CN114014894A - Cobalt-containing organic-inorganic hybrid molecule ferroelectric material and preparation method thereof - Google Patents
Cobalt-containing organic-inorganic hybrid molecule ferroelectric material and preparation method thereof Download PDFInfo
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- CN114014894A CN114014894A CN202111401591.XA CN202111401591A CN114014894A CN 114014894 A CN114014894 A CN 114014894A CN 202111401591 A CN202111401591 A CN 202111401591A CN 114014894 A CN114014894 A CN 114014894A
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 17
- 239000010941 cobalt Substances 0.000 title claims abstract description 17
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 10
- BZRRQSJJPUGBAA-UHFFFAOYSA-L cobalt(ii) bromide Chemical compound Br[Co]Br BZRRQSJJPUGBAA-UHFFFAOYSA-L 0.000 claims abstract description 7
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical class C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000015654 memory Effects 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 2
- 230000007306 turnover Effects 0.000 abstract description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 8
- 229910019131 CoBr2 Inorganic materials 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 230000010287 polarization Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 230000005621 ferroelectricity Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic System
- C07F15/06—Cobalt compounds
- C07F15/065—Cobalt compounds without a metal-carbon linkage
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10B—ELECTRONIC MEMORY DEVICES
- H10B51/00—Ferroelectric RAM [FeRAM] devices comprising ferroelectric memory transistors
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10B—ELECTRONIC MEMORY DEVICES
- H10B53/00—Ferroelectric RAM [FeRAM] devices comprising ferroelectric memory capacitors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Abstract
The invention discloses a cobalt-containing organic-inorganic hybrid molecule ferroelectric material and a preparation method thereof, wherein the molecular formula of the ferroelectric material is C10N2H21CoBr3The 296K crystal belongs to an orthorhombic system, and the space group is Pca21The highest temperature for keeping the ferroelectric property is 603K, the ferroelectric can realize ferroelectric domain turnover under the voltage of 30V, and the ferroelectric material has application potential in a plurality of fields such as piezoelectric transducers, ferroelectric memories (FRAM), ferroelectric photovoltaic materials and the like; the ferroelectric material adopts triethylene diamine derivative [ CH3(CH2)3‑Dabco]+Br and cobalt bromide react, and the obtained product is evaporated and crystallized, and the preparation method is simple to operate, safe and environment-friendly, and the prepared crystal has large volume, good quality, uniform particles, high yield and good repeatability.
Description
Technical Field
The invention relates to a ferroelectric material and a preparation method thereof, in particular to a cobalt-containing organic-inorganic hybrid molecule ferroelectric material and a preparation method thereof.
Background
Ferroelectric materials are receiving wide attention due to their great potential for applications in the fields of storage, energy harvesting and photovoltaics. Since ferroelectricity is found in inorganic ceramic ferroelectrics BTO and PZT, the inorganic ceramic ferroelectrics have a dominant role due to excellent ferroelectricity, piezoelectricity and thermal stability, but the ceramic ferroelectrics have high preparation cost, large energy consumption and serious pollution, and are difficult to miniaturize and lighten in practical application.
Thus, molecular ferroelectrics have emerged, including organic and organic-inorganic hybrid ferroelectrics, which are structurally diverse, tunable and easy to handle, and which have a combination of properties, e.g., Ps, d33And the optical property is excellent, and the material is expected to be a feasible supplement of inorganic ceramic ferroelectrics, and solves the increasingly serious energy and environmental problems. However, the highest temperature at which the molecular ferroelectric maintains ferroelectric properties is low compared to the inorganic ceramic ferroelectrics. Ferroelectric material in Chemical Science,2021, advanced Article (C9H14N)2CdBr4The highest temperature for maintaining the ferroelectric property is only 395K; ferroelectric material [ TMAEA ] in the Journal of the American Chemical Society,2020,142,4604-4608 article]Pb2Cl6The highest temperature for maintaining ferroelectric property is only 412K; ferroelectric material (EATMP) PbBr in the Journal of the American Chemical Society,2021,143,1664-4The highest temperature for keeping the ferroelectric property is 534K; ferroelectric material [ FEtDabco ] in article 946 of Chemical Communications,2021,57,943-]ZnI3The maximum temperature at which ferroelectric properties are maintained is 540K. The highest temperature at which molecular ferroelectrics retain their ferroelectric properties is low, severely limiting the use of such ferroelectric materials.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a cobalt-containing organic-inorganic hybrid molecule ferroelectric material, which has high highest temperature for keeping ferroelectric property; the invention also aims to provide a preparation method of the ferroelectric material.
