CN106947977A - A kind of copper-based low-temp reversible thermochromic material and preparation method thereof - Google Patents

A kind of copper-based low-temp reversible thermochromic material and preparation method thereof Download PDF

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CN106947977A
CN106947977A CN201710292798.5A CN201710292798A CN106947977A CN 106947977 A CN106947977 A CN 106947977A CN 201710292798 A CN201710292798 A CN 201710292798A CN 106947977 A CN106947977 A CN 106947977A
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reversible thermochromic
thermochromic material
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吴玉程
余翠平
崔接武
王岩
张勇
舒霞
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Hefei University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/54—Contact plating, i.e. electroless electrochemical plating
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    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract

A kind of copper-based low-temp reversible thermochromic material, the low-temp reversible thermochromic material is Cu (OH)2The composites of/HKUST 1, discoloring temperature is low, Coloring Time is fast, color-recovering time is short, and its preparation method includes following steps：By high-purity Cu pieces, the cleaning of high-purity Ti piece, drying；Using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, and Cu (OH) is prepared by anodizing2Nano-wire array；By Cu (OH)2Nano-wire array, which is placed in the ethanol solution of 1,3,5 benzenetricarboxylic acids, to be soaked, and deionized water cleaning produces Cu (OH) after drying2/ HKUST 1 low-temp reversible thermochromic material.The simple ripe, low cost of the copper-based low-temp reversible thermochromic material preparation method of the present invention, and change color contrast is high, discoloring temperature is low, Coloring Time is short, color-recovering time is short, invertibity is high.

