CN106637161B - A method of regulation lanthanum calcium manganese oxygen film magnetic property - Google Patents
A method of regulation lanthanum calcium manganese oxygen film magnetic property Download PDFInfo
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- CN106637161B CN106637161B CN201510736240.2A CN201510736240A CN106637161B CN 106637161 B CN106637161 B CN 106637161B CN 201510736240 A CN201510736240 A CN 201510736240A CN 106637161 B CN106637161 B CN 106637161B
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Abstract
The present invention relates to a kind of methods of regulation lanthanum calcium manganese oxygen film magnetic property, the described method includes: on a silicon substrate, lanthanum calcium manganese oxygen film is prepared using chemical solution deposition, iron ion is mixed in the solution, by adjusting the doping of iron ion, realizes and the regularity of lanthanum-strontium-manganese-oxygen film magnetic property is regulated and controled.Film iron ion prepared by the present invention is evenly distributed, surface roughness is low, non-microcracked, performance is stablized, and there is preferable magnetic performance, the LCMO film prepared using the regulation method, its Curie temperature can be changed in wide temperature range, this has great significance for the research of magnetic field sensor and magnetic electric compound material, has potential important application prospect in fields such as microwave communication, information, computer, aerospaces.
Description
Technical field
The present invention relates to a kind of methods of lanthanum calcium manganese oxygen film and regulation lanthanum calcium manganese oxygen film magnetic property, belong to magnetic material
Expect technical field.
Background technique
La0.7Ca0.3MnO3It (LCMO) is a kind of ferromagnetism functional material, because it is with giant magnetoresistance effect, induced by magnetic field
The behaviors such as insulator-metal phase transition and lattice structure transformation, in high density magnetic reading head, Magnetic Sensor, magneto-resistor random storage
Device, spin polarization transistor etc. are with a wide range of applications.However, LCMO only can obtain huge magnetic near Curie temperature
Electricresistance effect, which greatly limits its application ranges.It is currently reported to pass through Fe3+Doping makes its part replace Mn3+, reduce
Mn3+/Mn4+Double exchange model, thus realize LCMO ceramic material magnetic property regularity regulation (Journal of Alloys
and Compounds 502,283(2010)).Researcher also attempts to mix Fe in LCMO film3+, e.g., S.Canulescu
Deng with pulse reaction laser cross-beam ablation in LaAlO3And SrTiO3It deposited Fe on substrate3+Adulterate LCMO film
(Progress in Solid State Chemistry 35,241 (2007)), the magnetron sputtering method such as O.Arnache exist
LaAlO3And SrTiO3Fe is prepared on substrate3+Doping LCMO film (Physical Review B 77,214430 (2008),
Microelectronics Journal 39,544(2008),Applied Physics A 117,937(2014)).But
So far there is no the regulation for realizing that LCMO thin film magnetic can be regular, the application which has limited it in micro element.
Summary of the invention
For the disadvantages described above of the prior art, the object of the present invention is to provide a kind of sides of regulation LCMO thin film magnetic energy
Method, the present invention prepare LCMO film using chemical solution deposition on a si substrate, by changing Fe in solution3+Doping, from
And realize the regulation that LCMO thin film magnetic can be regular.
Here, the present invention provides a kind of method of regulation lanthanum calcium manganese oxygen film magnetic property, which comprises in silicon substrate
On, lanthanum calcium manganese oxygen film is prepared using chemical solution deposition, mixes iron ion in the solution, by the doping for adjusting iron ion
Amount is realized and is regulated and controled to the regularity of lanthanum calcium manganese oxygen film magnetic property.
Firstly, prepare LCMO film using chemical solution deposition, not only simple process, at low cost, and can be very
It is convenient to change Fe3+Doping concentration, so as to the regulation of its magnetic property.Secondly, selecting Si as film-substrate, it is thin to be conducive to LCMO
Film is integrated with current microelectronic material.Importantly, film iron ion prepared by the present invention is evenly distributed, surface roughness
It is low, non-microcracked, performance stablize, and have preferable magnetic performance, using the regulation method prepare LCMO film, can compared with
Change its Curie temperature in wide temperature range, this has important meaning for the research of magnetic field sensor and magnetic electric compound material
Justice has potential important application prospect in fields such as microwave communication, information, computer, aerospaces.
Preferably, the doping of iron ion is 0~20%.
