CN101104949A - Zn(1-x)Mn(x)O crystal thin film with cube phase and rock salt ore structure - Google Patents
Zn(1-x)Mn(x)O crystal thin film with cube phase and rock salt ore structure Download PDFInfo
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- CN101104949A CN101104949A CNA2007100680946A CN200710068094A CN101104949A CN 101104949 A CN101104949 A CN 101104949A CN A2007100680946 A CNA2007100680946 A CN A2007100680946A CN 200710068094 A CN200710068094 A CN 200710068094A CN 101104949 A CN101104949 A CN 101104949A
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Abstract
The invention provides a Zn1-xMnxO film with cubic phase and rock salt ore structure and the preparation method thereof, belonging to the technical field of preparation of oxide diluted magnetic semiconductors. The invention is characterized in that the invention is implemented by electron beam reactive evaporation method, utilizes (MnO)y(ZnO)1-y ceramic target with high MnO content (y is molar ratio and equal to 0.2-0.3) as evaporation source and high-purity Ar/O2 mixed gas as reactant gas, and produces Zn1-xMnxO film with cubic phase and rock salt ore structure on a quartz glass substrate, wherein the Mn content (x, atom number ratio) in the film is 0.6-1.0, the optical bandgap of the film is continuously adjustable within a range of 4.5-5.7eV, and has the Zn1-xMnxO film with cubic phase and rock salt ore structure in the 200-1000nm thickness.
Description
Technical field
The invention belongs to the preparing technical field of oxide lanthanon magnetic semiconductor crystal film, be specifically related to a kind of on the silica glass substrate growth to visible light highly transparent, optical band gap continuously adjustable Zn in 4.5～5.7eV scope with a cube phase, salt mine structure
1-xMn
xO film and preparation technology thereof.
Technical background
In recent years, very popular to the research of dilute magnetic semiconductor (DMS) material in the world, this is because compare with common non magnetic semiconductor material, dilute magnetic semiconductor material has elementary charge degree of freedom and the electron spinning degree of freedom that can regulate simultaneously, thereby comprises in magneto-optic, the magnetoelectricity device that at novel spintronics device important application will be arranged.Especially, quite active to the research of zno-based DMS material in the world, this is because broad-band gap (3.37eV under the room temperature) characteristic of ZnO will make the Curie temperature of zno-based DMS material surpass room temperature.It is same because the broad-band gap characteristic of ZnO will make transition metal element doped ZnO material still have the feature to visible transparent.But preparation-obtained up to now zno-based DMS material for example adopts laser molecular beam epitaxy (S.W.Jung, S.-J.An, G.C.Yi, C.U.Jung, S.I.Lee, S.Cho, Ferromagneticproperties of Zn
1-xMn
xO epitaxial thin films, Applied Physics Letters, 80 (2002) 4561), pulsed laser deposition (T.Fukumura, Z.Jin, M.Kawasaki, T.Shono, T.Hasegawa, S.Koshihara, H.Koinuma, Magnetic properties of Mn-doped ZnO, Applied Physics Letters, 78 (2001) 958; M.Ivill, S.J.Pearton, D.P.Norton, J.Kelly, A.F.Hebard, Magnetization dependence on electron density inepitaxial ZnO thin films codoped with Mn and Sn, Journal ofApplied Physics, 97 (2005) 053904), metal organic chemical vapor deposition (E.Chikoidze, Y.Dumont, F.Jomard, D.Ballutaud, P.Galtier, O.Gorochov, D.Ferrand, Semiconducting and magnetic properties of Zn
1-xMn
xO films grown bymetalorganic chemical vapor deposition, Journal of Applied Physics, 97 (2005) 10D327), magnetron sputtering (X.M.Cheng, C.L.Chien, Magnetic properties of epitaxial Mn-doped ZnO thin films, Journal ofApplied Physics, 93 (2003) 7876) etc. the prepared adulterated ZnO of Mn of method (is Zn
1-xMn
xO) material, its crystalline structure are six side's phases, the wurtzite structure of class ZnO, and for the cubic structure Zn with single crystalline phase
1-xMn
xThe O material, not seeing as yet so far has report.In fact, Zn
1-xMn
xThe O material also might form cube phase, the salt mine crystalline structure of class MnO except six side's phases that can form class ZnO, wurtzite structure, this depends on Zn on the one hand
1-xMn
