CN106637161A - Method for regulating magnetic performance of lanthanum calcium manganese oxygen film - Google Patents
Method for regulating magnetic performance of lanthanum calcium manganese oxygen film Download PDFInfo
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- CN106637161A CN106637161A CN201510736240.2A CN201510736240A CN106637161A CN 106637161 A CN106637161 A CN 106637161A CN 201510736240 A CN201510736240 A CN 201510736240A CN 106637161 A CN106637161 A CN 106637161A
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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Abstract
The invention relates to a method for regulating the magnetic performance of a lanthanum calcium manganese oxygen film. The method includes the steps that the lanthanum calcium manganese oxygen film is prepared on a silicon substrate through a chemical solution deposition method; iron ions are doped in the solution; and regular regulation on the magnetic performance of the lanthanum calcium manganese oxygen film is achieved by adjusting the doping amount of the iron ions. The prepared film in even in iron ion distribution, low in surface roughness, free of micro cracks and stable in performance and has the good magnetic performance; by means of the LCMO film prepared through the regulating method, the Curie temperature of the film can be changed in a wide temperature range, and the great significance is achieved in study of magnetic field sensors and magnetoelectric composite materials; and the film has a potential important application prospect in the fields of microwave communication, information, computers, aerospace and the like.
Description
Technical field
The present invention relates to a kind of method of lanthanum calcium manganese oxygen film and regulation and control lanthanum calcium manganese oxygen film magnetic property, belongs to magnetic material
Technical field.
Background technology
La0.7Ca0.3MnO3(LCMO) it is a kind of ferromagnetism functional material, because it has giant magnetoresistance effect, induced by magnetic field exhausted
The behavior such as edge body-metal phase change and lattice structure transformation, in high density magnetic reading head, Magnetic Sensor, magneto-resistor random storage
The aspects such as device, spin polarization transistor are with a wide range of applications.However, LCMO only can obtain huge near Curie temperature
Magneto-resistance effect, which greatly limits its range of application.It is currently reported by Fe3+Doping so as to which part replaces
Mn3+, reduce Mn3+/Mn4+Double exchange model, so as to realize the regular regulation and control of LCMO ceramic material magnetic properties
(Journal of Alloys and Compounds 502,283(2010)).Researcher also attempts being mixed in LCMO films
Fe3+, e.g., the pulse reaction laser cross-beam ablation such as S.Canulescu is in LaAlO3And SrTiO3Deposited on substrate
Fe3+Doping LCMO films (Progress in Solid State Chemistry 35,241 (2007)), the magnetic control such as O.Arnache splashes
Method is penetrated in LaAlO3And SrTiO3Fe is prepared on substrate3+Doping LCMO films (Physical Review B 77,
214430(2008)、Microelectronics Journal 39,544(2008)、Applied Physics A 117,937(2014)).But
It is not realize the regulation and control that LCMO thin film magnetics can be regular so far, which has limited its application in micro element.
The content of the invention
For the disadvantages described above of prior art, it is an object of the invention to provide a kind of side of regulation and control LCMO thin film magnetics energy
Method, the present invention prepares on a si substrate LCMO films using chemical solution deposition, by Fe in change solution3+Doping
Amount, so as to realize the regulation and control that LCMO thin film magnetics can be regular.
Here, the present invention provides a kind of method of regulation and control lanthanum calcium manganese oxygen film magnetic property, methods described includes：In silicon substrate
On, lanthanum calcium manganese oxygen film is prepared using chemical solution deposition, iron ion is mixed in the solution, by the doping for adjusting iron ion
Amount, realizes the regularity regulation and control to lanthanum-strontium-manganese-oxygen film magnetic property.