Description

A kind of copper-based low-temp reversible thermochromic material and preparation method thereof
Technical field
The present invention relates to a kind of copper-based low-temp reversible thermochromic material and preparation method thereof, belong to field of material technology.
Background technology
The phenomenon that in temperature change color change occurs for some mixtures or compound is referred to as thermochromism, possesses this and shows The material of elephant is thermochromic material.In recent years, the thermic based on inorganic, organic, liquid crystal, polymer and large biological molecule etc. Off-color material causes increasing concern, and being widely used in national defence, military affairs, anti-fake mark, daily decoration etc., each is led Domain, such as daily-use electrical appliance temperature alarm, mechanical devices measuring temperature distribution.The colourshifting process of thermochromic material is a heat The process of physics or heat induced chemical change is caused, mainly including crystal transfer, the gain and loss crystallization water, electro transfer and coordination geometry structure Type change etc., spectral quality of the material in visible-range is changed in change procedure, therefore shows changing for color Become phenomenon.Thermochromic material can be divided into polytype, according to discoloring temperature scope, can be divided into low temperature (T<100 DEG C) thermic Off-color material, middle temperature (100<T<600 DEG C) thermochromic material, low temperature (T>600 DEG C) thermochromic material；From thermodynamics For, thermochromic material can be divided into Reversible Thermochromic Materials and irreversible thermochromic material, wherein, reversible thermochromic Material reaches that the change of color can occur for discoloring temperature, can still recover original color after cooling, and it has memory for color Function, can be with Reusability.Since the eighties, thermochromic material gradually develops in terms of middle low temperature, reversible two.In view of Current part thermochromic material discoloring temperature is high, small discoloration aberration, color-recovering time length, it is irreversible the shortcomings of, such as how it is low into Originally, prepared by simple maturation process to become color contrast height, the thermochromic material that discoloring temperature is low, color-recovering time is short, invertibity is high, Possess and its important actual application value.
The characteristics of due to having both organic compound and inorganic compound, metal-organic framework (MOFs) has been increasingly becoming newly The function supramolecular materials of type, be widely used in lighting, energy storage, the field such as small molecule absorption and separation, catalysis and sensing. Research worker is prepared for a series of MOFs bases thermochromic materials, the metal center when colourshifting process is mainly due to heating Coordination environment is changed, however, the discoloring temperature of part MOFs base thermochromic materials is high, colourshifting process is irreversible, because This limits its further application.In addition, MOFs is substantially based on dusty material, the report for rarely having MOFs Ordered Materials. In the recent period, PaoloFalcaro and its partner orderly CuMOF preparation in NatureMaterials magazine rans, with Cu (OH)2For presoma, by the reaction with organic crosslinking ligand, orderly MOF materials are successfully prepared.Based on this, the present invention with Cu (OH) prepared by anodic oxidation2Nano-wire array is presoma, and 1,3,5- benzenetricarboxylic acid is organic crosslinking ligand, is prepared for low Warm Reversible Thermochromic Materials, and the material discoloration acumen, discoloring temperature low (40 DEG C or so), color-recovering time short (within 5s), Invertibity is high, possesses high application potential.
The content of the invention：
It is an object of the invention to：A kind of copper-based low-temp reversible thermochromic material and preparation method thereof, the copper are provided The simple ripe, low cost of base low-temp reversible thermochromic material preparation technology, and change color contrast is high, discoloring temperature is low, secondary color Time is short, invertibity is high.
To achieve these goals, the present invention provides following technical scheme：
A kind of copper-based low-temp reversible thermochromic material, the low-temp reversible thermochromic material is Cu (OH)2/HKUST-1 Composite, discoloring temperature is low, Coloring Time is short, color-recovering time is short.
Preferably, described discoloring temperature is 35~45 DEG C, and Coloring Time is within 5s, and color-recovering time is within 5s.
Further, a kind of preparation method of copper-based low-temp reversible thermochromic material, including following steps：
(1) by high-purity Cu pieces, the cleaning of high-purity Ti piece, drying；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, passes through anode Oxidizing process prepares Cu (OH)2Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array is placed in the ethanol solution of 1,3,5- benzenetricarboxylic acids Immersion, 5~80 DEG C of reaction temperature, deionized water cleaning produces Cu (OH) after drying2/ HKUST-1 low-temp reversible thermochromism Material.
Preferably, a kind of preparation method of copper-based low-temp reversible thermochromic material, including following steps：
(1) by high-purity Cu pieces, high-purity Ti piece successively in acetone, absolute ethyl alcohol and deionized water respectively ultrasound 5~ 30min, to remove the greasy dirt and oxide on surface, is then dried stand-by in an oven；
(2) using high-purity Cu pieces after cleaning, drying as anode, high-purity Ti piece after cleaning, drying is negative electrode, it is placed in 1~ 3mol/LKOH aqueous solution Anodic Oxidation reacts 5~30min, 1~5mA/cm of current density2, 5~20 DEG C of reaction temperature, acquisition Cu(OH)2Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array is placed in the nothing of 5~100mmol/L1,3,5- benzenetricarboxylic acids In hydrous ethanol solution, 5s~5h is soaked, 5~80 DEG C of reaction temperature, deionized water cleaning produces Cu (OH) after drying2/HKUST- 1 low-temp reversible thermochromic material.
Preferably, described high-purity Cu pieces are the Cu pieces that purity is more than 99.9%, and high-purity Ti piece is that purity is more than 99.7% Ti pieces.
Preferably, by adjusting Cu (OH)2Leaching of the nano-wire array in the ethanol solution of 1,3,5- benzenetricarboxylic acids The bubble time, realize Cu (OH)2Portions turn or completely transformation of the nano-wire array to HKUST-1.
Preferably, as Cu (OH)2Soak time of the nano-wire array in the ethanol solution of 1,3,5- benzenetricarboxylic acids During less than 2h, Cu (OH)2Portions turn from nano-wire array to HKUST-1；As Cu (OH)2Nano-wire array is in 1,3,5- benzene three When soak time in the ethanol solution of formic acid is more than 2h, Cu (OH)2Complete transformation from nano-wire array to HKUST-1.
The beneficial effects of the present invention are：The copper-based low-temp reversible thermochromic material preparation method of the present invention it is simple into Ripe, low cost, and change color contrast is high, discoloring temperature is low, Coloring Time is short, color-recovering time is short, invertibity is high, operation is easy to control System.
