CN113340948A - Preparation method of high-response humidity sensor based on halogenated perovskite microcrystal and product thereof - Google Patents
Preparation method of high-response humidity sensor based on halogenated perovskite microcrystal and product thereof Download PDFInfo
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- CN113340948A CN113340948A CN202110642013.9A CN202110642013A CN113340948A CN 113340948 A CN113340948 A CN 113340948A CN 202110642013 A CN202110642013 A CN 202110642013A CN 113340948 A CN113340948 A CN 113340948A
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- 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
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Abstract
The invention relates to a preparation method of a high-response humidity sensor based on halogenated perovskite microcrystal and a product thereof, belonging to the technical field of semiconductor sensor preparation. The invention provides a preparation method of a high-response humidity sensor based on halogenated perovskite microcrystal, which mainly adopts oleylamine passivated Cs3Cu2Br5Perovskite microcrystalline or octylamine passivated Cs3Cu2Br5The perovskite microcrystal is coated on the interdigital electrode to form the sensor, and the prepared sensor has the characteristics of high responsiveness and good detection stability. The sensitive material adopted in the preparation method is nontoxic, and the sensitivity of the material is improved by a surface passivation technology in the preparation process; meanwhile, the preparation process is simple to operate, low in preparation cost and suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of semiconductor sensor preparation, and relates to a preparation method of a high-response humidity sensor based on halogenated perovskite microcrystal and a product thereof.
Background
Humidity is an indispensable physical quantity affecting industrial production, agricultural planting, medical diagnosis and treatment. The impedance type humidity sensor has the characteristics of miniaturization, integration, low cost and the like, and is suitable for being used as a biological detector. Porous perovskite thin films and bulk materials are considered the first detection materials for the preparation of resistive moisture traps. Today, most of the research on sensitive materials for humidity sensing is focused on oxide perovskites; however, in rapid practical applications, time measurement systems such as breath monitoring are hampered due to the relatively long response time of oxide perovskite humidity sensors. In addition, the synthesis of oxide perovskites requires high temperature calcination, which places higher demands on production costs and manufacturing processes.
Therefore, there is a need to develop a new method for preparing a humidity sensor with high sensitivity and low cost. Halogenated perovskites have received much attention for their excellent optoelectronic properties, and are suitable for sensing because of their sensitive surface properties and solution processable characteristics. However, the inherent instability of conventional organohalide perovskite lead and the toxicity of lead limit its application and commercial exploitation. Lead-free halide perovskite Cs due to excellent stability and low cost3Cu2Br5Has great application potential in the field of perovskite sensing. So far, based on Cs3Cu2Br5Humidity sensors for perovskites have not been publicly reported.
Based on the above background, use of Cs3Cu2Br5The high-response impedance type humidity sensor developed by the perovskite microcrystal particles and convenient and fast in preparation method is beneficial to promoting the progress and the industrialized development of the semiconductor sensing technology.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a humidity sensor based on halogenated perovskite crystallites; it is a further object of the present invention to provide a highly responsive humidity sensor based on perovskite crystallites.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a preparation method of a high-response humidity sensor based on halogenated perovskite microcrystal comprises the following specific steps:
deactivating Cs with oleylamine3Cu2Br5Perovskite microcrystalline or octylammonium passivated Cs3Cu2Br5And mixing the perovskite microcrystals, dispersing the perovskite microcrystals into n-hexane to form dispersion liquid, repeatedly dripping the dispersion liquid on the interdigital electrode to form a coating layer with the thickness of 4-5 mu m, annealing at 60 ℃ for 30min, and packaging by using a chip protection shell.
Preferably, said oleylamine deactivated Cs3Cu2Br5The perovskite microcrystal is prepared according to the following method:
mixing Octadecene (ODE) and CuBr, stirring for 1h at 120-150 ℃ in a nitrogen atmosphere, adding oleic acid and oleylamine, raising the reaction temperature to 140 ℃ along with the dissolution of the CuBr, adding cesium oleate precursor (OA-Cs) for reacting for 5s, cooling to room temperature with ice water, centrifuging at 9000rpm for 5min, washing to obtain precipitate, continuously dispersing the precipitate in n-hexane for secondary washing to obtain the oleylamine passivated Cs3Cu2Br5Perovskite crystallites.
More preferably, the volume-to-mass ratio of the Octadecene (ODE) to the CuBr is 10:44.5, ml: mg.
Further preferably, the volume ratio of Octadecene (ODE), oleic acid and oleylamine is 10:0.5: 0.5.
Further preferably, the volume ratio of Octadecene (ODE) and cesium oleate precursor (OA-Cs) is 10: 3.