First, LCMO films are prepared using chemical solution deposition, not only process is simple, low cost, and can be with ten
Divide and easily change Fe3+Doping content, so as to the regulation and control of its magnetic property.Secondly, select Si as film-substrate, be beneficial to
LCMO films are integrated with current microelectronic material.Importantly, the present invention prepare film iron ion be evenly distributed, table
Surface roughness is low, non-microcracked, stable performance, and with preferable magnetic performance, the LCMO prepared using the regulation and control method
Film, can change its Curie temperature in wide temperature range, and this has for the research of magnetic field sensor and magnetic electric compound material
Important meaning, has potential important application prospect in fields such as microwave communication, information, computer, Aero-Space.
It is preferred that the doping of iron ion is 0～20%.
In the present invention, the chemical solution deposition includes：
Step 1) lanthanum acetate, calcium acetate, manganese acetate and ferric nitrate are added the mixed liquor being made up of acetic acid and water according to stoichiometric proportion
In solvent, it is heated to reflux being completely dissolved solvent, obtains mixed solution, adds complexing agent, continuation to heat back in mixed solution
After stream certain hour, solution is cooled to into room temperature, acetic acid and the volume ratio of water are 5 in the mixed solvent:1～2:1, the network
Mixture is 1 with the volume ratio of the mixed solution:5～1:7；
Step 2) by step 1) solution left standstill that obtains after 72～96 hours, filters, and obtains iron ion doping lanthanum calcium manganese oxygen presoma
Solution；
Step 3) by step 2) the iron ion doping lanthanum calcium manganese oxygen precursor solution for preparing is added drop-wise to through pretreatment and the silicon of rotation at a high speed
On substrate, iron ion doping lanthanum calcium manganese oxygen gel mould is obtained；
Step 4) by step 3) in the gel mould that obtains carry out Fractional Heat-treatment：First 5～10 minutes are incubated at 150～200 DEG C, so
It is pyrolyzed 10～15 minutes at 300～400 DEG C afterwards；
Step 5) repeat step 3) and 4), it is to be achieved needed for after film thickness, gel mould annealed at 700～850 DEG C 20～60
Minute.
It is preferred that step 1) in the temperature that is heated to reflux be 70～90 DEG C, add the time being heated to reflux after complexing agent to be
1～2 hour, solute reacted completely.
It is preferred that step 1) described in complexing agent be acetylacetone,2,4-pentanedione.
It is preferred that step 2) in 0.2 micron of filtering with microporous membrane.
It is preferred that step 2) in, the molar concentration of the iron ion doping lanthanum calcium manganese oxygen precursor solution for obtaining is 0.1～
0.3mol/L。
It is preferred that step 3) in, the preprocessing process of silicon substrate is：During silicon substrate is respectively placed in into acetone, second alcohol and water
It is cleaned by ultrasonic, then anneals 20～40 minutes at 300～500 DEG C.
It is preferred that step 3) in, silicon substrate rotating speed is 3000～6000 revs/min.
It is preferred that step 5) in, Fractional Heat-treatment is carried out under oxygen atmosphere.
Description of the drawings
Fig. 1 is the XRD of the film prepared by case study on implementation 1 to 6；
Fig. 2 is zero magnetic-field cooling (ZFC) thermomagnetization curve of the film prepared by case study on implementation 1 to 5；
Fig. 3 is that the film prepared by case study on implementation 1 to 5 has magnetic-field cooling (FC) thermomagnetization curve；
Fig. 4 is the differential curve of the intensity of magnetization to temperature when having magnetic-field cooling of the film prepared by case study on implementation 1 to 5；
Fig. 5 is the resistance variation with temperature curve of film prepared by case study on implementation 1,2,3 and 5；
Fig. 6 is film prepared by case study on implementation 1,2, the 3 and 5 magneto-resistor variation with temperature curve at additional 3T magnetic fields.
Specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following embodiments, it should be appreciated that following embodiments are only used for
The bright present invention, and the unrestricted present invention.
The present invention prepares on a si substrate LCMO films using chemical solution deposition, by Fe in change solution3+Doping
Amount, so as to realize the regulation and control that LCMO thin film magnetics can be regular.
