CN106987811B - A kind of temperature magnetic field film-sensing material and preparation method thereof - Google Patents
A kind of temperature magnetic field film-sensing material and preparation method thereof Download PDFInfo
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- CN106987811B CN106987811B CN201710178568.6A CN201710178568A CN106987811B CN 106987811 B CN106987811 B CN 106987811B CN 201710178568 A CN201710178568 A CN 201710178568A CN 106987811 B CN106987811 B CN 106987811B
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- C—CHEMISTRY; METALLURGY
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
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- C01G45/00—Compounds of manganese
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- C—CHEMISTRY; METALLURGY
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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Abstract
The present invention discloses a kind of temperature magnetic field film-sensing material and preparation method thereof, replaces lanthanum ion in Mn oxide with calcium ion and barium ions part, is modulated to the magnetoresistance characteristics and Curie temperature of Mn oxide material.Mn oxide material presoma is prepared using sol-gal process first, then by the material precursor powdered and block target is made, finally block target material deposition on substrate and is annealed with pulsed laser deposition.Mn oxide presoma is prepared using sol-gal process, so that the relatively uniform, particle size of Mn oxide material mixing is nanoscale and particle size uniformity is higher, sol-gal process has the characteristics that easy to operate, mild condition, easy to control；Deposit manganese-salt phosphating with pulsed laser deposition, have the characteristics that high-quality, uniformity is high and material component is stablized, be effectively guaranteed obtained by film and target material composition it is consistent.In addition, membrane structure has also widened paramagnetic state-ferrimagnetic state transformation warm area of Mn oxide material.
Description
Technical field
The present invention relates to sensor material technical field more particularly to a kind of temperature magnetic field film-sensing material and its preparations
Method.
Background technique
Scientific technological advance makes rapid progress, the especially rapid development of intelligent robot technology and technology of Internet of things, people
There is higher hope to existing sensor technology.It is desirable to acquire equipment by simple sensor to obtain more
Information, this is that traditional sensor can not be accomplished.Traditional sensor function purposes is all relatively simple, it is generally the case that one
A sensor can only measure a type of external parameter.For example, thermocouple temperature sensor can only measure the temperature in environment,
Without being capable of measuring other kinds of environmental physics amount；Tesla meter can only also measure the magnetic field size in environment.With material skill
Art is constantly progressive, and the new material with special nature of a batch is developed, and calcium titanium ore manganose oxide is exactly one such.
Calcium titanium ore manganose oxide is a kind of material with CMR effect, the magneto-resistor which has traditional material incomparable
Change rate.Research shows that the magneto-resistor of the perovskite manganese oxide material can generate response to temperature and change of magnetic field strength, and
It and near Curie temperature is linear response, but, magnetoresistive ratio lower since there are its Curie temperature be smaller and paramagnetic
The disadvantages of state-ferrimagnetic state transformation warm area is relatively narrow, limits application of the material in terms of sensor.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of temperature magnetic field film-sensing material and its systems
Preparation Method.
The technical solution adopted by the present invention is that:
A kind of temperature magnetic field film-sensing material prepares Mn oxide material presoma using sol-gal process first, so
By Mn oxide material precursor powder and block target is made afterwards, finally the block target is sunk with pulsed laser deposition
Product calcium titanium ore manganose oxide film obtained on the substrate of insulation.
Invention additionally discloses a kind of preparation method of temperature magnetic field film-sensing material, it is used to prepare a kind of temperature
Magnetic field film-sensing material, preparation method the following steps are included:
Step 1: Mn oxide material presoma is prepared using sol-gal process,
Step 2: by Mn oxide material precursor powder and block target is made,
Step 3: the block target material deposition being obtained into calcium titanium ore manganose oxidation on the substrate of insulation with pulsed laser deposition
Object film.
Further, when preparing Mn oxide material presoma with sol-gal process material used include lanthanum source material,
Calcium source material, barium source material, manganese source material, the lanthanum source material, calcium source material, barium source material, manganese source material respectively correspond for
Lanthanum nitrate, calcium acetate, barium nitrate, manganese acetate.
