CN101183595B - P type doping ZnO based rare magnetic semiconductor material and method of producing the same - Google Patents
P type doping ZnO based rare magnetic semiconductor material and method of producing the same Download PDFInfo
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 47
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 41
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- 238000000034 method Methods 0.000 title abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000011701 zinc Substances 0.000 claims abstract description 16
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 11
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000004246 zinc acetate Substances 0.000 claims abstract description 10
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 9
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 9
- 239000001632 sodium acetate Substances 0.000 claims abstract description 9
- 238000004528 spin coating Methods 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- -1 transition metal salt Chemical class 0.000 claims abstract description 6
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 4
- 239000010980 sapphire Substances 0.000 claims abstract description 4
- 239000011734 sodium Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 13
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 10
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract 2
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- 239000010408 film Substances 0.000 description 10
- 229910001428 transition metal ion Inorganic materials 0.000 description 5
- 229940011182 cobalt acetate Drugs 0.000 description 4
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
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Abstract
The invention discloses a p-type doped ZnO-based diluted magnetic semiconductor material and the preparation method. The material molecular structure formula is Zn<SUB>TM<SUB>y</SUB>x</SUB>O, in which Tm represents transition metal element, Co, Ni, Mn and other elements, x=0-10%, y=0-20%. Method is that zinc acetate, sodium acetate and transition metal salt are dissolved in ethylene glycol monomethyl ether as precursor; then ethanol is added as stabilizer; after stirring, the stable sol is formed. After the sol being dried and heat treated, the power sample is obtained; or by spin coating, the sol is coated uniformly on the Si wafer cleaned in advance or other substrates (quartz glass, sapphire, SiC and other materials), after being dried and heat treated, the thin film sample is obtained. The sol-gel method of preparing material has the advantage of simple technology, low cost, and obtaining easily large area thin films; based on the preparation of the room-temperature ferromagnetic ZnO-based diluted magnetic semiconductor, the Na ion is introduced successfully to obtain the p-type doping; therefore the magnetic property is improved, and by regulating concentration of the Na ion,the magnetic property is controlled.
Description
Technical field
The present invention relates to a kind of p type doping ZnO based rare magnetic semiconductor material and preparation method.Main zno-based dilute magnetic semiconductor powder and the film that adopts sol-gel process and have room-temperature ferromagnetic in conjunction with codope approach (as transition metal and Na codope) preparation.
Background technology
The present information industry mainly is to utilize the electric charge degree of freedom of electronics in the semiconductor device to handle and transmission information, and memory devices such as tape, hard disk and magneto optical disk then are to utilize the electronic spin degree of freedom to come stored information.How these two kinds of character being combined the new functional material of exploration, further strengthen the performance of semiconductor and magnetic device, will be the target of next step development.The main cause that the spin of charge carrier is not fully used in traditional semi-conducting material is that the material overwhelming majority used in the information industry all is diamagnetic (as Si and GaAs etc.).Started the frontier of in semiconductor, utilizing and study electron spin character with the dilute magnetic semiconductor (DMS) that the part component in magnetic ion (transiting group metal elements or rare earth element) the alternative compounds semiconductor forms.
Dilute magnetic semiconductor had been subjected to paying close attention to widely in the last few years, because this material is because of itself and distinct characteristic of general semiconductor such as huge Faraday effect, big exciton division, huge Zeeman splittings etc. have important application prospects at aspects such as spinning LED, spin laser, spin field effect device, the information processings of spin quantum, the spintronics of Chan Shenging has also caused worldwide research boom therefrom, is wherein key issue and explore the dilute magnetic semiconductor with room-temperature ferromagnetic.
ZnO is a wide bandgap semiconductor, band gap is 3.36eV, in a lot of different field application is arranged, as piezoelectric transducer, fluorescence, transparent conductive film etc., and low price, reserves are abundant, has environment friendly again, succeed in developing in case have the zno-based dilute magnetic semiconductor material of room-temperature ferromagnetic, can produce extensive use in a large number.
