CN101211764A - Chromium doped titanium dioxide ferromagnetic film room temperature preparation method - Google Patents
Chromium doped titanium dioxide ferromagnetic film room temperature preparation method Download PDFInfo
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- CN101211764A CN101211764A CNA2006101707195A CN200610170719A CN101211764A CN 101211764 A CN101211764 A CN 101211764A CN A2006101707195 A CNA2006101707195 A CN A2006101707195A CN 200610170719 A CN200610170719 A CN 200610170719A CN 101211764 A CN101211764 A CN 101211764A
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Abstract
The invention provides a method for preparing a chromium-doped titanium dioxide (TiO2)(CrxTi<1-x>O2) room-temperature ferromagnetic film, which belongs to the field of the preparation of the novel semiconductor spin electric devices. In the method, a Cr-doped titanium dioxide sol is first prepared adopting the sol-gel method and the sol is rotationally coated on a silicon substrate to form a CrxTi<1-x>O2 sol-gel film. The CrxTi<1-x>O2 sol-gel film has weak ferromagnetic characteristic at the room temperature after being annealed and crystallized in the air atmosphere; the CrxTi<1-x>O2 film has increased ferromagnetic characteristic after being secondarily annealed in the atmosphere in which the hydrogen is contained or under a vacuum environment. The adoption of the invention can prepare the CrxTi<1-x>O2 film having favorable room-temperature ferromagnetism.
Description
Technical field
The invention belongs to novel semi-conductor spin electric device preparation field, relate in particular to a kind of Cr doped Ti O with room-temperature ferromagnetic
2(Cr
xTi
1-xO
2) preparation method of film.
Background technology
Dilute magnetic semiconductor combines the information storage characteristic of semi-conductive charge transport characteristic and magnetic material, is the important materials of preparation novel semi-conductor spin electric device.Because the introducing of magnetic element, dilute magnetic semiconductor material also have a series of general semi-conductive unusual character that are different from, and comprise abundant physical connotation.Therefore, the research for dilute magnetic semiconductor all has very important significance in basic theory and practical application.Oxide based diluted magnetic semiconductor is a kind of dilute magnetic semiconductor material with high temperature ferromagnetism and high spinning polarizability that gets a good chance of, and has broad application prospects and use value in semiconductor spintronics field.
From application point of view, the dilute magnetic semiconductor that the preparation Curie temperature is higher than room temperature is very important.Comparatively extensive based on the research of the dilute magnetic semiconductor of II-VI family and III-V compound semiconductor, such as (Cd, Mn) Te and (Ga, Mn) As, but the Curie temperature of these materials generally is lower than 110K, has limited their practical application.In recent years, discovered the TiO that transition metal Co, Cr, Fe and Ni etc. mix
2Oxide lanthanon magnetic semiconductor has the ferromagnetism that is higher than room temperature, has caused people's extensive interest.TiO
2The preparation method of based diluted magnetic semiconductor thin film is mainly coating techniques such as molecular beam epitaxy, metal organic chemical vapor deposition, reactive sputtering and pulsed laser deposition and ion implantation technique etc.The doped Ti O that different preparation methods obtains
2The ion magnetic moment of material is widely different.In addition, different substrates is very big to the magnetic characteristic influence of material.Preparation has the transient metal doped TiO of high temperature ferromagnetism and macroion magnetic moment
2Thin-film material has important and practical meanings for its application in the semiconductor spin electric device.
Summary of the invention
The purpose of this invention is to provide a kind of sol-gel process that utilizes and prepare Cr
xTi
1-xO
2The method of ferromagnetic film room temperature.
Technical scheme of the present invention is: the TiO that a kind of Cr mixes
2The preparation method of ferromagnetic film room temperature comprises the steps:
1) adopts sol-gel process, prepare the titanium dioxide (TiO of chromium-doped (Cr)
2) colloidal sol, the Cr of doping and the atomic ratio of Ti are controlled at 3: 97-10: 90;
2) colloidal sol is spin-coated on the monocrystalline substrate uniformly, forms Cr doped Ti O
2Colloidal sol-gel film, 0.03≤x≤0.1 wherein;
3) with Cr
xTi
1-xO
2Colloidal sol-gel film carries out dried in 80-150 ℃ of temperature range;
4) to Cr
xTi
1-xO
2Colloidal sol-gel film carries out annealing in process, finishes Cr doped Ti O
2The preparation of ferromagnetic thin film.