Further, Mn oxide material presoma is prepared with sol-gal process in the step 1 specifically include following step
It is rapid:
Lanthanum nitrate material, acetic acid calcium material, barium nitrate material, acetic acid manganese material are pressed La2/3 (Ca1-xBax) 1/ by 1-1
The ratio between cationic amount of substance carries out precise in 3MnO3, wherein 0.2≤x≤0.8, in the feelings of 80 DEG C of water-baths and stirring
It under condition, is completely dissolved in suitable deionized water, obtains transparent no precipitation solution A；
1-2, uses citric acid as dispersing agent, weighs by the ratio between amount of substance of citric acid and metal cation for 1.2: 1
Citric acid is dissolved in suitable ethylene glycol and is stirred continuously, and into solution, dropwise addition dilute nitric acid solution is transparent to solution, obtains solution
B；
Solution B is slowly added into solution A in the case where water-bath, constantly stirs by 1-3, until obtaining dry solidifying
Glue；
Xerogel is placed in 120 DEG C of air dry ovens and is dried by 1-4, until it is dry to obtain loose porous sepia
Gel.
Further, the dosage of ethylene glycol described in the step 1-2 determines its use according to the requirement of solution B viscosity
Amount.
Further, in the step 2 by the Mn oxide material precursor powder and that packaged target is made is specific
The following steps are included:
The sepia xerogel is ground into no granular sensation powder by 2-1；
2-2 holds the powder with porcelain crucible, is placed in 6 hours in 400 DEG C of Muffle furnaces, and removal organic matter obtains powder
C；
Suitable polyvinyl alcohol is placed in deionized water by 2-3, and water-bath to debita spissitudo obtains polyvinyl alcohol colloid；
Suitable polyvinylidene alcohol colloid is added drop-wise in the powder C by 2-4, is ground and uniformly obtains powder
D；
The powder D is pressed into diameter 28mm round shape target with metal die by 2-5, and pressure size used is 25MPa；
The round shape target is placed in 3 hours in 500 DEG C of Muffle furnaces by 2-6, removes polyvinylidene alcohol colloid；
The round shape target is placed in 1050 DEG C of 10 hours of annealing in tube furnace, obtains Mn oxide bulk target by 2-7
Material.
Further, the Mn oxide block target material deposition is being insulated with pulsed laser deposition in the step 3
On substrate specifically includes the following steps:
The Mn oxide bulk target and insulating substrate are respectively placed on corresponding position by 3-1, close vacuum
Room successively opens mechanical pump and molecular pump vacuumizes vacuum chamber；
3-2, when the vacuum degree in vacuum chamber reaches 10-4When Pa, molecular pump is closed, opens oxygen valve, adjusts vacuum chamber
Oxygen pressure is 50Pa；
3-3, setting vacuum chamber liner bottom temperature are 700 DEG C, and the insulating substrate is covered with baffle；
3-4, the energy that pulse laser is arranged is 280mJ, and frequency is 3Hz and is beaten in advance:
3-5 removes the baffle, starts to deposit, and keeps the temperature 20min in situ after deposition 90min and is cooled to room temperature, manganese oxygen is made
Compound film.
The manganese-salt phosphating is placed in Muffle furnace by 3-6, and 800 DEG C of annealing 120min, naturally cool to room in air
Temperature obtains calcium titanium ore manganose oxide film.
Further, the sedimentation time that manganese-salt phosphating is made is adjusted according to the thickness of aimed thin film, adjustment
Rate is 500nm/h.
Further, the insulating substrate material includes simple glass, quartz glass and corundum.
The invention adopts the above technical scheme, by replacing lanthanum ion in Mn oxide with calcium ion and barium ions part,
And the ratio by adjusting each metal cation in Mn oxide material, magnetoresistance characteristics, residence to the Mn oxide material
In temperature be modulated, make the Curie temperature of the Mn oxide material near room temperature and have biggish magneto-resistor variation
Rate；Because preparing Mn oxide presoma using sol-gal process, so that the Mn oxide material mixes relatively uniform, product grain
Diameter is Nano grade and relatively uniform, and this method has the characteristics that synthesis process mild condition, easy to control；Finally use pulse laser
Sedimentation deposits manganese-salt phosphating, and the film that this method obtains has high-quality, uniformity is high and material component is stablized etc.
