CN110231371A - A kind of Au/g-C3N4The preparation method of humidity-sensitive material - Google Patents

A kind of Au/g-C3N4The preparation method of humidity-sensitive material Download PDF

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Publication number
CN110231371A
CN110231371A CN201910633834.9A CN201910633834A CN110231371A CN 110231371 A CN110231371 A CN 110231371A CN 201910633834 A CN201910633834 A CN 201910633834A CN 110231371 A CN110231371 A CN 110231371A
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China
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preparation
humidity
sensitive material
concentration
mmol
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CN201910633834.9A
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张红燕
于淑国
张军
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Xinjiang University
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Xinjiang University
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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
    • G01N27/121—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 for determining moisture content, e.g. humidity, of the fluid
    • 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

Abstract

The present invention provides a kind of Au/g-C3N4The preparation method of humidity-sensitive material, this method include block g-C3N4Preparation, two-dimensional nano stratiform g-C3N4Preparation and Au/g-C3N4Three steps of preparation.Preferably, in Au/g-C3N4It further include HAuCl in the preparation step of humidity-sensitive material4The step of adding proportion preferably optimizes with preparation technology parameter, works as HAuCl4When concentration is 0.5 mM, Au nanoparticle enters g-C3N4Interlayer, 2D Au/g-C3N4It can accelerate H2O's is decomposed to form conductive ion (H3O+), further improve the conductivity of sensor.High-performance Au/g-C can be obtained by above-mentioned processing3N4Humidity-sensitive material.

Description

A kind of Au/g-C3N4The preparation method of humidity-sensitive material
Technical field
The invention belongs to two-dimensional nano semiconductor sensitive material development fields, and in particular to a kind of Au/g-C3N4Humidity-sensitive material Preparation method.
Background technique
With the fast development of science and technology, humidity sensor is in industrial production, food safety, environmental Kuznets Curves, pharmaceutical processing, agriculture It is played an important role in the application such as industry.There is high sensitivity in order to obtain, good reproducibility, low cost, easily fabricated and length The humidity sensor of phase stability, semiconductor material, polymer material, organic and inorganic materials are frequently used to humidity sensor material Material.Graphite carbonitride (the g-C of two-dimentional (2D)3N4) it is a kind of polymer of intermediate band gap (2.65eV) without metal semiconductor material There is material big specific surface area, unique physical and chemical stability and special structure development to be relatively suitble to be humidity-sensitive material.But It is to lack g-C in existing report3N4The exploitation of humidity-sensitive material.By research, find due to H2O is adsorbed on g-C3N4When surface, H2O and g-C3N4Adsorption capacity can be strong, be not easy to form conductive ion, limit g-C3N4Application in moisture sensor.In order to Overcome this disadvantage, when with Au modify 2D g-C3N4When, 2D g-C3N4To H2The suction-operated of O molecule weakens, and makes 2D Au/g- C3N4Electric conductivity enhancing.And only short grained noble metal nano particles (2 nm) dimensional effect can accelerate point of water Solution.Therefore, with the nano-particle modified 2D g-C of the Au of small particle3N4It can promote the decomposition of water, to be effectively improved humidity sensor The response of device.The advantages of in view of above-mentioned material, developing a kind of New Two Dimensional Au/g-C3N4 humidity sensor has potential work Industry production and environmentally friendly application value.
Present inventor obtains Au/g-C by the control to Au concentration3N4High performance wet sensitive sensing material.It is real It tests and shows Au/g-C3N4A kind of simple and effective of preparation method wet sensitive sensing material preparation method.
Summary of the invention
The present invention provides a kind of Au/g-C3N4The preparation method of humidity-sensitive material, this method include block g-C3N4System Standby, two-dimensional nano stratiform g-C3N4Preparation and Au/g-C3N4Three steps of preparation.Preferably, in Au/g-C3N4Humidity-sensitive material Preparation step in further include the steps that Au adding proportion preferably optimizes with preparation parameter, can be excellent by above-mentioned processing available Good Au/g-C3N4Humidity-sensitive material.
In view of g-C3N4With different-shape structure, 2D Au/g-C is prepared using ultrasonic stripping method3N4Humidity-sensitive material, both The deficiency that technique is cumbersome, regulation is difficult in tradition preparation is overcome, and the Au/ of the two-dimensional nano stratiform of bigger serface can be obtained g-C3N4Humidity-sensitive material provides effective preparation method to find the synthesis of simple, low cost and high wet sensitive energy material.
Wherein, g-C3N4The ratio of middle addition Au is to influence g-C3N4The key link of wet sensitive performance, therefore, including the source Au Selection and the adding proportion of Au be Au/g-C3N4Preparation first has to solve the problems, such as.By XRD the study found that observing obvious G-C3N4The peak XRD (see figure 1), do not find the peak Au since the carrying capacity of Au is too low.The Au modification of various concentration limited can change Become g-C3N4Forbidden bandwidth, forbidden bandwidth is reduced to 2.59 eV when the concentration of Au is 0.3 mmol/L, the concentration of Au is 0.5, Forbidden bandwidth is increased to 2.92 eV respectively when 0.7 mmol/L, 2.97 eV(are shown in Fig. 2).By SEM the study found that g-C3N4For The two-dimensional material of larger hole configurations is that material hole becomes smaller when the concentration of Au is 0.5 mmol/L, is intended to that sheet knot is presented Structure (see figure 3) illustrates that Au is successfully modified in g-C3N4Surface.By TEM the study found that when the concentration of Au is 0.5 mmol/L, Au/g-C3N4Lamella is relatively thin, observes that the diameter of Au is about that 2.5 nm(are shown in Fig. 4).
The Au of various concentration is to g-C3N4The wet sensitive performance of sensor has significant impact.The study found that the concentration of Au is When 0.5 mmol/L, Au/g-C3N4The sensitivity highest of moisture sensor, best test frequency are that 100Hz(is shown in Fig. 5)；Lag compared with Small, the response time is fast (see Fig. 6,7), and sensor has long-term stability (see figure 8), it is seen that such method can prepare high property The Au/g-C of energy3N4Humidity-sensitive material.
This method is verified repeatedly in an experiment, the results showed that this method is a kind of practical preparation high-performance Au/g-C3N4The preparation method of humidity-sensitive material.
Detailed description of the invention
The Au/g-C of Fig. 1 various concentration3N4XRD spectrum.The concentration of Au is respectively as follows: (1) 0 mmol/L；(2) 0.3 mmol/ L；(3) 0.5 mmol/L；(4) 0.7 mmol/L.
The Au/g-C of Fig. 2 various concentration3N4Forbidden bandwidth map.The concentration of Au is respectively as follows: (1) 0 mmol/L；(2) 0.3 mmol/L；(3) 0.5 mmol/L；(4) 0.7 mmol/L.
The Au/g-C of Fig. 3 various concentration3N4SEM figure.(a) 0 mmol/L；(b) 0.5 mmol/L.
Fig. 4 concentration is the Au/g-C of 0.5 mmol/L3N4TEM figure.(a) TEM；(b) HR-TEM.
The Au/g-C of Fig. 5 various concentration3N4Sensitivity map and frequency test figure.(a) sensitivity map；(b) frequency test Figure.
Fig. 6 concentration is the Au/g-C of 0.5 mmol/L3N4Hysteresis quality.
Fig. 7 concentration is the Au/g-C of 0.5 mmol/L3N4Response time figure.
Fig. 8 concentration is the Au/g-C of 0.5 mmol/L3N4Long-time stability figure.
Specific embodiment
A kind of preparation method of the Au/g-C3N4 humidity-sensitive material of embodiment 1
Au/g-C3N4The preparation method of humidity-sensitive material includes block g-C3N4Preparation, two-dimensional nano stratiform g-C3N4Preparation and Au modifies g-C3N4Three processes of preparation.
(1), block g-C3N4Preparation
A certain amount of urea is placed in silica crucible, with 550 DEG C of calcining 2h in Muffle furnace, it is spare to be cooled to room temperature grinding.
(2), two-dimensional nano stratiform g-C3N4Preparation
By 400mg block g-C3N4It is dissolved into the beaker containing 80mL isopropanol, is ultrasonically treated 3h, with turning for 10000r/min Speed centrifugation 4min, obtains fluffy faint yellow solid；Above-mentioned solid is dissolved in the deionized water of 100mL and is ultrasonically treated 1h, with The revolving speed of 3000r/min is centrifuged 10min, takes supernatant liquid that two-dimensional nano stratiform g-C can be obtained3N4Colloid, it is finally dry with 80 DEG C It is dry.
(3), Au/g-C3N4Preparation
Au modifies g-C3N4Preparation: by the two-dimensional nano g-C of 100mg3N4It is dissolved in 10mL, 0.3mmol/L, 0.5mmol/ respectively L, the HAuCl of 0.7mmol/L4In solution, Au/g-C is can be obtained with 80 DEG C of dryings in 80 DEG C of stirring in water bath 1h3N4Humidity-sensitive material.
Pass through above-mentioned specific embodiment, it is easier to understand the present invention.Above-described embodiment is the description of illustrative, without It should be understood as limiting the scope of the invention.