Wherein step 1 prepares Cr doped Ti O
2Colloidal sol, adopting the alkoxide (as tetra-n-butyl titanate etc.) of titanium, the inorganic salts (as chromium acetate or chromium chloride etc.) of chromium is predecessor, two kinds of predecessors are dissolved in organic solvent altogether (as absolute ethyl alcohol, ethylene glycol etc.) in, the complexing agent that has added stabilization is (as acetylacetone,2,4-pentanedione, glacial acetic acid etc.) and promote catalyst for reaction (as nitric acid, hydrochloric acid etc.), add then to stir under deionized water (amount of deionized water not produce in the colloidal sol the be precipitated as should) room temperature solution is fully mixed, again through heating ageing or in air, be placed to the acquisition stable sol.The temperature of ageing of heating is advisable with 30-80 ℃.
In order to obtain certain thickness Cr
xTi
1-xO
2Colloidal sol-gel film, can be before step 4 repeating step 2 and 3.
The Cr that said method obtains
xTi
1-xO
2Film has room-temperature ferromagnetic, but saturation magnetic moment is less usually, in order to strengthen its magnetic, and further Cr to obtaining
xTi
1-xO
2Ferromagnetic thin film carries out the annealing in process second time, specifically can adopt one of following dual mode: (1) is in hydrogeneous atmosphere, as carrying out annealing in process in the mixed atmosphere of hydrogen, hydrogen and nitrogen or inert gas, air pressure is not higher than atmospheric pressure, annealing temperature is 300-900 ℃, wherein hydrogen content is 5-100% in the mixed atmosphere, and described inert gas is selected argon gas usually; (2) carry out annealing in process under vacuum condition, vacuum degree is≤10
-3Pa, annealing temperature is 300-1000 ℃.
Technique effect of the present invention: adopt sol-gel process to prepare Cr doped Ti O
2Colloidal sol is spin-coated on colloidal sol on the Si single crystalline substrate and forms Cr
xTi
1-xO
2Colloidal sol-gel film, the film that obtains after the annealing crystallization has room-temperature ferromagnetic.But, a Cr through annealing in process in air atmosphere
xTi
1-xO
2The saturation magnetic moment of film is very little, as Cr
0.05Ti
0.95O
2The saturation magnetic moment of ferromagnetic thin film only is 0.31emu/cm
3Yet, after the double annealing under nitrogen atmosphere or the vacuum, Cr
xTi
1-xO
2The saturation magnetic moment of film obviously improves, and has reached 3.39emu/cm respectively
3And 2.35emu/cm
3Double annealing under nitrogen atmosphere or the vacuum does not influence Cr
0.05Ti
0.95O
2The crystal structure of ferromagnetic thin film is (with reference to figure 1, Fig. 2, Cr
xTi
1-xO
2The structure of film and Magnetic Measurement result).The present invention can obtain to have the Cr of room-temperature ferromagnetic
xTi
1-xO
2Film, after double annealing under hydrogeneous atmosphere or the vacuum condition, the ferromagnetism of this film has obtained enhancing.
Description of drawings
Fig. 1 is the Cr of sol-gel process preparation
0.05Ti
0.95O
2Film and the X-ray diffractogram after double annealing under nitrogen atmosphere or the vacuum;
Fig. 2 is the M-H magnetic hysteresis loop figure that utilizes the film that records under alternating gradient sample magnetometer (AGM) room temperature.