The technical scheme is as follows: the molecular formula of the cobalt-containing organic-inorganic hybrid molecule ferroelectric material is C10N2H21CoBr3The structure is simple as follows:
the maximum temperature of the ferroelectric material for maintaining the ferroelectric property is 603K, and the ferroelectric domain switching voltage is 30V.
The preparation method of the ferroelectric material comprises the following steps:
(1) reacting a triethylenediamine derivative [ CH3(CH2)3-Dabco]+·Br-Putting into a beaker, adding distilled water for dissolving, adding cobalt bromide into the beaker, reacting until the solid is dissolved, and filtering to obtain filtrate;
(2) evaporating and crystallizing the filtrate to obtain the crystal which is the cobalt-containing organic-inorganic hybrid molecule ferroelectric material.
The preparation method of the cobalt-containing organic-inorganic hybrid molecule ferroelectric material comprises the step (1) of obtaining a triethylene diamine derivative [ CH3(CH2)3-Dabco]+·Br-The molar ratio of the cobalt bromide to the cobalt bromide is 1: 1-3.
The reaction temperature in the step (1) is 20-60 ℃.
The reaction time in the step (1) is 0.5-1 hour.
The evaporation crystallization temperature of the step (2) is 20-45 ℃.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: (1) the ferroelectric material has the highest temperature for keeping the ferroelectric property of 603K and good ferroelectric property; (2) the ferroelectric body of the ferroelectric material can turn over the ferroelectric domain only by a driving voltage of 30V, and has great application advantages in the aspect of ferroelectric memories; (3) the preparation method is simple to operate, safe and environment-friendly, and the prepared crystal has large volume, good quality, uniform particles, high yield and good repeatability; (4) the ferroelectric material has application potential in the fields of piezoelectric transducers, ferroelectric memories (FRAM), ferroelectric photovoltaic materials and the like.
Drawings
FIG. 1 shows a cobalt-containing organic-inorganic hybrid ferroelectric material C of the present invention10N2H21CoBr3Synthetic roadmaps of (a);
FIG. 2 is a graph of the cell stacking of the synthetic ferroelectric material of example 2 at 296K;
FIG. 3 is a powder diffraction XRD pattern of the synthetic ferroelectric material of example 2;
FIG. 4 is an infrared spectrum of the synthetic ferroelectric material of example 2;
fig. 5 is a ferroelectric hysteresis loop of the synthetic ferroelectric material of example 2;
FIG. 6 is a TG-DSC analysis chart of the synthetic ferroelectric material of example 2;
FIG. 7 is a frequency doubling (SHG) graph of the synthetic ferroelectric material of example 2;
FIG. 8 is a temperature-varying powder diffraction XRD pattern of the synthetic ferroelectric material of example 2;
FIG. 9 is a diagram of ferroelectric domains of a synthetic ferroelectric material of example 2;
fig. 10 is a diagram of the inversion of ferroelectric domains of the synthetic ferroelectric material of example 2.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
Example a cobalt-containing organic-inorganic hybrid molecular ferroelectric material was prepared according to the synthetic route of fig. 1.
Example 1
At 20 deg.C, 10mmol of [ CH ]3(CH2)3-Dabco]+·Br-Placing into a beaker, adding 20ml of distilled water, stirring to dissolve, and adding 10mmol of CoBr2Stirred for 0.5 hour, CoBr2The solid was dissolved and filtered to give a clear filtrate. Standing the filtrate at 20 deg.C for volatilization to obtain C10N2H21CoBr3And (4) crystals.
