CN106596651B - A kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application - Google Patents
A kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application Download PDFInfo
- Publication number
- CN106596651B CN106596651B CN201611103265.XA CN201611103265A CN106596651B CN 106596651 B CN106596651 B CN 106596651B CN 201611103265 A CN201611103265 A CN 201611103265A CN 106596651 B CN106596651 B CN 106596651B
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- composite material
- nanoparticle composite
- hydroxide nanoparticle
- hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
A kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application, are related to molybdenum disulfide/magnesium hydroxide material and its preparation and application.Sensitivity is low at room temperature, response speed is slow in order to solve the problems, such as existing detection oxynitrides sensitive material by the present invention.The composite material is prepared by molybdenum disulfide, magnesium nitrate, surfactant and thiocarbamide.Method: ammonium molybdate, thiocarbamide and polyethylene glycol are weighed as hydro-thermal reaction and obtains molybdenum disulfide crude product；Washing, drying；It grinds at powder；Hydro-thermal reaction prepares crude product；It is washed, drying box obtains molybdenum disulfide/hydroxide nanoparticle composite material；Using: molybdenum disulfide/hydroxide nanoparticle composite material is prepared into gas sensor to NOxIt is detected.Composite material sensitive membrane response and recovery response are fast and preferable to the selectivity of oxynitrides gas, and method and process is simple.The present invention is suitable for preparing and applying molybdenum disulfide/hydroxide nanoparticle composite material.
Description
Technical field
The present invention relates to a kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and applications.
Background technique
With NO and NO2Based on NOx(nitrogen oxides) is the major reason 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 through ultraviolet light with hydrocarbon, it is photochemical
Learning smog has special odor, stimulates eyes, injures plant, and atmospheric visibility can be made to reduce；In addition, NOxIn air
The nitric acid that water reaction generates and the ingredient that nitrous acid is acid rain；NO in atmospherexIt is mostly derived from burning and the plant of fossil fuel
The conversion of nitrogenous compound in the burning of body, and agricultural land soil and animal excrements.Therefore, research and development are to NOxIt is highly sensitive, fast
The gas sensor of speed response has a very important significance daily life and industrial production.
Molybdenum disulfide is as novel nano material, in catalyst, solid lubricant, lithium battery, hydrogen storage, liberation of hydrogen, sensing
Device, photoelectricity etc. have huge application prospect, are widely studied by people.In molybdenum disulfide structure, each molybdenum is former
All there are six sulphur atoms to wrap up around sub, shows triangular prism column, especially more Mo-S faceted pebbles is exposed, due to Mo-S faceted pebble ratio
Surface area is big, and surface-active is very high, so there is very high apparent activation energy, therefore, molybdenum disulfide/hydroxide nanoparticle is compound
Material will more be of practical significance in fields such as gas sensing techniques.There is document report MoS2The inspection of/graphene mixing aeroge
Survey NO2, the sensor is to NO2The testing result of gas is shown in more sensitive, MoS when operating temperature is 200 DEG C2/ graphene is mixed
It is higher to close aeroge senor operating temperature, can not detect at room temperature, be unfavorable for practical application.And MoS2/ graphene is mixed
It closes aeroge to need to calcine at 450 DEG C, sensor preparation temperature is high, is unfavorable for industrialized production.Document report ZnO modification
MoS2Nanosheet composite material detects ethyl alcohol, and it is 240 DEG C which, which is shown in operating temperature to the testing result of alcohol gas,
When it is more sensitive, but ZnO modify MoS2Nanosheet composite material senor operating temperature is higher, can not detect at room temperature, also
It is unfavorable for practical application.SnO2It modifies molybdenum disulfide nano sheet composite material and detects NO2, detect 0.5ppm NO2Sensitivity is about
0.6%, sensitivity is lower, and practical application value is not high.
Summary of the invention
The present invention is in order to which sensitivity is low at room temperature, response speed for the sensitive material that solves existing detection oxynitrides
Slow problem, and a kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application are provided.