In 2000, people such as Dietl foretell based on mean field theory, in ZnO and GaN, carry out doped transition metal ions and high temperature ferromagnetism may occur, people such as Sato also calculate by the density function based on double crossing over mechanism and point out, mix 3d transition metal atoms such as Mn, Co and Ni among the ZnO and will show ferromagnetic ordering.Although but magnetic ion can enter and obtain certain room-temperature ferromagnetic in the compound semiconductor, because the restriction of process conditions, doping content can not be too high, caused magnetic property to be in reduced levels all the time.
2004, people such as Spaldine were through COMPUTER CALCULATION, and prophesy is mixed by introducing the room, can improve the room-temperature ferromagnetic in the zno-based dilute magnetic semiconductor; People such as Sluiter have also proved by theory analysis that the p type is doped with and have been beneficial to the raising room-temperature ferromagnetic.But for ZnO, exist the defective of p type doping difficulty all the time, how to explore effective and efficient manner and introduce the difficult point that the room has just become the research.
On the preparation means of zno-based dilute magnetic semiconductor material, sol-gal process is compared with traditional high-octane preparation method, it is simple to have method, needing no vacuum equipment, chemical uniformity is good, can prepare large-area zno-based diluted semi-conductor thin-film with room-temperature ferromagnetic on various substrates, and on this basis, can successfully introduce p type alloy and change carrier concentration in the sample, improve the structural behaviour of zno-based dilute magnetic semiconductor with this, optical characteristics and magnetism characteristic.
Summary of the invention
The purpose of this invention is to provide a kind of p type doping ZnO based rare magnetic semiconductor material and preparation method.
The molecular structural formula of p type doping ZnO based rare magnetic semiconductor material is Zn
1-x-yTm
yNa
xO, Tm represent transition metal Co, Ni, Mn etc., x=0-10%, y=0-20%.
P type doped ZnO-based diluted magnetic semiconductor method for manufacturing thin film comprises the steps:
1) be that zinc acetate, sodium acetate and the transition metal salt of 1-x-y: x: y joins in the EGME with molar percentage, the concentration of configuration solution is 0.5～0.7mol/L, adds and the equimolar monoethanolamine of metal cation then; After at room temperature being stirred to dissolving fully, continue to stir 12～15 hours, still aging then 24～36 hours, obtain transparent, uniform sol;
2) cleaned in advance substrate is placed on the spin coating instrument, more above-mentioned colloidal sol is dropped on the substrate, open the spin coating instrument, make colloidal sol evenly be coated on the substrate;
3) substrate that will be coated with colloidal sol is placed in the baking oven, and in 100～120 ℃ of following preheatings 3～5 minutes, repetitive coatings, preheating were 15～20 times then;
4) to the substrate of finishing coating 300～350 ℃ of following heat treatments 3～5 hours, obtain p type doped ZnO-based diluted magnetic semiconductor material film.
P type doped ZnO-based diluted magnetic semiconductor powder preparation method comprises the steps:
1) be that zinc acetate, sodium acetate and the transition metal salt of 1-x-y: x: y joins in the EGME with molar percentage, the concentration of configuration solution is 0.5～0.7mol/L, adds and the equimolar monoethanolamine of metal cation then; After at room temperature being stirred to dissolving fully, continue to stir 12～15 hours, still aging then 24～36 hours, obtain transparent, uniform sol;
2) colloidal sol was placed 100～120 ℃ of baking ovens 24～36 hours, obtain gel;
3) gel was heat-treated under 300～350 ℃ 3～5 hours, and, obtain required p type doped ZnO-based diluted magnetic semiconductor powder with the stove cooling.
Described transition metal is Co, Ni or Mn.The material of substrate is single crystalline Si, quartz glass, sapphire, SiC or simple glass.
