CN107177834B - A method of regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field - Google Patents
A method of regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field Download PDFInfo
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- CN107177834B CN107177834B CN201710405411.2A CN201710405411A CN107177834B CN 107177834 B CN107177834 B CN 107177834B CN 201710405411 A CN201710405411 A CN 201710405411A CN 107177834 B CN107177834 B CN 107177834B
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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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/406—Oxides of iron group metals
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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Abstract
The invention discloses a kind of methods for regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field, it is therefore intended that, the Fe of preparation3O4The magnetic anisotropy of film is obvious, has higher Wan strong, and Fe3O4Film surface appearance is uniform, rough overshoot is small, and used technical solution is, comprising: 1) clean substrate is placed on the magnetic pole of permanent magnet, and substrate and permanent magnet are placed in vacuum reaction cavity heat it is spare, and heating temperature be less than permanent magnet Curie temperature；2) using ferrocene steam as source of iron, using oxygen as oxygen source, ferrocene steam and oxygen ALT pulse are sent into vacuum reaction cavity, atomic layer deposition cycles several times are carried out to substrate, until uniform deposition has conformal Fe on the surface of substrate3O4Film；3) it is filled with inert gas into vacuum reaction cavity, is taken out after substrate cooled to room temperature.
Description
Technical field
The invention belongs to atomic layer deposition methods to prepare thin film technique field, and in particular to a kind of to be regulated and controled using situ Magnetic Field
The method of atomic layer deposition thin film magnetism.
Background technique
In the latest 20 years, in order to apply magneto-electronics in semiconductor industry highly developed till now, Hen Duoren
Gradually concentrate on on semiconductor magnetoeletronic.The major advantage of this new branch of science is can be with traditional metal
Oxide semiconductor technology is compatible, thus it is traditional by charge based on semiconductor on addition spin freedom degree, make now
The function of electronics device be expanded, performance is improved, and the speed and integration density and reduction of data processing are improved
Power consumption etc. makes current very mature microelectric technique be expanded.Now, semiconductor magnetoeletronic is considered as magnetoelectricity
Son learns the main flow direction of extensive practical most realistic approach and Future Development.Spintronics and microelectronics push super
Thin and three-dimensional conformal high quality magnetic oxide film demand, so that ultra-thin and three-dimensional conformal magnetic oxide controllable growth
Magnetic controllable growth as key technique problem urgently to be solved, especially magnetic oxide is that the technology of bottleneck is difficult
Topic, such as high density data storage, sensor and spintronics.However, so far, preparing magnetic oxide film
Method is mainly include the following types: (1) utilizes pulsed laser deposition (PLD), and the method technics comparing is simple, the crystalline of film
It measures, but large-area uniformity and film thickness accurately control poor, and cannot achieve three-dimensional uniformly conformal covering.(2) magnetic control
Sputtering is most common magnetic oxide film growth method, and the method has preferable planar uniformity and quality of forming film, so
And cannot achieve the controllable precise of Subnano-class in terms of film thickness accurately control, especially with complex three-dimensional nano junction
It cannot achieve three-dimensional uniformly conformal covering on the substrate of structure.(3) can be prepared using chemical vapor deposition (CVD) method is had centainly
The Fe of three-dimensional uniformity3O4Film, but since Fe has Fe2O3And Fe3O4Two kinds of stable oxides, so pure to prepare
The Fe of phase3O4Film is relatively difficult.Furthermore CVD accurately controlled in film thickness and in the three-dimensional structure with larger depth-to-width ratio still
It cannot achieve uniform conformal covering.In conclusion existing preparation Fe3O4The conventional method of film has film thickness to be unable to accurately control
With the bottleneck problem that cannot achieve three-dimensional uniformly conformal covering.However the rapid development of current microelectric technique, 22nm and with
The microelectronic circuit of lower line width has used three-dimensional structure as Fin-FET or Tri-Get.This indicate microelectronic circuit from
Flatness structural transition has been trend of the times to three-dimensional structure, how to solve after being transitioned into three-dimensional structure from plane tradition PVD and
The technical bottleneck problem (three-dimensional conformal uniformity and magnetic controllability etc.) that CVD technology faces is key problem.