Molybdenum disulfide of the present invention/hydroxide nanoparticle composite material is by molybdenum disulfide, magnesium nitrate, surfactant and thiocarbamide
It is prepared；The surfactant is lauryl sodium sulfate；
In the molybdenum disulfide/hydroxide nanoparticle composite material: the mass fraction of molybdenum disulfide is 10~14%, nitric acid
The mass fraction of magnesium is 26~30%, and the mass fraction of surfactant is 18~22%, and surplus is thiocarbamide；The magnesium nitrate is
Crystal magnesium nitrate；
The molybdenum disulfide/hydroxide nanoparticle composite material preparation method sequentially includes the following steps:
One, ammonium molybdate, thiocarbamide and polyethylene glycol are weighed as raw material, by dissolution of raw material in 6 for 25:150:1 in molar ratio
In the distilled water of times raw material volume, stirs 25~35 minutes, be then ultrasonically treated 25~35 minutes, it then will be molten in 10 minutes
The pH value of liquid is adjusted to 1.5~2.5, finally moves to solution in the water heating kettle that liner is polytetrafluoroethylene (PTFE), at 180~220 DEG C
At a temperature of carry out 18~26h of hydro-thermal reaction, cooled to room temperature obtains molybdenum disulfide crude product；
The molecular weight of the polyethylene glycol is 1000~10000；The stirring rate is 400~500r/min；The tune
The reagent for saving the pH of solution is the sulfuric acid solution of 6~12mol/kg or the hydrochloric acid solution of 6~12mol/kg；
Two, molybdenum disulfide crude product is washed with deionized three times, then again with ethanol washing three times, finally ethyl alcohol is washed
Molybdenum disulfide crude product after washing is placed in 55~65 DEG C of dry casees dry 10~14h, obtains molybdenum disulfide nano sheet；
Three, molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, grind at partial size be 200~500 purposes
Powder；
Four, molybdenum disulfide powder that the step of weighing 10~14% by mass fraction three obtains, 26~30% magnesium nitrate,
18~22% surfactant and the thiocarbamide of surplus；In the ratio of molybdenum disulfide powder quality and distilled water volume be (0.3~
0.5g): 40ml disperses weighed molybdenum disulfide powder in distilled water, and weighed nitric acid is added after 15~25 minutes in ultrasound
Then magnesium, surfactant and thiocarbamide obtain mixed solution in magnetic agitation 30 minutes, it is poly- that mixed solution, which is finally moved to 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, naturally cools to room after the completion
Temperature obtains molybdenum disulfide/hydroxide nanoparticle composite material crude product；The surfactant is lauryl sodium sulfate；Institute
Stating magnesium nitrate is crystal magnesium nitrate；
Five, molybdenum disulfide/hydroxide nanoparticle composite material crude product is washed three times with deionized water first, so
It is washed three times with ethyl alcohol again afterwards, the product obtained after washing is placed in 55~65 DEG C of dry casees dry 10~14h, obtains two
Molybdenum sulfide/hydroxide nanoparticle composite material；
The application of the molybdenum disulfide/hydroxide nanoparticle composite material is molybdenum disulfide/hydroxide nanoparticle composite wood
Material is for detecting NOx, specifically sequentially include the following steps:
Molybdenum disulfide/hydroxide nanoparticle composite material is placed in mortar to the powder for being ground to that partial size is 200~500 mesh
Then end powder is added in the dehydrated alcohol of 6 times of volumes, ultrasonic treatment obtains molybdenum disulfide/hydroxide nanoparticle composite wood
Expect solution；Finally molybdenum disulfide/hydroxide nanoparticle composite material solution is coated in golden interdigital electrode, is dried in the air at room temperature
It is dry, gas sensor is obtained, it is 15 DEG C~30 DEG C, under conditions of humidity is 25%~35% that the gas sensor of preparation, which is placed in temperature,
To NOxIt is detected.The ratio of the powder and dehydrated alcohol is 1:10；The time of ultrasonic treatment is 5min.
The present invention have it is following the utility model has the advantages that
Molybdenum disulfide of the present invention/hydroxide nanoparticle composite material sensitive membrane response and recovery response are fast, and to nitrogen oxygen
The selectivity of chemical compound gas is preferable.This method simple process, environmental-friendly, at low cost, favorable repeatability, are easy to apply.
