CN103787290B - Based on intercalation configuration C 3n 4nanometer sheet high-performance humidity-sensitive material and preparation method - Google Patents

Based on intercalation configuration C 3n 4nanometer sheet high-performance humidity-sensitive material and preparation method Download PDF

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CN103787290B
CN103787290B CN201410022785.2A CN201410022785A CN103787290B CN 103787290 B CN103787290 B CN 103787290B CN 201410022785 A CN201410022785 A CN 201410022785A CN 103787290 B CN103787290 B CN 103787290B
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humidity
sensitive material
alkali metal
intercalation
nanometer sheet
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CN103787290A (en
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张振翼
董斌
黄金斗
苑青
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Dalian Minzu University
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Dalian Nationalities University
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Abstract

A kind of based on intercalation configuration C 3n 4nanometer sheet high-performance humidity-sensitive material, it is a kind of with C 3n 4starting material and alkali metal chloride carry out with 100:0.5 ~ 10 mass ratio reacting the alkali metal chloride intercalation C obtained 3n 4the high-performance humidity-sensitive material of nanometer sheet, its preparation method is as follows: take C 3n 4starting material and alkali metal chloride, after grinding is mixed, loads in retort furnace, rise to 450 ~ 600 DEG C with the speed of 5 ~ 20 DEG C/min, and keep 1 ~ 4 hour in this temperature; Take out material porphyrize after cooling, put into solvent supersound process 10 ~ 40 minutes; The suspension liquid centrifugation obtained by previous step, removes supernatant liquor, with 40 ~ 100 DEG C of dryings 1 ~ 8 hour in loft drier, obtains alkali metal chloride intercalation C 3n 4nanometer sheet humidity-sensitive material.This preparation method's technique is simple, easily operation, with low cost, and prepared high-performance humidity-sensitive material has the stability of highly sensitive, quick-speed response-recovery speed and excellence.