The method of the regulation and control LCMO thin film magnetics energy that the present invention is provided includes：On a silicon substrate, using chemical solution deposition
Method prepares lanthanum calcium manganese oxygen film, and iron ion is mixed in the solution, by the doping for adjusting iron ion, realizes thin to lanthanum strontium manganese oxygen
The regular regulation and control of film magnetic property.
Specifically include following steps：
1) during lanthanum acetate, calcium acetate, manganese acetate and ferric nitrate to be added in molar ratio the mixed liquor solvent being made up of acetic acid and water, plus
Heat backflow is completely dissolved solvent, obtains mixed solution, and acetic acid and the volume ratio of water are 5 in the mixed solvent:1～2:1, plus
Temperature is preferably in the range of 70～90 DEG C during heat backflow；
2) to step 1) appropriate complexing agent acetylacetone,2,4-pentanedione is added in the mixed solution for preparing, and continue to be heated to reflux after certain hour, will
Solution is cooled to room temperature, is selected at 70～90 DEG C, is heated to reflux 1～2 hour；
3) by step 2) in mixed solution stand 72-96 hours after, with 0.2 μm of filtering with microporous membrane, obtain iron ion doping
LCMO precursor solutions；
4) by step 3) the iron ion doping LCMO precursor solutions that prepare are added drop-wise to through pretreatment and at a high speed Si substrates of rotation
On, obtain iron ion doping LCMO gel moulds；
5) by step 4) in the gel mould that obtains Fractional Heat-treatment is carried out in quick anneal oven：The first insulation 5 at 150～200 DEG C～
10 minutes, then it is pyrolyzed 10～15 minutes at 300～400 DEG C；
6) repeat step 4) and 5), gel mould is first carried out into Fractional Heat-treatment under oxygen atmosphere after required film thickness to be achieved：First
Be incubated 5～10 minutes at 150～200 DEG C, be then pyrolyzed 10～15 minutes at 300～400 DEG C, finally 700～
Anneal 20～60 minutes at 850 DEG C.
Wherein, step 1) in, the doping of ferro element is 0～20%, the doping of preferred iron ion be ＞ 0 and≤
10%.
Step 2) in, acetylacetone,2,4-pentanedione is preferably 1 with the volume ratio of mixed solution:5～1:7.
Step 3) in the molar concentration of precursor solution that obtains be preferably 0.1～0.3mol/L.
Step 4) in Si substrate pre-treatment processes be：It is cleaned by ultrasonic in first Si substrates being respectively placed in into acetone, second alcohol and water,
Then anneal 20～40 minutes at 300～500 DEG C preferably in quick anneal oven.
The invention has the beneficial effects as follows：
1) present invention selects Si as substrate, integrated with current microelectronic material beneficial to LCMO films；
2) present invention provide method, solute used be lanthanum acetate, calcium acetate, manganese acetate, ferric nitrate, solvent be acetic acid, water and
Acetylacetone,2,4-pentanedione, raw material is cheap, nontoxic, discharges without toxic gas in preparation process, and environmental pollution is little；
3) film iron ion prepared by the present invention is evenly distributed, surface roughness is low, non-microcracked, stable performance, and with preferable
Magnetic performance；
4) preparation process is simple of the present invention, without the need for special installation, is conducive to large-scale production；
5) present invention with the chemical ratios of very convenient regulation and control each element, can be conducive to the regulation and control of LCMO thin film magnetics energy.
The present invention is further illustrated below in conjunction with drawings and embodiments, but accompanying drawing and following embodiments are merely to illustrate this
Invention, and the unrestricted present invention, those skilled in the art according to some nonessential improvement that the above of invention is made and
Adjustment belongs to protection scope of the present invention.In addition, concrete proportioning, time, temperature of following technological parameters etc. are also only examples
Property, those skilled in the art can select suitable value in the range of above-mentioned restriction.
Embodiment 1
A) cleaning of silicon substrate
First surface of silicon pollutant is blown off with nitrogen, then silicon chip is successively placed on into ultrasound in acetone, ethanol and deionized water clear
Wash 10 minutes, after the cleaning of Si substrates is finished, dry at 450 DEG C, it is standby after natural cooling.