Molybdenum disulfide of the present invention/hydroxide nanoparticle composite material can be used 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 high sensitivity of gas is up to 72%, response time 3.3s；And minimum mole of the detectable gas of composite material
Concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Detailed description of the invention:
Fig. 1 is 40000 times of scanning electron microscope (SEM) photographs of molybdenum disulfide/hydroxide nanoparticle composite material prepared by embodiment 1；
Fig. 2 is gas sensor detection NO prepared by testing example 1xSensitivity curve；
Fig. 3 be embodiment 1 prepare molybdenum disulfide/hydroxide nanoparticle composite material as gas sensor to NOxSpirit
Sensitivity and NOxRelation curve between concentration；
Fig. 4 is NO of the molybdenum disulfide/hydroxide nanoparticle composite material to 100ppm of the preparation of embodiment 1xGas-sensitive
Spend stability test curve；
Fig. 5 is molybdenum disulfide/hydroxide nanoparticle composite material of the preparation of embodiment 1 to N2Adsorption-desorption curve；
Fig. 6 is 15000 times of transmission electron microscope pictures of molybdenum disulfide/hydroxide nanoparticle composite material prepared by embodiment 1；
Fig. 7 is 400000 times of transmission electron microscope pictures of molybdenum disulfide/hydroxide nanoparticle composite material prepared by embodiment 1；
Fig. 8 is molybdenum disulfide/hydroxide nanoparticle composite material selective electron diffraction figure prepared by embodiment 1.
Specific embodiment:
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any reasonable combination.
Specific embodiment 1: present embodiment molybdenum disulfide/hydroxide nanoparticle composite material, the composite material is by two
Molybdenum sulfide, magnesium nitrate, surfactant and thiocarbamide are prepared；
In the molybdenum disulfide/hydroxide nanoparticle composite material: the mass fraction of molybdenum disulfide is 10~14%, nitric acid
The mass fraction of magnesium is 26~30%, and the mass fraction of surfactant is 18~22%, and surplus is thiocarbamide.
Present embodiment have it is following the utility model has the advantages that
Present embodiment molybdenum disulfide/hydroxide nanoparticle composite material sensitive membrane response and recovery response are fast and right
The selectivity of oxynitrides gas is preferable.This method simple process, environmental-friendly, at low cost, favorable repeatability, are easy to answer
With.
Present embodiment molybdenum disulfide/hydroxide nanoparticle composite material can be used as sensitive material, be 15 for temperature
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 multiple
Condensation material is to NOxThe high sensitivity of gas is up to 72%, response time 3.3s；And the detectable gas of composite material is minimum
Molar concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: the magnesium nitrate is crystal nitre
Sour magnesium.Other steps and parameter are same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: the surfactant
For lauryl sodium sulfate.Other steps and parameter are the same as one or two specific embodiments.
Specific embodiment 4: present embodiment molybdenum disulfide/hydroxide nanoparticle composite material preparation method press with
Lower step carries out:
One, ammonium molybdate, thiocarbamide and polyethylene glycol are weighed as raw material, by dissolution of raw material in 6 for 25:150:1 in molar ratio
In the distilled water of times raw material volume, stirs 25~35 minutes, be then ultrasonically treated 25~35 minutes, it then will be molten in 10 minutes
The pH value of liquid is adjusted to 1.5~2.5, finally moves to solution in the water heating kettle that liner is polytetrafluoroethylene (PTFE), at 180~220 DEG C
At a temperature of carry out 18~26h of hydro-thermal reaction, cooled to room temperature obtains molybdenum disulfide crude product；
Two, molybdenum disulfide crude product is washed with deionized three times, then again with ethanol washing three times, finally ethyl alcohol is washed
Molybdenum disulfide crude product after washing is placed in 55~65 DEG C of dry casees dry 10~14h, obtains molybdenum disulfide nano sheet；
Three, molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, grind at partial size be 200~500 purposes
Powder；
Four, molybdenum disulfide powder that the step of weighing 10~14% by mass fraction three obtains, 26~30% magnesium nitrate,
18~22% surfactant and the thiocarbamide of surplus；In the ratio of molybdenum disulfide powder quality and distilled water volume be (0.3~
0.5g): 40ml disperses weighed molybdenum disulfide powder in distilled water, and weighed nitric acid is added after 15~25 minutes in ultrasound
Then magnesium, surfactant and thiocarbamide obtain mixed solution in magnetic agitation 30 minutes, it is poly- that mixed solution, which is finally moved to 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, naturally cools to room after the completion
Temperature obtains molybdenum disulfide/hydroxide nanoparticle composite material crude product；The surfactant is lauryl sodium sulfate；Institute
Stating magnesium nitrate is crystal magnesium nitrate；
Five, molybdenum disulfide/hydroxide nanoparticle composite material crude product is washed three times with deionized water first, so
It is washed three times with ethyl alcohol again afterwards, the product obtained after washing is placed in 55~65 DEG C of dry casees dry 10~14h, obtains two
Molybdenum sulfide/hydroxide nanoparticle composite material.
