CN101428843A - Process for producing ferromagnetic monodisperse nano-zinc oxide at room temperature - Google Patents
Process for producing ferromagnetic monodisperse nano-zinc oxide at room temperature Download PDFInfo
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- CN101428843A CN101428843A CNA2008101629937A CN200810162993A CN101428843A CN 101428843 A CN101428843 A CN 101428843A CN A2008101629937 A CNA2008101629937 A CN A2008101629937A CN 200810162993 A CN200810162993 A CN 200810162993A CN 101428843 A CN101428843 A CN 101428843A
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Abstract
The invention discloses a preparation method of mono-dispersed nanometer zinc oxide with room temperature ferromagnetism. The preparation method comprises the following steps: placing the zinc acetylacetonate hydrate of analytically pure and the oleyl amine of technical pure with the molar percentage of 1:50 to 1:200 into a container; heating the temperature to 200 to 300 DEG C; insulating for 0.5 to 2 hours; carrying out centrifugal separation when reaction solution is cooled into the room temperature to obtain a solid product; dispersing the solid product again by absolute ethyl alcohol and carrying out centrifugal separation; and drying under the room temperature to obtain mono-dispersed nanometer zinc oxide powder with the different grain size of 7 to 10 nm after the steps are performed repeatedly for 2 to 3 times. The invention has the advantages of simple process, low cost, no limit of high-temperature high-pressure reaction conditions, good controllability and no pollution to environment; and the saturation magnetization of the nanometer zinc oxide is improved by eight to ten times than that in the background art. The invention has high use value in aspects of the research on the source of the room temperature ferromagnetism of the nanometer zinc oxide and the design and the manufacture of a low power dissipation novel spinning electronic device integrating magnetism, light and electron into a whole.
Description
Technical field
The present invention relates to the preparation of semi-conductor spintronics material, particularly relate to a kind of preparation method with ferromagnetic monodisperse nano-zinc oxide at room temperature.
Background technology
The semiconductor material that preparation has room-temperature ferromagnetic is the gordian technique of semi-conductor spintronics practicality.Zinc oxide is a very important representative materials of II-VI family composite semiconductor, exciton bind energy (60mev) is big, have tangible magneto-optic effect, be development visible-preferred material of new device aspect such as ultraviolet band light emission, optical detection, piezoelectricity and magneto-optic function be integrated.The magneticsubstance that has electric charge and spin characters concurrently that forms with part zine ion in the transition metal alternative semiconductors zinc oxide, to become the information processing of a new generation and the important materials in fields such as storage, quantum calculation and quantum communication, cause that people greatly pay close attention to.Recently, people have observed room-temperature ferromagnetic in the pure zinc oxide of containing transition metal not.For example, adopt laser to melt method growing zinc oxide film [N.H.Hong, J.Sakai, and V.Brize, J.Phys.:Condens.Matter 19 (2007) 036219], Hydrothermal Preparation goes out zinc-oxide nano column [Z.J.Yan, Y.W.Ma, D.L.Wang, J.H.Wang, Z.S.Gao, L.Wang, P.Yu, and T.Song, Appl.Phys.Lett.92 (2008) 081911] and by argon gas injection [R P Borges, R C Da Silva, S Magalhaes, MM Cruz, and M Godinho, J.Phys.:Condens.Matter 19 (2007) 476207], mechanical force [K.Potzger, S.Q.Zhou, J.Grenzer, M.Helm, and J.Fassbender, Appl.Phys.Lett.92 (2008) 182504] and annealing [S.Banerjee, M.Mandal, N.Gayathri, and M.Sardar, Appl.Phys.Lett.91 (2007) 182501] etc. method obtain the semiconductor material zinc oxide of room-temperature ferromagnetic, for the practicability of spin electric device provides material foundation.There is the preparation process complexity in the above-mentioned synthetic method, needs expensive device, shortcomings such as high-temperature and high-pressure conditions.