Preferably, the octylammonium passivated Cs3Cu2Br5The perovskite microcrystal is prepared according to the following method:
mixing Octadecene (ODE) and CuBr, stirring for 1h at 120 ℃ in a nitrogen atmosphere, adding oleic acid and octylammonium, raising the reaction temperature to 140 ℃ along with the dissolution of CuBr, adding an oleic acid cesium precursor (OA-Cs) for reaction for 5s, cooling to room temperature by using ice water, centrifuging at 9000rpm for 5min, washing to obtain a precipitate, continuously dispersing the precipitate in n-hexane for secondary washing to obtain the octylamine passivated Cs3Cu2Br5Perovskite crystallites.
More preferably, the volume-to-mass ratio of the Octadecene (ODE) to the CuBr is 10:44.5, ml: mg.
Further preferably, the volume ratio of Octadecene (ODE), oleic acid and octylamine is 10:0.5: 0.5.
Further preferably, the volume ratio of Octadecene (ODE) and cesium oleate precursor (OA-Cs) is 10: 3.
Preferably, the cesium oleate precursor (OA-Cs) is prepared as follows:
mixing Cs2CO3Octadecene (ODE) and Oleic Acid (OA) are mixed according to the mass-volume ratio of 305:15:0.95, mg: ml: ml, and stirred for 1h at the temperature of 120 ℃ in a nitrogen atmosphere.
Preferably, the inter-finger distance of the interdigital electrodes is 200-500 nm.
Preferably, the annealing treatment is annealing treatment at 60 ℃ for 30 min.
Preferably, said oleylamine deactivated Cs3Cu2Br5The mass-volume ratio of the perovskite microcrystal to the n-hexane is 30:3, mg: ml.
Preferably, the octylammonium passivated Cs3Cu2Br5The mass-volume ratio of the perovskite microcrystal to the n-hexane is 30:3, mg: ml.
2. The high-response humidity sensor based on the halogenated perovskite microcrystal is prepared according to the preparation method.
The invention has the beneficial effects that: the invention provides a preparation method of a high-response humidity sensor based on halogenated perovskite microcrystal, which mainly adopts oleylamine passivated Cs3Cu2Br5Perovskite crystallites and octylamine passivated Cs3Cu2Br5The sensor is formed by coating the mixture formed by the perovskite microcrystal on the interdigital electrode, and the prepared sensor has the characteristics of high responsiveness and good detection stability. The sensitive material adopted in the preparation method is nontoxic, and the sensitivity of the material is improved by a surface passivation technology in the preparation process; meanwhile, the preparation process is simple to operate, low in preparation cost and suitable for industrial production.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 shows passivated Cs prepared in the examples3Cu2Br5A structure diagram of perovskite crystallites;
FIG. 2 shows passivated Cs prepared in example 1(OLA) and example 2(OAm)3Cu2Br5SEM images of perovskite crystallites;
FIG. 3 shows passivated Cs prepared in example 1(OLA) and example 2(OAm)3Cu2Br5X-ray diffraction spectroscopy of perovskite crystallites;
FIG. 4 is the result of elemental analysis on the coating layer (where a and b are coating layers in OLA, and c and d are coating layers in OAm);
FIG. 5 is a graph of the dynamic response of various sensors;
FIG. 6 is a hysteresis characteristic curve for different sensors;
FIG. 7 shows the results of measuring the contact angle of the sensors prepared in examples 1(a) and 2 (b);
fig. 8 is a result of a long-term stability test of the sensors prepared in example 1(a) and example 2 (b).
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.
Wherein the showings are for the purpose of illustrating the invention only and not for the purpose of limiting the same, and in which there is shown by way of illustration only and not in the drawings in which there is no intention to limit the invention thereto; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The chemicals used in the following examples are as follows:
cesium carbonate (Cs)2CO399.95%), cuprous bromide (CuBr, 99%), 1-octadecene (ODE, 90%), oleylamine (OAm,>70%), octylamine (OLA,. gtoreq.99%), oleic acid (OA, 90%), n-hexane, the above chemicals need no further purification.