The beneficial effect that the present invention has:
The dilute magnetic semiconductor material that adopts sol-gel process and have the room-temperature ferromagnetic feature in conjunction with codope approach (transition metal ions and Na codope ZnO) preparation is increased to Curie temperature more than the room temperature.On structure, the doping content of control Co and Na is in certain scope, and the doping ZnO that obtains still has hexagonal wurtzite structure, not because of producing the impurity phase-splitting.
The present invention adopts sol-gel process to possess skills simply, expends lowly, is easy to obtain advantages such as large-area film.Because colloid obtains by solution, chemical composition is just the same in the micelle and between micelle, can prepare the even alloy of multicomponent (uniformity coefficient can reach the molecular level level), and can prepare that some conventional methods are difficult to obtain or not getable product.
Among the present invention, sol-gel process is evenly mixed transition metal ions and Na ion and is entered ZnO, the successful introducing of Na ion can significantly improve the carrier concentration among the ZnO, regulate the magnetic exchange-coupling interaction between transition metal ions effectively, make the more simple ZnO:Co dilute magnetic semiconductor material of ferromagnetic property of this diluted magnetic semiconductor film material be significantly improved, for better condition has been created in the application under the zno-based dilute magnetic semiconductor room temperature.
Description of drawings
Fig. 1 is the Zn that does not mix Na of embodiment 1,2 preparations
0.95Co
0.05O powder, Zn
0.94Co
0.05Na
0.01O powder and pure ZnO powder XRD figure spectrum relatively can know that Co and Na all enter the ZnO lattice, except the buergerite of ZnO itself, do not produce second phase;
Fig. 2 be utilize superconducting quantum interference device (SQUID) (SQUID) at room temperature (300 ℃ time) record the Zn of embodiment 1,2 preparations
0.95Co
0.05O and Zn
0.8Na
0.1Co
0.1The M-H figure of O dilute magnetic semiconductor powder compares, and as can be seen, the introducing of Na ion has improved the room-temperature ferromagnetic of ZnCoO, and its saturation magnetization has risen to 0.14emu/g by 0.10emu/g.
Embodiment
With zinc acetate (Zn (CH
3COO)
22H
2O), sodium acetate (CH
3COONa) and transition metal salt be solute, EGME is a solvent, monoethanolamine is a stabilizer.Take by weighing solute by certain molar percentage (transition metal ions: 0～20%, Na:0～10%) and add in the EGME, add and the equimolar monoethanolamine of metal cation then, the concentration of configuration solution is 0.5～0.7mol/L.At room temperature be stirred to dissolving fully, continue to stir 12～15 hours, still aging then 24～36 hours, obtain transparent, uniform sol.Colloidal sol is placed and was not produced precipitation in 1～2 day, go up dropping colloidal solution at cleaned in advance Si sheet or other substrates (quartz glass, sapphire, SiC etc.), mode with the rotation substrate on the spin coating instrument makes colloid evenly apply one deck, place 100～120 ℃ baking oven preheating 3～5 minutes then, repetitive coatings, warm can obtain the film of different-thickness then, final sample is at 300～350 ℃ of air atmospheres, and cools off with stove.The process of preparation powder sample only need be omitted the spin coating process, after oven dry under 100～120 ℃, adopts same heat-treat condition can obtain powder colloidal sol.
Embodiment 1: preparation Zn
0.95Co
0.05O dilute magnetic semiconductor powder
1) 95: 5 zinc acetate of molar percentage (5.21g) and cobalt acetate (0.31g) are joined in the 50ml EGME, add the monoethanolamine of 0.5ml then, be made into the solution that concentration is 0.5mol/L; After at room temperature being stirred to dissolving fully, continue to stir 12 hours, still aging then 24 hours, obtain transparent, uniform sol;
2) colloidal sol was placed 100 ℃ of baking ovens 24 hours, obtain gel;
3) gel was heat-treated under 300 ℃ 3 hours, and, obtain required Zn with the stove cooling
0.95Co
0.05O dilute magnetic semiconductor powder.