xThe content x of Mn in the O material also depends on the processing condition of material preparation on the other hand.At first, from the doping angle, when Mn content x is low (x＜0.45 usually), Mn is incorporated into the ZnO lattice as substitutional impurity (Mn that promptly mixes replaces the position of Zn in the ZnO lattice), forms six side's phases, the wurtzite structure Zn of class ZnO structure
1-xMn
xO; When Mn content x is higher (x＞0.5 usually), then Zn is incorporated into the MnO lattice as impurity component, finally forms cube phase, the salt mine structure Zn of class MnO structure
1-xMn
xO; And o'clock often obtain six sides in 0.45＜x＜0.5 mutually and a cube Zn who coexists mutually
1-xMn
xThe O material.Secondly, from the angle of material growth conditions, form the wurtzite structure Zn of c-axle preferrel orientation
1-xMn
xThe required energy of O material is lower, and to have a minimum surface can this feature relevant with (0001) crystal face of wurtzite structure material for this, Zn in relatively low growth temperature and under than the high growth rates condition
1-xMn
xThe O material grows up to the crystalline structure of six side's phases, wurtzite easily; And to make other crystal faces as (100) face and (110) face preferential growth, then need higher relatively underlayer temperature, higher reaction particle energy and lower growth velocity.Therefore, actually or the height of Mn content x and growth conditions whether suitably for form the six sides Zn of cube phase mutually at early growth period
1-xMn
xThe O nucleus is very crucial.If can successfully prepare transition metal element doped cube phase zno-based DMS material, for example Zn of cube phase, salt mine structure
1-xMn
xThe O material for the structure diversity that enriches the zno-based material, study it and form mutual relationship between mechanism and microstructure and the magnetic properties or the like, all has great scientific meaning and using value.
Summary of the invention
The object of the invention provides a kind of transition metal element doped cube phase zno-based DMS material of preparing, and has cube phase of class MnO, the Zn of salt mine structure
1-xMn
xO film and preparation method thereof enriches the structure diversity of zno-based material.
The Zn of of the present invention cube of phase, salt mine structure
1-xMn
xThe O film, the Mn content x in the film is adjustable continuously in 0.6～1.0 scope, and x is meant the normalization method atom number ratio of Zn and Mn element, and the optical band gap of film is adjustable continuously in 4.5～5.7eV scope, and thickness is adjustable continuously in 200～1000nm scope.
The Zn of of the present invention cube of phase, salt mine structure
1-xMn
xThe preparation technology of O film is the method that adopts electric beam evaporation, with (MnO)
y(ZnO)
1-y(y=0.2～0.3) ceramic target is a source material, with highly purified Ar/O
2Gas mixture is a reactant gases, and growing on the silica glass substrate obtains.
The Zn of of the present invention cube of phase, salt mine structure
1-xMn
xO thin film preparation process step is as follows:
(1) quartz substrate of cleaning is packed into substrate holder in the growth room is put (MnO)
y(ZnO)
1-yTarget separates target and substrate with baffle plate in crucible.
(2) take out the growth room to≤1 * 10 with the vacuum pump unit
-3The vacuum tightness of Pa.
(3) substrate is heated to 500 ℃, is incubated 15 minutes, make the residue desorb that is adsorbed on substrate surface to obtain the growth surface that cleans.While unlocking electronic rifle high pressure, the bundle spot position of regulating electron beam gather 4～5mA so that heat target with electron beam, to its degasification to target material surface.
(4) underlayer temperature is turned down certain suitable growth temperature from 500 ℃, charge into highly purified Ar/O
2Gas mixture makes charging into Ar/O
2Air pressure in the growth room behind the gas mixture is 2.5～3.5 * 10
-2The Pa scope.Strengthen electron beam line to 20～30mA then, (MnO)
y(ZnO)
1-yThe target start vaporizer, by regulate electron beam spot area, position and line size make target evenly, evaporation stably, the vapour pressure of target is controlled at 1.0～2.0 * 10
-2The Pa scope is opened baffle plate growth Zn
1-xMn
xThe O crystal film.