Feature, in addition, membrane structure has also widened paramagnetic state-ferrimagnetic state transformation warm area of Mn oxide material.Method of the invention is not
It only may insure the homogeneity of film thickness, moreover it is possible to improve thin-film material quality.
Detailed description of the invention
The present invention is described in further details below in conjunction with the drawings and specific embodiments；
Fig. 1 is a kind of flow diagram of temperature magnetic field film-sensing material preparation method of the present invention；
Fig. 2 is the present invention a kind of intensity of magnetization variation with temperature curve and dM/dT of temperature magnetic field film-sensing material
Curve；
Fig. 3 is a kind of magneto-resistor variation with temperature curve of temperature magnetic field film-sensing material of the present invention；
Fig. 4 is a kind of change curve of the magneto-resistor of temperature magnetic field film-sensing material of the present invention with magnetic field strength.
Specific embodiment
Shown in one of picture 1-4, invention additionally discloses a kind of preparation methods of temperature magnetic field film-sensing material, for making
A kind of standby temperature magnetic field film-sensing material, preparation method the following steps are included:
Step 1: Mn oxide material presoma is prepared using sol-gal process,
Step 2: by Mn oxide material precursor powder and block target is made,
Step 3: the block target material deposition being obtained into calcium titanium ore manganose oxidation on the substrate of insulation with pulsed laser deposition
Object film.
Further, when preparing Mn oxide material presoma with sol-gal process material used include lanthanum source material,
Calcium source material, barium source material, manganese source material, the lanthanum source material, calcium source material, barium source material, manganese source material respectively correspond for
Lanthanum nitrate, calcium acetate, barium nitrate, manganese acetate.
Further, Mn oxide material presoma is prepared with sol-gal process in the step 1 specifically include following step
It is rapid:
Lanthanum nitrate material, acetic acid calcium material, barium nitrate material, acetic acid manganese material are pressed La2/3 (Ca1-xBax) 1/ by 1-1
The ratio between the amount (unit: mole) of cationic substance carries out precise in 3MnO3, wherein 0.2≤x≤0.8, such as manganese acetate
Material can carry out precise by 10: 3: 2: 15 the ratio between stoichiometric number, completely molten in the case where 80 DEG C of water-baths and stirring
In suitable deionized water, transparent no precipitation solution A is obtained；
1-2, uses citric acid as dispersing agent, weighs by the ratio between amount of substance of citric acid and metal cation for 1.2: 1
Citric acid is dissolved in suitable ethylene glycol and is stirred continuously, and into solution, dropwise addition dilute nitric acid solution is transparent to solution, obtains solution
B；
Solution B is slowly added into solution A in the case where water-bath, constantly stirs by 1-3, until obtaining dry solidifying
Glue；
Xerogel is placed in 120 DEG C of air dry ovens and is dried by 1-4, until it is dry to obtain loose porous sepia
Gel.
Further, the dosage of ethylene glycol described in the step 1-2 determines its use according to the requirement of solution B viscosity
Amount.
Further, in the step 2 by the Mn oxide material precursor powder and that packaged target is made is specific
The following steps are included:
The sepia xerogel is ground into no granular sensation powder by 2-1；
2-2 holds the powder with porcelain crucible, is placed in 6 hours in 400 DEG C of Muffle furnaces, and removal organic matter obtains powder
C；
Suitable polyvinyl alcohol is placed in deionized water by 2-3, and water-bath to debita spissitudo obtains polyvinyl alcohol colloid；
Suitable polyvinylidene alcohol colloid is added drop-wise in the powder C by 2-4, is ground and uniformly obtains powder
D；
The powder D is pressed into diameter 28mm round shape target with metal die by 2-5, and pressure size used is 25MPa；
The round shape target is placed in 3 hours in 500 DEG C of Muffle furnaces by 2-6, removes polyvinylidene alcohol colloid；
The round shape target is placed in 1050 DEG C of 10 hours of annealing in tube furnace, obtains Mn oxide bulk target by 2-7
Material.