B) preparation of precursor solution
First by La:Ca:Mn:Fe elemental mole ratios are 0.7:0.3:1:0.01 lanthanum acetate, calcium acetate, manganese acetate and ferric nitrate are dissolved in
In the mixed solvent of acetic acid and deionized water, being heated to 60～80 DEG C is completely dissolved solute, is subsequently adding complexing agent levulinic
Ketone, and continuing heating makes solute react completely, the volume ratio of acetic acid and acetylacetone,2,4-pentanedione is 5:1:1, manganese element concentration in solution
For 0.1M/L, the solution room temperature for obtaining is placed into 72～96h, obtain stable with 0.2 micron of filtering with microporous membrane solution
Iron ion doping amount is 1% LCMO thin film precursor solution.
C) preparation of film
Precursor solution is at the uniform velocity added dropwise first on the clean silicon chip of high speed rotation, silicon substrate rotating speed is 5000 revs/min, during holding
Between be 30 seconds, you can layer of gel film is obtained on silicon chip.It is placed on Fractional Heat-treatment in quick anneal oven：First 200
5 minutes are incubated at DEG C, 400 DEG C are then raised temperature to, 10 minutes is incubated at this temperature, repeat this process 7 times, finally existed
Anneal 30 minutes at 750 DEG C, that is, obtain the LCMO films that the iron ion doping amount that thickness is 140nm is 1%.
Embodiment 2
The present embodiment is with the difference of embodiment 1：The doping of iron ion is 3%, remaining content and the complete phase of embodiment 1
Together.
Embodiment 3
The present embodiment is with the difference of embodiment 1：The doping of iron ion is 5%, remaining content and the complete phase of embodiment 1
Together.
Embodiment 4
The present embodiment is with the difference of embodiment 1：The doping of iron ion is 10%, remaining content and the complete phase of embodiment 1
Together.
Embodiment 5
The present embodiment is with the difference of embodiment 1：The doping of iron ion is not carried out, remaining content and the complete phase of embodiment 1
Together.
Embodiment 6
The present embodiment is with the difference of embodiment 1：Manganese ion is all replaced by iron ion, and remaining content is complete with embodiment 1
It is identical.
Performance detection：
1. crystal structure detection
Table 1：The lattice paprmeter of the film of case study on implementation 1 to 6
The crystallinity of film 1 to 6 can be seen that well by Fig. 1 and Biao 1 and orthohormbic structure, iron ion doping is
The lattice paprmeter of LCMO films can fluctuate with the different of doping, but its unit cell volume is all the time between unadulterated
Between LCMO and LCFO.
2. magnetic property detection
As shown in Figures 2 to 4, with the increase of iron ion doping amount, the Curie temperature of LCMFO is moved to low temperature direction, is being occupied
In below temperature, all show good ferromagnetism.
3. electronic transport performance
As shown in Figure 5 and Figure 6, with the increase of iron ion doping amount, the metal-insulator transition temperature of LCMFO films constantly to
Low temperature direction is moved, while the maximum magnetic flux resistance value of film is also continuously increased, when iron ion doping amount is 5%, its magneto-resistor
Value is up to 75%.
Industrial applicability：The LCMO films prepared using the regulation and control method, can change its Curie in wide temperature range
Temperature, this has great significance for the research of magnetic field sensor and magnetic electric compound material, in microwave communication, information, calculating
There is potential important application prospect in the fields such as machine, Aero-Space.
Claims (10)
1. it is a kind of regulation and control lanthanum calcium manganese oxygen film magnetic property method, it is characterised in that methods described includes：
On a silicon substrate, lanthanum calcium manganese oxygen film is prepared using chemical solution deposition, iron ion is mixed in the solution, by the doping for adjusting iron ion, realize the regularity regulation and control to lanthanum-strontium-manganese-oxygen film magnetic property.