(5) a certain value in thickness reaches 200～1000nm scope finishes growth, treats that underlayer temperature reduces to 100 ℃ and close gas mixture, treats to take out sample after underlayer temperature is reduced to room temperature.
Processing step of the present invention is mentioned (MnO) in (1)
y(ZnO)
1-yCeramic target is to be prepared from according to certain molar ratio mixing, compacting and through 600 ℃ vacuum sintering technology by the ZnO of purity 99.99% and MnO powder, and wherein the shared molar percentage of MnO is y=0.2～0.3.
The suitable underlayer temperature of mentioning in the processing step of the present invention (4) is certain temperature between 350 ℃～450 ℃.
The Ar/O that mentions in the processing step of the present invention (4)
2Gas mixture is that employing purity is 99.99% Ar gas and O
2Gas mixes, wherein Ar gas and O
2The volume percent of gas is 1: 1～3: the 1 a certain ratio in the scope.
Mention in the processing step of the present invention (4), fill into the Ar/O in the growth room before the film growth
2The partial pressure of gas mixture is 2.5 * 10
-2Pa～3.5 * 10
-2In the Pa scope, can control the partial pressure of gas mixture by the airshed that needle-valve is regulated gas mixture.
(MnO) that mentions in the processing step of the present invention (4), evaporate by high-power electron beam during film growth
y(ZnO)
1-yThe vapour pressure of target is 1.0 * 10
-2Pa～2.0 * 10
-2Pa can control by line and two parameters of bundle spot sweep rate of regulating electron beam gun.
Mention in the processing step of the present invention (4), during film growth the line of high-power electron beam in 20mA～30mA scope.
Of the present invention cube of phase Zn
1-xMn
xThe technology of preparing of O film realizes in the electric beam evaporation depositing system, with this method six sides Zn mutually that grows
1-xMn
xAdopt relatively low (MnO) of MnO content during the O film
y(ZnO)
1-yTarget (usually y≤0.1), charge into O
2And underlayer temperature lower (200～300 ℃ of scopes), target vapour pressure are big (2.0～4.0 * 10
-2The Pa scope) etc. process parameter is compared, growth cube phase Zn
1-xMn
xNeed adopt MnO content higher relatively (MnO) during the O film
y(ZnO)
1-yTarget (y=0.2～0.3), in the growth room, charge into Ar/O
2Gas mixture, and underlayer temperature higher relatively (350～450 ℃ of scopes), and the target partial pressure in the reaction chamber is relatively low (1.0～2.0 * 10
-2The Pa scope).At first, select MnO content higher (MnO) for use
y(ZnO)
1-yTarget is for the Zn that forms cubic structure at early growth period
1-xMn
xThe O nucleus is necessary; Secondly, fill into the Ar/O of growth room
2Gas mixture has part to be ionized into Ar by high-power electron beam
+And O
2-Ion, O
2-Ionic has to be beneficial to and reduces the Zn that grows
1-xMn
xOxygen vacancy defect quantity in the O film, and high energy Ar
+Ionic exists and can give Zn with its transmission ofenergy
1-xMn
xO molecule or Zn, Mn atom; The 3rd, target partial pressure relatively low in higher relatively underlayer temperature and the growth room can improve Zn equally
1-xMn
xThe kinetic energy of O molecule and Zn, Mn atom and mean free path thereof, thus help the Zn of cubic structure
1-xMn
xThe formation of O nucleus with grow up.
Finished product characteristics of the present invention are: measure Zn respectively with energy dispersion X-ray feature energy spectrometer (EDX), x-ray diffractometer (XRD) and ultraviolet-visible-near-infrared spectrum instrument
1-xMn
xThe Mn content of O film, the crystalline structure and the transmitted spectrum of film.The result shows, the Zn that grows
1-xMn
xThe Mn content of the sample of O film is a cube phase crystalline structure between 0.6～1.0, optical band gap is in 4.5～5.7eV scope.