Atomic layer deposition (Atomic Layer Deposition, ALD) film deposition techniques are a kind of from limitation (self-
Limiting surface growth pattern) has extraordinary three-dimensional uniformity.In fact in microelectronic field ALD conduct
A kind of high-quality dielectric layer and CMOS transistor high-k preparing dynamic random access memory (DRAMs) trench capacitor
The key technology of layer.ALD is a kind of film deposition techniques that can be realized self limitation that monoatomic layer is successively grown, feature
For can in the three-dimensional structure of any shape all deposition thickness controllable precise and 100% uniform conformal film, this satisfies systems
The urgent need of standby three dimensional microelectronic device.However Fe is prepared with ALD3O4Film usually has weaker magnetic anisotropic, this is
Because of the Fe of ALD preparation3O4Film crystal unity is low, and crystal grain is smaller, so the Fe of ALD preparation3O4It is usually isotropic
Superparamagnetism, so we pass through in Fe in the invention3O4Add in-place magnetic field induces Fe in the growth course of film3O4Film
In magnetic moment orientation, and then induce magnetic anisotropic, had no so far using situ Magnetic Field and ALD is induced to prepare Fe3O4It is thin
The relevant report of magnetic anisotropy in film.
Summary of the invention
In order to solve the problems in the prior art, the present invention proposes that a kind of using situ Magnetic Field to regulate and control atomic layer deposition thin
The method of film magnetism, method is easy to operate, raw material is cheap and safe and non-toxic, it is pollution-free, conducive to volume production and with existing IC technique
It is compatible, the Fe of method preparation3O4The magnetic anisotropy of film is obvious, has higher Wan strong, and Fe3O4Film surface appearance
Uniformly, rough overshoot is small.
In order to achieve the goal above, the technical scheme adopted by the invention is as follows: the following steps are included:
1) clean substrate is placed on the magnetic pole of permanent magnet, and substrate and permanent magnet is placed in vacuum reaction cavity
Heat it is spare, and heating temperature be less than permanent magnet Curie temperature；
2) using ferrocene steam as source of iron, using oxygen as oxygen source, ferrocene steam and oxygen ALT pulse are sent into
In vacuum reaction cavity, atomic layer deposition cycles several times are carried out to substrate, until on the surface of substrate uniform deposition have it is conformal
Fe3O4Film；
3) it is filled with inert gas into vacuum reaction cavity, is taken out after substrate cooled to room temperature.
The clean processing of substrate includes: successively to clean substrate 10 with acetone and dehydrated alcohol respectively first in the step 1)
~15 minutes；Then it is cleaned by ultrasonic repeatedly with deionized water 3~5 times, each 5~10 minutes every time；By base after the completion of finally cleaning
Piece takes out dry be dried with nitrogen.
Substrate and permanent magnet are heated to 350~450 DEG C under an inert atmosphere in the step 1).
The substrate is Au/Si substrate or Pt/Si substrate, and the Curie temperature of the permanent magnet is greater than 450 DEG C.
The permanent magnet be diameter be 10mm-50mm, the cylindrical SnCo magnet with a thickness of 5mm-10mm.
Each atomic layer deposition cycles include: progress 1~4s source of oxygen pulse first in the step 2)；Then nitrogen is used
Clean 6-16s；Secondly the source pulse of 0.1~0.4s ferrocene is carried out；Finally 6~16s is cleaned with nitrogen.
Ferrocene steam is to add ferrocene in the Solid Source heating device of atomic layer deposition apparatus in the step 2)
Heat is to obtaining after 140~160 DEG C.