Present embodiment have it is following the utility model has the advantages that
Present embodiment molybdenum disulfide/hydroxide nanoparticle composite material sensitive membrane response and recovery response are fast and right
The selectivity of oxynitrides gas is preferable.This method simple process, environmental-friendly, at low cost, favorable repeatability, are easy to answer
With.
Present embodiment molybdenum disulfide/hydroxide nanoparticle composite material can be used as sensitive material, be 15 for temperature
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 multiple
Condensation material is to NOxThe high sensitivity of gas is up to 72%, response time 3.3s；And the detectable gas of composite material is minimum
Molar concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Specific embodiment 5: present embodiment is unlike specific embodiment four: polyethylene glycol described in step 1
Molecular weight be 1000~10000.Other steps and parameter are identical as specific embodiment four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: described in step 1
Stirring rate is 400~500r/min.Other steps and parameter are identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: described in step 1
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 as one of specific embodiment one to six.
Specific embodiment 8: the application of one molybdenum disulfide of present embodiment/hydroxide nanoparticle composite material is two sulphur
Change molybdenum/hydroxide nanoparticle composite material for detecting NOx, specifically sequentially include the following steps:
Molybdenum disulfide/hydroxide nanoparticle composite material is placed in mortar to the powder for being ground to that partial size is 200~500 mesh
Then end powder is added in the dehydrated alcohol of 6 times of volumes, ultrasonic treatment obtains molybdenum disulfide/hydroxide nanoparticle composite wood
Expect solution；Finally molybdenum disulfide/hydroxide nanoparticle composite material solution is coated in golden interdigital electrode, is dried in the air at room temperature
It is dry, gas sensor is obtained, it is 15 DEG C~30 DEG C, under conditions of humidity is 25%~35% that the gas sensor of preparation, which is placed in temperature,
To NOxIt is detected；The ratio of the powder and dehydrated alcohol is 1:10.
Present embodiment have it is following the utility model has the advantages that
Present embodiment molybdenum disulfide/hydroxide nanoparticle composite material sensitive membrane response and recovery response are fast and right
The selectivity of oxynitrides gas is preferable.This method simple process, environmental-friendly, at low cost, favorable repeatability, are easy to answer
With.
Present embodiment molybdenum disulfide/hydroxide nanoparticle composite material can be used as sensitive material, be 15 for temperature
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 multiple
Condensation material is to NOxThe high sensitivity of gas is up to 72%, response time 3.3s；And the detectable gas of composite material is minimum
Molar concentration is 0.1ppm, and sensitivity is about 28.4%, response time 5.3s.
Specific embodiment 9: present embodiment is unlike specific embodiment eight: the time of the ultrasonic treatment
For 5min.Other steps and parameter are identical as specific embodiment eight.