Embodiment
Of the present invention to as if a kind of sol-gel process that utilizes prepare Cr
xTi
1-xO
2Ferromagnetic film room temperature and strengthen the ferromagnetic method of this film.Cr
xTi
1-xO
2Having the ferromagnetic characteristic that is higher than room temperature, is a kind of candidate material of the preparation semiconductor spin electric device that gets a good chance of.Generally be to adopt methods such as molecular beam epitaxy, pulsed laser deposition and reactive sputtering to prepare room-temperature ferromagnetic Cr now
xTi
1-xO
2Film, the present invention adopts sol-gel process, the TiO that utilizes sol evenning machine that Cr is mixed
2Colloidal sol evenly is coated on Si (001) single crystalline substrate and forms Cr
xTi
1-xO
2Colloidal sol-gel film, acquisition has the Cr of room-temperature ferromagnetic after air is annealed crystallization down
xTi
1-xO
2Film.The room temperature magnetic characteristic of sample utilizes alternating gradient magnetometer (AGM) to measure.Cr
xTi
1-xO
2Ferromagnetic thin film has less saturated ion magnetic moment, after handling through the double annealing in hydrogeneous atmosphere or the vacuum, and Cr
xTi
1-xO
2The saturated ion magnetic moment of film is greatly improved.
TiO in the Cr doping
2During the colloidal sol preparation, the alkoxide (as tetra-n-butyl titanate) of employing Ti, the inorganic salts of Cr are (as chromium acetate, chromium chloride etc.) be predecessor, be dissolved in altogether (such as absolute ethyl alcohol, ethylene glycol etc.) in the suitable solvent, add complexing agent (as acetylacetone,2,4-pentanedione, glacial acetic acid etc.) and catalyst (as nitric acid, hydrochloric acid etc.), add appropriate amount of deionized water then, stirring a period of time is fully mixed solution under the room temperature, passes through and heats ageing or form stable sol after placement a period of time in air.When wherein colloidal sol prepared, the kind of the predecessor of employing, solvent, complexing agent and catalyst was not limited in list above several, comprised that also other can be used for Cr doped Ti O
2The substitute of colloidal sol preparation substitutes the inorganic salts of Cr etc. such as the alkoxide that can adopt Cr.By the mol ratio of Ti and Cr in the adjusting predecessor, can obtain the Cr of different Cr content x
xTi
1-xO
2Film.
Embodiment 1 sol-gel process prepares Cr
xTi
1-xO
2(x=0.05) film
Utilize sol-gel process on Si (001) single crystalline substrate, to prepare Cr
0.05Ti
0.95O
2Film.Utilize tetra-n-butyl titanate and chromium chloride as predecessor (Cr: the Ti mol ratio is 5: 95), they are dissolved in (concentration of solution is 0.1mol/L) in the absolute ethyl alcohol, add acetylacetone,2,4-pentanedione as complexing agent, nitric acid is as catalyst, splash into appropriate amount of deionized water, utilize magnetic stirring apparatus to make solution fully mix, in air, place the TiO of the Cr doping that obtained performance is stable two days later in 3 hours stirring under the solution room temperature
2Colloidal sol.The TiO that utilizes sol evenning machine that Cr is mixed
2Colloidal sol evenly is coated on Si (001) single crystalline substrate, and the spin coating process of colloidal sol was at first carried out under the 500rpm rotating speed 10 seconds, carries out under the 3000rpm rotating speed 40 seconds then, obtains the Cr of uniform thickness
0.05Ti
0.95O
2Colloidal sol-gel film.Film carried out film spin coating next time after under 100 ℃ of temperature dry 10 minutes, repeat the film that spin coating obtains suitable thickness then.This experiment repeats spin coating 3 times, and the thickness of preparation film is about 60nm.Film carries out annealing in process in air atmosphere, temperature is 550 ℃, and the time is 1 hour.Step annealing time-division three carries out in air atmosphere, carries out under 100 ℃, 280 ℃ and 550 ℃ of temperature respectively, 550 ℃ of insulations 1 hour down, helps not having the preparation of be full of cracks film like this.Through the sample after the air annealing further under 400 ℃ or vacuum under the nitrogen atmosphere (～10
-3Pa) 550 ℃ are carried out the double annealing processing, and the time is 1 hour.