The ferrocene steam and oxygen use response speed to carry out ALT pulse for the ALD pulse valve of Millisecond and are sent into vacuum
In reaction cavity.
Compared with prior art, the present invention selects the permanent magnet of high-curie temperature to provide situ Magnetic Field to induce ALD former
Position preparation Fe3O4The magnetic anisotropy of film, the precursor source used are cheap ferrocene and oxygen as iron and oxygen
Precursor source makes ferrocene react with oxygen, in Au/Si or Pt/Si substrate surface by atomic layer deposition (ALD) equipment
The Fe of depositing homogeneous3O4Film, film thickness and the ingredient all uniform, controllables deposited, surface are smooth.The method of the present invention not only may be used
To prepare three-dimensional uniform conformal Fe3O4Film can also induce apparent magnetic anisotropy and ferrous iron using situ Magnetic Field
It is magnetic.The method of the present invention is easy to operate, and advantages of nontoxic raw materials is pollution-free, it can be achieved that large area and batch production.Through the method for the present invention system
The Fe obtained3O4Film is tested and is analyzed by electronic paramagnetic resonance spectrometer (ESR), is determined and is had the property that 1 plus original
The Fe of position magnetic field growth3O4Fe of the film than not adding situ Magnetic Field3O4Film has in stronger face with magnetic outside face respectively to different
Property；2, add the Fe of situ Magnetic Field growth3O4Fe of the film than not adding situ Magnetic Field3O4Film has higher Wan strong；3,
Fe3O4Film surface appearance is uniform, and rough overshoot is small；4, add the Fe of situ Magnetic Field growth3O4Film is with and without adding situ Magnetic Field
The Fe of growth3O4Surface topography having the same.
Further, each atomic layer deposition cycles include following four step: progress 1~4s source of oxygen pulse first；Then
6-16s is cleaned with nitrogen；Secondly the source pulse of 0.1~0.4s ferrocene is carried out；6~16s finally is cleaned with nitrogen, will not reacted
Ferrocene drain, repeat above procedure for several times until the film thickness grown reaches the requirement of oneself, the thickness of film
Controllable precise can be simply implemented by setting ALD cycle number.
Detailed description of the invention
Fig. 1 grows Fe under the conditions of not adding situ Magnetic Field using ALD3O4The FMR curve graph of/Au/Si sample；
Fig. 2 grows Fe under the conditions of added with situ Magnetic Field using ALD3O4The FMR curve graph of/Au/Si sample；
Fig. 3 grows Fe under the conditions of not adding situ Magnetic Field using ALD3O4The FMR curve graph of/Pt/Si sample；
Fig. 4 grows Fe under the conditions of added with situ Magnetic Field using ALD3O4The FMR curve graph of/Pt/Si sample.
Specific embodiment
Below with reference to specific embodiment and Figure of description the present invention will be further explained explanation.
1) present invention is the following steps are included: use acetone and dehydrated alcohol successively respectively first for Au/Si Pt/Si substrate
Cleaning 10~15 minutes；Then it is cleaned by ultrasonic repeatedly with deionized water 3~5 times, each 5~10 minutes every time；It will after the completion of cleaning
It is spare that Au/Si Pt/Si substrate takes out being dried with nitrogen for drying.