2. method according to claim 1, it is characterised in that the doping of iron ion is 0～20%.
3. method according to claim 1 and 2, it is characterised in that the chemical solution deposition includes：
Step 1）Lanthanum acetate, calcium acetate, manganese acetate and ferric nitrate are added in the mixed liquor solvent being made up of acetic acid and water according to stoichiometric proportion, it is heated to reflux being completely dissolved solvent, obtain mixed solution, complexing agent is added in mixed solution, continue to be heated to reflux after certain hour, solution is cooled to into room temperature, acetic acid and the volume ratio of water are 5 in the mixed solvent:1～2:1, the complexing agent is 1 with the volume ratio of the mixed solution:5～1:7；
Step 2）By step 1) solution left standstill that obtains after 72～96 hours, filters, and obtains iron ion doping lanthanum calcium manganese oxygen precursor solution；
Step 3）By step 2) the iron ion doping lanthanum calcium manganese oxygen precursor solution for preparing is added drop-wise to through pretreatment and at a high speed on the silicon substrate of rotation, obtains iron ion doping lanthanum calcium manganese oxygen gel mould；
Step 4）By step 3) in the gel mould that obtains carry out Fractional Heat-treatment：First 5～10 minutes are incubated at 150～200 DEG C, are then pyrolyzed 10～15 minutes at 300～400 DEG C；
Step 5）Repeat step 3) and 4), after required film thickness to be achieved, gel mould is annealed 20～60 minutes at 700～850 DEG C.
4. method according to claim 3, it is characterised in that step 1）In the temperature that is heated to reflux be 70～90 DEG C, add the time being heated to reflux after complexing agent to be 1～2 hour.
5. the method according to claim 3 or 4, it is characterised in that step 1）Described in complexing agent be acetylacetone,2,4-pentanedione.
6. the method according to any one of claim 3～5, it is characterised in that step 2）It is middle to use 0.2 micron of filtering with microporous membrane.
7. the method according to any one of claim 3～6, it is characterised in that step 2）In, the molar concentration of the iron ion doping lanthanum calcium manganese oxygen precursor solution for obtaining is 0.1～0.3mol/L.
8. the method according to any one of claim 3～7, it is characterised in that step 3）In, the preprocessing process of silicon substrate is：It is cleaned by ultrasonic during silicon substrate is respectively placed in into acetone, second alcohol and water, then anneals 20～40 minutes at 300～500 DEG C.
9. the method according to any one of claim 3～8, it is characterised in that step 3）In, silicon substrate rotating speed is 3000～6000 revs/min.
10. the method according to any one of claim 3～9, it is characterised in that step 5）In, Fractional Heat-treatment is carried out under oxygen atmosphere.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1785906A (en) * | 2005-11-04 | 2006-06-14 | 北京工业大学 | Preparation method of lanthanum calcium manganese oxygen functional ceramic |
| KR20110051955A (en) * | 2009-11-11 | 2011-05-18 | 한국과학기술연구원 | Method of non-shrinkage fabrication of metal oxide thin film for solid oxide fuel cell by low temperature |
| CN103774227A (en) * | 2014-01-20 | 2014-05-07 | 华东师范大学 | Manganite epitaxial thin film and preparation method thereof |
-
2015
- 2015-11-03 CN CN201510736240.2A patent/CN106637161B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1785906A (en) * | 2005-11-04 | 2006-06-14 | 北京工业大学 | Preparation method of lanthanum calcium manganese oxygen functional ceramic |
| KR20110051955A (en) * | 2009-11-11 | 2011-05-18 | 한국과학기술연구원 | Method of non-shrinkage fabrication of metal oxide thin film for solid oxide fuel cell by low temperature |
| CN103774227A (en) * | 2014-01-20 | 2014-05-07 | 华东师范大学 | Manganite epitaxial thin film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李阿丹: ""La2/3Ca1/3Mn(1-x)FexO3溶胶凝胶制备和表征"", 《硅酸盐通报》 * |
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