Claims (3)

1. the present invention discloses a kind of Au/g-C3N4The preparation method of humidity-sensitive material, it is characterised in that: (1) block g-C3N4Preparation: A certain amount of urea is placed in silica crucible, with 550 DEG C of calcining 2h in Muffle furnace, it is spare to be cooled to room temperature grinding；(2) two Tie up nano lamellar g-C3N4Preparation: by the block g-C of 400mg3N4It is dissolved into the beaker containing 80mL isopropanol, at ultrasound 3h is managed, 4min is centrifuged with the revolving speed of 10000r/min, obtains fluffy faint yellow solid；Above-mentioned solid is dissolved in going for 100mL It is ultrasonically treated 1h in ionized water, 10min is centrifuged with the revolving speed of 3000r/min, takes supernatant liquid that two-dimensional nano stratiform can be obtained g-C3N4Colloid, finally with 80 DEG C of dryings；(3) preparation of Au/g-C3N4: by the two-dimentional g-C of 100mg3N4It is dissolved in 10mL respectively, The HAuCl of various concentration4In solution, Au/g-C is can be obtained with 80 DEG C of dryings in 80 DEG C of stirring in water bath 1h3N4Humidity-sensitive material.
2. with according to described in claim 1, which is characterized in that the HAuCl4The concentration of solution is 0.3,0.5,0.7 mmol/ respectively L。
3. with according to described in claim 2, which is characterized in that the HAuCl4The optium concentration of solution is 0.5 mmol/L.
CN201910633834.9A 2019-07-15 2019-07-15 A kind of Au/g-C3N4The preparation method of humidity-sensitive material Pending CN110231371A (en)

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CN111189887A (en) * 2020-01-09 2020-05-22 中国石油大学(华东) Humidity sensor and manufacturing method and application thereof

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Application publication date: 20190913