2) substrate of clean plane or three-dimensional structure is placed on to the magnetic of cylindrical permanent magnet of the Curie temperature greater than 450 DEG C
On pole and it is sent into ALD vacuum reaction cavity, then in N2Be heated under atmosphere 350~450 DEG C it is spare；
4) using ferrocene as source of iron, ferrocene is heated to 140 in the Solid Source heating device of atomic layer deposition system
Ferrocene steam is obtained after~160 DEG C, and using oxygen as oxygen source, ferrocene steam and oxygen are passed through atomic layer deposition apparatus
Then carrier gas system is sent into vacuum reaction cavity by carrier gas system, is controlled by the ALD pulse valve of Millisecond response speed
Ferrocene steam and oxygen enter the amount of vacuum reaction cavity, and atomic layer deposition cycles, each atom are opened in nitrogen atmosphere
Layer deposition cycle are as follows: first carry out the pulse of 1~4s source of oxygen, and clean 6~16s with nitrogen；Then 0.1~0.4s ferrocene is carried out
Source pulse, finally cleans 6~16s with nitrogen, until heavy in Au/Si the Pt/Si substrate surface of plane or three-dimensional structure
Fe uniformly conformal in product3O4Film；
4)Fe3O4After the completion of film deposition, a certain amount of N is filled with toward vacuum reaction cavity the inside2And allow sample natural cooling
Sample is taken out from cavity after to room temperature；
Embodiment 1
The present invention the following steps are included:
A, Au/Si substrate prepares: Au/Si substrate needed for testing takes turns doing following cleaning: respectively with acetone and anhydrous second
Alcohol successively cleans 10~15 minutes；Then it is cleaned by ultrasonic repeatedly with deionized water 3~5 times, each 5~10 minutes every time；It has cleaned
The use of vacuum reaction cavity is immediately fed into after Au/Si Pt/Si substrate is taken out dry be dried with nitrogen after；
B, ferrocene source is packed into the Solid Source heating source bottle of ALD equipment, pre- pumping processing is carried out to source bottle, to take dress away
The air introduced in source capsule line in source procedure, setting source bottle heater strip temperature heats source, until the steaming of every subpulse
Until vapour pressure is stablized, to guarantee that ferrocene there are enough vapour pressure pulses to enter carrier gas system, reaction chamber is finally brought by carrier gas
Body；
C, start to heat substrate after ready Au/Si substrate being sent into reaction cavity by vacuum mechanical-arm,
In order to guarantee that gas is pure N inside reaction cavity2Gas, need to be by the N of every source capsule line2Carrier gas flux is set as 2000sccm,
And simultaneously close off vacuum pump extraction valve V6, carrier gas can be automatically closed in system after the pressure of reaction cavity reaches an atmospheric pressure
And open vacuum pump extraction valve V6Pumping, the intracorporal gas of reaction chamber is taken away, repeats above step 3 times, can both guarantee anti-
Answering inside cavity is purer N2, furthermore maintain the nitrogen flow of every pipe source line 50sccm always during heating, with
Guarantee that reaction cavity pressure maintains 800Pa or so, furnace silk temperature is set as 500~600 DEG C in heating process, and substrate temperature is set as
350~450 DEG C, after base reservoir temperature is stablized, the ALD deposition program set is executed, specific procedure is as follows:
First pulse is pulse of oxygen, and the pulse of oxygen time is 1~4 second；The nitrogen cleaning burst length is 6~16 seconds；Two
The luxuriant iron burst length is 0.1~0.4 second；Nitrogen cleans 6~16 seconds, and the carrier gas flux of ferrocene and oxygen is set to
150sccm and 200sccm, the N of other source capsule lines2Carrier gas flux is set as 80sccm, and growth thickness is that execution 400 is above-mentioned
ALD cycle；
D, by Fe made from the original position ALD3O4Film is in N2Room temperature is naturally cooled under atmosphere and is taken out.