Summary of the invention
The object of the present invention is to provide easy, a kind of preparation method cheaply with ferromagnetic monodisperse nano-zinc oxide at room temperature.
The technical solution used in the present invention is:
The present invention is that analytically pure zinc acetylacetonate and the commercially pure oleyl amine of 1:50-1:200 is placed in the container with molar percentage, be warmed up to 200~300 ℃, be incubated 0.5-2 hour, during the reaction soln cool to room temperature, centrifugation obtains solid product, with dehydrated alcohol disperse once more, centrifugation, after repeating 2~3 times, at room temperature be dried to pressed powder.
Control reaction temperature obtains the monodisperse nano-zinc oxide powder of 7~10nm various grain sizes.
The beneficial effect that the present invention has:
Technology of the present invention is simple, and cost is low, is not subjected to the high-temperature high-voltage reaction condition restriction, and controllability is good, environmentally safe, and the saturation magnetization of the nano zine oxide that obtains is than improving eight to tens times in the above-mentioned document.It has great scientific meaning for the room-temperature ferromagnetic source of research nano zine oxide, simultaneously in the design of the novel spin electric device of reduce power consumption of collection magnetic, light, electronics one, have very high practical value in making.
Description of drawings
Fig. 1 is the nano zine oxide TEM and the SAED photo of embodiment 1 preparation.
Fig. 2 is the M-H curve of the nano zine oxide of embodiment 1 preparation.
Embodiment
Embodiment 1:
Carrying out according to preparation process, is the methyl ethyl diketone zinc powder 0.106g of 1:100 with molar percentage, and oleyl amine 12.4ml puts into there-necked flask respectively, is warmed up to 250 ℃ with the temperature rise rate of 4 ℃/min, is incubated 1 hour.During the reaction soln cool to room temperature, centrifugation 15min, the solid dispersed that obtains is washed in dehydrated alcohol, and recentrifuge repeats the powder Air drying 3 times.The test that transmission electron microscope observation and selected area electron diffraction are observed (TEM and SAED) is that dried powder supersound process is dispersed in the toluene, then with drips of solution on the copper mesh that is coated with carbon film, drying at room temperature, TEM model are JEOL200CX.As shown in Figure 1, be TEM with room-temperature ferromagnetic Zinc oxide nanoparticle and the SAED photo for preparing by embodiment 1.Wherein (a) is the TEM photo of monodisperse nano-zinc oxide among Fig. 1, and particle diameter is 9.6 ± 0.2nm; (b) be the SAED polycrystalline diffractogram of nano zine oxide, illustrate that product is a wurtzite structure zinc oxide, the inclusion-free peak.As shown in Figure 2, be the M-H curve under the nano zine oxide room temperature, can see that sample at room temperature still has tangible magnetic hysteresis loop, saturation magnetization is 34memu/g under the room temperature, illustrates that nano zine oxide has room-temperature ferromagnetic.
Embodiment 2:
Carrying out according to preparation process, is the methyl ethyl diketone zinc powder 0.106g of 1:100 with molar percentage, and oleyl amine 12.4ml puts into there-necked flask respectively, is warmed up to 200 ℃ with the temperature rise rate of 4 ℃/min, is incubated 1.5 hours.During the reaction soln cool to room temperature, centrifugation 15min, the solid dispersed that obtains is washed in dehydrated alcohol, and recentrifuge repeats the powder Air drying 3 times.
Embodiment 3:
Carrying out according to preparation process, is the methyl ethyl diketone zinc powder 0.106g of 1:50 with molar percentage, and oleyl amine 6.2ml puts into there-necked flask respectively, is warmed up to 250 ℃ with the temperature rise rate of 4 ℃/min, is incubated 0.5 hour.During the reaction soln cool to room temperature, centrifugation 15min, the solid dispersed that obtains is washed in dehydrated alcohol, and recentrifuge repeats the powder Air drying 3 times.
