CN105084330A - Ferromagnetic semiconductor material Li (Cd, Mn) P and preparation method thereof - Google Patents
Ferromagnetic semiconductor material Li (Cd, Mn) P and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a ferromagnetic semiconductor material having the formula of Liy (Cd1-xMnx) P, wherein y is greater than 0.6 and less than 1.4, and x is greater than 0 and less than 0.4. The present invention also provides a preparation method of the ferromagnetic semiconductor material, the Liy (Cd1-xMnx) P is prepared by sintering a precursor in an oxygen-isolated environment by solid phase reaction method, wherein y is greater than 0.6 and less than 1.4, x is greater than 0 and less than 0.4, and the sintering temperature is 550-950 DEG C.
Description
Technical field
The present invention relates to a kind of ferromagnetic semiconductor material based on I-II-V race semiconductor material, particularly relate to the ferromagnetic semiconductor material that a kind of chemical structure of general formula is Li (Cd, Mn) P.
Background technology
Ferromegnetism dilute magnetic semiconductor is by realizing to doped magnetic ion in semi-conductor.Due to the application prospect of spin electric device aspect, as far back as the nineties in 20th century ferromegnetism dilute magnetic semiconductor system be just widely studied (Zutic, I.etal., Rev.Mod.Phys.76,323,2004).Studying so far is dilute magnetic semiconductor based on iii-v the most widely, namely with the semi-conductor (Ohno, H., Science281,951,1998) that III element V group element compound is parent phase.But also there is manufacture craft in iii-v dilute magnetic semiconductor, the problems such as current carrier and magnetic moment binding.
The ferromegnetism dilute magnetic semiconductor Li (Zn based on I-II-V race semiconductor material of nearest report, Mn) As more successfully solves the problem (Deng that current carrier and magnetic moment are bound, Z.etal., NatureCommunications2:422,2011), current carrier wherein and magnetic moment are provided by Li ion and Mn ion respectively, and this is that the research of ferromagnetic semiconductor mechanism is provided convenience.
Can be put to practical semiconductor material needs carrier type and concentration to be controlled, so just can be obtained the material of expection by doping.Wherein one of of paramount importance application is exactly elementary cell PN junction electron doping semi-conductor and hole property doped semiconductor being combined to form transistor.But the carrier concentration of Li (Zn, Mn) As is about 10
19-10
20cm
-3, its electrical conductive behavior all shows as very strong metallicity.This means, by its carrier type of very difficult change, also just cannot obtain PN junction.
In addition, containing toxic element As in Li (Zn, Mn) As, in the use and manufacturing processed of material, the somatic damage of personnel is easily caused.
Summary of the invention
Therefore, the object of the invention is to the defect overcoming above-mentioned prior art, provide a kind of ferromegnetism dilute magnetic semiconductor based on I-II-V race semiconductor material, its semiconductive is stronger, and carrier type and concentration are more easily conditioned, and not containing toxic element As.
The invention provides a kind of ferromagnetic semiconductor material, its chemical formula is Li
y(Cd
1-xmn
x) P, wherein 0.6<y<1.4,0<x<0.4.
According to ferromagnetic semiconductor material provided by the invention, the crystalline structure of wherein said ferromagnetic semiconductor material belongs to isometric system.
The present invention also provides a kind of method preparing above-mentioned ferromagnetic semiconductor material, utilizes solid reaction process, in the environment of isolating with oxygen, sinter precursor, forms Li
y(Cd
1-xmn
x) P, wherein 0.6<y<1.4,0<x<0.4, the material of wherein said precursor is selected from the group of following material formation: Li, Cd, Mn, P, Li
3p, CdP, MnP, wherein the content of various material meets ferromagnetic semiconductor material Li to be prepared
y(Cd
1-xmn
x) proportioning of various element in P, wherein sintering temperature is 550-950 DEG C.
According to method provided by the invention, wherein said sintering process is carried out at ambient pressure, and sintering temperature is 600-900 DEG C.