Main technological features of the present invention is:
The Zn of cube phase, salt mine structure
1-xMn
xThe O film is to adopt electric beam evaporation equipment, polycrystalline (MnO)
y(ZnO)
1-yCeramic target is that the source material growth obtains.With adopt similar approach (as laser molecular beam epitaxy, pulsed laser deposition, magnetron sputtering etc.) growth six sides Zn mutually in the world
1-xMn
xThe situation of O film is compared, and technical characterictic of the present invention is to charge into Ar/O in thin film growth process in reaction chamber
2Gas mixture, rather than only charge into O
2On the other hand, with the electric beam evaporation method six sides Zn mutually that grows
1-xMn
xThe O film is compared, growth cube phase Zn
1-xMn
xNot only adopted MnO content higher (MnO) during the O film
y(ZnO)
1-y(y=0.2～0.3) target has also cooperated other process parameter, for example charges into Ar/O
2Gas mixture, suitably improve underlayer temperature to 350～450 ℃ scope certain temperature, reduce target partial pressure to 1.0～2.0 * 10
-2The a certain numerical value of Pa scope etc.In other words, only adopt MnO content higher (MnO)
y(ZnO)
1-yTarget is not enough, and essential other growth conditionss that cooperate are such as charging into Ar/O
2Gas mixture, raising underlayer temperature just can obtain the cubic structure Zn of single crystalline phase to appropriate value, reduction target partial pressure etc.
1-xMn
xThe O thin-film material, otherwise can only obtain the Zn of six sides, cube mixed phase
1-xMn
xThe O material.
The quartz glass substrate that the present invention obtains cube phase Zn
1-xMn
xThe O film, its Mn content x is in 0.6～1.0 scope, and this x value is than six side's phases, wurtzite structure Zn
1-xMn
xThe Mn content value of O film is big [from existing document, six side's phase Zn
1-xMn
xThe Mn content maximum of O is no more than 0.45 (E.Chikoidze, Y.Dumont, F.Jomard, D.Ballutaud, P.Galtier, O.Gorochov, D.Ferrand, " Semiconducting and magnetic properties of Zn
1-xMn
xO films grown bymetalorganic chemical vapor deposition ", Journal of Applied Physics, 97 (2005) 10D327), otherwise can cause six sides mutually with two being separated cube mutually]; Adjustable continuously in 4.5～5.7eV scope that do not coexist of its optical band gap along with Mn content x in the film, this optical band gap numerical value is also than six side's phases, wurtzite structure Zn
1-xMn
xThe optical band gap value of O film is big.
Description of drawings
Fig. 1 is the Zn that is grown on the silica glass substrate according to embodiments of the invention 1
1-xMn
xX-ray diffraction (XRD) spectrogram of O (x=0.68) film sample.As seen film has cube phase, the salt mine crystalline structure of class MnO.
Fig. 2 is cube phase Zn that is grown on the silica glass substrate according to embodiments of the invention 1
1-xMn
xUltraviolet-visible-near-infrared transmission the spectrum of O (x=0.68) film sample, the optical band gap of visible film is 5.04eV.
Embodiment
Embodiment 1
1, the silica glass substrate of cleaning is packed into substrate holder in the growth room.(MnO) that high temperature sintering is crossed
0.3(ZnO)
0.7The ceramic target material place crucible, with baffle plate target source and substrate are separated.
2, take out growth room to 1.0 * 10 with the vacuum pump unit
-3The vacuum tightness of Pa.
3, heated substrate to 500 ℃ is incubated 15 minutes, unlocking electronic rifle high pressure then, and the bundle spot position of regulating electron beam is to target material surface, and electron beam is gathered 5mA with to the target degasification.
4, with substrate to reducing to 350 ℃, charge into 1: 1 by volume Ar/O proportioning, purity 99.99%
2Gas mixture, the flow by adjusting gas mixture is with the air pressure adjustment to 3.0 in the growth room * 10
-2The Pa scope.Regulate the electron beam line then to 25mA, total gas pressure reaches 4.5 * 10 in the growth room at this moment
-2Pa, i.e. (MnO) that is evaporated by high-power electron beam
0.3(ZnO)
0.7The partial pressure of target steam is 1.5 * 10
-2Pa.
