CN102087900A - Salen-like and diketone-base dysprosium tetranuclear cluster compound type monomolecular magnetic material and preparation method thereof - Google Patents

Salen-like and diketone-base dysprosium tetranuclear cluster compound type monomolecular magnetic material and preparation method thereof Download PDF

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CN102087900A
CN102087900A CN2010105867791A CN201010586779A CN102087900A CN 102087900 A CN102087900 A CN 102087900A CN 2010105867791 A CN2010105867791 A CN 2010105867791A CN 201010586779 A CN201010586779 A CN 201010586779A CN 102087900 A CN102087900 A CN 102087900A
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dysprosium
cluster compound
diketo
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salen
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孙文彬
闫鹏飞
田永梅
李洪峰
李光明
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Heilongjiang University
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Abstract

The invention provides a salen-like and diketone-base dysprosium tetranuclear cluster compound type monomolecular magnetic material and a preparation method thereof and relate to a cluster compound and a preparation method thereof. The invention aims at solving the technical problem that the existing dysprosium tetranuclear cluster compound type monomolecular magnetic material has low effective revolving and inverting energy barrier. The molecular formula of the salen-like and diketone-base dysprosium tetranuclear cluster compound type monomolecular magnetic material is [Dy4(mu3-OH)2L2(acac)4].H2LCH3CN. The method comprises the following steps of: firstly, at a room temperature, dissolving 1,2-hexamethylene diamine salicylaldehyde and diacetone in an aprotic polar solvent, and adding organic base to obtain a mixture A; secondly, adding dysprosium chloride salt to a protonic polar solvent to obtain a mixture B; and thirdly, dripping the mixture B in the mixture A, then agitating, reacting, filtering, and settling filtrate for 14 days. The cluster compound is used in the fields of high density information storage, quantum computer and the like.