The thickness of film utilizes ESEM to carry out sample in cross section and measures mensuration, utilizes X-ray diffraction (XRD) method to analyze the structures of samples characteristic, and the room temperature magnetic characteristic of sample utilizes alternating gradient magnetometer (AGM) to measure.The X-ray diffraction of prepared film (XRD) as shown in Figure 1, wherein: a is the sample of annealing after the crystallization under 550 ℃ of air atmospheres; B is the sample after double annealing under 400 ℃ of hydrogeneous atmosphere; C is the sample after double annealing under 550 ℃ of vacuum.Cr after 550 ℃ of air atmospheres annealing crystallization as can be seen from Figure 1
0.05Ti
0.95O
2Film is anatase structured (the anatase structured diffraction maximum of A representative among Fig. 1).Do not find CrO
2Peak etc. any cenotype.Structurally do not have significant change through hydrogen or vacuum double annealing rear film, show that double annealing does not influence original Cr
0.05Ti
0.95O
2The structure of film.Magnetic Measurement shows, the Cr after air atmosphere is annealed crystallization down
0.05Ti
0.95O
2Film has the room temperature ferromagnetic characteristic, and its saturation magnetic moment is 0.31emu/Gm
3, and after hydrogen or vacuum double annealing, its saturation magnetic moment obviously is improved, and has reached 3.39emu/cm respectively
3And 2.35emu/cm
3The Magnetic Measurement of sample the results are shown in shown in Figure 2, and wherein: a is the sample after the annealing crystallization under 550 ℃ of air atmospheres; B is the sample after double annealing under 400 ℃ of hydrogeneous atmosphere; C is the sample after double annealing under 550 ℃ of vacuum.
Utilize sol-gel process on Si (001) single crystalline substrate, to prepare Cr
0.03Ti
0.97O
2Film.Utilize tetra-n-butyl titanate and chromium acetate as predecessor (Cr: the Ti mol ratio is 3: 97), they are dissolved in (concentration of solution is 0.1mol/L) in the ethylene glycol altogether, add glacial acetic acid as complexing agent, nitric acid is as catalyst, splash into appropriate amount of deionized water, utilize magnetic stirring apparatus solution fully to be mixed in 3 hours, the ageing 12 hours of under 60 ℃, heating, the TiO that the Cr that obtained performance is stable mixes with stirring under the solution room temperature
2Colloidal sol.The TiO that utilizes sol evenning machine that Cr is mixed
2Colloidal sol is coated on Si (001) substrate, and at first spin coating 10 seconds under the 500rpm rotating speed was carried out under the 3000rpm rotating speed 40 seconds then, obtains the Cr of uniform thickness
0.03Ti
0.97O
2Colloidal sol-gel film.Film carried out film spin coating next time after under 80 ℃ of temperature dry 15 minutes, repeat the film that spin coating obtains suitable thickness then.This experiment repeats spin coating 3 times, and the thickness of preparation film is about 60nm.Film carries out annealing in process in air atmosphere, temperature is 400 ℃, and the time is 1 hour.Step annealing time-division three carries out in air atmosphere, carries out under 100 ℃, 280 ℃ and 400 ℃ of temperature respectively, 400 ℃ of insulations 1 hour down.This sample is further at 10%H
2Carry out double annealing under the following 400 ℃ of temperature of/Ar atmosphere and handle, the time is 1 hour.
Magnetic Measurement shows, the Cr after air atmosphere is annealed crystallization down
0.03Ti
0.97O
2Film has the room temperature ferromagnetic characteristic, has less saturation magnetic moment, and after the double annealing, its saturation magnetic moment is improved under the hydrogeneous atmosphere.
Utilize sol-gel process on Si (001) single crystalline substrate, to prepare Cr
0.1Ti
0.9O
2Film.Utilize tetra-n-butyl titanate and chromium chloride as predecessor (Cr: the Ti mol ratio is 10: 90), they are dissolved in (concentration of solution is 0.1mol/L) in the ethylene glycol, add acetylacetone,2,4-pentanedione as complexing agent, hydrochloric acid is as catalyst, splash into appropriate amount of deionized water, utilize magnetic stirring apparatus solution fully to be mixed in 3 hours, the ageing 12 hours of under 60 ℃, heating, the TiO that the Cr that obtained performance is stable mixes with stirring under the solution room temperature
2Colloidal sol.The TiO that utilizes sol evenning machine that Cr is mixed
2Colloidal sol is coated on Si (001) substrate, and at first spin coating 10 seconds under the 500rpm rotating speed was carried out under the 3000rpm rotating speed 40 seconds then, obtains the Cr of uniform thickness
0.1Ti
0.9O
2Colloidal sol-gel film.Film carried out film spin coating next time after under 120 ℃ of temperature dry 10 minutes, repeat the film that spin coating obtains suitable thickness then.This experiment repeats spin coating 3 times, and the thickness of preparation film is about 60nm.Film carries out annealing in process in air atmosphere, temperature is 650 ℃, and the time is 1 hour.Step annealing time-division three carries out in air atmosphere, carries out under 100 ℃, 280 ℃ and 650 ℃ of temperature respectively, 650 ℃ of insulations 1 hour down.This sample is further in vacuum (～10
-3Pa) carry out the double annealing processing under 650 ℃ of temperature, the time is 1 hour.
