationxSensitivity curve, as can be seen from Figure 2, sensitive membrane absorption NOxAfterwards, resistance relatively rapidly drops
It is low, continuous 5 circulation absorptions-desorption NOxAfterwards, its sensitivity starts to reduce.Fig. 3 is molybdenum bisuphide/hydrogen-oxygen prepared by embodiment 1
Change magnesium nano composite material as gas sensor to NOxSensitivity and NOxRelation curve between concentration；From the figure 3, it may be seen that with
NOxThe increase of concentration, gas sensor is to NOxSensitivity increase therewith；Fig. 4 is molybdenum bisuphide/hydrogen-oxygen prepared by embodiment 1
Change NO of the magnesium nano composite material to 100ppmxGas sensitivity stability test curve：In Fig. 4 it can be seen that molybdenum bisuphide/
The change of sensitivity of hydroxide nanoparticle composite is almost a straight line, shows molybdenum bisuphide/hydroxide prepared by embodiment 1
The Sensitivity Stability of magnesium nano composite material is good；Fig. 5 is that molybdenum bisuphide/hydroxide nanoparticle prepared by embodiment 1 is combined
Material is to N2Adsorption-desorption curve；It can be seen that the sample specific surface area is 46.697m in Fig. 52g-1, can from Fig. 5
Go out the sample and can be very good adsorption/desorption under test gas；Fig. 6 is that molybdenum bisuphide/hydroxide nanoparticle prepared by embodiment 1 is multiple
15000 times of transmission electron microscope pictures of condensation material；Fig. 7 is molybdenum bisuphide/hydroxide nanoparticle composite prepared by embodiment 1
400000 times of transmission electron microscope pictures：MoS can be clearly seen from Fig. 72(002) of crystal, (100) crystal face and Mg (OH)2Crystal
(001), (011) crystal face；Fig. 8 is the SEAD of molybdenum bisuphide/hydroxide nanoparticle composite prepared by embodiment 1
Figure：As can be seen from Figure 8, electronic diffraction ring ecto-entad corresponds respectively to MoS2(100) crystal face of crystal, Mg (OH)2Crystal
(001) crystal face, Mg (OH)2(110) crystal face of crystal, MoS2(110) crystal face of crystal and Mg (OH)2(201) of crystal are brilliant
Face.
Claims (9)
1. a kind of molybdenum bisuphide/hydroxide nanoparticle composite, it is characterised in that：The composite is by molybdenum bisuphide, nitric acid
Magnesium, surfactant and thiourea are prepared from；
In the molybdenum bisuphide/hydroxide nanoparticle composite：The mass fraction of molybdenum bisuphide is 10～14%, magnesium nitrate
Mass fraction is 26～30%, and the mass fraction of surfactant is 18～22%, balance of thiourea.
2. molybdenum bisuphide according to claim 1/hydroxide nanoparticle composite, it is characterised in that：The magnesium nitrate
For crystal magnesium nitrate.
3. molybdenum bisuphide according to claim 1/hydroxide nanoparticle composite, it is characterised in that：Live on the surface
Property agent be sodium lauryl sulphate.