In the present invention, the chemical solution deposition includes:
Lanthanum acetate, calcium acetate, manganese acetate and ferric nitrate are added according to stoichiometric ratio and are made of acetic acid and water by step 1)
In the mixed solvent, being heated to reflux is completely dissolved solvent, obtains mixed solution, complexing agent is added into mixed solution, continue
It being heated to reflux after a certain period of time, solution is cooled to room temperature, the volume ratio of the in the mixed solvent acetic acid and water is 5:1~2:1,
The volume ratio of the complexing agent and the mixed solution is 1:5~1:7；
Behind solution left standstill 72~96 hours that step 2) obtains step 1), filtering obtains iron ion doping lanthanum calcium manganese oxygen
Precursor solution；
Iron ion doping lanthanum calcium manganese oxygen precursor solution prepared by step 2) is added drop-wise to by pretreatment and height by step 3)
On the silicon substrate of speed rotation, iron ion doping lanthanum calcium manganese oxygen gel mould is obtained；
Gel mould obtained in step 3) is carried out Fractional Heat-treatment by step 4): 5~10 are first kept the temperature at 150~200 DEG C
Minute, then it is pyrolyzed 10~15 minutes at 300~400 DEG C；
Step 5) repeats step 3) with 4), and after required film thickness to be achieved, gel mould is annealed at 700~850 DEG C
20~60 minutes.
Preferably, the temperature being heated to reflux in step 1) is 70~90 DEG C, it is 1 that the time being heated to reflux after complexing agent, which is added,
~2 hours, solute reacted completely.
Preferably, complexing agent described in step 1) is acetylacetone,2,4-pentanedione.
Preferably, with 0.2 micron of filtering with microporous membrane in step 2).
Preferably, in step 2), the molar concentration of obtained iron ion doping lanthanum calcium manganese oxygen precursor solution is 0.1~
0.3mol/L。
Preferably, in step 3), the preprocessing process of silicon substrate are as follows: silicon substrate is respectively placed in acetone, in second alcohol and water
Ultrasonic cleaning, then anneals 20~40 minutes at 300~500 DEG C.
Preferably, silicon substrate revolving speed is 3000~6000 revs/min in step 3).
Preferably, carrying out Fractional Heat-treatment under oxygen atmosphere in step 5).
Detailed description of the invention
Fig. 1 is the XRD diagram of film prepared by case study on implementation 1 to 6；
Fig. 2 is zero magnetic-field cooling (ZFC) thermomagnetization curve of film prepared by case study on implementation 1 to 5；
Fig. 3 is that film prepared by case study on implementation 1 to 5 has magnetic-field cooling (FC) thermomagnetization curve；
Fig. 4 is differential curve of the intensity of magnetization to temperature when having magnetic-field cooling of 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 that the magneto-resistor variation with temperature when adding the magnetic field 3T outside of film prepared by case study on implementation 1,2,3 and 5 is bent
Line.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that following embodiments are only used for
Illustrate the present invention, is not intended to limit the present invention.
The present invention prepares LCMO film using chemical solution deposition on a si substrate, by changing Fe in solution3+Doping
Amount, to realize the regulation that LCMO thin film magnetic can be regular.
The method of regulation LCMO thin film magnetic energy provided by the invention includes: on a silicon substrate, using chemical solution deposition
Method prepares lanthanum calcium manganese oxygen film, mixes iron ion in the solution, by adjusting the doping of iron ion, realizes thin to lanthanum calcium manganese oxygen
The regularity regulation of film magnetic property.
Specifically includes the following steps:
1) lanthanum acetate, calcium acetate, manganese acetate and ferric nitrate are added to the mixed solvent being made of acetic acid and water in molar ratio
In, being heated to reflux is completely dissolved solvent, obtain mixed solution, the volume ratio of the in the mixed solvent acetic acid and water be 5:1~
2:1, temperature is preferably within the scope of 70~90 DEG C when being heated to reflux；
2) appropriate complexing agent acetylacetone,2,4-pentanedione is added in the mixed solution prepared to step 1), and continues to be heated to reflux a timing
Between after, solution is cooled to room temperature, is selected at 70~90 DEG C, is heated to reflux 1~2 hour；
3) after the mixed solution in step 2) being stood 72-96 hours, with 0.2 μm of filtering with microporous membrane, iron ion is obtained
Adulterate LCMO precursor solution；
4) by step 3) prepare iron ion doping LCMO precursor solution be added drop-wise to by pretreatment and it is high-speed rotating
On Si substrate, iron ion doping LCMO gel mould is obtained；
5) gel mould obtained in step 4) is subjected to Fractional Heat-treatment in quick anneal oven: first at 150~200 DEG C
Heat preservation 5~10 minutes, is then pyrolyzed 10~15 minutes at 300~400 DEG C；
6) step 4) is repeated with 5), and gel mould is first carried out to segmentation heat under oxygen atmosphere after required film thickness to be achieved
Processing: 5~10 minutes first are kept the temperature at 150~200 DEG C, is then pyrolyzed 10~15 minutes at 300~400 DEG C, finally 700
It anneals 20~60 minutes at~850 DEG C.
