CN102659166B - Method for preparing CuO/Cu2O block composite material with room-temperature ferromagnetism - Google Patents
Method for preparing CuO/Cu2O block composite material with room-temperature ferromagnetism Download PDFInfo
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- CN102659166B CN102659166B CN201210157576.XA CN201210157576A CN102659166B CN 102659166 B CN102659166 B CN 102659166B CN 201210157576 A CN201210157576 A CN 201210157576A CN 102659166 B CN102659166 B CN 102659166B
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Abstract
The invention discloses a method for preparing a CuO/Cu2O block composite material with room-temperature ferromagnetism. The method comprises the following specific preparation processes of: A-, paving a high-purity CuO (99.99 percent) powder in a clean quartz boat; B-, putting the quartz boat in a tube furnace; heating along with the furnace to 950 DEG C; then, performing heat preservation for 0-8 hours under the atmosphere of 950 DEG C; and then, rapidly taking out the quartz boat or cooling along with the furnace to obtain the CuO/Cu2O block composite material with the room-temperature ferromagnetism. According to the method disclosed by the invention, the CuO/Cu2O block composite material with the room-temperature ferromagnetism is prepared by utilizing a high-temperature sintering CuO powder. The invention relates to a method of obtaining the intrinsic room-temperature ferromagnetism (the CuO/Cu2O block material is paramagnetic) by utilizing CuO and Cu2O in a nonmagnetic substance CuO/Cu2O block composite material. The method for preparing the CuO/Cu2O block composite material with the room-temperature ferromagnetism has the advantages that the required equipment (tube furnace) is simple; the raw materials are low in cost; the process is simple and easy to implement; the cost is low; the reaction condition is controllable; products and a byproduct (oxygen) are environmental-friendly; and the product yield is high.
Description
Technical field
The invention belongs to technical field of electronic materials, specifically one has room-temperature ferromagnetic CuO/Cu
2the preparation method of O block composite material.
Background technology
Along with the develop rapidly of electronics technology and electronic industry, investigator is just being devoted to introduce electron spinning at present in conventional electrical device, thereby makes the spin of electronics be applied to storage, transmission, process quantum information and become possibility.In to spin electric device performance history of new generation, dilute magnetic semiconductor owing to having magnetic substance and semi-conductive characteristic concurrently, be easy to be considered to the next generation and utilize the spin degree of freedom of electronics to make the main raw of microelectronic device with conventional semiconductor technology is compatible.In recent years, investigator both domestic and external has observed obvious room-temperature ferromagnetic in transient metal doped oxide system, and this makes the actual application prospect of dilute magnetic semiconductor device become optimistic.But up to the present in view of existing the cluster, magnetic second-phase, current carrier and the defect that comprise doped magnetic element to induce the multiple possible magnetic sources such as ferromegnetism in these dilute magnetic semiconductor systems that have been found that, make for the verifying and its ferromagnetic control is all become to complex of these dilute magnetic semiconductor magnetic source, thereby greatly affected the practical application of material.
2004, the people such as Coey were first at the HfO for doping
2in film, find Curie temperature higher than the ferrimagnetism of room temperature and proposed
d 0(electronic configuration of this type of material is generally
d 0or
d 10) ferromagnetic concept (M. Venkatesan, C. B. Fitzgerald, J. M. D. Coey.
nature 430,630 (2004); J. M. D. Coey, M. Venkatesan, C. B. Fitzgerald,
nat. Mater. 4, 173 (2005) .): he points out in the time that magnetic-doped concentration goes to zero, and the specific magnetising moment that experiment provides is also non-vanishing, seems a kind of magnetic moment relevant with defect to be activated by magnetic impurity in sample.Subsequently, researchist is in succession at pure ZnO, TiO
2, SnO
2, In
2o
3, Al
2o
3, also observed obvious room temperature ferromagnetic phenomenon in the system such as CuO, MgO.