Description

Class salen and diketo dysprosium four nuclear cluster compound type unimolecule magnetic materials and preparation method thereof
Technical field
The present invention relates to a kind of cluster compound and preparation method thereof.
Background technology
Single molecular magnets can be regarded the crosspoint of molecular based ferromagnet and nano magnetic material as.It provides first the mono-dispersed nano magnet truly that is made of individual molecule.Owing to showing under its low temperature very slowly that magnetic relaxation phenomenon can be applied in that high density information stores and fields such as quantum computer receive much concern.Research to single molecular magnets also helps the physical understanding of nano-scale magnetic particle.
Since people (J.Appl.Phys.1996,79,6031) such as Friedman in 1996 had reported the single molecular magnets that contains Mn12 cluster complex for the first time, people began containing the broad research of transition metal single molecular magnets.Yet, the research of rare earth unimolecule material is rarely had report, with respect to transition metal, the high-spin of rare earth ion itself, height revolve the rail coupling has brought up very big easy magnetic axis magnetic anisotropy, make its desirable feedstock that becomes single molecular magnets, as rare earth Ho, Tb and Dy etc.This type of unimolecule magnetic material has organic-dissolvable preferably, makes things convenient for the preparation of its molecular magnetism Coating Materials.Why single molecular magnets can show above-mentioned all special magnetic property at low temperatures, is that the energy barrier that has near room temperature makes the practical application of unimolecule magnetic material become possibility because it has bigger spin flip conversion energy barrier U under the low temperature.
The multinuclear cluster compound that contains Dy is that people study a more class unimolecule magnetic material in recent years.A kind of dysprosium four nuclear cluster compound [Dy that published at present 4(μ 3-OH) 2(mdeaH) 2(piv) 8] (effectively spin flip conversion energy barrier Ueff is 6.9K, and the magnetization relaxation time is 4.8 * 10 -5S) (Inorg.Chem.2010,49,8067).
Summary of the invention
The present invention will solve the low technical problem of the existing dysprosium four nuclear cluster compound effective spin flip conversion energy barriers of unimolecule magnetic material; And provide class salen and diketo dysprosium four to examine cluster compound type unimolecule magnetic materials and preparation method thereof.
The molecular formula of class salen and diketo dysprosium four nuclear cluster compound type unimolecule magnetic materials is [Dy among the present invention 4(μ 3-OH) 2L 2(acac) 4] H 2LCH 3CN is to have zero dimension, four nuclear and dysprosium cluster compounds of coplanar structure, structural formula as shown in Figure 1, effective spin flip conversion energy barrier U EffBe 20.72K, the magnetization relaxation time is τ 0Be 4.55 * 10 -6S.
The preparation method of class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials is undertaken by following step among the present invention:
Step 1, at room temperature, with 1,2-cyclohexanediamine salicylaldehyde and acetylacetone,2,4-pentanedione are dissolved in the non-proton property polar solvent, the acetylacetone,2,4-pentanedione consumption is 1, three times of 2-cyclohexanediamine salicylaldehyde quality, 1, the quality of 2-cyclohexanediamine salicylaldehyde and non-proton property polar solvent volume ratio are 0.33g: 10mL, add organic base, the organic base consumption is the twice of cyclohexanediamine salicylaldehyde amount, obtains mixture A;
Step 2, dysprosium chloride add in the protic polar solvent, dysprosium chloride salt consumption and 1, and 2-cyclohexanediamine salicylaldehyde identical in quality, the quality of dysprosium chloride salt and protic polar solvent volume ratio are 0.33g: 10mL, obtain mixture B;
Step 3, mixture B dropwise is added drop-wise among the mixture A, 70～80 ℃ of following stirring reactions 5～6 hours, filters then, with static 14 days of filtrate; Obtain class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials.
Reactional equation of the present invention is as follows:
Figure BDA0000038109970000021
Effective spin flip conversion energy barrier height under class salen of the present invention and the diketo dysprosium four nuclear cluster compound type unimolecule magnetic material low temperature.Effective spin flip conversion energy barrier U EffBe 20.72K, the magnetization relaxation time is τ 0Be 4.55 * 10 -6S.The inventive method is simple, is convenient to operation.Be applied in fields such as high density information storage and quantum computer.
Description of drawings