Further, the Mn oxide block target material deposition is being insulated with pulsed laser deposition in the step 3
On substrate specifically includes the following steps:
The Mn oxide bulk target and insulating substrate are respectively placed on corresponding position by 3-1, close vacuum
Room successively opens mechanical pump and molecular pump vacuumizes vacuum chamber；
3-2, when the vacuum degree in vacuum chamber reaches 10-4When Pa, molecular pump is closed, opens oxygen valve, adjusts vacuum chamber
Oxygen pressure is 50Pa；
3-3, setting vacuum chamber liner bottom temperature are 700 DEG C, and the insulating substrate is covered with baffle；
3-4, the energy that pulse laser is arranged is 280mJ, and frequency is 3Hz and is beaten in advance:
3-5 removes the baffle, starts to deposit, and keeps the temperature 20min in situ after deposition 90min and is cooled to room temperature, manganese oxygen is made
Compound film.
The manganese-salt phosphating is placed in Muffle furnace by 3-6, and 800 DEG C of annealing 120min, naturally cool to room in air
Temperature obtains calcium titanium ore manganose oxide (La2/3(Ca0.6Ba0.4)1/3MnO3) film.
Further, the sedimentation time that manganese-salt phosphating is made is adjusted according to the thickness of aimed thin film, adjustment
Rate is 500nm/h, and sedimentation time is longer, and the thickness of gained film is thicker.
Further, the insulating substrate material includes simple glass, quartz glass and corundum.
The present invention discloses a kind of temperature magnetic field film-sensing material, prepares Mn oxide material using sol-gal process first
Then by Mn oxide material precursor powder and block target is made in presoma, finally should with pulsed laser deposition
Block target material deposition calcium titanium ore manganose oxide film obtained on the substrate of insulation.
As shown in one of figures 2-4, the invention adopts the above technical scheme, by replacing manganese with calcium ion and barium ions part
Lanthanum ion in oxide, and the ratio by adjusting each metal cation in Mn oxide material, to the Mn oxide material
Magnetoresistance characteristics, Curie temperature be modulated, make the Curie temperature of the Mn oxide material near room temperature and have compared with
Big magnetoresistive ratio；Because preparing Mn oxide presoma using sol-gal process, so that the Mn oxide material mixes
Relatively uniform, particle size is Nano grade and relatively uniform, and this method has the spies such as synthesis process mild condition, easy to control
Point；Manganese-salt phosphating is finally deposited with pulsed laser deposition, the film that this method obtains is with high-quality, uniformity is high
The features such as stablizing with material component, in addition, membrane structure has also widened paramagnetic state-ferrimagnetic state transformation temperature of Mn oxide material
Area.Method of the invention not only may insure the homogeneity of film thickness, moreover it is possible to improve thin-film material quality.
Claims (8)
1. a kind of preparation method of temperature magnetic field film-sensing material, is used to prepare and can be used for temperature and magnetic field film-sensing material
Calcium titanium ore manganose oxide film, it is characterised in that: preparation method the following steps are included:
Step 1: Mn oxide material presoma is prepared using sol-gal process,
Step 2: by Mn oxide material precursor powder and block target is made,
Step 3: it is thin that the block target material deposition being obtained into calcium titanium ore manganose oxide on the substrate of insulation with pulsed laser deposition
Film.
2. a kind of preparation method of temperature magnetic field film-sensing material according to claim 1, it is characterised in that: use colloidal sol
Gel method material used when preparing Mn oxide material presoma includes lanthanum source material, calcium source material, barium source material, manganese source material
Material, the lanthanum source material, calcium source material, barium source material, manganese source material are respectively lanthanum nitrate, calcium acetate, barium nitrate, manganese acetate.