Description

Based on intercalation configuration C 3n 4nanometer sheet high-performance humidity-sensitive material and preparation method
Technical field
The present invention relates to a kind of humidity sensor material and preparation method.
Background technology:
Humidity sensor is widely used in meteorological observing and controlling, environmental monitoring, food storing, industrial production and even military field, is even in indispensable status.The core of humidity sensor is humidity sensitive material (being called for short: humidity-sensitive material), and it mainly utilizes the change of physics or chemical property before and after humidity-sensitive material adsorbed water molecule to measure the change of ambient humidity.Therefore, the kind of humidity-sensitive material, yardstick and the quality of structure to humidity sensor performance play vital effect.Along with the fast development of nanoscale science and technology, there is the appearance of many structural performance nano materials such as high-specific surface area, quantum size effect and small-size effect, bringing new opportunity for developing high-performance humidity sensor of new generation.At present, also metal oxide ceramic aspect is mainly concentrated on to the research of nanoscale humidity-sensitive material.Although metal oxide ceramic nano material has demonstrated the wet sensitive performance being better than its body phase material, its sensitivity and response-recovery speed or not ideal enough.
Summary of the invention:
The object of this invention is to provide a kind of have highly sensitive, quick-speed response-recovery speed and high stability based on intercalation configuration C 3n 4nanometer sheet high-performance humidity-sensitive material and preparation method.
The present invention is a kind of with C 3n 4starting material and alkali metal chloride carry out with 100:0.5 ~ 10 mass ratio reacting the alkali metal chloride intercalation C obtained 3n 4the high-performance humidity-sensitive material of nanometer sheet.
High-performance humidity-sensitive material preparation method of the present invention is as follows:
1) C is taken 3n 4starting material and alkali metal chloride, C of the present invention 3n 4starting material are one in urea, Dicyanodiamide or trimeric cyanamide; Alkali metal chloride is the one in lithium chloride, sodium-chlor or Repone K, and they are all anhydrous chloride crystal powders, best, lithium chloride purity>=97.0%; Sodium-chlor purity>=99.5%; Repone K purity>=99.5%.
2) by the above-mentioned material taken through grinding be mixed after, load alumina crucible add a cover after put into retort furnace, rise to 450 ~ 600 DEG C with the speed of 5 ~ 20 DEG C/min in air atmosphere, and this temperature keep 1 ~ 4 hour.
3) taking out material porphyrize after cooling, is that 0.1g/L ~ 5g/L puts into solvent supersound process 10 ~ 40 minutes according to concentration ratio.Solvent of the present invention is the one in water, methyl alcohol or ethanol.
4) suspension liquid obtained in step 3) is carried out centrifugation, remove supernatant liquor, with 40 ~ 100 DEG C of dryings 1 ~ 8 hour in loft drier, obtain alkali metal chloride intercalation C 3n 4nanometer sheet humidity-sensitive material.
Graphite-like structure C of the present invention 3n 4nanometer sheet is a kind of two-dimensional layer material with stable chemical structure, and its larger interlamellar spacing is conducive to other small-sized compound and carries out intercalation to it, thus forms two-dimentional intercalation configuration nano material.Alkali metal chloride has the features such as size is little, water-absorbent is strong.Therefore, alkali metal chloride intercalation C can be utilized 3n 4nanometer sheet, by the water absorbing properties of alkali metal chloride and C 3n 4nanometer sheet two-dimensional layered structure characteristic organically combines, thus is expected to obtain the high performance humidity-sensitive material highly sensitive, response-recovery speed is fast, stability is high and humidity hysteresis is little.
The present invention compared with prior art tool has the following advantages:
1) product of the present invention be a kind of highly sensitive, the response-recovery time is short and the performance alkali metal chloride intercalation C of excellent in stability 3n 4nanometer sheet humidity-sensitive material, it to be made in 11% ~ 95% gamut relative humidity and responding fast;
2) preparation technology of the present invention is simple, with low cost, is applicable to large-scale commercial production.
Accompanying drawing explanation
The humidity-sensitive material electron scanning micrograph figure of Fig. 1 prepared by the embodiment of the present invention 10;
The humidity-sensitive material transmission electron microscope photo figure of Fig. 2 prepared by the embodiment of the present invention 10;
The humidity-sensitive material X-ray diffraction spectrogram of Fig. 3 prepared by the embodiment of the present invention 10;
The humidity-sensitive material Fourier infrared spectrum figure of Fig. 4 prepared by the embodiment of the present invention 10;
The impedance of the humidity-sensitive material of Fig. 5 prepared by the embodiment of the present invention 10 is with relative humidity variations graphic representation;
The kinetic curve figure of the humidity-sensitive material of Fig. 6 prepared by the embodiment of the present invention 10;
The response-recovery graphic representation of the humidity-sensitive material of Fig. 7 prepared by the embodiment of the present invention 10;
Response-recovery ten cyclic curve figure of the humidity-sensitive material of Fig. 8 prepared by the embodiment of the present invention 10;
The humidity hysteresis graphic representation of the humidity-sensitive material of Fig. 9 prepared by the embodiment of the present invention 10.
Embodiment
In the mode of specific embodiment, the invention will be further described below:
Embodiment 1:
Take 10g trimeric cyanamide and 0.2g lithium chloride purity>=97.0% respectively, make the mass ratio of trimeric cyanamide and lithium chloride be 100:2; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 500 DEG C with the speed of 5 DEG C/min in air atmosphere, and keep 4 hours in this temperature; Taking out material porphyrize after cooling, is that 0.5g/L puts into ethanolic soln supersound process 10 minutes according to concentration ratio; The alcohol suspending liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 50 DEG C of dryings 6 hours in loft drier, obtains lithium chloride intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 2:
Take 10g urea and 0.1g lithium chloride purity>=97.0% respectively, make the mass ratio of urea and lithium chloride be 100:1; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 550 DEG C with the speed of 10 DEG C/min in air atmosphere, and keep 1 hour in this temperature; Taking out material porphyrize after cooling, is that 3g/L puts into water supersound process 10 minutes according to concentration ratio; The aqueous suspension that previous step is obtained carries out centrifugation, removes supernatant liquor, with 80 DEG C of dryings 8 hours in loft drier, obtains lithium chloride intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 3:
Take 10g trimeric cyanamide and 0.6g Repone K purity>=99.5% respectively, make the mass ratio of trimeric cyanamide and Repone K be 100:6; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 500 DEG C with the speed of 20 DEG C/min in air atmosphere, and keep 2 hours in this temperature; Taking out material porphyrize after cooling, is that 5g/L puts into methanol solution supersound process 10 minutes according to concentration ratio; The methyl alcohol suspension liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 50 DEG C of dryings 6 hours in loft drier, obtains Repone K intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 4:
Take 10g trimeric cyanamide and 0.4g lithium chloride purity>=97.0% respectively, make the mass ratio of trimeric cyanamide and lithium chloride be 100:4; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 550 DEG C with the speed of 10 DEG C/min in air atmosphere, and keep 2 hours in this temperature; Taking out material porphyrize after cooling, is that 1g/L puts into methanol solution supersound process 10 minutes according to concentration ratio; The methyl alcohol suspension liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 60 DEG C of dryings 4 hours in loft drier, obtains lithium chloride intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 5:
Take 10g urea and 0.05g sodium-chlor purity>=99.5% respectively, make the mass ratio of urea and sodium-chlor be 100:0.5; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 500 DEG C with the speed of 10 DEG C/min in air atmosphere, and keep 3 hours in this temperature; Taking out material porphyrize after cooling, is that 0.8g/L puts into ethanolic soln supersound process 20 minutes according to concentration ratio; The alcohol suspending liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 50 DEG C of dryings 6 hours in loft drier, obtains sodium-chlor intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 6:
Take 10g Dicyanodiamide and 0.1g sodium-chlor purity>=99.5% respectively, make the mass ratio of Dicyanodiamide and sodium-chlor be 100:1; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 450 DEG C with the speed of 10 DEG C/min in air atmosphere, and keep 1 hour in this temperature; Taking out material porphyrize after cooling, is that 0.2g/L puts into water supersound process 20 minutes according to concentration ratio; The aqueous suspension that previous step is obtained carries out centrifugation, removes supernatant liquor, with 100 DEG C of dryings 6 hours in loft drier, obtains sodium-chlor intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 7:
Take 10g urea and 0.3g sodium-chlor purity>=99.5% respectively, make the mass ratio of urea and sodium-chlor be 100:3; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 500 DEG C with the speed of 20 DEG C/min in air atmosphere, and keep 1 hour in this temperature; Taking out material porphyrize after cooling, is that 4.5g/L puts into methanol solution supersound process 30 minutes according to concentration ratio; The methyl alcohol suspension liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 50 DEG C of dryings 6 hours in loft drier, obtains sodium-chlor intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 8:
Take 10g trimeric cyanamide and 1g Repone K purity>=99.5% respectively, make the mass ratio of trimeric cyanamide and Repone K be 100:10; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 500 DEG C with the speed of 10 DEG C/min in air atmosphere, and keep 2 hours in this temperature; Taking out material porphyrize after cooling, is that 3g/L puts into ethanolic soln supersound process 10 minutes according to concentration ratio; The alcohol suspending liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 60 DEG C of dryings 4 hours in loft drier, obtains Repone K intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 9:
Take 10g Dicyanodiamide and 0.8g Repone K purity>=99.5% respectively, make the mass ratio of Dicyanodiamide and Repone K be 100:8; By the above-mentioned material taken after grinding is mixed, load after alumina crucible is added a cover and put into retort furnace, rise to 500 DEG C with the speed of 10 DEG C/min in air atmosphere, and keep 2 hours in this temperature; Taking out material porphyrize after cooling, is that 1.5g/L puts into methanol solution supersound process 10 minutes according to concentration ratio; The methyl alcohol suspension liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 50 DEG C of dryings 6 hours in loft drier, obtains Repone K intercalation C 3n 4nanometer sheet humidity-sensitive material.
Embodiment 10:
Take 10g urea and 0.3g lithium chloride purity>=97.0% respectively, make the mass ratio of urea and lithium chloride be 100:3; By the above-mentioned material taken after grinding is mixed, load alumina crucible and add a cover and put into retort furnace and rise to 550 DEG C with the speed of 20 DEG C/min in air atmosphere, and keep 2 hours in this temperature; Taking out material porphyrize after cooling, is that 0.5g/L puts into methanol solution supersound process 20 minutes according to concentration ratio; The methyl alcohol suspension liquid that previous step is obtained carries out centrifugation, removes supernatant liquor, with 60 DEG C of dryings 4 hours in loft drier, obtains lithium chloride intercalation C 3n 4the high-performance humidity-sensitive material of nanometer sheet.
As can be seen from the humidity-sensitive material electron scanning micrograph figure prepared by the present embodiment shown in Fig. 1, obtained humidity-sensitive material is the nanometer sheet of thickness at 20 ~ 30nm.As can be seen from the humidity-sensitive material transmission electron microscope photo figure prepared by the present embodiment shown in Fig. 2, obtained humidity-sensitive material is curling nanometer sheet.Can see from the humidity-sensitive material X-ray diffraction spectrogram prepared by the present embodiment shown in Fig. 3, the C caused by lithium chloride intercalation 3n 4(100) crystallographic plane diffraction peak slightly broadening, and its (002) crystallographic plane diffraction peak slightly moves to little angular direction.Can see from the humidity-sensitive material Fourier infrared spectrum figure prepared by the present embodiment shown in Fig. 4, be positioned at 1150 ~ 1650cm -1and 810cm -1c 3n 4infrared signature vibration peak, and be positioned at 2157cm -1li-N=CR 2stretching vibration peak.Can find out that the impedance of this material with humidity change obviously, spans about 3 orders of magnitude, and present good linear relationship from the impedance of the humidity-sensitive material prepared by the present embodiment shown in Fig. 5 with relative humidity variations graphic representation.As can be seen from the kinetic curve figure of the humidity-sensitive material prepared by the present embodiment shown in Fig. 6, the non-stop run under different humidity of this material, still keeps good performance.As can be seen from the response-recovery graphic representation of the humidity-sensitive material prepared by the present embodiment shown in Fig. 7, the time of response of this material from 11%RH to 95%RH is 0.9s, and the time of recovery from 95%RH to 11%RH is 1.4s.As can be seen from response-recovery ten cyclic curve figure of the humidity-sensitive material prepared by the present embodiment shown in Fig. 8, this material has high stability.As can be seen from the humidity hysteresis graphic representation of the humidity-sensitive material prepared by the present embodiment shown in Fig. 9, this material has excellent adsorption/desorption performance, can Reusability.