Fe is grown under the conditions of no situ Magnetic Field using ALD referring to Fig. 13O4The electron paramagnetic resonance wave of/Au/Si sample
Spectrometer (ESR) test result shows the Fe prepared on Au/Si substrate under the conditions of not adding situ Magnetic Field3O4Film has very
Strong magnetic anisotropy is magnetic beach axis (resonant fields are up to 5580Oe) outside face, is magnetic easy axis (resonant fields 1753Oe), face in face
Interior and face external resonance field differs 3827Oe.Comparison diagram 2 grows Fe under the conditions of added with situ Magnetic Field using ALD3O4/ Au/Si sample
Electronic paramagnetic resonance spectrometer (ESR) test result, it can be clearly seen that after adding situ Magnetic Field, Fe3O4The magnetic of film is respectively to different
Property weakens significantly.It is remained as outside face magnetic beach axis (but face external resonance field is reduced to 3297 Oe), remains as magnetic easy axis (face in face
It is 2710 Oe that internal resonance field, which increases), the difference in face with face external resonance field is reduced to 587Oe.Situ Magnetic Field allows Fe3O4The face of film
Magnetic anisotropy reduces 3240 Oe (3827-587=3240 Oe) outside interior and face, this is sufficiently demonstrated in ALD growing film
In the process, add in-place magnetic field can effectively change the magnetic anisotropy of film.
Embodiment 2
The present invention the following steps are included:
A, Pt/Si substrate prepares: Pt/Si substrate needed for testing takes turns doing following cleaning: respectively with acetone and anhydrous second
Alcohol successively cleans 10~15 minutes；Then it is cleaned by ultrasonic repeatedly with deionized water 3~5 times, each 5~10 minutes every time；It has cleaned
The use of vacuum reaction cavity is immediately fed into after Pt/Si substrate is taken out dry be dried with nitrogen after；
B, ferrocene source is packed into the Solid Source heating source bottle of ALD equipment, pre- pumping processing is carried out to source bottle, to take dress away
The air introduced in source capsule line in source procedure, setting source bottle heating temperature heats source, until the steam of every subpulse
Until pressure is stablized, to guarantee that ferrocene there are enough vapour pressure pulses to enter carrier gas system, reaction cavity is finally brought by carrier gas；
C, start to heat substrate after ready Pt/Si substrate being sent into reaction cavity by vacuum mechanical-arm,
In order to guarantee that gas is pure N inside reaction cavity2Gas, need to be by the N of every source capsule line2Carrier gas flux is set as 2000sccm,
And simultaneously close off vacuum pump extraction valve V6, carrier gas can be automatically closed in system after the pressure of reaction cavity reaches an atmospheric pressure
And open vacuum pump extraction valve V6Pumping, the intracorporal gas of reaction chamber is taken away, repeats above step 3 times, can both guarantee anti-
Answering inside cavity is purer N2, furthermore maintain the nitrogen flow of every pipe source line 50sccm always during heating, with
Guarantee that reaction cavity pressure maintains 800Pa or so, furnace silk temperature is set as 500~600 DEG C in heating process, and substrate temperature is set as
350~450 DEG C, after base reservoir temperature is stablized, the ALD deposition program set is executed, specific procedure is as follows:
First pulse is pulse of oxygen, and the pulse of oxygen time is 1~4 second；The nitrogen cleaning burst length is 6~16 seconds；Two
The luxuriant iron burst length is 0.1~0.4 second；Nitrogen cleans 6~16 seconds, and the carrier gas flux of ferrocene and oxygen is set to
150sccm and 200sccm, the N of other source capsule lines2Carrier gas flux is set as 80sccm, and growth thickness is that execution 400 is above-mentioned
ALD cycle；
D, by Fe made from the original position ALD3O4Film is in N2Room temperature is naturally cooled under atmosphere and is taken out.
Fe is grown under the conditions of no situ Magnetic Field using ALD referring to Fig. 33O4The electron paramagnetic resonance wave of/Pt/Si sample
Spectrometer (ESR) test result shows the Fe prepared on Pt/Si substrate under the conditions of not adding situ Magnetic Field3O4Film has very
Strong magnetic anisotropy is magnetic beach axis (resonant fields are up to 5915Oe) outside face, is magnetic easy axis (resonant fields 1890Oe), face in face
Interior and face external resonance field differs 4025Oe.Comparison diagram 4 grows Fe under the conditions of added with situ Magnetic Field using ALD3O4/ Pt/Si sample
Electronic paramagnetic resonance spectrometer (ESR) test result, it can be clearly seen that after adding situ Magnetic Field, Fe3O4The magnetic of film is respectively to different
Property weakens significantly.Add outside behind situ Magnetic Field and remain as magnetic beach axis (but face external resonance field is reduced to 3350Oe), in face still
For magnetic easy axis (face internal resonance field increase be 2603Oe), the difference in face with face external resonance field is reduced to 747Oe.Situ Magnetic Field allows
The Fe that Pt/Si substrate is grown above3O4Magnetic anisotropy reduces 3278Oe (4025-747=outside in the face of film and face
3278Oe), this again demonstrate during ALD growing film, add in-place magnetic field can effectively change the magnetic of film respectively to
It is anisotropic.