Embodiment 1:
Molybdenum disulfide described in the present embodiment/hydroxide nanoparticle composite material preparation method sequentially includes the following steps:
One, ammonium molybdate, thiocarbamide and polyethylene glycol are weighed as raw material, by dissolution of raw material in 6 for 25:150:1 in molar ratio
In the distilled water of times raw material volume, stirs 30 minutes, be then ultrasonically treated 30 minutes, then by the pH value of solution in 10 minutes
2 are adjusted to, finally solution is moved in the water heating kettle that liner is polytetrafluoroethylene (PTFE), carries out hydro-thermal reaction at a temperature of 220 DEG C
26h, cooled to room temperature obtain molybdenum disulfide crude product；
The molecular weight of the polyethylene glycol is 1000；The stirring rate 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；
Two, molybdenum disulfide crude product is washed with deionized three times, then again with ethanol washing three times, finally ethyl alcohol is washed
Molybdenum disulfide crude product after washing is placed in 60 DEG C of dry casees dry 12h, obtains molybdenum disulfide nano sheet；
Three, molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, grind at partial size be 400 mesh powders；
Four, it weighs the resulting molybdenum disulfide powder of 0.5g step 3 to be scattered in 40ml distilled water, ultrasound makes it in 20 minutes
It is uniformly dispersed, the Mg (NO of 0.35g is then added3)2·6H2O, the thiocarbamide of the lauryl sodium sulfate of 0.2g and 0.3g, then magnetic
Power stirs 30 minutes and obtains mixed solution, finally moves to mixed solution in the water heating kettle that liner is polytetrafluoroethylene (PTFE), at 150 DEG C
At a temperature of carry out hydro-thermal reaction 2h, cooled to room temperature, it is thick to obtain molybdenum disulfide/hydroxide nanoparticle composite material after the completion
Product；
Five, molybdenum disulfide/hydroxide nanoparticle composite material crude product is washed three times with deionized water first, so
Washed three times with ethyl alcohol again afterwards, the product obtained after washing be placed in 60 DEG C of dry casees dry 12h, obtain molybdenum disulfide/
Hydroxide nanoparticle composite material；The surfactant is lauryl sodium sulfate；The magnesium nitrate is crystal magnesium nitrate.
Obtained molybdenum disulfide/hydroxide nanoparticle composite material is placed in mortar to the powder for being ground to that partial size is 500 mesh
Then end powder is added in the dehydrated alcohol of 6 times of volumes, ultrasonic treatment obtains molybdenum disulfide/hydroxide nanoparticle composite wood
Expect solution；Finally molybdenum disulfide/hydroxide nanoparticle composite material solution is coated in golden interdigital electrode, is dried in the air at room temperature
It is dry, obtain gas sensor, by the gas sensor of preparation be placed in temperature be 25 DEG C, under conditions of humidity is 35% to NOxIt is examined
It surveys；The ratio of the powder and dehydrated alcohol is 1:10.
The present embodiment molybdenum disulfide/hydroxide nanoparticle composite material sensitive membrane response and recovery response are fast, and to nitrogen
The selectivity of oxygen compound gas is preferable.This method simple process, environmental-friendly, at low cost, favorable repeatability, are easy to apply.
Present embodiment molybdenum disulfide/hydroxide nanoparticle composite material can be used as sensitive material, be 25 for temperature
DEG C, humidity be 35% under conditions of to NOxThe detection of gas, works as NOxWhen gas concentration is 100ppm, the composite material is to NOxGas
The high sensitivity of body is up to 72%, response time 3.3s；And the minimum molar concentration of the detectable gas of composite material is
0.1ppm, sensitivity are about 28.4%, response time 5.3s.