Brief description of the drawings
Fig. 1 is the Cu (OH) that embodiment 1 is obtained2The FESEM photos of nano-wire array；
Fig. 2 is the Cu (OH) that embodiment 2 is obtained2The FESEM photos of/HKUST-1 low-temp reversible thermochromic materials；
Fig. 3 is the Cu (OH) that embodiment 3 is obtained2The FESEM photos of/HKUST-1 low-temp reversible thermochromic materials；
Fig. 4 is the Cu (OH) that embodiment 4 is obtained2The FESEM photos of/HKUST-1 low-temp reversible thermochromic materials；
Fig. 5 is the Cu (OH) that embodiment 5 is obtained2The FESEM photos of/HKUST-1 low-temp reversible thermochromic materials；
Fig. 6 is the Cu (OH) that embodiment 1 is obtained2The XRD spectrum of nano-wire array；
Fig. 7 is the Cu (OH) that embodiment 5 is obtained2The XRD spectrum of/HKUST-1 low-temp reversible thermochromic materials.
Specific embodiment
To enable the above objects, features and advantages of the present invention more obvious understandable, below in conjunction with the accompanying drawings to the present invention Embodiment be described in detail.Many details are elaborated in the following description to fully understand this hair It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not Similar improvement is done in the case of running counter to intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Embodiment 1
Cu(OH)2The preparation method of nano-wire array, including following steps：
(1) by purity be more than 99.9% Cu pieces, purity be more than 99.7% Ti pieces successively acetone, absolute ethyl alcohol and In deionized water distinguish ultrasound 10min, with remove dried in the greasy dirt and oxide on surface, baking oven it is stand-by；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, is placed in 2mol/LKOH aqueous solution Anodic Oxidation reacts 10min, current density 2.5mA/cm2, 10 DEG C of reaction temperature, acquisition Cu (OH)2 Nano-wire array.
Embodiment 2
A kind of preparation method of copper-based low-temp reversible thermochromic material, including following steps：
(1) by purity be more than 99.9% Cu pieces, purity be more than 99.7% Ti pieces successively acetone, absolute ethyl alcohol and In deionized water distinguish ultrasound 10min, with remove dried in the greasy dirt and oxide on surface, baking oven it is stand-by；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, is placed in 2mol/LKOH aqueous solution Anodic Oxidation reacts 10min, current density 2.5mA/cm2, 10 DEG C of reaction temperature, acquisition Cu (OH)2 Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array is placed in the anhydrous second of 50mmol/L1,3,5- benzenetricarboxylic acids In alcoholic solution, 5min is soaked, 25 DEG C of reaction temperature, deionized water cleaning obtains Cu (OH) after drying2/ HKUST-1 low temperature Reversible Thermochromic Materials.
Embodiment 3
A kind of preparation method of copper-based low-temp reversible thermochromic material, including following steps：
(1) by purity be more than 99.9% Cu pieces, purity be more than 99.7% Ti pieces successively acetone, absolute ethyl alcohol and In deionized water distinguish ultrasound 10min, with remove dried in the greasy dirt and oxide on surface, baking oven it is stand-by；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, is placed in 2mol/LKOH aqueous solution Anodic Oxidation reacts 10min, current density 2.5mA/cm2, 10 DEG C of reaction temperature, acquisition Cu (OH)2 Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array is placed in the anhydrous second of 50mmol/L1,3,5- benzenetricarboxylic acids In alcoholic solution, 10min is soaked, 25 DEG C of reaction temperature, deionized water cleaning obtains Cu (OH) after drying2/ HKUST-1's is low Warm Reversible Thermochromic Materials.
Embodiment 4
A kind of preparation method of copper-based low-temp reversible thermochromic material, including following steps：
(1) by purity be more than 99.9% Cu pieces, purity be more than 99.7% Ti pieces successively acetone, absolute ethyl alcohol and In deionized water distinguish ultrasound 10min, with remove dried in the greasy dirt and oxide on surface, baking oven it is stand-by；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, is placed in 2mol/LKOH aqueous solution Anodic Oxidation reacts 10min, current density 2.5mA/cm2, 10 DEG C of reaction temperature, acquisition Cu (OH)2 Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array is placed in the anhydrous second of 50mmol/L1,3,5- benzenetricarboxylic acids In alcoholic solution, 30min is soaked, 25 DEG C of reaction temperature, deionized water cleaning obtains Cu (OH) after drying2/ HKUST-1's is low Warm Reversible Thermochromic Materials.
Embodiment 5
A kind of preparation method of copper-based low-temp reversible thermochromic material, including following steps：
(1) by purity be more than 99.9% Cu pieces, purity be more than 99.7% Ti pieces successively acetone, absolute ethyl alcohol and In deionized water distinguish ultrasound 10min, with remove dried in the greasy dirt and oxide on surface, baking oven it is stand-by；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, is placed in 2mol/LKOH aqueous solution Anodic Oxidation reacts 10min, current density 2.5mA/cm2, 10 DEG C of reaction temperature, acquisition Cu (OH)2 Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array is placed in the anhydrous second of 50mmol/L1,3,5- benzenetricarboxylic acids In alcoholic solution, 2h is soaked, 25 DEG C of reaction temperature, deionized water cleaning obtains Cu (OH) after drying2/ HKUST-1 low temperature can Inverse thermochromic material.
Embodiment 6
The performance of copper-based low-temp reversible thermochromic material obtained by test above-described embodiment, by the Cu of the gained of embodiment 4 (OH)2/ HKUST-1, which is placed on heating magnetic stirring apparatus table top, to be heated, and is studied its discoloring temperature, Coloring Time, is answered Color time and invertibity etc..As a result show, by the Cu (OH) of the gained of embodiment 42/ HKUST-1 is placed in 40 DEG C of heating magnetic force After agitator table top, the Cu (OH) of the gained of embodiment 4 within 5s2/ HKUST-1 is changed into navy blue from original light green, leaves Original color can be still returned in 40 DEG C of heating magnetic stirring apparatus table top 5s, and be can be repeated several times, its discoloration is embodied Temperature is low, become the advantages of color contrast is high, Coloring Time is fast, color-recovering time is short, invertibity is high.
With reference to accompanying drawing, the present invention is further described as follows：
The copper-based low-temp reversible thermochromic material presoma of the present invention is Cu (OH)2Nano-wire array, its pattern and X are penetrated Ray diffraction diagram is composed as a shown in Figure 6.It can be seen that from Fig. 2~4：Compared to presoma Cu (OH) in Fig. 12The shape of nano-wire array Looks, soak by the ethanol solution short time of 1,3,5- benzenetricarboxylic acid and (are less than 2h), Cu (OH)2Nano-wire array can part It is changed into HKUST-1, nano wire remains to be retained, has obtained Cu (OH)2/ HKUST-1 composite construction；Can be with from Fig. 5 Find out：When soak time is more than or equal to 2h, Cu (OH)2Nano-wire array is fully converted to HKUST-1.In addition, from Fig. 7 X X ray diffraction collection of illustrative plates can be seen that：HKUST-1 successful preparation.