Example 2
At 25 deg.C, 10mmol of [ CH ]3(CH2)3-Dabco]+·Br-Placing into a beaker, adding 20ml of distilled water, stirring to dissolve, and adding 10mmol of CoBr2Reaction with stirring for 1 hour, CoBr2The solid was dissolved and filtered to give a clear filtrate. Standing the filtrate at 25 deg.C for volatilization to obtain C10N2H21CoBr3And (4) crystals.
Example 3
At 60 deg.C, 10mmol of [ CH ]3(CH2)3-Dabco]+·Br-Placing into a beaker, adding 20ml of distilled water, stirring to dissolve, and adding30mmol of CoBr2Stirred for 0.5 hour, CoBr2The solid was dissolved and filtered to give a clear filtrate. Standing the filtrate at 45 deg.C for volatilization to obtain C10N2H21CoBr3And (4) crystals.
Taking the sample of example 2, a single crystal of suitable size was selected under a microscope and monochromated at 296K with Mo Ka radiation using graphite
The X-ray diffraction structure of the single crystals was measured on a Bruker Apex II CCD diffractometer. The SADABS method is used for carrying out semi-empirical absorption correction, the unit cell parameters are determined by the least square method, data reduction and structure analysis are respectively completed by using SAINT and SHELXL program packages, all non-hydrogen atoms are anisotropically refined by the full matrix least square method and participate in structural factor calculation, and related crystallography data are shown in Table 1.
TABLE 1 crystallographic data of Fe-O-compound in example 1
As shown in fig. 3, the simulated diffraction peaks compare well with the diffraction peaks measured in the actual experiment, indicating that the compound is of high purity.
As shown in FIG. 4, at 2900cm-1The nearby strong absorption peak is-CH3"and" -CH2- "stretching vibration absorption peak of group; at 1420cm-1The strong absorption peak in the vicinity is a C-C single bond bending vibration absorption peak.
As shown in FIG. 5, the ferroelectric material had a saturation polarization value of 2.1. mu.C cm-2The remanent polarization value is 1.8 mu C cm-2Coercive electric field of 30kV cm-1。
As shown in FIG. 6, the TG curve shows that the compound has high thermal stability, and the compound structure begins to collapse after 603K and completely collapses around 1000K along with the increase of temperature; from the DSC curve, no structural phase change of the compound occurred below 603K, and the compound began to decompose after 603K. The two figures combined with TG and DSC illustrate that the material is structurally stable below 603K.
As shown in fig. 7, the frequency doubling signal below 603K is active, and it is proved that the compound is in a non-centrosymmetric structure before collapse, and has ferroelectric properties.
As shown in fig. 8, all diffraction peaks remained stable and did not change significantly at 603K and below, which proves that the structure of the compound was not changed and the ferroelectric properties could be guaranteed; and as the structure of the compound with the voltage of above 603K collapses and loses weight, most of derived peaks of the ferroelectric structure disappear, and properties such as ferroelectric property and the like are lost along with the collapse of the structure.
The ferroelectric material of the application has no phase change below 603K, and loses ferroelectric property with structural collapse after 603K. As can be illustrated by fig. 5 to 8, the ferroelectric material has ferroelectric properties below 603K, so the highest temperature at which the ferroelectric material of the present application maintains ferroelectric properties is 603K.
As shown in fig. 10, the ferroelectric domain switching voltage of the molecular ferroelectric is 30V. Based on the electric hysteresis phenomenon in ferroelectricity, the ferroelectric domain can be used for forming high polarization charges by inversion under an electric field or forming low polarization charges without inversion to judge that the memory cell is in a state of '1' or '0', thereby manufacturing the ferroelectric memory. The ferroelectric domain is switched without high electric field, and the state of the memory cell in '1' or '0' can be changed only by using common working voltage; and a charge pump is not needed to generate high-voltage data erasing, so that the phenomenon of erasing delay is avoided. The characteristic enables the ferroelectric memory to still keep data after power failure, has high writing speed and infinite writing service life, and is not easy to be damaged. The molecular ferroelectrics mentioned in the article j.am.chem.soc.2020,142,1995-2000 require a voltage of 70V to switch the ferroelectric domain; the molecular ferroelectric in the article adv.funct.mater.2021,2102848 needs 110V to realize the ferroelectric domain inversion, while the material ferroelectric in the present invention needs only 30V of driving voltage to invert the ferroelectric domain, which is very advantageous for the application of the material in the ferroelectric memory.
