CN117385463A - Method for realizing giant expansion material, giant expansion material and application - Google Patents
Method for realizing giant expansion material, giant expansion material and application Download PDFInfo
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- CN117385463A CN117385463A CN202311524621.5A CN202311524621A CN117385463A CN 117385463 A CN117385463 A CN 117385463A CN 202311524621 A CN202311524621 A CN 202311524621A CN 117385463 A CN117385463 A CN 117385463A
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- Prior art keywords
- lithium metaborate
- phase
- giant
- tetragonal
- expansion material
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- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 claims abstract description 43
- 230000008859 change Effects 0.000 claims abstract description 40
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000013078 crystal Substances 0.000 claims description 18
- 230000007704 transition Effects 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 3
- 239000010432 diamond Substances 0.000 abstract description 10
- 230000009466 transformation Effects 0.000 abstract description 10
- 229910003460 diamond Inorganic materials 0.000 abstract description 8
- 229910052582 BN Inorganic materials 0.000 abstract description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 125000003010 ionic group Chemical group 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 150000002894 organic compounds Chemical class 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- 239000011147 inorganic material Substances 0.000 description 4
- 230000035772 mutation Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
Abstract
According to the giant expansion material and the realization method thereof, tetragonal phase lithium metaborate is annealed at the temperature of 600-740 ℃, the tetragonal phase lithium metaborate is changed in shape, the structure of the tetragonal phase lithium metaborate provided by the application has atomic distribution similar to diamond and cubic boron nitride, structural gaps are occupied by ionic groups, the structure has compactness, the structural internal stress can be provided in the heating process to force atoms to be redistributed, the tetragonal structure lithium metaborate structure causes huge volume expansion before and after phase change, the structural transformation is initiated and can be directly reflected to macroscopic size, the phase change condition is mild, the material can be suitable for occasions of practical application, and the function of a thermal switch can be better realized through larger macroscopic shape change.
Description
Technical Field
The application relates to the technical field of thermal expansion, in particular to a realization method of a giant expansion material lithium metaborate, a giant expansion material and application.
Background
Thermal expansion phenomenon is common in nature. The temperature influences the change of the crystal size, wherein the lattice parameter of one type of material can be suddenly changed under the action of the temperature, and the change can be transferred to the macroscopic structure through the periodicity of the lattice, so that the macroscopic shape is finally deformed severely. The material with huge shape change under the temperature stimulus has potential application value in the field of thermal switches.
The bulk crystals of crystalline organic compounds having giant expansion properties often accompany large macroscopic shape changes during the temperature rise. By entropy driving the redirection of organic molecules in a specific framework structure, induced structural phase changes result in a change in crystal dimensions of about 10%. In contrast, most inorganic structures generally exhibit a change in unit cell volume of around 5% due to thermal phase transformation, while ICSD shows 53% expansion of unit cell volume before and after phase transformation of diamond and cubic boron nitride, indicating the potential of inorganic materials in thermally induced deformation. However, the phase change conditions of the two materials are harsh, so that the inorganic materials have huge lattice parameter mutation and meanwhile have mild phase change conditions, which is still a difficult problem for research in the field.
Disclosure of Invention
In view of the above, it is necessary to provide a method for realizing a giant expansion material with mild phase change conditions, a giant expansion material and application thereof, aiming at the technical defects existing in the prior art.
In order to solve the problems, the following technical scheme is adopted in the application:
one of the purposes of the application is to provide a method for realizing a giant expansion material, which comprises the following steps:
annealing tetragonal lithium metaborate at a temperature of 600-740 ℃, wherein the tetragonal lithium metaborate undergoes shape change.
In some of these embodiments, the tetragonal phase lithium metaborate is converted to a monoclinic phase lithium metaborate.
In some of these embodiments, the tetragonal phase lithium metaborate is a powder or bulk crystal.
In some of these embodiments, the lithium metaborate has a rate of change of lattice parameters a, b, c and unit cell volume V of 37.7%,2.6% and 33.6%, respectively, before and after the phase change.
In some embodiments, the lithium metaborate expands significantly in macroscopic size after phase transition, and the expansion ratio is 30-60% calculated as the area enclosed by the envelope.