Example 1
The high-response humidity sensor based on the halogenated perovskite microcrystal comprises the following steps:
(1) preparation of OA-Cs precursor: 305mg of Cs2CO3Adding 15ml of ODE (octadecene) and 0.95ml of OA (oleic acid) into a 100ml three-neck flask, uniformly mixing, and stirring for 1h at the temperature of 120 ℃ in a nitrogen atmosphere to obtain an OA-Cs precursor;
(2) preparation of oleylamine deactivated Cs3Cu2Br5Perovskite crystallites: adding 10ml of ODE (octadecene) and 44.5mg of CuBr into a 100ml three-neck flask, mixing, stirring for 1h at 120 ℃ in a nitrogen atmosphere, adding 0.5ml of oleic acid and 0.5ml of oleylamine, raising the reaction temperature to 140 ℃ along with the dissolution of the CuBr, adding 3ml of OA-Cs precursor, reacting for 5s, cooling to room temperature with ice water, centrifuging at 9000rpm for 5min, washing to obtain precipitate, continuously dispersing the precipitate in n-hexane for secondary washing to obtain the oleylamine passivated Cs3Cu2Br5Perovskite crystallites (OLA);
(4) 30mg of oleylamine deactivated Cs prepared in the above step (2)3Cu2Br5And dispersing the perovskite microcrystal in 3ml of n-hexane to form a dispersion liquid, coating the dispersion liquid on an interdigital electrode with a finger spacing of 200nm in a dripping mode (repeated dripping can be performed for many times) to form a coating layer with the thickness of 4.5 mu m, annealing at 60 ℃ for 30min, and packaging with a chip protective shell to obtain the high-response humidity sensor (OLA sensor) based on the halogenated perovskite microcrystal.
Example 2
The high-response humidity sensor based on the halogenated perovskite microcrystal comprises the following steps:
(1) preparation of OA-Cs precursor: 305mg of Cs2CO3Adding 15ml of ODE (octadecene) and 0.95ml of OA (oleic acid) into a 100ml three-neck flask, uniformly mixing, and stirring for 1h at the temperature of 120 ℃ in a nitrogen atmosphere to obtain an OA-Cs precursor;
(2) preparation of octylamine passivated Cs3Cu2Br5Perovskite crystallites: adding 10ml of ODE (octadecene) and 44.5mg of CuBr into a 100ml three-neck flask, mixing, stirring for 1h at 120 ℃ in a nitrogen atmosphere, adding 0.5ml of oleic acid and 0.5ml of octylammonium, raising the reaction temperature to 140 ℃ along with the dissolution of the CuBr, adding 3ml of OA-Cs precursor, reacting for 5s, cooling to room temperature with ice water, centrifuging at 9000rpm for 5min, washing to obtain precipitate, continuously dispersing the precipitate in n-hexane for secondary washing to obtain octylamine passivated Cs3Cu2Br5Perovskite crystallites (OAm);
(3) deactivating the oleylamine prepared in step (2) above with Cs3Cu2Br5Perovskite microcrystals and octylamine passivated Cs prepared in step (3) above3Cu2Br5Mixing perovskite microcrystals, dispersing the perovskite microcrystals into 3ml of n-hexane to form dispersion, coating the dispersion on interdigital electrodes with the finger spacing of 200nm in a dripping mode to form a coating layer with the thickness of 4.1 mu m, annealing at 60 ℃ for 30min, and packaging with a chip protective shell to obtain the high-response humidity sensor (O) based on halogenated perovskite microcrystalsAm sensor).
Wherein the finger pitch of the interdigital electrodes used in examples 1 and 2 can be selected from 200 to 500 μm, and the thickness of the coating layer formed during the coating of the dispersion can be limited to 4 to 5 μm, all of which enable the production of humidity sensors having a composite performance requirement.
Example 3
The performance of the high-response humidity sensor based on halogenated perovskite microcrystals prepared in example 1 was tested, and the results are as follows:
passivated Cs prepared in the examples3Cu2Br5The structure of the perovskite crystallites is shown in fig. 1, the SEM image thereof is shown in fig. 2 (wherein the product prepared in example 1 is OLA and the product prepared in example 1 is OAm), the X-ray diffraction spectrum is shown in fig. 3, and the elemental analysis on the coating layer is shown in fig. 4 (wherein a and b are the coating layers in OLA and c and d are the coating layers in OAm). It can be seen that the product formed by the preparation method of the present invention is indeed two ligand-inactivated Cs3Cu2Br5Perovskite crystallites.
The dynamic response test of the sensors prepared in example 1 and example 2 is shown in fig. 5, which illustrates the two ligand-passivated Cs prepared according to the present invention3Cu2Br5Perovskite crystallites (OLA sensors and OAm sensors) have the ability to detect different relative humidities.
Hysteresis characteristics of the sensors prepared in examples 1 and 2 are shown in FIG. 6, which illustrates Cs passivated based on two ligands3Cu2Br5Both the moisture sensors (OLA sensor and OAm sensor) of the perovskite crystallites have good stability.