Claims (2)

1. one kind based on intercalation configuration C 3n 4the preparation method of nanometer sheet high-performance humidity-sensitive material, is characterized in that: with C 3n 4starting material and alkali metal chloride carry out with 100:0.5 ~ 10 mass ratio reacting the alkali metal chloride intercalation C obtained 3n 4the high-performance humidity-sensitive material of nanometer sheet, its preparation process is as follows:
1) C is taken 3n 4starting material and alkali metal chloride;
2) by the above-mentioned material taken through grinding be mixed after, load alumina crucible add a cover after put into retort furnace, rise to 450 ~ 600 DEG C with the speed of 5 ~ 20 DEG C/min in air atmosphere, and this temperature keep 1 ~ 4 hour;
3) taking out material porphyrize after cooling, is that 0.1g/L ~ 5g/L puts into solvent supersound process 10 ~ 40 minutes according to concentration ratio;
4) by step 3) in obtained suspension liquid carry out centrifugation, remove supernatant liquor, with 40 ~ 100 DEG C of dryings 1 ~ 8 hour in loft drier, obtain alkali metal chloride intercalation C 3n 4nanometer sheet humidity-sensitive material.
2. according to claim 1 based on intercalation configuration C 3n 4the preparation method of nanometer sheet high-performance humidity-sensitive material, is characterized in that: solvent is the one in water, methyl alcohol or ethanol.
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