Embodiment 4:
Carrying out according to preparation process, is the methyl ethyl diketone zinc powder 0.106g of 1:50 with molar percentage, and oleyl amine 6.2ml puts into there-necked flask respectively, is warmed up to 200 ℃ with the temperature rise rate of 4 ℃/min, is incubated 1 hour.During the reaction soln cool to room temperature, centrifugation 15min, the solid dispersed that obtains is washed in dehydrated alcohol, and recentrifuge repeats the powder Air drying 3 times.
Embodiment 5:
Carrying out according to preparation process, is the methyl ethyl diketone zinc powder 0.503g of 1:200 with molar percentage, and oleyl amine 12.4ml puts into there-necked flask respectively, is warmed up to 250 ℃ with the temperature rise rate of 4 ℃/min, is incubated 2 hours.During the reaction soln cool to room temperature, centrifugation 15min, the solid dispersed that obtains is washed in dehydrated alcohol, and recentrifuge repeats the powder Air drying 3 times.
Embodiment 6:
Carrying out according to preparation process, is the methyl ethyl diketone zinc powder 0.503g of 1:200 with molar percentage, and oleyl amine 12.4ml puts into there-necked flask respectively, is warmed up to 300 ℃ with the temperature rise rate of 4 ℃/min, is incubated 1 hour.During the reaction soln cool to room temperature, centrifugation 15min, the solid dispersed that obtains is washed in dehydrated alcohol, and recentrifuge repeats the powder Air drying 3 times.
Claims (2)
1, a kind of preparation method with ferromagnetic monodisperse nano-zinc oxide at room temperature, it is characterized in that: with molar percentage is that analytically pure zinc acetylacetonate and the commercially pure oleyl amine of 1:50-1:200 is placed in the container, be warmed up to 200~300 ℃, be incubated 0.5-2 hour, during the reaction soln cool to room temperature, centrifugation, obtain solid product, with dehydrated alcohol disperse once more, centrifugation, repeat 2~3 times after, at room temperature be dried to pressed powder.
2, according to right 1 described a kind of preparation method with ferromagnetic monodisperse nano-zinc oxide at room temperature, it is characterized in that: control reaction temperature obtains the monodisperse nano-zinc oxide powder of 7~10nm various grain sizes.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101979324A (en) * | 2010-11-02 | 2011-02-23 | 上海大学 | Method for preparing monodisperse zinc oxide microspheres |
CN102161499A (en) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | Quantum size zinc oxide and preparation method and application thereof |
CN103280532A (en) * | 2013-05-21 | 2013-09-04 | 华北电力大学 | Preparation method of polymer solar cell zinc oxide film with inverted structure |
CN113058623A (en) * | 2019-12-12 | 2021-07-02 | 中国科学技术大学 | Preparation method and application of molybdenum selenide-based nanocomposite |
-
2008
- 2008-12-11 CN CNA2008101629937A patent/CN101428843A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101979324A (en) * | 2010-11-02 | 2011-02-23 | 上海大学 | Method for preparing monodisperse zinc oxide microspheres |
CN101979324B (en) * | 2010-11-02 | 2012-05-02 | 上海大学 | Method for preparing monodisperse zinc oxide microspheres |
CN102161499A (en) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | Quantum size zinc oxide and preparation method and application thereof |
CN103280532A (en) * | 2013-05-21 | 2013-09-04 | 华北电力大学 | Preparation method of polymer solar cell zinc oxide film with inverted structure |
CN103280532B (en) * | 2013-05-21 | 2016-04-20 | 华北电力大学 | A kind of preparation method of reverse geometry polymer solar cells Zinc oxide film |
CN113058623A (en) * | 2019-12-12 | 2021-07-02 | 中国科学技术大学 | Preparation method and application of molybdenum selenide-based nanocomposite |
CN113058623B (en) * | 2019-12-12 | 2022-07-15 | 中国科学技术大学 | Preparation method and application of molybdenum selenide-based nanocomposite |
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