Claims (6)
1. A cobalt-containing organic-inorganic hybrid molecule ferroelectric material is characterized in that the molecular formula of the ferroelectric material is C10N2H21CoBr3The structure is simple as follows:
2. a method for preparing the cobalt-containing organic-inorganic hybrid molecule ferroelectric material according to claim 1, comprising the steps of:
(1) reacting a triethylenediamine derivative [ CH3(CH2)3-Dabco]+·Br-Putting into a beaker, adding distilled water for dissolving, adding cobalt bromide into the beaker, reacting until the solid is dissolved, and filtering to obtain filtrate;
(2) evaporating and crystallizing the filtrate to obtain the crystal which is the cobalt-containing organic-inorganic hybrid molecule ferroelectric material.
3. The method for preparing a cobalt-containing organic-inorganic hybrid molecule ferroelectric material according to claim 2, wherein the triethylenediamine derivative [ CH ] in the step (1)3(CH2)3-Dabco]+·Br-The molar ratio of the cobalt bromide to the cobalt bromide is 1: 1-3.
4. The preparation method of the cobalt-containing organic-inorganic hybrid molecule ferroelectric material as claimed in claim 2, wherein the reaction temperature in the step (1) is 20-60 ℃.
5. The method for preparing the cobalt-containing organic-inorganic hybrid molecule ferroelectric material as claimed in claim 2, wherein the reaction time in the step (1) is 0.5-1 hour.
6. The method for preparing the cobalt-containing organic-inorganic hybrid molecule ferroelectric material according to claim 2, wherein the temperature of the evaporative crystallization in the step (2) is 20-45 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992019564A1 (en) * | 1991-05-01 | 1992-11-12 | The Regents Of The University Of California | Amorphous ferroelectric materials |
| CN110590858A (en) * | 2019-08-27 | 2019-12-20 | 江苏科技大学 | Cobalt-containing coordination compound with low-temperature phase change and preparation method thereof |
| KR20210007169A (en) * | 2019-07-10 | 2021-01-20 | 한국전력공사 | Method for measuring efficiency of ferroelectric materials containing transition elements and the pellet for measuring efficiency of ferroelectric materials |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992019564A1 (en) * | 1991-05-01 | 1992-11-12 | The Regents Of The University Of California | Amorphous ferroelectric materials |
| KR20210007169A (en) * | 2019-07-10 | 2021-01-20 | 한국전력공사 | Method for measuring efficiency of ferroelectric materials containing transition elements and the pellet for measuring efficiency of ferroelectric materials |
| CN110590858A (en) * | 2019-08-27 | 2019-12-20 | 江苏科技大学 | Cobalt-containing coordination compound with low-temperature phase change and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| LIAO, WEI-QIANG: "Synthesis, structures and dielectric properties of two five-coordinate copper(II) complexes based on N-chloromethyl-1, 4-diazabicyclo[2.2.2]octane", 《INORGANIC CHEMISTRY COMMUNICATIONS》, vol. 33, pages 161 - 164, XP028555918, DOI: 10.1016/j.inoche.2013.04.031 * |
| LUACHAN, SANCHAI: ""(1-Butyl-1, 4-diazabicyclo[2.2.2]octon-1-ium-κN4)trichloridocobalt(II)"", 《ACTA CRYSTALLOGRAPHICA, SECTION E: STRUCTURE REPORTS ONLINE》, vol. 65, no. 3, pages 321 * |
| V. L. GOEDKEN: "Donor properties of positively charged ligands. Five-coordinate transition metal complexes containing a monoquaternized tertiary diamine", 《INORG. CHEM》, vol. 8, no. 11, pages 2331 * |
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