According to method provided by the invention, wherein said sintering process is carried out under higher than an atmospheric pressure, and sintering temperature is 550-950 DEG C.
According to method provided by the invention, wherein said pressure is 1-20GPa.
According to method provided by the invention, wherein said precursor comprises Li, Cd, Mn, P.
According to method provided by the invention, wherein said precursor comprises Li
3p, Cd, Mn, P, CdP, MnP.
According to method provided by the invention, wherein said sintering process is carried out in rare gas element.
According to method provided by the invention, wherein said sintering process is carried out in vacuum environment.
Ferromagnetic semiconductor Li (Cd provided by the invention, Mn) no longer toxic element As is contained in P, and comparatively As element is higher due to the electronegativity of P element, and the positive polarity of Cd element is stronger than Zn element, make Li (Cd, Mn) P has good semiconductive, and carrier concentration more easily regulates, and can perform well in the various devices such as spin electric device.
Accompanying drawing explanation
Referring to accompanying drawing, embodiments of the present invention is further illustrated, wherein:
Fig. 1 is the crystalline structure schematic diagram of ferromagnetic semiconductor provided by the invention;
Fig. 2 is Li in embodiment 1
0.6cd
0.9mn
0.1the temperature variant graphic representation of resistivity of P;
Fig. 3 is Li in embodiment 1
0.6cd
0.9mn
0.1the X ray diffracting spectrum of P;
Fig. 4 is Li in embodiment 1
0.6cd
0.9mn
0.1the temperature variant graphic representation of DC magnetic susceptibility of P;
Fig. 5 is Li in embodiment 2
1.4cd
0.6mn
0.4the temperature variant graphic representation of resistivity of P;
Fig. 6 is Li in embodiment 2
1.4cd
0.6mn
0.4the X ray diffracting spectrum of P;
Fig. 7 is Li in embodiment 2
1.4cd
0.6mn
0.4the temperature variant graphic representation of DC magnetic susceptibility of P;
Fig. 8 is Li in embodiment 3
1.2cd
0.95mn
0.05the temperature variant graphic representation of resistivity of P;
Fig. 9 is Li in embodiment 3
1.2cd
0.95mn
0.05the X ray diffracting spectrum of P;
Figure 10 is Li in embodiment 3
1.2cd
0.95mn
0.05the DC magnetic susceptibility of P varies with temperature graphic representation;
Figure 11 is Li in embodiment 4
1.1cd
0.9mn
0.1the temperature variant graphic representation of resistivity of P;
Figure 12 is Li in embodiment 4
1.1cd
0.9mn
0.1the X ray diffracting spectrum of P;
Figure 13 is Li in embodiment 4
1.1cd
0.9mn
0.1the temperature variant graphic representation of DC magnetic susceptibility of P;
Figure 14 is Li in embodiment 5
0.6cd
0.8mn
0.2the temperature variant graphic representation of resistivity of P;
Figure 15 is Li in embodiment 5
0.6cd
0.8mn
0.2the X ray diffracting spectrum of P;
Figure 16 is Li in embodiment 5
0.6cd
0.8mn
0.2the temperature variant graphic representation of DC magnetic susceptibility of P;
Figure 17 is Li in embodiment 6
1.4cd
0.6mn
0.4the temperature variant graphic representation of resistivity of P;
Figure 18 is Li in embodiment 6
1.4cd
0.6mn
0.4the X ray diffracting spectrum of P;
Figure 19 is Li in embodiment 6
1.4cd
0.6mn
0.4the temperature variant graphic representation of DC magnetic susceptibility of P;
Figure 20 is Li in embodiment 7
1.05cd
0.7mn
0.3the temperature variant graphic representation of resistivity of P;
Figure 21 is Li in embodiment 7
1.05cd
0.7mn
0.3the X ray diffracting spectrum of P;
Figure 22 is Li in embodiment 7
1.05cd
0.7mn
0.3the temperature variant graphic representation of DC magnetic susceptibility of P.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with specific embodiment, the present invention is described in more detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The invention provides a kind of ferromagnetic semiconductor material based on I-II-V race semiconductor material, its chemical structure of general formula is Li