In conclusion the method for the present invention proposes one kind adds situ Magnetic Field during ALD growth in situ thin magnetic film
By comparison plus situ Magnetic Field and institute under the conditions of situ Magnetic Field is not added in method to regulate and control grown thin magnetic film magnetic anisotropy
The magnetic anisotropy in thin magnetic film face and outside face is grown, discovery grows magnetism in various substrates (Au/Si and Pt/Si) above
The magnetic anisotropy of film is all largely by the regulation of situ Magnetic Field.
The method have the advantages that can by ALD grow thin magnetic film during by add in-place magnetic field come
Regulate and control ALD just in the magnetism of thin magnetic film.The thickness of thin magnetic film can also be accurately controlled by control ALD cycle number
Degree, preparation process is simple and easy, compatible with existing semiconductor preparing process.
Claims (6)
1. a kind of method for regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field, which comprises the following steps:
1) clean substrate is placed on the magnetic pole of permanent magnet, and substrate and permanent magnet is placed in vacuum reaction cavity and heated
It is spare, and heating temperature is less than the Curie temperature of permanent magnet；
The clean processing of substrate includes: successively to clean substrate 10~15 with acetone and dehydrated alcohol respectively first in the step 1)
Minute；Then it is cleaned by ultrasonic repeatedly with deionized water 3~5 times, each 5~10 minutes every time；Substrate is taken after the completion of finally cleaning
It is dried with nitrogen out with dry；
2) using ferrocene steam as source of iron, using oxygen as oxygen source, ferrocene steam and oxygen ALT pulse are sent into vacuum
In reaction cavity, atomic layer deposition cycles several times are carried out to substrate, until conformal on uniform deposition on the surface of substrate
Fe3O4Film；
Each atomic layer deposition cycles include: progress 1~4s source of oxygen pulse first in the step 2)；Then it is cleaned with nitrogen
6-16s；Secondly the source pulse of 0.1~0.4s ferrocene is carried out；Finally 6~16s is cleaned with nitrogen；
3) it is filled with inert gas into vacuum reaction cavity, is taken out after substrate cooled to room temperature.
2. a kind of method for regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field according to claim 1, special
Sign is that substrate and permanent magnet are heated to 350~450 DEG C under an inert atmosphere in the step 1).
3. a kind of method for regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field according to claim 2, special
Sign is that the substrate is Au/Si substrate or Pt/Si substrate, and the Curie temperature of the permanent magnet is greater than 450 DEG C.
4. a kind of method for regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field according to claim 3, special
Sign is, the permanent magnet be diameter be 10mm-50mm, the cylindrical SnCo magnet with a thickness of 5mm-10mm.
5. a kind of method for regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field according to claim 1, special
Sign is that ferrocene steam is to heat ferrocene in the Solid Source heating device of atomic layer deposition apparatus in the step 2)
It is obtained after to 140~160 DEG C.
6. a kind of method for regulating and controlling atomic layer deposition thin film magnetism using situ Magnetic Field according to claim 5, special
Sign is, the ferrocene steam and oxygen use response speed to control two provenance alternating pulses for the ALD pulse valve of Millisecond
Punching is sent into vacuum reaction cavity.
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