Claims (7)

1. a kind of copper-based low-temp reversible thermochromic material, it is characterised in that the low-temp reversible thermochromic material is Cu (OH)2/ HKUST-1 composites, discoloring temperature is low, Coloring Time is short, color-recovering time is short.
2. a kind of copper-based low-temp reversible thermochromic material according to claim 1, it is characterised in that described color temperature Spend for 35~45 DEG C, Coloring Time is within 5s, and color-recovering time is within 5s.
3. a kind of preparation method of copper-based low-temp reversible thermochromic material, it is characterised in that including following steps：
(1) by high-purity Cu pieces, the cleaning of high-purity Ti piece, drying；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, passes through anodic oxidation Method prepares Cu (OH)2Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array, which is placed in the ethanol solution of 1,3,5- benzenetricarboxylic acids, to be soaked, 5~80 DEG C of reaction temperature, deionized water cleaning, Cu (OH) is produced after drying2/ HKUST-1 low-temp reversible thermochromic material.
4. a kind of preparation method of copper-based low-temp reversible thermochromic material according to claim 3, it is characterised in that bag Include following steps：
(1) high-purity Cu pieces, high-purity Ti piece are distinguished into 5~30min of ultrasound in acetone, absolute ethyl alcohol and deionized water successively, To remove the greasy dirt and oxide on surface, then dry in an oven stand-by；
(2) using high-purity Cu pieces after cleaning, drying as anode, the high-purity Ti piece after cleaning, drying is negative electrode, is placed in 1~3mol/ LKOH aqueous solution Anodic Oxidation reacts 5~30min, 1~5mA/cm of current density2, 5~20 DEG C of reaction temperature, acquisition Cu (OH)2Nano-wire array；
(3) Cu (OH) for obtaining step (2)2Nano-wire array is placed in the anhydrous second of 5~100mmol/L1,3,5- benzenetricarboxylic acids In alcoholic solution, 5s~5h is soaked, 5~80 DEG C of reaction temperature, deionized water cleaning produces Cu (OH) after drying2/ HKUST-1's Low-temp reversible thermochromic material.
5. a kind of preparation method of copper-based low-temp reversible thermochromic material according to claim 4, it is characterised in that institute The high-purity Cu pieces stated are the Cu pieces that purity is more than 99.9%, and high-purity Ti piece is the Ti pieces that purity is more than 99.7%.
6. the preparation method of a kind of copper-based low-temp reversible thermochromic material according to claim 3, it is characterised in that logical Overregulate Cu (OH)2Soak time of the nano-wire array in the ethanol solution of 1,3,5- benzenetricarboxylic acid, realizes Cu (OH)2 Portions turn or completely transformation of the nano-wire array to HKUST-1.
7. a kind of preparation method of copper-based low-temp reversible thermochromic material according to claim 6, it is characterised in that when Cu(OH)2When soak time of the nano-wire array in the ethanol solution of 1,3,5- benzenetricarboxylic acid is less than 2h, Cu (OH)2Receive Portions turn from nanowire arrays to HKUST-1；As Cu (OH)2Ethanol solution of the nano-wire array in 1,3,5- benzenetricarboxylic acids In soak time be more than 2h when, Cu (OH)2Complete transformation from nano-wire array to HKUST-1.
CN201710292798.5A 2017-04-28 2017-04-28 A kind of copper-based low-temp reversible thermochromic material and preparation method thereof Pending CN106947977A (en)

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CN109293940A (en) * 2018-11-22 2019-02-01 苏州大学 One-dimensional HKUST-1 nanobelt and preparation method thereof
CN109679111A (en) * 2019-01-14 2019-04-26 济南大学 A kind of preparation method of HKUST-1 complex nanoparticle

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Application publication date: 20170714