d 0ferromagnetic occurred overturning before investigator's viewpoint, make to utilize magnetic element doping to obtain dilute magnetic semiconductor and become inessential means, simultaneously owing to having avoided the use of magnetic element, thereby get rid of the interference to sample magnetic source by magnetic second-phase or magnetic particle cluster.Cu and oxide compound thereof (CuO and Cu
2o) be at room temperature all paramagnetic characteristic, so thereby Cu has been used for doped oxide semiconductors in a large number as a kind of non magnetic ion realizes coupling (T. S. Herng, the D. C. Qi of the ferromagnetic and characteristic of semiconductor of room temperature, T. Berlijn, J. B. Yi, K. S. Yang, Y. Dai, Y. P. Feng, I. Santoso, C. H. Sanchez, X. Y. Gao, A. T. S. Wee, W. Ku, J. Ding, and A. Rusydi
physical Review Letters, 105,207201 (2010) .) and ferroelectric-ferromagnetic coupling (T.S. Herng, M.F. Wong, D.C. Qi, J.B. Yi, A, Kumar, A. Huang, F.C. Kartawidjaja, S. Smadici, P. Abbamonte, C. Sanchez-Hanke, S. Shannigrahi, J.M. Xue, J. Wang, Y.P. Feng, A. Rusydi, K.Y. Zeng, J. Ding
advanced Materials, 23,1635 (2011)) research.People have prepared CuO/Cu by collosol and gel and hydrothermal method at present
2o matrix material, but CuO/Cu prepared by this method
2o matrix material does not all have room-temperature ferromagnetic.
Summary of the invention
Technical problem to be solved by this invention is to provide one and prepares and have room-temperature ferromagnetic CuO/Cu
2the preparation method of O block composite material.
Adopt following technical scheme for solving technical problem of the present invention:
One has room-temperature ferromagnetic CuO/Cu
2the preparation method of O block composite material, concrete preparation technology is as follows:
A, by high-purity CuO(99.99%) powder is laid in clean quartz boat;
B, quartz boat is put into tube furnace, be warming up to 950 degrees Celsius with stove, then under 950 degrees Celsius of air atmosphere, be incubated after 0-8 hour, quartz boat is taken out or furnace cooling fast, obtain having the CuO/Cu of room-temperature ferromagnetic
2o block composite material.
The temperature rise rate of described tube furnace is 10 degrees celsius/minute.
The present invention utilizes high temperature sintering CuO powder to prepare to have room-temperature ferromagnetic CuO/Cu
2o block composite material is that one is utilized non-magnetic substance CuO/Cu
2in O block composite material, obtain room-temperature ferromagnetic (CuO and the Cu of intrinsic
2the block materials of O is paramagnetic characteristic) method.Due to its presoma CuO and last sintered product Cu
2o is at room temperature paramagnetic characteristic, this preparation method's condition is high temperature sintering simultaneously, and all samples all have the experiment condition being equal to except sintering time, so we can get rid of sample because preparation process is subject to ferromagnetic pollution, thereby obtain the attribute of sample intrinsic, regulate CuO and Cu in matrix material by the change of sintering time
2the ratio of O, the saturation magnetization of sample is with the increase first increases and then decreases of sintering time, and the sample of sintering after 2 hours has maximum saturation magnetization 0.04 emu/g.This invention, for the development and application of spintronics device provides material foundation, at spin fet, has potential commercial application prospect in spin resonance tunnelling device isospin electron device.The equipment simple (tube furnace) that the present invention requires, raw material cheapness, simple for process, cost is low, and reaction conditions is controlled, product and by product (oxygen) environmentally safe, product production is large.
accompanying drawing explanation
Fig. 1 is the thermogravimetric Heat Flow Analysis figure of high-purity CuO powder.
Fig. 2 is that sintering time is 0 hour, 1.5 hours, 2 hours, 4 hours, 6 hours, 8 hours lower CuO/Cu
2the X ray diffracting spectrum of O block composite material.