Wherein, in step 1), the doping of ferro element is 0~20%, preferably the doping of iron ion be > 0 and≤
10%.
In step 2), the volume ratio of acetylacetone,2,4-pentanedione and mixed solution is preferably 1:5~1:7.
The molar concentration of precursor solution obtained in step 3) is preferably 0.1~0.3mol/L.
Si substrate pre-treatment process in step 4) are as follows: Si substrate is first respectively placed in acetone, is cleaned by ultrasonic in second alcohol and water,
Then it anneals 20~40 minutes at 300~500 DEG C preferably in quick anneal oven.
The beneficial effects of the present invention are:
1) present invention select Si as substrate, conducive to integrating for LCMO film and current microelectronic material；
2) method provided by the invention, 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 in preparation process without toxic gas, and environmental pollution is small；
3) film iron ion prepared by the present invention is evenly distributed, surface roughness is low, non-microcracked, and performance is stablized, and has
There is preferable magnetic performance；
4) preparation process of the present invention is simple, is not necessarily to special installation, is conducive to large-scale production；
5) chemical ratios for the regulation each element that the present invention can be very convenient are conducive to the tune of LCMO thin film magnetic energy
Control.
The present invention is further illustrated below in conjunction with drawings and embodiments, but attached drawing and following embodiments are merely to illustrate
The present invention is not intended to limit the present invention, and those skilled in the art some nonessential changes according to what the above content of invention was made
It is all belonged to the scope of protection of the present invention into adjustment.In addition, the specific proportion of following technological parameters, time, temperature etc. are also only
Exemplary, those skilled in the art can select suitably to be worth in the range of above-mentioned restriction.
Embodiment 1
A) cleaning of silicon substrate
Surface of silicon pollutant is blown off with nitrogen first, then silicon wafer is successively placed on to acetone, ethyl alcohol and deionization
It is cleaned by ultrasonic 10 minutes in water, after Si substrate cleans, is dried at 450 DEG C, it is spare after natural cooling.
B) preparation of precursor solution
Lanthanum acetate, calcium acetate, manganese acetate and the nitre for being first 0.7:0.3:1:0.01 by La:Ca:Mn:Fe elemental mole ratios
For sour dissolved ferric iron in the in the mixed solvent of acetic acid and deionized water, being heated to 60~80 DEG C is completely dissolved solute, and network is then added
Mixture acetylacetone,2,4-pentanedione, and continuing heating reacts solute completely, the volume ratio of acetic acid and acetylacetone,2,4-pentanedione is 5:1:1, manganese in solution
Concentration of element is 0.1M, and obtained solution is placed at room temperature for 72~96h, is obtained with 0.2 micron of filtering with microporous membrane solution
The LCMO thin film precursor solution that stable iron ion doping amount is 1%.
C) preparation of film
Precursor solution is at the uniform velocity added dropwise on high-speed rotating clean silicon chip first, silicon substrate revolving speed be 5000 turns/
Point, the retention time is 30 seconds, and layer of gel film can be obtained on silicon wafer.Place it in Fractional Heat-treatment in quick anneal oven:
5 minutes first are kept the temperature at 200 DEG C, then raises temperature to 400 DEG C, keeps the temperature 10 minutes at this temperature, repetition this process 7 times, finally
30 minutes are annealed at 750 DEG C to get the LCMO film for being 1% to the iron ion doping amount with a thickness of 140nm.
Embodiment 2
The present embodiment difference from example 1 is that: the doping of iron ion is 3%, remaining content and embodiment 1
It is identical.
Embodiment 3
The present embodiment difference from example 1 is that: the doping of iron ion is 5%, remaining content and embodiment 1
It is identical.
Embodiment 4
The present embodiment difference from example 1 is that: the doping of iron ion is 10%, remaining content and embodiment
1 is identical.
Embodiment 5
The present embodiment difference from example 1 is that: do not carry out the doping of iron ion, remaining content and embodiment 1
It is identical.
Embodiment 6
The present embodiment difference from example 1 is that: manganese ion is all replaced by iron ion, remaining content and implement
Example 1 is identical.