Magnetic Measurement shows, the Cr after air atmosphere is annealed crystallization down
0.1Ti
0.9O
2Film performance room temperature ferromagnetic characteristic, but have less saturation magnetic moment, and after double annealing under the vacuum, its saturation magnetic moment is improved.
Above-mentioned is detailed description 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 (10)
1. the TiO that mixes of a Cr
2The preparation method of ferromagnetic film room temperature comprises the steps:
1) adopts sol-gel process, the TiO of preparation doping Cr
2Colloidal sol, the Cr of doping and the atomic ratio of Ti are controlled at 3: 97-10: 90;
2) colloidal sol is spin-coated on the monocrystalline substrate uniformly, forms Cr doped Ti O
2Cr
xTi
1-xO
2Colloidal sol-gel film, wherein 0.03≤x≤0.1;
3) with Cr
xTi
1-xO
2Colloidal sol-gel film carries out dried in 80-150 ℃ of temperature range;
4) to Cr
xTi
1-xO
2Colloidal sol-gel film carries out annealing in process, finishes Cr doped Ti O
2The preparation of ferromagnetic thin film.
2. the TiO that Cr as claimed in claim 1 mixes
2The preparation method of ferromagnetic film room temperature, it is characterized in that, it is predecessor that described step 1 adopts the alkoxide of titanium, the inorganic salts of chromium, be dissolved in two kinds of predecessors in the organic solvent altogether, add the complexing agent of stabilization and promoted catalyst for reaction, add deionized water then, stirring fully mixes solution under the room temperature, passes through and heats ageing or be placed to the acquisition stable sol in air.
3. the TiO that Cr as claimed in claim 2 mixes
2The preparation method of ferromagnetic film room temperature is characterized in that, the alkoxide of described titanium is a tetra-n-butyl titanate, the inorganic salts of chromium are chromium acetate or chromium chloride, organic solvent is absolute ethyl alcohol or ethylene glycol, and complexing agent is acetylacetone,2,4-pentanedione or glacial acetic acid, and catalyst is nitric acid or hydrochloric acid.
4. the TiO that Cr as claimed in claim 2 mixes
2The preparation method of ferromagnetic film room temperature is characterized in that, the temperature of the described ageing of heating is 30-80 ℃.
5. the TiO that Cr as claimed in claim 1 mixes
2The preparation method of ferromagnetic film room temperature is characterized in that, repeating step 2 and 3 before described step 4 is to obtain certain thickness Cr
xTi
1-xO
2Colloidal sol-gel film.
6. the TiO that Cr as claimed in claim 1 mixes
2The preparation method of ferromagnetic film room temperature, it is characterized in that described step 4 adopts air atmosphere annealing, annealing process is: earlier 80-150 ℃ of following process annealing, 240-300 ℃ of annealing down, in 400-1000 ℃ of temperature range, carry out the annealing in process of higher temperature at last then.
7. the TiO that Cr as claimed in claim 6 mixes
2The preparation method of ferromagnetic film room temperature is characterized in that, after described step 4 is annealed in air atmosphere, and further annealing in process for the second time in hydrogeneous atmosphere, air pressure is not higher than atmospheric pressure, and annealing temperature is 300-900 ℃.