Fig. 1 is 40000 times of scanning electron microscope (SEM) photographs of molybdenum disulfide/hydroxide nanoparticle composite material prepared by embodiment 1；From
It can be seen that molybdenum disulfide/hydroxide nanoparticle composite material is the petal-like structures of curling in Fig. 1；Fig. 2 is testing example 1
The gas sensor of preparation detects NOxSensitivity curve, as can be seen from Figure 2, sensitive membrane adsorb NOxAfterwards, resistance relatively rapidly drops
It is low, continuous 5 circulation absorptions-desorption NOxAfterwards, sensitivity starts to reduce.Fig. 3 is molybdenum disulfide/hydrogen-oxygen prepared by embodiment 1
Change magnesium nanocomposite 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 with it；Fig. 4 is molybdenum disulfide/hydrogen-oxygen prepared by embodiment 1
Change magnesium nanocomposite to the NO of 100ppmxGas sensitivity stability test curve: in Fig. 4 it can be seen that molybdenum disulfide/
The change of sensitivity of hydroxide nanoparticle composite material is almost a straight line, shows molybdenum disulfide/hydroxide prepared by embodiment 1
The Sensitivity Stability of magnesium nanocomposite is good；Fig. 5 is that molybdenum disulfide/hydroxide nanoparticle prepared by embodiment 1 is compound
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
The sample can be very good adsorption/desorption under test gas out；Fig. 6 is that molybdenum disulfide/hydroxide nanoparticle prepared by embodiment 1 is multiple
15000 times of transmission electron microscope pictures of condensation material；Fig. 7 is molybdenum disulfide/hydroxide nanoparticle composite material 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 molybdenum disulfide/hydroxide nanoparticle composite material selective electron diffraction prepared by embodiment 1
Figure: as can be seen from Figure 8, electronic diffraction ring ecto-entad corresponds respectively to MoS2(100) crystal face, the Mg (OH) of crystal2Crystal
(001) crystal face, Mg (OH)2(110) crystal face, the MoS of crystal2(110) crystal face and Mg (OH) of crystal2(201) of crystal are brilliant
Face.
Claims (8)
1. a kind of molybdenum disulfide/hydroxide nanoparticle composite material, it is characterised in that: the composite material is by molybdenum disulfide, nitric acid
Magnesium, surfactant and thiocarbamide are prepared；
In the molybdenum disulfide/hydroxide nanoparticle composite material: the mass fraction of molybdenum disulfide is 10~14%, magnesium nitrate
Mass fraction is 26~30%, and the mass fraction of surfactant is 18~22%, and surplus is thiocarbamide；
The surfactant is lauryl sodium sulfate.
2. molybdenum disulfide according to claim 1/hydroxide nanoparticle composite material, it is characterised in that: the magnesium nitrate
For crystal magnesium nitrate.
3. molybdenum disulfide as described in claim 1/hydroxide nanoparticle composite material preparation method, it is characterised in that the party
Method sequentially includes the following steps:
One, ammonium molybdate, thiocarbamide and polyethylene glycol are weighed as raw material, by dissolution of raw material in 6 times of originals for 25:150:1 in molar ratio
In the distilled water of Material product, stirs 25~35 minutes, be then ultrasonically treated 25~35 minutes, then by solution in 10 minutes
PH value is adjusted to 1.5~2.5, finally moves to solution in the water heating kettle that liner is polytetrafluoroethylene (PTFE), in 180~220 DEG C of temperature
Degree is lower to carry out 18~26h of hydro-thermal reaction, and cooled to room temperature obtains molybdenum disulfide crude product；
Two, molybdenum disulfide crude product is washed with deionized three times, then again with ethanol washing three times, finally will be after ethanol washing
Molybdenum disulfide crude product be placed in 55~65 DEG C of dry casees dry 10~14h, obtain molybdenum disulfide nano sheet；
Three, molybdenum disulfide nano sheet obtained in step 2 is placed in mortar, grind at partial size be 200~500 mesh powders；
Four, molybdenum disulfide powder that the step of weighing 10~14% by mass fraction three obtains, 26~30% magnesium nitrate, 18~
22% surfactant and the thiocarbamide of surplus；In the ratio of molybdenum disulfide powder quality and distilled water volume be (0.3~
0.5g): 40ml disperses weighed molybdenum disulfide powder in distilled water, and weighed nitric acid is added after 15~25 minutes in ultrasound
Then magnesium, surfactant and thiocarbamide obtain mixed solution in magnetic agitation 30 minutes, it is poly- that mixed solution, which is finally moved to 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, naturally cools to room after the completion
Temperature obtains molybdenum disulfide/hydroxide nanoparticle composite material crude product；The surfactant is lauryl sodium sulfate；Institute
Stating magnesium nitrate is crystal magnesium nitrate；
Five, molybdenum disulfide/hydroxide nanoparticle composite material crude product is washed three times with deionized water first, then again
It is washed three times with ethyl alcohol, the product obtained after washing is placed in 55~65 DEG C of dry casees dry 10~14h, obtains curing
Molybdenum/hydroxide nanoparticle composite material.