y(Cd
1-xmn
x) P, wherein 0.6<y<1.4,0<x<0.4, x, y represent atom percentage content.Li
y(Cd
1-xmn
x) P crystalline structure as shown in Figure 1, there is the space symmetr group of F-43m, belong to isometric system, lattice constant range is:
Embodiment 1
The present embodiment provides a kind of preparation method of ferromagnetic semiconductor material, comprising:
1) in inert gas filled glove box by high-purity Li block, Cd powder, Mn powder, P powder according to predetermined proportion (Li
0.6cd
0.9mn
0.1p, quality is respectively Li block 0.21 gram, 5.06 grams, Cd powder, 0.27 gram, Mn powder, 1.55 grams, P powder) Homogeneous phase mixing, and mixture is loaded in alumina-ceramic test tube;
2) the ceramic test tube Vacuum Package of sample will be housed in silica tube;
3) sinter 20 hours under silica tube being placed on the temperature of in High Temperature Furnaces Heating Apparatus 600 DEG C, after having sintered, obtain Li
0.6cd
0.9mn
0.1p.
The resistivity of the sample that the method for the present embodiment obtains varies with temperature behavior as shown in Figure 2, shows good semiconductive.As shown in Figure 3, all diffraction peaks can find the corresponding indices of diffraction to the X ray diffracting spectrum of sample, illustrate that method that the present embodiment provides has prepared the good ferromagnetic semiconductor material Li of high purity, crystallinity
0.6cd
0.9mn
0.1p.The DC magnetic susceptibility of sample and the relation curve of temperature are as Fig. 4, and ferromagnetic transformation temperature is 12K.
Embodiment 2
The present embodiment provides a kind of preparation method of ferromagnetic semiconductor material, comprising:
1) in inert gas filled glove box by high-purity Li block, Cd powder, Mn powder, P powder according to predetermined proportion (Li
1.4cd
0.6mn
0.4p, quality is respectively Li block 0.49 gram, 3.37 grams, Cd powder, 1.10 grams, Mn powder, 1.55 grams, P powder) Homogeneous phase mixing, and mixture is loaded in alumina-ceramic test tube;
2) the ceramic test tube Vacuum Package of sample will be housed in silica tube, and be filled with a certain amount of rare gas element in silica tube;
3) sinter 5 hours under silica tube being placed on the temperature of in High Temperature Furnaces Heating Apparatus 900 DEG C, after having sintered, obtain Li
1.4cd
0.6mn
0.4p.
The resistivity of the sample that the method for the present embodiment obtains varies with temperature behavior as shown in Figure 5, shows good semiconductive.As shown in Figure 6, all diffraction peaks can find the corresponding indices of diffraction to the X ray diffracting spectrum of sample, illustrate that ferromagnetic semiconductor material purity prepared by the method that the present embodiment provides is high, crystallinity is good.As shown in Figure 7, ferromagnetic transformation temperature is 25K for the DC magnetic susceptibility of sample and the relation curve of temperature.
Embodiment 3
The present embodiment provides a kind of preparation method of ferromagnetic semiconductor material, comprising:
1) in inert gas filled glove box by high-purity Li
3p, P, Cd, Mn, CdP, MnP are according to predetermined proportion (Li
1.2cd
0.95mn
0.05p, quality is respectively Li
3p1.24 gram, P0.20 gram, Cd3.37 gram, Mn0.20 gram, CdP3.87 gram, MnP0.21 gram) Homogeneous phase mixing, mixture is loaded niobium pipe, and by the niobium seal of tube under the protection of rare gas element;
2) by niobium pipe Vacuum Package in silica tube;
3) sinter 15 hours under silica tube being placed on the temperature of in High Temperature Furnaces Heating Apparatus 750 DEG C, after having sintered, obtain Li
1.2cd
0.95mn
0.05p.