8. the TiO that Cr as claimed in claim 7 mixes
2The preparation method of ferromagnetic film room temperature is characterized in that, described hydrogeneous atmosphere is the mixed atmosphere of hydrogen or hydrogen and nitrogen or inert gas, and wherein hydrogen content is 5-100% in the mixed atmosphere.
9. the TiO that Cr as claimed in claim 8 mixes
2The preparation method of ferromagnetic film room temperature is characterized in that, described inert gas is an argon gas.
10. the TiO that Cr as claimed in claim 6 mixes
2The preparation method of ferromagnetic film room temperature is characterized in that, after described step 4 is annealed in air atmosphere, further carries out annealing in process under vacuum condition, and vacuum degree is≤10
-3Pa, annealing temperature is 300-1000 ℃.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079886A (en) * | 2010-11-30 | 2011-06-01 | 南京理工大学 | Method for preparing metal ion-doped titanium dioxide sol |
| CN102181825A (en) * | 2011-03-10 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | Seed layer-assisted high performance TiO2-based transparent conductive film and preparation method thereof |
| CN103526263A (en) * | 2013-10-21 | 2014-01-22 | 电子科技大学 | Preparation method of Cr-doped TiO2 nanometer magnetic film with room-temperature ferromagnetic effect |
| CN106268765A (en) * | 2016-07-15 | 2017-01-04 | 辽宁大学 | A kind of metal ion doped titanium dioxide method for manufacturing thin film |
| CN109411599A (en) * | 2018-10-22 | 2019-03-01 | 西安理工大学 | A kind of preparation method of zirconium adulterated TiOx memristor film |
| CN109594067A (en) * | 2019-01-08 | 2019-04-09 | 工业和信息化部电子第五研究所华东分所 | A method of in the red schorl phase titanium dioxide nano linear array of (001) Solute Content in Grain growth |
| CN113026002A (en) * | 2021-03-03 | 2021-06-25 | 陕西雷翔新材料科技有限公司 | Thin film metal oxide structure and manufacturing method thereof |
-
2006
- 2006-12-26 CN CNA2006101707195A patent/CN101211764A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079886A (en) * | 2010-11-30 | 2011-06-01 | 南京理工大学 | Method for preparing metal ion-doped titanium dioxide sol |
| CN102181825A (en) * | 2011-03-10 | 2011-09-14 | 中国科学院上海硅酸盐研究所 | Seed layer-assisted high performance TiO2-based transparent conductive film and preparation method thereof |
| CN102181825B (en) * | 2011-03-10 | 2013-03-13 | 中国科学院上海硅酸盐研究所 | Seed layer-assisted high performance TiO2-based transparent conductive film and preparation method thereof |
| CN103526263A (en) * | 2013-10-21 | 2014-01-22 | 电子科技大学 | Preparation method of Cr-doped TiO2 nanometer magnetic film with room-temperature ferromagnetic effect |
| CN103526263B (en) * | 2013-10-21 | 2016-02-03 | 电子科技大学 | There is the Cr doped Ti O of room temperature ferromagnetic effect 2the preparation method of nano-magnetic thin films |
| CN106268765A (en) * | 2016-07-15 | 2017-01-04 | 辽宁大学 | A kind of metal ion doped titanium dioxide method for manufacturing thin film |
| CN106268765B (en) * | 2016-07-15 | 2019-01-08 | 辽宁大学 | A kind of metal ion doped titanium dioxide method for manufacturing thin film |
| CN109411599A (en) * | 2018-10-22 | 2019-03-01 | 西安理工大学 | A kind of preparation method of zirconium adulterated TiOx memristor film |
| CN109594067A (en) * | 2019-01-08 | 2019-04-09 | 工业和信息化部电子第五研究所华东分所 | A method of in the red schorl phase titanium dioxide nano linear array of (001) Solute Content in Grain growth |
| CN109594067B (en) * | 2019-01-08 | 2021-07-09 | 工业和信息化部电子第五研究所华东分所 | Method for preparing rutile phase titanium dioxide nanowire array growing in preferred orientation of (001) crystal face |
| CN113026002A (en) * | 2021-03-03 | 2021-06-25 | 陕西雷翔新材料科技有限公司 | Thin film metal oxide structure and manufacturing method thereof |
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