5, open baffle plate and begin the Zn that grows
1-xMn
xThe O crystal film, and suitably finely tune electron beam line size and bundle spot position stablizing with maintenance growth room internal reaction air pressure.Grow and close baffle plate after 100 minutes, close electron beam gun high pressure and line, the substrate cooling is closed and is mixed air valve.After treating that temperature is reduced to room temperature, take out sample.
The Zn for preparing
1-xMn
xO film sample even grain size adopts energy dispersion X-ray (EDX) feature energy spectrometer that the proximate analysis of film is shown, x=0.68, and promptly institute's growing film is Zn
0.32Mn
0.68O; Recording thickness is 920nm; The X-ray diffraction measurement shows Zn
0.32Mn
0.68The O film belongs to cube salt mine structure of single crystalline phase, and no dephasign segregation can be pointed out (111), the diffraction of (200) and (220) crystal face into a cube phase, salt mine structure respectively referring to 1, three diffraction peak of accompanying drawing; To Zn
0.32Mn
0.68The ultraviolet-visible transmitted spectrum measurement of O film shows that referring to accompanying drawing 2, its optical band gap is 5.04eV.
Embodiment 2
● with pack into substrate holder in the growth room of the silica glass substrate of cleaning.(MnO) that high temperature sintering is crossed
0.2(ZnO)
0.8The ceramic target material place crucible, with baffle plate target source and substrate are separated.
● take out growth room to 1.0 * 10 with the vacuum pump unit
-3The vacuum tightness of Pa.
● heated substrate to 500 ℃, be incubated 15 minutes, unlocking electronic rifle high pressure then, the bundle spot position of regulating electron beam is to target material surface, and electron beam is gathered 4mA with to the target degasification.
● underlayer temperature is adjusted to 400 ℃, charges into 2: 1 by volume Ar/O proportioning, purity 99.99%
2Gas mixture, the flow by adjusting gas mixture is with the air pressure adjustment to 3.5 in the growth room * 10
-2The Pa scope.Regulate the electron beam line then to 20mA, total gas pressure reaches 4.5 * 10 in the growth room at this moment
-2Pa, i.e. (MnO) that is evaporated by high-power electron beam
0.2(ZnO)
0.8The partial pressure of target steam is 1.0 * 10
-2Pa.
● open baffle plate and begin the Zn that grows
1-xMn
xThe O crystal film, and suitably finely tune electron beam line size and bundle spot position stablizing with maintenance growth room internal reaction air pressure.Grow and close baffle plate after 60 minutes, close electron beam gun high pressure and line, the substrate cooling is closed and is mixed air valve.After treating that temperature is reduced to room temperature, take out sample.
Prepare the Zn that thickness is 460nm
1-xMn
xThe O film sample shows with the proximate analysis of energy dispersion X-ray (EDX) feature energy spectrometer to film, x=0.63, and promptly institute's growing film is Zn
0.37Mn
0.63O; The X-ray diffraction measurement shows Zn
0.37Mn
0.63The O film belongs to cube salt mine structure of single crystalline phase, no dephasign segregation, and two diffraction peaks can be pointed out the diffraction into (111) and (200) crystal face of a cube phase, salt mine structure respectively; To Zn
0.37Mn
0.63The ultraviolet-visible transmitted spectrum measurement of O film shows that its optical band gap is 4.64eV.
Claims (5)
1. the Zn of one kind of cube of phase, salt mine structure
1-xMn
xThe O film is characterized in that the Mn content x in the film is adjustable continuously in 0.6～1.0 scope, and x is meant the normalization method atom number ratio of Zn and Mn element, and the optical band gap of film is adjustable continuously in 4.5～5.7eV scope, and thickness is adjustable in 200～1000nm scope.