Performance detection:
1. crystal structure detects
Table 1: the lattice constant of 1 to 6 film of case study on implementation
。
1 to 6 crystallinity of film is good it can be seen from Fig. 1 and table 1 and is orthohormbic structure, and iron ion doping LCMO is thin
The lattice constant of film can be fluctuated with the difference of doping, but its unit cell volume always between undoped LCMO and
Between LCFO.
2. magnetic property detects
As shown in Figures 2 to 4, with the increase of iron ion doping amount, the Curie temperature of LCMFO is mobile to low temperature direction,
In Curie temperature hereinafter, all showing 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 film
It is constantly mobile to low temperature direction, while the maximum magnetic flux resistance value of film is also continuously increased, when iron ion doping amount is 5%,
Magnetoelectricity resistance value is up to 75%.
Industrial applicability: the LCMO film prepared using the regulation 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, aerospace.
Claims (7)
1. a kind of method of regulation lanthanum calcium manganese oxygen film magnetic property, which is characterized in that the method is in lanthanum calcium manganese oxygen film
La0.7Ca0.3MnO3Middle doping iron ion, wherein the doping of iron ion is > 0 and≤10%, which comprises
Lanthanum acetate, calcium acetate, manganese acetate and ferric nitrate are added according to stoichiometric ratio and are mixed by what acetic acid and water formed by step 1)
In bonding solvent, being heated to reflux is completely dissolved solute, obtains mixed solution, and complexing agent is added into mixed solution, continues to heat
Reflux is completely dissolved solute, and solution is cooled to room temperature, and the volume ratio of the in the mixed solvent acetic acid and water is 5:1~2:1,
The volume ratio of the complexing agent and the mixed solution is 1:5~1:7；
Behind solution left standstill 72~96 hours that step 2 obtains step 1), filtering obtains iron ion doping lanthanum calcium manganese oxygen forerunner
Liquid solution；
Iron ion doping lanthanum calcium manganese oxygen precursor solution prepared by step 2) is added drop-wise to by step 3) to be revolved by pretreatment and high speed
On the silicon substrate turned, iron ion doping lanthanum calcium manganese oxygen gel mould is obtained, silicon substrate revolving speed is 3000~6000 revs/min；
Gel mould obtained in step 3) is carried out Fractional Heat-treatment by step 4): 5~10 minutes first are kept the temperature at 150~200 DEG C,
Then it is pyrolyzed 10~15 minutes at 300~400 DEG C；
Step 5) repeats step 3) and 4), it is to be achieved needed for after film thickness, gel mould annealed to 20 at 700~850 DEG C~
60 minutes；
In the method, by adjusting the doping of iron ion, realizes and the regularity of lanthanum calcium manganese oxygen film magnetic property is regulated and controled.
2. adding the method according to claim 1, wherein the temperature being heated to reflux in step 1) is 70~90 DEG C
Entering the time being heated to reflux after complexing agent is 1~2 hour.
3. the method according to claim 1, wherein complexing agent described in step 1) is acetylacetone,2,4-pentanedione.
4. the method according to claim 1, wherein with 0.2 micron of filtering with microporous membrane in step 2.
5. the method according to claim 1, wherein in step 2, before obtained iron ion doping lanthanum calcium manganese oxygen
The molar concentration for driving liquid solution is 0.1~0.3mol/L.
6. the method according to claim 1, wherein in step 3), the preprocessing process of silicon substrate are as follows: serve as a contrast silicon
Bottom is respectively placed in acetone, is cleaned by ultrasonic in second alcohol and water, then anneals 20~40 minutes at 300~500 DEG C.
7. method described according to claim 1~any one of 6, which is characterized in that in step 5), required film to be achieved is thick
After degree, Fractional Heat-treatment is first carried out under oxygen atmosphere and is annealed 20~60 minutes at 700~850 DEG C again.
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Citations (2)
| 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 |
| CN103774227A (en) * | 2014-01-20 | 2014-05-07 | 华东师范大学 | Manganite epitaxial thin film and preparation method thereof |
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| KR101186929B1 (en) * | 2009-11-11 | 2012-09-28 | 한국과학기술연구원 | Method of non-shrinkage fabrication of metal oxide thin film for solid oxide fuel cell by low temperature |
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Patent Citations (2)
| 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 |
| 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 |
|---|
| "La2/3Ca1/3Mn(1-x)FexO3溶胶凝胶制备和表征";李阿丹;《硅酸盐通报》;20070430;第26卷(第2期);第401-403页 * |
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