3. a kind of preparation method of temperature magnetic field film-sensing material according to claim 2, it is characterised in that: the step
With sol-gal process prepare Mn oxide material presoma in rapid 1 specifically includes the following steps:
Lanthanum nitrate material, acetic acid calcium material, barium nitrate material, acetic acid manganese material are pressed La2/3 (Ca1-xBax) 1/3MnO3 by 1-1
The ratio between amount of substance of middle cation carries out precise, wherein 0.2≤x≤0.8, in the case where 80 DEG C of water-baths and stirring,
It is completely dissolved in suitable deionized water, obtains transparent no precipitation solution A；
1-2, uses citric acid as dispersing agent, weighs lemon by the ratio between amount of substance of citric acid and metal cation for 1.2: 1
Acid is dissolved in suitable ethylene glycol and is stirred continuously, and into solution, dropwise addition dilute nitric acid solution is transparent to solution, obtains solution B；
Solution B is slowly added into solution A in the case where water-bath, constantly stirs by 1-3, until obtaining xerogel；
Xerogel is placed in 120 DEG C of air dry ovens and is dried by 1-4, until obtaining loose porous sepia xerogel.
4. a kind of preparation method of temperature magnetic field film-sensing material according to claim 3, it is characterised in that: the step
The dosage of ethylene glycol described in rapid 1-2 determines its dosage according to the requirement of solution B viscosity.
5. a kind of preparation method of temperature magnetic field film-sensing material according to claim 3, it is characterised in that: the step
By the Mn oxide material precursor powder and bulk target is made in rapid 2, specifically includes the following steps:
The sepia xerogel is ground into no granular sensation powder by 2-1；
2-2 holds the powder with porcelain crucible, is placed in 6 hours in 400 DEG C of Muffle furnaces, and removal organic matter obtains powder C；
Suitable polyvinyl alcohol is placed in deionized water by 2-3, and water-bath to debita spissitudo obtains polyvinyl alcohol colloid；
Suitable polyvinylidene alcohol colloid is added drop-wise in the powder C by 2-4, is ground and uniformly obtains powder D；
The powder D is pressed into diameter 28mm round shape target with metal die by 2-5, and pressure size used is 25MPa；
The round shape target is placed in 3 hours in 500 DEG C of Muffle furnaces by 2-6, removes polyvinylidene alcohol colloid；
The round shape target is placed in 1050 DEG C of 10 hours of annealing in tube furnace, obtains Mn oxide bulk target by 2-7.
6. a kind of preparation method of temperature magnetic field film-sensing material according to claim 5, it is characterised in that: the step
In rapid 3 with pulsed laser deposition by the Mn oxide block target material deposition on an insulating substrate specifically includes the following steps:
The Mn oxide bulk target and insulating substrate are respectively placed on corresponding position by 3-1, close vacuum chamber, first
It opens mechanical pump afterwards and molecular pump vacuumizes vacuum chamber；
3-2, when the vacuum degree in vacuum chamber reaches 10-4When Pa, molecular pump is closed, opens oxygen valve, adjusts vacuum chamber oxygen
Pressure is 50Pa；
3-3, setting vacuum chamber liner bottom temperature are 700 DEG C, and the insulating substrate is covered with baffle；
3-4, the energy that pulse laser is arranged is 280mJ, and frequency is 3Hz and is beaten in advance:
3-5 removes the baffle, starts to deposit, and keeps the temperature 20min in situ after deposition 90min and is cooled to room temperature, Mn oxide is made
Film；
The manganese-salt phosphating is placed in Muffle furnace by 3-6,800 DEG C of annealing 120min in air, cooled to room temperature,
Obtain calcium titanium ore manganose oxide film.
7. a kind of preparation method of temperature magnetic field film-sensing material according to claim 6, it is characterised in that: manganese is made
The sedimentation time of sull is adjusted according to the thickness of aimed thin film, and the rate of adjustment is 500nm/h.
8. a kind of preparation method of temperature magnetic field film-sensing material according to claim 1 or 6, it is characterised in that: institute
The insulating substrate material stated includes simple glass, quartz glass and corundum.
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