Embodiment 2: preparation Zn
0.94Co
0.05Na
0.01O dilute magnetic semiconductor powder
1) 94: 5: 1 zinc acetate of molar percentage (5.16g), cobalt acetate (0.31g) and sodium acetate (0.02g) are joined in the 50ml EGME, add the monoethanolamine of 0.5ml then, be made into the solution that concentration is 0.5mol/L; After at room temperature being stirred to dissolving fully, continue to stir 15 hours, still aging then 36 hours, obtain transparent, uniform sol;
2) colloidal sol was placed 120 ℃ of baking ovens 24 hours, obtain gel;
3) gel was heat-treated under 350 ℃ 5 hours, and, obtain required Zn with the stove cooling
0.94Co
0.05Na
0.01O dilute magnetic semiconductor powder.
Embodiment 3: preparation Zn
0.8Co
0.15Na
0.5The O diluted semi-conductor thin-film
1) 80: 15: 5 zinc acetate of molar percentage (4.39g), cobalt acetate (0.93g) and sodium acetate (0.1g) are joined in the 50ml EGME, add the monoethanolamine of 0.5ml then, be made into the solution that concentration is 0.5mol/L; After at room temperature being stirred to dissolving fully, continue to stir 12 hours, still aging then 24 hours, obtain transparent, uniform sol;
2) drip colloidal solution on cleaned in advance quartz glass substrate, the mode with the rotation substrate on the spin coating instrument evenly applies colloid, and 100 ℃ of following preheatings 3 minutes;
3) repetitive coatings, warm are 20 times, finish pre-plated film;
4) the quartz glass substrate of finishing pre-plated film was heat-treated under 300 ℃ 3 hours, and, obtain required Zn with the stove cooling
0.8Co
0.15Na
0.5The O diluted semi-conductor thin-film.
Embodiment 4: preparation Zn
0.7Co
0.2Na
0.1The O diluted semi-conductor thin-film
1) 7: 2: 1 zinc acetate of molar percentage (3.84g), cobalt acetate (1.24g) and sodium acetate (0.2g) are joined in the 50ml EGME, add the monoethanolamine of 0.5ml then, be made into the solution that concentration is 0.7mol/L; After at room temperature being stirred to dissolving fully, continue to stir 15 hours, still aging then 36 hours, obtain transparent, uniform sol;
2) drip colloidal solution on cleaned in advance quartz glass substrate, the mode with the rotation substrate on the spin coating instrument evenly applies colloid, and 100 ℃ of following preheatings 5 minutes;
3) repetitive coatings, warm are 20 times, finish pre-plated film;
4) the quartz glass substrate of finishing pre-plated film was heat-treated under 300 ℃ 5 hours, and, obtain required Zn with the stove cooling
0.7Co
0.2Na
0.1The O diluted semi-conductor thin-film.
Above-mentioned is detailed presentations for most preferred embodiment processing step of the present invention; but obviously; the researcher in the technology of the present invention field can make the change of form and content aspect unsubstantiality and not depart from the scope that institute of the present invention essence is protected according to above-mentioned step; therefore, the present invention is not limited to above-mentioned concrete form and details.
Claims (4)
1. a p type doping ZnO based rare magnetic semiconductor material is characterized in that molecular structural formula is Zn
1-x-yTM
yNa
xO, TM represent transition metal Co, Ni, Mn, 0＜x≤10%, y=0-20%.
2. p type doping ZnO based rare magnetic semiconductor material preparation method as claimed in claim 1 is characterized in that comprising the steps:
1) be that zinc acetate, sodium acetate and the transition metal salt of 1-x-y: x: y joins in the EGME with molar percentage, the concentration of configuration solution is 0.5～0.7mol/L, add and the equimolar monoethanolamine of metal cation then, after at room temperature being stirred to dissolving fully, continue to stir 12～15 hours, still aging then 24～36 hours, obtain transparent, uniform sol;
2) cleaned in advance substrate is placed on the spin coating instrument, more above-mentioned colloidal sol is dropped on the substrate, open the spin coating instrument, make colloidal sol evenly be coated on the substrate;
3) substrate that will be coated with colloidal sol is placed in the baking oven, and in 100～120 ℃ of following preheatings 3～5 minutes, repetitive coatings, preheating were 15～20 times then;
4) substrate of finishing coating was heat-treated under 300～350 ℃ 3～5 hours, obtain p type doped ZnO-based diluted magnetic semiconductor film.