4. the preparation method of molybdenum bisuphide as claimed in claim 1/hydroxide nanoparticle composite, it is characterised in that the party
Method is carried out according to the following steps：
First, it is in molar ratio 25：150：1 weighs ammonium molybdate, thiourea and Polyethylene Glycol as raw material, by material dissolution in 6 times of originals
In the distilled water of material volume, stir 25～35 minutes, then supersound process 25～35 minutes, then by solution in 10 minutes
PH value is adjusted to 1.5～2.5, finally solution is moved in the water heating kettle that liner is politef, in 180～220 DEG C of temperature
18～26h of hydro-thermal reaction is carried out under degree, room temperature is naturally cooled to and is obtained molybdenum bisuphide crude product；
2nd, molybdenum bisuphide crude product three times is washed with deionized, then again with washing with alcohol three times, finally by after washing with alcohol
Molybdenum bisuphide crude product be placed in 55～65 DEG C of dry casees be dried 10～14h, obtain molybdenum disulfide nano sheet；
3rd, the molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, is ground to into the powder that particle diameter is 200～500 mesh；
4th, molybdenum disulfide powder that the step of weighing 10～14% by mass fraction three obtains, 26～30% magnesium nitrate, 18～
22% surfactant and the thiourea of surplus；In molybdenum disulfide powder quality and distilled water volume ratio for (0.3～
0.5g)：40ml is scattered in the molybdenum disulfide powder for weighing in distilled water, and ultrasound adds the nitric acid for weighing after 15～25 minutes
Magnesium, surfactant and thiourea, then magnetic agitation obtain mixed solution within 30 minutes, it is poly- finally mixed solution to be moved to into liner
In the water heating kettle of tetrafluoroethene, 1.5～2.5h of hydro-thermal reaction is carried out at a temperature of 140～160 DEG C, after the completion of naturally cool to room
Temperature, obtains molybdenum bisuphide/hydroxide nanoparticle composite crude product；The surfactant is sodium lauryl sulphate；Institute
Magnesium nitrate is stated for crystal magnesium nitrate；
5th, first deionized water carries out three washings, Ran Houzai to molybdenum bisuphide/hydroxide nanoparticle composite crude product
Three washings are carried out with ethanol, the product obtained after washing is placed in 55～65 DEG C of dry casees and is dried 10～14h, obtain curing
Molybdenum/hydroxide nanoparticle composite.
5. the preparation method of molybdenum bisuphide according to claim 4/hydroxide nanoparticle composite, it is characterised in that：
The molecular weight of Polyethylene Glycol described in step one is 1000～10000.
6. the preparation method of molybdenum bisuphide according to claim 4/hydroxide nanoparticle composite, it is characterised in that：
Stir speed (S.S.) described in step one is 400～500r/min.
7. the preparation method of molybdenum bisuphide according to claim 4/hydroxide nanoparticle composite, it is characterised in that：
The reagent that the pH of solution is adjusted described in step one is the sulfuric acid solution of 6～12mol/kg or the hydrochloric acid solution of 6～12mol/kg.
8. the application of molybdenum bisuphide as claimed in claim 1/hydroxide nanoparticle composite, it is characterised in that curing
Molybdenum/hydroxide nanoparticle composite is used to detect NOx, specifically carry out according to the following steps：
Molybdenum bisuphide/hydroxide nanoparticle composite is placed in mortar the powder for being ground to that particle diameter is 200～500 mesh, so
During powder to be added afterwards the dehydrated alcohol of 6 times of volumes, supersound process obtains molybdenum bisuphide/hydroxide nanoparticle composite material sol
Liquid；Finally molybdenum bisuphide/hydroxide nanoparticle composite solution is coated in golden interdigital electrode, is dried at room temperature, obtained
To gas sensor, it is to NO under conditions of 25%～35% that the gas sensor of preparation is placed in into temperature for 15 DEG C～30 DEG C, humidityx
Detected；The ratio of the powder and dehydrated alcohol is 1:10.
9. the application of molybdenum bisuphide according to claim 8/hydroxide nanoparticle composite, it is characterised in that：It is described
The time of supersound process is 5min.
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| CN112680748A (en) * | 2020-12-01 | 2021-04-20 | 江南大学 | A/B/Si ternary composite silicon-based photoelectrode with bionic structure and preparation method thereof |
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| CN113418960A (en) * | 2021-05-07 | 2021-09-21 | 电子科技大学 | Flexible humidity sensor based on hydrophilicity-enhanced molybdenum disulfide and preparation method thereof |
| CN114058084A (en) * | 2021-11-29 | 2022-02-18 | 江西广源化工有限责任公司 | Molybdenum substrate layer modified magnesium hydroxide and preparation method and application thereof |
| CN114609197A (en) * | 2022-03-25 | 2022-06-10 | 电子科技大学 | Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor |
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