The resistivity of the sample that the method for the present embodiment obtains varies with temperature behavior as shown in Figure 8, shows good semiconductive.As shown in Figure 9, all diffraction peaks can find the corresponding indices of diffraction to the X ray diffracting spectrum of sample, illustrate that ferromagnetic semiconductor material purity prepared by the method that the present embodiment provides is high, crystallinity is good.As shown in Figure 10, ferromagnetic transformation temperature is 28K. for the DC magnetic susceptibility of sample and the relation curve of temperature
Embodiment 4
The present embodiment provides a kind of preparation method of ferromagnetic semiconductor material, comprising:
1) in inert gas filled glove box by high-purity Li
3p, P, Cd, Mn, CdP, MnP are according to predetermined proportion (Li
1.1cd
0.9mn
0.1p, quality is respectively Li
3p1.14 gram, P0.25 gram, Cd3.03 gram, Mn0.16 gram, CdP3.87 gram, MnP0.26 gram) Homogeneous phase mixing, mixture is loaded niobium pipe, and by the niobium seal of tube under the protection of rare gas element;
2) by niobium pipe Vacuum Package in silica tube;
3) 20 hours are sintered under silica tube being placed on the temperature of in High Temperature Furnaces Heating Apparatus 750 DEG C;
4) under the protection of rare gas element, grinding mixing and compressing tablet by obtaining sample after having sintered, mixture being loaded in niobium pipe, and by the niobium seal of tube under the protection of rare gas element;
5) by niobium pipe Vacuum Package in silica tube;
6) sinter 20 hours under silica tube being placed on the temperature of in High Temperature Furnaces Heating Apparatus 750 DEG C, obtain Li
1.1cd
0.9mn
0.1p.
The resistivity of the sample that the present embodiment provides varies with temperature behavior as shown in figure 11, shows good semiconductive.As shown in figure 12, all diffraction peaks can find the corresponding indices of diffraction to the X ray diffracting spectrum of sample, illustrate that ferromagnetic semiconductor material purity prepared by the method that the present embodiment provides is high, crystallinity is good.As shown in figure 13, ferromagnetic transformation temperature is 30K for the DC magnetic susceptibility of sample and the relation curve of temperature.
Embodiment 5
The present embodiment provides a kind of preparation method of ferromagnetic semiconductor material, comprising:
1) in inert gas filled glove box by high-purity Li block, Cd powder, Mn powder, P powder according to predetermined proportion (Li
0.6cd
0.8mn
0.2p, quality is respectively Li block 0.025 gram, 0.540 gram, Cd powder, 0.066 gram, Mn powder, 0.186 gram, P powder) Homogeneous phase mixing, load high pressure assembly;
2) high pressure assembly is put into high-tension unit and carry out high-pressure sinter.Sintering procedure is slowly boost to 1GPa under room temperature, restarts heating schedule and is heated to 550 DEG C, and be down to room temperature be incubated 2 hours under high-temperature and high-pressure conditions after, then release, obtains Li
0.6cd
0.8mn
0.2p.
The resistivity of the sample that the method for the present embodiment obtains varies with temperature behavior as shown in figure 14, shows good semiconductive.As shown in figure 15, all diffraction peaks can find the corresponding indices of diffraction to the X ray diffracting spectrum of sample, illustrate that ferromagnetic semiconductor material purity prepared by the method that the present embodiment provides is high, crystallinity is good.As shown in figure 16, ferromagnetic transformation temperature is 13K for the DC magnetic susceptibility of sample and the relation curve of temperature.
Embodiment 6
The present embodiment provides a kind of preparation method of ferromagnetic semiconductor material, comprising:
1) in inert gas filled glove box by high-purity Li
3p, P, Cd, Mn, CdP, MnP are according to predetermined proportion (Li
1.4cd
0.6mn
0.4p, quality is respectively Li
3p0.145 gram, P0.025 gram, Cd0.202 gram, Mn0.099 gram, CdP0.258 gram, MnP0.052 gram) Homogeneous phase mixing, load high pressure assembly;
2) high pressure assembly is put into high-tension unit and carry out high-pressure synthesis.Sintering procedure is slowly boost to 8GPa under room temperature, restarts heating schedule and is heated to 950 DEG C, and be down to room temperature be incubated 0.1 hour under high-temperature and high-pressure conditions after, then release, obtains Li
1.4cd
0.6mn
0.4p.