3. a kind of p type doping ZnO based rare magnetic semiconductor material preparation method as claimed in claim 2, the material that it is characterized in that described substrate is single crystalline Si, quartz glass, sapphire or SiC.
4. p type doping ZnO based rare magnetic semiconductor material preparation method as claimed in claim 1 is characterized in that comprising the steps:
1) be that zinc acetate, sodium acetate and the transition metal salt of 1-x-y: x: y joins in the EGME with molar percentage, the concentration of configuration solution is 0.5～0.7mol/L, adds and the equimolar monoethanolamine of metal cation then; After at room temperature being stirred to dissolving fully, continue to stir 12～15 hours, still aging then 24～36 hours, obtain transparent, uniform sol;
2) colloidal sol was placed 100～120 ℃ of baking ovens 24～36 hours, obtain gel;
3) gel was heat-treated under 300～350 ℃ 3～5 hours, and, obtain required p type doped ZnO-based diluted magnetic semiconductor powder with the stove cooling.
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| CN101481817B (en) * | 2008-12-31 | 2010-08-25 | 浙江大学 | Growth method of nonpolar ZnO crystal film |
| CN101698932B (en) * | 2009-10-30 | 2011-04-27 | 北京工业大学 | Method for preparing P type cobalt-doped zinc oxide film |
| WO2012037729A1 (en) * | 2010-09-25 | 2012-03-29 | Ye Zhizhen | METHOD FOR MANUFACTURING P-TYPE ZnO-BASED MATERIAL |
| CN102062770A (en) * | 2010-12-03 | 2011-05-18 | 厦门大学 | Ternary oxide air-sensitive material and synthesis method thereof |
| CN103107291A (en) * | 2011-11-11 | 2013-05-15 | 海洋王照明科技股份有限公司 | Substrate of organic electroluminescence device and production method thereof |
| CN104064314B (en) * | 2014-06-17 | 2017-01-04 | 北京理工大学 | A kind of preparation method of dilute magnetic semiconductor |
| CN105314672B (en) * | 2015-10-15 | 2017-04-05 | 西安工业大学 | A kind of sol-gel process for preparing of Co-doped ZnO nanometer rods |
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| US5191223A (en) * | 1991-07-03 | 1993-03-02 | International Business Machines Corporation | Device for selective magnetization and method |
| CN1725446A (en) * | 2005-06-15 | 2006-01-25 | 浙江大学 | Zn1-x CoxO rare magnetic semiconductor film and its preparation technology |
| CN101016164A (en) * | 2007-02-09 | 2007-08-15 | 北京大学 | Method of preparing zinc oxide doped ambient temperature diluted magnetic semi-conducting material |
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|---|---|---|---|---|
| US5191223A (en) * | 1991-07-03 | 1993-03-02 | International Business Machines Corporation | Device for selective magnetization and method |
| CN1725446A (en) * | 2005-06-15 | 2006-01-25 | 浙江大学 | Zn1-x CoxO rare magnetic semiconductor film and its preparation technology |
| CN101016164A (en) * | 2007-02-09 | 2007-08-15 | 北京大学 | Method of preparing zinc oxide doped ambient temperature diluted magnetic semi-conducting material |
Non-Patent Citations (2)
| Title |
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| 赵青等.溶胶-凝胶法制备Fe掺杂ZnO基稀磁半导体的结构与磁性.功能材料38 11.2007,38(11),p1780-1782. |
| 赵青等.溶胶-凝胶法制备Fe掺杂ZnO基稀磁半导体的结构与磁性.功能材料38 11.2007,38(11),p1780-1782. * |
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