One of the purposes of the application is to provide a giant expansion material, which is prepared by the realization method of the giant expansion material.
The second purpose of the application is to provide the application of the giant expansion material in a thermal switch.
By adopting the technical scheme, the application has the following beneficial effects:
according to the giant expansion material and the realization method thereof, tetragonal phase lithium metaborate is annealed at the temperature of 600-740 ℃, the shape of tetragonal phase lithium metaborate is changed, the structure of the tetragonal phase lithium metaborate provided by the application has the atomic distribution similar to diamond and cubic boron nitride, structural gaps are occupied by ionic groups, the structure has compactness, the structural internal stress can be provided in the heating process to force atoms to be redistributed, the tetragonal structure lithium metaborate causes huge volume expansion before and after phase change, the structural transformation is initiated and can be directly reflected to macroscopic size, the phase change condition is mild, the material can be suitable for occasions of practical application, and the function of a thermal switch can be better realized through larger macroscopic shape change.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings used in the embodiments of the present application or the description of the prior art will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows the change of lattice parameter and unit cell volume of lithium metaborate with temperature according to the embodiment of the present application, blue circles, diamonds and squares correspond to a, b and c of the crystal, respectively, and red spheres represent the unit cell volume of the crystal.
Fig. 2 is a photograph under a microscope of a 587 ℃ low temperature phase and a 640 ℃ high temperature phase, respectively, provided in the examples of the present application.
FIG. 3 is a schematic illustration of differential scanning calorimetry results at 25-1200℃as provided in the examples of the present application.
Fig. 4 is a schematic diagram showing the morphology of bulk crystals provided in the embodiment of the present application at different temperatures, wherein the bulk crystals undergo the processes of non-phase transformation, surface phase transformation and complete phase transformation from 584 ℃ to 687 ℃ and the morphology of the crystals is disintegrated from bulk to powder.
Fig. 5 is a schematic diagram of a phase transition provided in an embodiment of the present application, wherein curves 1-5 respectively represent a low temperature phase, a high temperature phase after heat treatment of low Wen Xiangjing, and a low temperature phase synthesized again from the high temperature phase, and thus two cycle processes are performed.
Detailed Description
Embodiments of the present application are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary and intended for the purpose of explaining the present application and are not to be construed as limiting the present application.
In the description of the present application, it should be understood that the terms "upper," "lower," "horizontal," "inner," "outer," and the like indicate an orientation or a positional relationship based on that shown in the drawings, and are merely for convenience of description and simplification of the description, and do not indicate or imply that the apparatus or element in question must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application will be further described in detail with reference to the accompanying drawings and examples.
The implementation method of the giant expansion material provided by the embodiment of the application comprises the following steps: annealing tetragonal lithium metaborate at a temperature of 600-740 ℃, wherein the tetragonal lithium metaborate undergoes shape change.
It should be noted that: although the crystalline organic compound has more free structural design and can easily obtain special structures with unconventional properties, the properties of the crystalline organic compound are not dependent on topological structures, so that the preparation process behind the properties is low in universality and the difficulty in exploring the structures required by the characteristics is high. The temperature induced change in macroscopic dimensions of the crystalline organic compound is still low (5-20%). Although diamond and cubic boron nitride exhibit a great abrupt change in this respect, they are not suitable for practical applications due to the severe phase change conditions (vacuum, high temperature or high pressure extreme conditions). The diamond and cubic boron nitride are similar in structure, and the unit cell change caused by phase change is the same, indicating that the characteristic depends on the topology in the inorganic material. However, in the current research, the volume mutation caused by the thermal phase change of the inorganic material is still very weak, and the directivity of structural design is low.
With reference to the structural features of diamond, we speculate that the material needs to possess two features: 1) The structure has compactness, so that the internal stress of the structure is provided in the heating process to force atoms to be redistributed so as to cause structural change; 2) Has ionic groups to satisfy the effect of reducing the phase change condition.
By searching the ICSD library, the lithium metaborate structure has atomic distributions similar to diamond and cubic boron nitride, and structural gaps are occupied by ionic groups, so that the requirements are met. Tests show that the volume mutation is increased by 34% after the thermally induced phase transition, the millimeter-sized monocrystal of the lithium metaborate has similar shape deformation, and the lithium metaborate has the structural characteristics, so that the lithium metaborate has the potential of a giant expansion material.