4. molybdenum disulfide according to claim 3/hydroxide nanoparticle composite material preparation method, it is characterised in that:
The molecular weight of polyethylene glycol described in step 1 is 1000~10000.
5. molybdenum disulfide according to claim 3/hydroxide nanoparticle composite material preparation method, it is characterised in that:
Stirring rate described in step 1 is 400~500r/min.
6. molybdenum disulfide according to claim 3/hydroxide nanoparticle composite material preparation method, it is characterised in that:
The reagent that the pH of solution is adjusted described in step 1 is the sulfuric acid solution of 6~12mol/kg or the hydrochloric acid solution of 6~12mol/kg.
7. the application of molybdenum disulfide as described in claim 1/hydroxide nanoparticle composite material, it is characterised in that curing
Molybdenum/hydroxide nanoparticle composite material is for detecting NOx, specifically sequentially include the following steps:
It is 200~500 mesh powders that molybdenum disulfide/hydroxide nanoparticle composite material, which is placed in mortar, and is ground to partial size, so
Powder is added afterwards in the dehydrated alcohol of 6 times of volumes, ultrasonic treatment obtains molybdenum disulfide/hydroxide nanoparticle composite material sol
Liquid；Finally molybdenum disulfide/hydroxide nanoparticle composite material solution is coated in golden interdigital electrode, dries, obtains at room temperature
To gas sensor, by the gas sensor of preparation be placed in temperature be 15 DEG C~30 DEG C, under conditions of humidity is 25%~35% to NOx
It is detected；The ratio of the powder and dehydrated alcohol is 1:10.
8. the application of molybdenum disulfide according to claim 7/hydroxide nanoparticle composite material, it is characterised in that: described
The time of ultrasonic treatment is 5min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611103265.XA CN106596651B (en) | 2016-12-05 | 2016-12-05 | A kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611103265.XA CN106596651B (en) | 2016-12-05 | 2016-12-05 | A kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106596651A CN106596651A (en) | 2017-04-26 |
| CN106596651B true CN106596651B (en) | 2019-02-12 |
Family
ID=58595849
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611103265.XA Expired - Fee Related CN106596651B (en) | 2016-12-05 | 2016-12-05 | A kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106596651B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085020B (en) * | 2017-05-26 | 2019-03-26 | 黑龙江大学 | A kind of molybdenum disulfide/indium hydroxide composite air-sensitive sensing material and preparation method and application |
| CN111796004A (en) * | 2019-04-08 | 2020-10-20 | 天津大学 | Nitrogen dioxide sensor based on two-dimensional molybdenum disulfide nano material |
| CN112680748B (en) * | 2020-12-01 | 2022-03-25 | 江南大学 | A/B/Si ternary composite silicon-based photoelectrode with bionic structure and preparation method thereof |
| 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 |
| CN114058084B (en) * | 2021-11-29 | 2023-05-09 | 江西广源化工有限责任公司 | Molybdenum substrate layer modified magnesium hydroxide and preparation method and application thereof |
| CN114609197B (en) * | 2022-03-25 | 2023-11-21 | 电子科技大学 | Gas-sensitive material, preparation method and NH (NH) thereof 3 Application in gas sensor |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5931449B2 (en) * | 1976-07-29 | 1984-08-02 | 東レ株式会社 | Polyamide film with excellent drawability |
| JPH0532850A (en) * | 1991-03-05 | 1993-02-09 | Showa Electric Wire & Cable Co Ltd | Flame-retardant resin composition |
| CN104495935B (en) * | 2014-12-03 | 2017-06-16 | 安徽百特新材料科技有限公司 | A kind of strip preparation method of molybdenum disulfide nano sheet layer |
| CN104409706B (en) * | 2014-12-22 | 2017-03-29 | 湖南大学 | A kind of molybdenum bisuphide/sulphur, nitrogen-doped graphene nanosheet composite material and its preparation method and application |
| CN104649324B (en) * | 2015-01-21 | 2016-04-20 | 济南大学 | A kind of preparation method of molybdenumdisulphide/zinc oxide nanometer composite material |