Fig. 3 (a) for sintering time be 0 hour, 1.5 hours, 2 hours, 4 hours, 6 hours, 8 hours lower CuO/Cu
2the room temperature mangneto loop line of O block composite material, 3 (b) for sintering time be 0 hour, 1.5 hours, 2 hours, 4 hours, 6 hours, 8 hours lower CuO/Cu
2the saturation magnetization of O block composite material is with the variation relation of sintering time.
Fig. 4 is that sintering time is 2 hours CuO/Cu
2the null field of O block composite material and have a cooling curve.
Fig. 5 is that sintering time is 2 hours CuO/Cu
2the scanning electron microscope picture of O block composite material.
Embodiment
Embodiment 1
By 1 gram of high-purity CuO(99.99%) powder is laid in clean quartz boat and puts into tube furnace, tube furnace temperature starts the speed rising with 10 degrees celsius/minute from room temperature, when temperature arrives 950 degrees Celsius time, quartz boat is taken out fast, obtain sample CuO(0h after cooling).
Utilize the structure of X-ray diffractometer assay products, as shown in Figure 2, result shows that product is pure monocline CuO structure, does not observe other dephasigns.Magnetic Measurement result shows that sample is at room temperature paramagnetic characteristic (shown in Fig. 3).
By 1 gram of high-purity CuO(99.99%) powder is laid in clean quartz boat and puts into tube furnace, tube furnace temperature starts to start to rise with the speed of 10 degrees celsius/minute from room temperature, when temperature arrives after being incubated 1.5 hours after 950 degrees Celsius, quartz boat is taken out fast, obtain CuO/Cu after cooling
2o block composite material.
Utilize the structure of X-ray diffractometer assay products, as shown in Figure 2, result shows that product is CuO and Cu
2the matrix material of O, along with the increase of sintering time, the diffraction peak of CuO phase weakens gradually, and Cu
2the diffraction peak of O phase strengthens gradually.Magnetic Measurement result shows the sintering CuO/Cu of 1.5 hours
2o matrix material has obvious room-temperature ferromagnetic, and its saturation magnetization is 0.02 emu/g.
Embodiment 3
Respectively by 1 gram of high-purity CuO(99.99%) powder is laid in clean quartz boat and puts into tube furnace, tube furnace temperature starts to start to rise with the speed of 10 degrees celsius/minute from room temperature, when temperature arrives after being incubated 2 hours after 950 degrees Celsius, quartz boat is taken out fast, obtain CuO/Cu after cooling
2o block composite material.
Utilize the structure of X-ray diffractometer assay products, as shown in Figure 2, result shows that product is CuO and Cu
2the matrix material of O, along with the increase of sintering time, the diffraction peak of CuO phase weakens gradually, and Cu
2the diffraction peak of O phase strengthens gradually.Magnetic Measurement result shows the sintering CuO/Cu of 2 hours
2o matrix material has maximum saturation magnetization 0.04 emu/g.Utilize superconducting quantum interference device (SQUID) to study the cold property of this sample.Figure 4 shows that null field and the extra show cooling curve of sample, interior (2~330 K) two curves of temperature range that result is presented at test never intersect, and this shows this CuO/Cu
2the Curie temperature of O matrix material, at least higher than 330 K, meanwhile, has a bag upwards centered by 220 K on the null field cooling curve of sample, it is corresponding to the Ne&1&el temperature of block CuO.Adopt the pattern of scanning electron microscopic observation sample, the sintering CuO/Cu of 2 hours as shown in Figure 5
2the particle size of O matrix material, between 7~10 microns, shows that it is block composite material.
By 1 gram of high-purity CuO(99.99%) powder is laid in clean quartz boat and puts into tube furnace, tube furnace temperature starts to start to rise with the speed of 10 degrees celsius/minute from room temperature, when temperature arrives after being incubated 4 hours after 950 degrees Celsius, quartz boat is taken out fast, obtain CuO/Cu after cooling
2o block composite material.