Fig. 1 is the molecular structure of four nuclear dysprosium unimolecule magnetic materials; Fig. 2 is the metal coplane molecular structure of four nuclear dysprosium unimolecule magnetic materials; Fig. 3 is the interchange alternating temperature frequency conversion magnetization curve figure of four nuclear dysprosium unimolecule magnetic materials, 1 for frequency be the magnetization curve of 10Hz, 2 expression frequencies are the magnetization curve of 100Hz, 3 expression frequencies are the magnetization curve of 250Hz, 4 expression frequencies are the magnetization curve of 500Hz, and 5 expression frequencies are the magnetization curve of 750Hz, and 6 expression frequencies are the magnetization curve of 1000Hz, 7 expression frequencies are the magnetization curve of 1250Hz, and 8 expression frequencies are the magnetization curve of 1500Hz; Fig. 4 is the Arrhenius plot of four nuclear dysprosium unimolecule magnetic materials.
Embodiment
Embodiment one: the molecular formula of present embodiment class salen and diketo dysprosium four nuclear cluster compound type unimolecule magnetic materials is [Dy 4(μ 3-OH) 2L 2(acac) 4] H 2LCH 3CN is the dysprosium cluster compound with zero dimension, four nuclears and coplanar structure, effectively spin flip conversion energy barrier U EffBe 20.72K, the magnetization relaxation time is τ 0Be 4.55 * 10 -6S.
Embodiment two: the preparation method of present embodiment class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials is undertaken by following step: step 1, at room temperature, with 1,2-cyclohexanediamine salicylaldehyde and acetylacetone,2,4-pentanedione are dissolved in the non-proton property polar solvent, the acetylacetone,2,4-pentanedione consumption is 1, three times of 2-cyclohexanediamine salicylaldehyde quality, 1, the quality of 2-cyclohexanediamine salicylaldehyde and non-proton property polar solvent volume ratio are 0.33g: 10mL, add organic base, the organic base consumption is the twice of cyclohexanediamine salicylaldehyde amount, obtains mixture A; Step 2, dysprosium chloride add in the protic polar solvent, dysprosium chloride salt consumption and 1, and 2-cyclohexanediamine salicylaldehyde identical in quality, the quality of dysprosium chloride salt and protic polar solvent volume ratio are 0.33g: 10mL, obtain mixture B; Step 3, mixture B dropwise is added drop-wise among the mixture A, 70～80 ℃ of following stirring reactions 5～6 hours, filters then, with static 14 days of filtrate; Obtain class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials; Molecular formula is [Dy 4(μ 3-OH) 2L 2(acac) 4] H 2LCH 3CN.
Effective spin flip conversion energy barrier U of the class salen of present embodiment preparation and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials EffBe 20.72K, the magnetization relaxation time is τ 0Be 4.55 * 10 -6S.
Embodiment three: what present embodiment and embodiment two were different is: the described non-proton property polar solvent of step 1 is an acetonitrile.Other step is identical with embodiment two with parameter.
Embodiment four: what present embodiment was different with embodiment two or three is: the described organic base of step 1 is a triethylamine.Other step is identical with embodiment two or three with parameter.
Embodiment five: what present embodiment was different with one of embodiment two to five is: the described protic polar solvent of step 2 is a methyl alcohol.Other step is identical with one of embodiment two to five with parameter.
Embodiment six: what present embodiment was different with one of embodiment two to six is: the step 3 rate of addition is 1 droplet/second.Other step is identical with one of embodiment two to six with parameter.
Embodiment seven: the preparation method of present embodiment class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials is undertaken by following step: one, at room temperature, with 0.33g1,2-cyclohexanediamine salicylaldehyde and 0.3g acetylacetone,2,4-pentanedione are dissolved in the 10mL acetonitrile, acetylacetone,2,4-pentanedione is 1, three times of 2-cyclohexanediamine salicylaldehyde quality, add the 0.66g triethylamine, obtain mixture A; Two, 0.33g dysprosium chloride salt adds in 10 ml methanol, obtains mixture B; Three, mixture B is dropwise dripped (1 droplet/second) in mixture A,, filter, static 14 days of filtrate then 70～80 ℃ of following stirring reactions 5～6 hours; Obtain class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials.
The structural formula of the magnetic material of present embodiment preparation is seen Fig. 1; As can be seen from Figure 2, four rare earth dysprosium metals are in same plane; Can prove absolutely its unimolecule magnetic behavior by Fig. 3; Calculate its effective spin flip conversion energy barrier U of acquisition by Fig. 4 and by Arrhenius curve (lnk=lnA-Ea/RT, k are speed constant, and R is a molar gas constant, and T is a thermodynamic temperature, and Ea is an apparent activation energy, and A is pre-exponential factor (also claiming frequency factor)) EffBe 20.72K, the magnetization relaxation time is τ 0Be 4.55 * 10 -6S.