In this embodiment, the tetragonal phase lithium metaborate is converted to monoclinic phase lithium metaborate.
In this embodiment, the tetragonal lithium metaborate is a powder or bulk crystal.
In this example, the rate of change of lattice parameters a, b, c and unit cell volume V of the lithium metaborate before and after phase transition was 37.7%,2.6% and 33.6%, respectively.
Referring to fig. 1, the lattice parameter and the unit cell volume of lithium metaborate provided in this embodiment change with temperature, blue circles, diamonds and squares correspond to a, b and c of the crystal, respectively, and red spheres represent the unit cell volume of the crystal. As can be seen from fig. 1, the unit cell parameters and unit cell volume mutation of the lithium metaborate before and after phase change are respectively 37.7%,2.6%,2.6% and 33.6%, and the lithium metaborate also shows obvious shape change under a macroscopic scale compared with the unit cell volume change of the organic compound by several times.
In this embodiment, the lithium metaborate expands significantly in macroscopic size after phase transition, and the expansion rate is 30-60% by calculating the area surrounded by the envelope.
Referring to fig. 2, in the pictures (upper pictures) of the low temperature phase at 587 ℃ and the high temperature phase at 640 ℃ under the microscope (lower pictures) provided in this embodiment, the outlines of the crystals are outlined by pink lines, and the macroscopic expansion behavior of the crystals can be clearly seen in the illustration, wherein the temperature rising rate is 0.6 ℃/min, the temperature rises from 570 ℃ to 650 ℃, and the front-rear envelope area expands by 50%.
Referring to FIG. 3, there is shown a schematic diagram of the phase transition and melting of the two front and rear peaks, respectively, as a result of differential scanning calorimetry at 25-1200 ℃.
As can be seen from fig. 3, DSC shows two peaks in the temperature rising process of 25-1200 ℃, which respectively show phase change and melting, and it should be mentioned that the phase change peak will change according to factors such as temperature rising rate and sample state, so that the phase change temperature interval from the first peak at 600 ℃ to the second peak at 740 ℃ is the phase change temperature interval of lithium metaborate.
Referring to fig. 4, the tetragonal lithium metaborate bulk crystal is in the form of tetragonal lithium metaborate at different temperatures, and undergoes the processes of non-phase transformation and surface phase transformation to complete phase transformation from 584 ℃ to 687 ℃, and the crystal form is disintegrated from bulk to powder state, and the whole process is subjected to 26min. .
It is understood that if the rate of temperature rise is increased, the lithium metaborate bulk crystal will disintegrate into a powder state, and that the dramatic change in morphology is of value in thermal switching applications. When the temperature exceeds the target temperature, the lithium metaborate is rapidly disintegrated into powder as a safety device, and the device switch is turned off. The tetragonal phase and the tetragonal phase can be mutually converted through temperature and pressure, so that the cyclic use is realized, and the cost is saved.
Referring to fig. 5, curves 1 to 5 respectively represent a low-temperature tetragonal phase (1), a high Wen Shanxie phase (2) of the low-temperature tetragonal phase after heat treatment, and a low-temperature monoclinic phase (3) synthesized again from the high-temperature tetragonal phase, and thus, the curves 4 to 5 undergo the same treatment for 2 to 3 cycles for the second time to indicate that the material can be recycled.
The lithium metaborate structure provided by the application has the atomic distribution similar to diamond and cubic boron nitride, structural gaps are occupied by ionic groups, the structure has compactness, the condition that structural internal stress is provided to force atoms to redistribute in the heating process can be met, huge volume expansion is caused before and after phase transition of the tetragonal lithium metaborate structure, structural transition is initiated, the structural transition can be directly reflected to macroscopic dimensions, the phase transition condition is mild, the lithium metaborate structure can be suitable for occasions of practical application, and the function of a thermal switch can be better realized through larger macroscopic shape change.
It will be understood that the technical features of the above-described embodiments may be combined in any manner, and that all possible combinations of the technical features in the above-described embodiments are not described for brevity, however, they should be considered as being within the scope of the description provided in the present specification, as long as there is no contradiction between the combinations of the technical features.