Utilize the structure of X-ray diffractometer assay products, as shown in Figure 2, result shows that product is CuO and Cu
2the matrix material of O, along with the increase of sintering time, the diffraction peak of CuO phase weakens gradually, and Cu
2the diffraction peak of O phase strengthens gradually.Magnetic Measurement result shows the sintering CuO/Cu of 4 hours
2o matrix material has obvious room-temperature ferromagnetic, and its saturation magnetization is 0.009emu/g.
Embodiment 5
By 1 gram of high-purity CuO(99.99%) powder is laid in clean quartz boat and puts into tube furnace, tube furnace temperature starts to start to rise with the speed of 10 degrees celsius/minute from room temperature, when temperature arrives after being incubated 6 hours after 950 degrees Celsius, quartz boat is taken out fast, obtain CuO/Cu after cooling
2o block composite material.
Utilize the structure of X-ray diffractometer assay products, as shown in Figure 2, result shows that product is CuO and Cu
2the matrix material of O, along with the increase of sintering time, the diffraction peak of CuO phase weakens gradually, and Cu
2the diffraction peak of O phase strengthens gradually.Magnetic Measurement result shows the sintering CuO/Cu of 6 hours
2o matrix material has obvious room-temperature ferromagnetic, and its saturation magnetization is 0.003 emu/g.
By 1 gram of high-purity CuO(99.99%) powder is laid in clean quartz boat and puts into tube furnace, tube furnace temperature starts to start to rise with the speed of 10 degrees celsius/minute from room temperature, after temperature arrives 950 degrees Celsius, be incubated 8 hours, after furnace cooling, obtain sample Cu
2o(8 h).
Utilize the structure of X-ray diffractometer assay products, as shown in Figure 2, result shows that product is pure cube Cu
2o structure, does not observe other dephasigns.Magnetic Measurement result shows that sample is at room temperature paramagnetic characteristic (shown in Fig. 3).
Claims (2)
1. one kind has room-temperature ferromagnetic CuO/Cu
2the preparation method of O block composite material, concrete preparation technology is as follows:
A, 99.99% high-purity CuO powder is laid in clean quartz boat;
B, quartz boat is put into tube furnace, be warming up to 950 degrees Celsius with stove, then under 950 degrees Celsius of air atmosphere, be incubated after 0-8 hour, quartz boat is taken out or furnace cooling fast, obtain having the CuO/Cu of room-temperature ferromagnetic
2o block composite material.
2. one according to claim 1 has room-temperature ferromagnetic CuO/Cu
2the preparation method of O block composite material, is characterized in that: in described step B, the temperature rise rate of tube furnace is 10 degrees celsius/minute.
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CN110436529B (en) * | 2019-09-08 | 2022-02-15 | 兰州大学第一医院 | Fe for magnetic thermal therapy3O4Preparation method of nano rod material |
Citations (2)
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CN102070181A (en) * | 2011-01-14 | 2011-05-25 | 浙江大学 | Preparation method of cuprous oxide |
CN102180509A (en) * | 2011-03-28 | 2011-09-14 | 浙江理工大学 | Method for preparing hollow CuO/Cu2O spheres with controllable ingredients |
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CN102070181A (en) * | 2011-01-14 | 2011-05-25 | 浙江大学 | Preparation method of cuprous oxide |
CN102180509A (en) * | 2011-03-28 | 2011-09-14 | 浙江理工大学 | Method for preparing hollow CuO/Cu2O spheres with controllable ingredients |
Non-Patent Citations (2)
Title |
---|
L.Liao et al..P-type electrical |
P-type electrical, photoconductive, and anomalous ferromagnetic properties of Cu2O nanowires;L. Liao, et al.;《Applied Physics Letters》;20090317;第113106-1页右栏第1段至第113106-3页右栏第1段 * |
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