Claims (6)

1. class salen and diketo dysprosium four nuclear cluster compound type unimolecule magnetic materials is characterized in that the molecular formula of class salen and diketo dysprosium four nuclear cluster compound type unimolecule magnetic materials is [Dy 4(μ 3-OH) 2L 2(acac) 4] H 2LCH 3CN is the dysprosium cluster compound with zero dimension, four nuclears and coplanar structure, effectively spin flip conversion energy barrier U EffBe 20.72K, the magnetization relaxation time is τ 0Be 4.55 * 10 -6S.
2. class salen and diketo dysprosium four are examined the preparation method of cluster compound unimolecule magnetic materials, it is characterized in that the preparation method of class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials is undertaken by following step:
Step 1, at room temperature, with 1,2-cyclohexanediamine salicylaldehyde and acetylacetone,2,4-pentanedione are dissolved in the non-proton property polar solvent, the acetylacetone,2,4-pentanedione consumption is 1, three times of 2-cyclohexanediamine salicylaldehyde amount, 1, the quality of 2-cyclohexanediamine salicylaldehyde and non-proton property polar solvent volume ratio are 0.33g: 10mL, add organic base, the organic base consumption is the twice of cyclohexanediamine salicylaldehyde amount, obtains mixture A;
Step 2, dysprosium chloride add in the protic polar solvent, dysprosium chloride salt consumption and 1, and 2-cyclohexanediamine salicylaldehyde identical in quality, the quality of dysprosium chloride salt and protic polar solvent volume ratio are 0.33g: 10mL, obtain mixture B;
Step 3, mixture B dropwise is added drop-wise among the mixture A, 70～80 ℃ of following stirring reactions 5～6 hours, filters then, with static 14 days of filtrate; Obtain class salen and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials; Molecular formula is [Dy 4(μ 3-OH) 2L 2(acac) 4] H 2LCH 3CN.
3. according to the preparation method of described class salen of claim 1 and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials, it is characterized in that the described non-proton property polar solvent of step 1 is an acetonitrile.
4. according to the preparation method of described class salen of claim 1 and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials, it is characterized in that the described organic base of step 1 is a triethylamine.
5. according to the preparation method of described class salen of claim 1 and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials, it is characterized in that the described protic polar solvent of step 2 is a methyl alcohol.
6. according to the preparation method of described class salen of claim 1 and diketo dysprosium four nuclear cluster compound unimolecule magnetic materials, it is characterized in that the step 3 rate of addition is 1 droplet/second.
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CN103219116A (en) * 2013-04-22 2013-07-24 黑龙江大学 Zn-Dy-Zn type single-molecule magnetic material and manufacturing method thereof
CN103310938A (en) * 2013-06-27 2013-09-18 黑龙江大学 Co-Dy type single molecule magnetic material and preparation method thereof
CN103714932A (en) * 2013-12-30 2014-04-09 北京工业大学 Co zero-dimension single-molecular magnet material, preparation method and application of Co zero dimension single-molecular magnet material
CN104031095A (en) * 2014-06-27 2014-09-10 广西师范大学 Isobutanolamine copper and rare earth 24-heteronuclear metal cluster and synthesis method thereof
CN104130295A (en) * 2014-07-18 2014-11-05 南开大学 Terbium iron dissimilar metallic compound with single-molecular magnet behavior
CN110931199A (en) * 2019-12-10 2020-03-27 黑龙江大学 Magnetic easy axis series type binuclear dysprosium molecular magnetic material constructed by 2, 6-dimethoxyphenol and preparation method thereof

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CN102982960B (en) * 2012-12-28 2015-01-07 南开大学 Trinuclear dysprosium cluster compound single-molecular magnet and preparation method thereof
CN102982960A (en) * 2012-12-28 2013-03-20 南开大学 Trinuclear dysprosium cluster compound single-molecular magnet and preparation method thereof
CN103219116A (en) * 2013-04-22 2013-07-24 黑龙江大学 Zn-Dy-Zn type single-molecule magnetic material and manufacturing method thereof
CN103219116B (en) * 2013-04-22 2015-07-08 黑龙江大学 Zn-Dy-Zn type single-molecule magnetic material and manufacturing method thereof
CN103310938A (en) * 2013-06-27 2013-09-18 黑龙江大学 Co-Dy type single molecule magnetic material and preparation method thereof
CN103310938B (en) * 2013-06-27 2015-07-08 黑龙江大学 Preparation method of Co-Dy type single molecule magnetic material
CN103714932A (en) * 2013-12-30 2014-04-09 北京工业大学 Co zero-dimension single-molecular magnet material, preparation method and application of Co zero dimension single-molecular magnet material
CN103714932B (en) * 2013-12-30 2016-04-20 北京工业大学 A kind of Co zero dimension single molecular magnets material and preparation method and application thereof
CN104031095A (en) * 2014-06-27 2014-09-10 广西师范大学 Isobutanolamine copper and rare earth 24-heteronuclear metal cluster and synthesis method thereof
CN104031095B (en) * 2014-06-27 2016-03-02 广西师范大学 Isobutyl hydramine copper-rare earth hetero 20 four-core metal duster compound and synthetic method thereof
CN104130295A (en) * 2014-07-18 2014-11-05 南开大学 Terbium iron dissimilar metallic compound with single-molecular magnet behavior
CN104130295B (en) * 2014-07-18 2017-05-10 南开大学 Terbium iron dissimilar metallic compound with single-molecular magnet behavior
CN110931199A (en) * 2019-12-10 2020-03-27 黑龙江大学 Magnetic easy axis series type binuclear dysprosium molecular magnetic material constructed by 2, 6-dimethoxyphenol and preparation method thereof
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