The resistivity of the sample that the method for the present embodiment obtains varies with temperature behavior as shown in figure 17, shows good semiconductive.As shown in figure 18, all diffraction peaks can find the corresponding indices of diffraction to the X ray diffracting spectrum of sample, illustrate that ferromagnetic semiconductor material purity prepared by the method that the present embodiment provides is high, crystallinity is good.As shown in figure 19, ferromagnetic transformation temperature is 8K for the DC magnetic susceptibility of sample and the relation curve of temperature.
Embodiment 7
The present embodiment provides a kind of preparation method of ferromagnetic semiconductor material, comprising:
1) in inert gas filled glove box by high-purity Li
3p, P, Cd, Mn, CdP, MnP are according to predetermined proportion (Li
1.05cd
0.7mn
0.3p, quality is respectively Li
3p0.109 gram, P0.028 gram, Cd0.236 gram, Mn0.049 gram, CdP0.301 gram, MnP0.077 gram) Homogeneous phase mixing, load high pressure assembly;
2) high pressure assembly is put into high-tension unit and carry out high-pressure synthesis.Sintering procedure, at room temperature slowly to boost to 20GPa, is restarted heating schedule and is heated to 700 DEG C, is down to room temperature, then release after being incubated 1 hour under high-temperature and high-pressure conditions;
3) under the protection of rare gas element, grinding mixing by obtaining sample, again loading high pressure assembly;
4) high pressure assembly is put into high-tension unit and carry out high-pressure synthesis.Sintering procedure, at room temperature slowly to boost to 20GPa, is restarted heating schedule and is heated to 700 DEG C, and be down to room temperature be incubated 1 hour under high-temperature and high-pressure conditions after, then release, obtains Li
1.05cd
0.7mn
0.3p.
The resistivity of the sample that the method for the present embodiment obtains varies with temperature behavior as shown in figure 20, shows good semiconductive.As shown in figure 21, all diffraction peaks can find the corresponding indices of diffraction to the X ray diffracting spectrum of sample, illustrate that ferromagnetic semiconductor material purity prepared by the method that the present embodiment provides is high, crystallinity is good.As shown in figure 22, ferromagnetic transformation temperature is 12.5K for the DC magnetic susceptibility of sample and the relation curve of temperature.
Each embodiment above-mentioned utilizes the solid reaction process under normal pressure (normal atmosphere) or high pressure (higher than a normal atmosphere) successfully to synthesize according to ferromagnetic semiconductor material Li of the present invention
y(Cd
1-xmn
x) P, 0.6<y<1.4,0<x<0.4.The ratio of the various materials in the precursor adopted in the method that wherein the various embodiments described above provide is only exemplary, and not intended to be limits the protection domain of the application, and those skilled in the art can easily according to the Li of required synthesis
y(Cd
1-xmn
x) concrete x and y value in P and determine the ratio of the weight of various material in precursor.
Adopt the mixture of simple substance Li, simple substance Cd, simple substance Mn and simple substance P as precursor in above-described embodiment 1,2 and 5, in the precursor adopted in embodiment 3,4,6,7, include compound L i
3p, CdP, MnP, all successfully synthesized according to ferromagnetic semiconductor material Li of the present invention
y(Cd
1-xmn
x) P.
According to other embodiments of the invention, ferromagnetic semiconductor material Li is synthesized
y(Cd
1-xmn
x) presoma that adopts of the solid phase method of P is the mixture of Li source material, Cd source material, Mn source material, P source material.Wherein Li source material, Cd source material, Mn source material, P source material can be simple substance, also can be compound, such as Li
3p, CdP, MnP.