The results of detecting the contact angles of the sensors prepared in examples 1 and 2 are shown in FIG. 7, wherein a and b are the sensors of examples 1 and 2, respectively, and the results show that OLA-passivated Cs prepared in example 13Cu2Br5The perovskite crystallites had OAm passivated Cs than the perovskite crystallites prepared in example 23Cu2Br5The perovskite crystallites are more hydrophilic.
The results of the long term stability tests of the sensors prepared in examples 1 and 2 are shown in FIG. 8, where a and b are the sensors of examples 1 and 2, respectively, and the results demonstrate two ligand-passivated Cs3Cu2Br5Humidity sensors of perovskite crystallites (OLA and OAm) have good long-term stability.
In summary, the invention provides a preparation method of a high-response humidity sensor based on halogenated perovskite microcrystal, and the Cs mainly adopts oleylamine passivated Cs3Cu2Br5Perovskite crystallites and octylamine passivated Cs3Cu2Br5The sensor is formed by coating the mixture formed by the perovskite microcrystal on the interdigital electrode, and the prepared sensor has the characteristics of high responsiveness and good detection stability. The sensitive material adopted in the preparation method is nontoxic, and the sensitivity of the material is improved by a surface passivation technology in the preparation process; meanwhile, the preparation process is simple to operate, low in preparation cost and suitable for industrial production.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a high-response humidity sensor based on halogenated perovskite microcrystal is characterized by comprising the following steps:
deactivating Cs with oleylamine3Cu2Br5Perovskite microcrystalline or octylammonium passivated Cs3Cu2Br5Mixing perovskite microcrystals, dispersing the mixture into n-hexane to form dispersion liquid, repeatedly dripping the dispersion liquid on an interdigital electrode to form a coating layer with the thickness of 4-5 mu m, annealing at 60 ℃ for 30min, and then processing by using a chipAnd (5) packaging the protective shell.
2. The method of claim 1, wherein the oleylamine deactivated Cs3Cu2Br5The perovskite microcrystal is prepared according to the following method:
mixing octadecene and CuBr, stirring for 1h at 120-150 ℃ in a nitrogen atmosphere, adding oleic acid and oleylamine, raising the reaction temperature to 140 ℃ along with the dissolution of the CuBr, adding a cesium oleate precursor for reaction for 5s, cooling to room temperature by using ice water, centrifuging at 9000rpm for 5min, washing to obtain a precipitate, continuously dispersing the precipitate in n-hexane for secondary washing to obtain the oleylamine passivated Cs3Cu2Br5Perovskite crystallites.
3. The preparation method according to claim 2, wherein the volume-to-mass ratio of octadecene to CuBr is 10:44.5, ml: mg;
the volume ratio of the octadecene to the oleic acid to the oleylamine is 10:0.5: 0.5;
the volume ratio of the octadecene to the cesium oleate precursor is 10: 3.
4. The method of claim 1, wherein the octylammonium passivated Cs3Cu2Br5The perovskite microcrystal is prepared according to the following method:
mixing octadecene and CuBr, stirring for 1h at 120 ℃ in a nitrogen atmosphere, adding oleic acid and octylammonium, raising the reaction temperature to 140 ℃ along with the dissolution of CuBr, adding a cesium oleate precursor for reaction for 5s, cooling to room temperature by using ice water, centrifuging at 9000rpm for 5min, washing to obtain a precipitate, continuously dispersing the precipitate in n-hexane for secondary washing to obtain the octylamine passivated Cs3Cu2Br5Perovskite crystallites.
5. The preparation method according to claim 4, wherein the volume-to-mass ratio of octadecene to CuBr is 10:44.5, ml: mg;
the volume ratio of octadecene to oleic acid to octylamine is 10:0.5: 0.5;
the volume ratio of the octadecene to the cesium oleate precursor is 10: 3.
6. The method according to any one of claims 2 to 5, wherein the cesium oleate precursor is prepared by a method comprising:
mixing Cs2CO3Octadecene and oleic acid were mixed according to a mass-to-volume ratio of 305:15:0.95, mg: ml: ml, and stirred at 120 ℃ under a nitrogen atmosphere for 1 hour.
7. The method according to claim 1, wherein the inter-finger distance between the interdigital electrodes is 200-500 nm.
8. The production method according to claim 1, wherein the annealing treatment is an annealing treatment at 60 ℃ for 30 min.
9. The method of claim 1, wherein the oleylamine deactivated Cs3Cu2Br5The mass-volume ratio of the perovskite microcrystal to the normal hexane is 30:3, mg: ml;
the octylammonium passivated Cs3Cu2Br5The mass-volume ratio of the perovskite microcrystal to the n-hexane is 30:3, mg: ml.
10. The halogenated perovskite microcrystal-based high-response humidity sensor prepared by the preparation method according to any one of claims 1 to 8.
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