2. the Zn of described cube of phase of claim 1, salt mine structure
1-xMn
xThe preparation technology of O film is characterized in that: adopt the electric beam evaporation method, with (MnO)
y(ZnO)
1-yCeramic target is an evaporation source, and wherein y is a mol ratio, with highly purified Ar/O
2Gas mixture is a reactant gases, and growing on the silica glass substrate obtains, and processing step is as follows:
A) the silica glass substrate of cleaning is packed into substrate holder in the growth room is put (MnO)
y(ZnO)
1-yTarget separates target and substrate with baffle plate in crucible;
B) take out reaction chamber to≤1 * 10 with vacuum pump
-3The vacuum tightness of Pa;
C) substrate is heated to 500 ℃ temperature, is incubated 15 minutes, make the residue desorb that is adsorbed on substrate surface, obtain the growth surface of cleaning; While unlocking electronic rifle high pressure, the bundle spot position of regulating electron beam gather 4～5mA so that heat target with electron beam, to its degasification to target material surface;
D) underlayer temperature is turned down certain suitable growth temperature from 500 ℃, charge into highly purified Ar/O
2Gas mixture makes charging into Ar/O
2Air pressure in the growth room behind the gas mixture is 2.5～3.5 * 10
-2The Pa scope; Strengthen electron beam line to 20～30mA then, (MnO)
y(ZnO)
1-yThe target start vaporizer, by regulate electron beam spot area, position and line size make target evenly, evaporation stably, the vapour pressure of target is controlled at 1.0～2.0 * 10
-2The Pa scope;
E) open baffle plate growth Zn
1-xMn
xThe O crystal film, and with measured film thickness instrument monitoring Zn
1-xMn
xThe thickness of O film, a certain value in thickness reaches 200～1000nm scope finishes growth, treats that underlayer temperature reduces to 100 ℃ and close gas mixture, treat that underlayer temperature is reduced to room temperature after, obtain having a cube phase, the Zn of salt mine structure
1-xMn
xThe O film.
3. the Zn of cube phase according to claim 2, salt mine structure
1-xMn
xThe preparation technology of O film is characterized in that described (MnO)
y(ZnO)
1-yTarget material be by the MnO of purity 99.99% and ZnO powder according to certain molar ratio mix, compacting and be prepared from, wherein mol ratio y=0.2～0.3 through 600 ℃ vacuum sintering technology.
4. the Zn of cube phase according to claim 2, salt mine structure
1-xMn
xThe preparation technology of O film is characterized in that described certain suitable growth temperature is a certain temperature in 350 ℃～450 ℃ scopes.
5. the Zn of cube phase according to claim 2, salt mine structure
1-xMn
xThe preparation technology of O film is characterized in that filling in the described thin film growth process Ar/O of reaction chamber
2The Ar of gas mixture: O
2Volume ratio was 1: 1～3: 1 scopes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100680946A CN101104949A (en) | 2007-04-24 | 2007-04-24 | Zn(1-x)Mn(x)O crystal thin film with cube phase and rock salt ore structure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100680946A CN101104949A (en) | 2007-04-24 | 2007-04-24 | Zn(1-x)Mn(x)O crystal thin film with cube phase and rock salt ore structure |
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| Publication Number | Publication Date |
|---|---|
| CN101104949A true CN101104949A (en) | 2008-01-16 |
Family
ID=38999024
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114555527A (en) * | 2019-11-13 | 2022-05-27 | 斯坦雷电气株式会社 | Wurtzite type manganese oxide particle and preparation method thereof |
-
2007
- 2007-04-24 CN CNA2007100680946A patent/CN101104949A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114555527A (en) * | 2019-11-13 | 2022-05-27 | 斯坦雷电气株式会社 | Wurtzite type manganese oxide particle and preparation method thereof |
| EP4059893A4 (en) * | 2019-11-13 | 2023-12-27 | Stanley Electric Co., Ltd. | Wrutzite-type manganese oxide particles and method for producing same |
| CN114555527B (en) * | 2019-11-13 | 2024-02-13 | 斯坦雷电气株式会社 | Wurtzite type manganese oxide particles and preparation method thereof |
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