The foregoing description of the preferred embodiments of the present application has been provided for the purpose of illustrating the general principles of the present application and is not meant to limit the scope of the present application in any way. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present application, and other embodiments of the present application, which may occur to those skilled in the art without the exercise of inventive faculty, are intended to be included within the scope of the present application, based on the teachings herein.
Claims (7)
1. A method for realizing a giant expansion material, comprising the steps of:
annealing tetragonal lithium metaborate at 600-740 ℃ to change shape.
2. The method of claim 1, wherein the tetragonal phase of lithium metaborate is converted to a monoclinic phase of lithium metaborate.
3. The method of claim 1, wherein the tetragonal lithium metaborate is a powder or a bulk crystal.
4. The method of claim 1, wherein the lithium metaborate has lattice parameters a, b, c and unit cell volume V of 37.7%,2.6% and 33.6%, respectively, before and after the phase transition.
5. The method for realizing the giant expansion material according to claim 1, wherein the lithium metaborate is obviously expanded in macroscopic size after phase transition, and the expansion rate is 30-60% when the area surrounded by an envelope line is calculated.
6. A giant expansion material prepared by the method of any one of claims 1 to 5.
7. Use of the giant expansion material of claim 6 in a thermal switch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311524621.5A CN117385463A (en) | 2023-11-15 | 2023-11-15 | Method for realizing giant expansion material, giant expansion material and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311524621.5A CN117385463A (en) | 2023-11-15 | 2023-11-15 | Method for realizing giant expansion material, giant expansion material and application |
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| CN117385463A true CN117385463A (en) | 2024-01-12 |
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| CN202311524621.5A Pending CN117385463A (en) | 2023-11-15 | 2023-11-15 | Method for realizing giant expansion material, giant expansion material and application |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050228166A1 (en) * | 2002-07-05 | 2005-10-13 | Kepert Cameron J | Anomalous expansion materials |
| WO2007148214A2 (en) * | 2006-06-23 | 2007-12-27 | Element Six (Production) (Pty) Ltd | Transformation toughened ultrahard composite materials |
| CN106917139A (en) * | 2015-12-24 | 2017-07-04 | 中国科学院新疆理化技术研究所 | The preparation method and purposes of lithium metaborate crystal |
| CN111640918A (en) * | 2020-05-11 | 2020-09-08 | 深圳新恒业电池科技有限公司 | Electrode material, preparation method thereof and electrode slice |
| US20200308684A1 (en) * | 2013-06-14 | 2020-10-01 | James Alan Monroe | Systems and methods for tailoring coefficients of thermal expansion between extreme positive and extreme negative values |
-
2023
- 2023-11-15 CN CN202311524621.5A patent/CN117385463A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050228166A1 (en) * | 2002-07-05 | 2005-10-13 | Kepert Cameron J | Anomalous expansion materials |
| WO2007148214A2 (en) * | 2006-06-23 | 2007-12-27 | Element Six (Production) (Pty) Ltd | Transformation toughened ultrahard composite materials |
| US20200308684A1 (en) * | 2013-06-14 | 2020-10-01 | James Alan Monroe | Systems and methods for tailoring coefficients of thermal expansion between extreme positive and extreme negative values |
| CN106917139A (en) * | 2015-12-24 | 2017-07-04 | 中国科学院新疆理化技术研究所 | The preparation method and purposes of lithium metaborate crystal |
| US20190345633A1 (en) * | 2015-12-24 | 2019-11-14 | Xinjiang Technical Institute Of Physics & Chemistry, Chinese Academy Of Sciences | Lithium Metaborate Crystal, Preparation Method and Use Thereof |
| CN111640918A (en) * | 2020-05-11 | 2020-09-08 | 深圳新恒业电池科技有限公司 | Electrode material, preparation method thereof and electrode slice |
Non-Patent Citations (1)
| Title |
|---|
| 梁敬魁, 柴璋, 赵书清: "LiBO_2玻璃晶化与相变的研究", 中国科学A辑, no. 01, 31 January 1990 (1990-01-31), pages 105 - 112 * |
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