| CN104961353B (en) * | 2015-06-24 | 2018-01-12 | 中国科学院上海光学精密机械研究所 | Hydro-thermal prepares large scale, the method for orthogonal unsymmetric structure platelike molybdenumdisulfide nano thin-film |
| CN105651999B (en) * | 2016-02-29 | 2018-02-27 | 江苏大学 | Molybdenum disulfide-based sensor and preparation method and application thereof |
| CN105664975B (en) * | 2016-03-14 | 2017-11-10 | 金堆城钼业股份有限公司 | A kind of stratiform MoS2‑Bi2MoO6The preparation method of nano composite material |
| CN105742602B (en) * | 2016-03-27 | 2018-07-20 | 华南理工大学 | A kind of sodium-ion battery cathode Sn/MoS2/ C composite and preparation method thereof |
| CN105879891B (en) * | 2016-04-20 | 2018-04-03 | 燕山大学 | A kind of preparation method of nickel phosphorus/molybdenum disulfide liberation of hydrogen composite |
-
2016
- 2016-12-05 CN CN201611103265.XA patent/CN106596651B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN106596651A (en) | 2017-04-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106596651B (en) | A kind of molybdenum disulfide/hydroxide nanoparticle composite material and preparation method and application | |
| Lv et al. | Sb-doped three-dimensional ZnFe2O4 macroporous spheres for N-butanol chemiresistive gas sensors | |
| Sun et al. | Fabrication of ZnO quantum dots@ SnO2 hollow nanospheres hybrid hierarchical structures for effectively detecting formaldehyde | |
| Yuan et al. | Rose-like MoO₃/MoS₂/rGO low-temperature ammonia sensors based on multigas detection methods | |
| Shakeel et al. | Advanced polymeric/inorganic nanohybrids: An integrated platform for gas sensing applications | |
| Ganesh et al. | Tuning the selectivity of NH3 gas sensing response using Cu-doped ZnO nanostructures | |
| Chen et al. | Ni-Co-P hollow nanobricks enabled humidity sensor for respiratory analysis and human-machine interfacing | |
| Meng et al. | High-sensitivity resistive humidity sensor based on graphitic carbon nitride nanosheets and its application | |
| Yu et al. | Peroxidase-like activity of FeVO4 nanobelts and its analytical application for optical detection of hydrogen peroxide | |
| CN106770544B (en) | Ni-MOF ultrathin nanometer band, synthetic method and its application | |
| CN104118904B (en) | The preparation method of three-dimensional hollow multilevel hierarchy stannic oxide gas sensitive and application thereof | |
| Chen et al. | Nanostructured gas sensors: From air quality and environmental monitoring to healthcare and medical applications | |
| CN102269693B (en) | Photonic crystal humidity sensor and preparation method thereof | |
| CN105883906B (en) | A kind of nano-stannic oxide and graphene composite material and preparation method and application | |
| CN104297464A (en) | Making method and application of mycotoxin photoelectrochemical sensor for in situ generation of CdS | |
| CN111579600B (en) | Camellia flower-shaped ZnO/SnO-SnO 2 Composite material and preparation method and application thereof | |
| CN108680610A (en) | One kind being based on MoS2The room temperature NO of-PbS composite materials2Gas sensor and preparation method thereof | |
| CN105628764A (en) | Uric acid detection electrochemical sensor and preparation and application thereof | |
| Chen et al. | High-response of NiO-modified self-assembled nanosheets formed with ZnO nanoparticles for n-butanol detection | |
| CN105885847B (en) | A kind of cadmium sulfoselenide solid solution quantum dot and preparation method thereof and Photocatalyzed Hydrogen Production application | |
| Wang et al. | Enhanced NH3 sensing properties of carboxyl functionalized carbon nanocoil | |
| CN105854898A (en) | Preparation method of cellulose-based core-shell CdS/ZnO (cadmium-sulfur/zinc oxide) photocatalyst | |
| CN103235123A (en) | Electrochemical immunosensor for detecting avian reoviruses and production method thereof | |
| Xu et al. | Synthesis of ZnO/ZnCo2O4 hollow tube clusters by a template method for high-sensitive H2S sensor | |
| CN104148626A (en) | Calixarene functionalized gold nanoparticle and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190212 Termination date: 20201205 |