According to other embodiments of the invention, wherein the container of splendid attire precursor is not limited to the alumina-ceramic test tube, niobium pipe etc. that adopt in above-described embodiment, also can be in other corrosion-resistant container, as BN pipe etc.
According to other embodiments of the invention; wherein the splendid attire mode of precursor in sintering process is not limited to the mode that provides in above-described embodiment; only need meet precursor to sinter under the environment of isolating with oxygen, such as, sinter under the protection of rare gas element, or sinter under vacuum conditions.
According to other embodiments of the invention, wherein normal pressure-sintered formation ferromagnetic semiconductor material Li
y(Cd
1-xmn
x) temperature of P is preferably 600-900 DEG C, sintering time is preferably more than 5 hours.
According to other embodiments of the invention, wherein high-pressure sinter forms ferromagnetic semiconductor material Li
y(Cd
1-xmn
x) temperature of P is preferably 550-950 DEG C, sintering time is preferably more than 0.1 hour, and sintering pressure, higher than a normal atmosphere, is preferably 1-20GPa.
According to other embodiments of the invention, the sintering process wherein under normal pressure and high pressure preferably carries out double sintering as embodiment 4 and 7, also can sinter repeatedly.
Ferromagnetic semiconductor material provided by the invention, its ferromagnetic transformation temperature is about below 30K, and the material of specific components has the ferromagnetic transformation temperature of 30K, and material shows good semiconductive at full warm area.
In ferromagnetic semiconductor material provided by the invention, instead of Zn and As in Li (Zn, Mn) As with Cd and P respectively, because the positive polarity of Cd element is stronger than Zn element, comparatively As element is higher for the electronegativity of P element, obtains material Li (Cd, the Mn) P that semiconductive is stronger.Carrier type and concentration in Li (Cd, Mn) P are more easily conditioned, and this is that the application of material provides guarantee.It is worth mentioning that not containing toxic element As in Li (Cd, Mn) P, is a kind of eco-friendly material.
It should be noted last that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted.Although with reference to embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, modify to technical scheme of the present invention or equivalent replacement, do not depart from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (10)
1. a ferromagnetic semiconductor material, its chemical formula is Li
y(Cd
1-xmn
x) P, wherein 0.6<y<1.4,0<x<0.4.
2. ferromagnetic semiconductor material according to claim 1, the crystalline structure of wherein said ferromagnetic semiconductor material belongs to isometric system.
3. prepare a method for ferromagnetic semiconductor material as claimed in claim 1, utilize solid reaction process, in the environment of isolating with oxygen, sinter precursor, form Li
y(Cd
1-xmn
x) P, wherein 0.6<y<1.4,0<x<0.4,
The material of wherein said precursor is selected from the group of following material formation: Li, Cd, Mn, P, Li
3p, CdP, MnP, wherein the content of various material meets ferromagnetic semiconductor material Li to be prepared
y(Cd
1-xmn
x) proportioning of various element in P, wherein sintering temperature is 550-950 DEG C.
4. method according to claim 3, wherein said sintering process is carried out at ambient pressure, and sintering temperature is 600-900 DEG C.
5. method according to claim 3, wherein said sintering process is carried out under higher than an atmospheric pressure, and sintering temperature is 550-950 DEG C.
6. method according to claim 5, wherein said pressure is 1-20GPa.
7. method according to claim 3, wherein said precursor comprises Li, Cd, Mn, P.
8. method according to claim 3, wherein said precursor comprises Li
3p, Cd, Mn, P, CdP, MnP.
9. method according to claim 3, wherein said sintering process is carried out in rare gas element.
10. method according to claim 3, wherein said sintering process is carried out in vacuum environment.
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Cited By (1)
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| CN110459377A (en) * | 2018-05-07 | 2019-11-15 | 中国科学院物理研究所 | A kind of ferromagnetic material and preparation method thereof with huge Negative magnetoresistance effect |
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Application publication date: 20151125 |