CN106011748B - A kind of preparation method of iron nitride thin film - Google Patents

A kind of preparation method of iron nitride thin film Download PDF

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CN106011748B
CN106011748B CN201610469979.6A CN201610469979A CN106011748B CN 106011748 B CN106011748 B CN 106011748B CN 201610469979 A CN201610469979 A CN 201610469979A CN 106011748 B CN106011748 B CN 106011748B
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iron
thin film
magnetic field
passed
nitride thin
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CN106011748A (en
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李静
彭晓领
杨艳婷
徐靖才
王攀峰
金红晓
金顶峰
洪波
王新庆
葛洪良
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China Jiliang University
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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
    • C23C14/08—Oxides
    • C23C14/085—Oxides of iron group metals
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/586—Nitriding

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Abstract

The present invention relates to a kind of preparation methods of iron nitride thin film.This method is the method using pulsed laser deposition, by controlling depositing temperature, time and oxygen flow, to prepare sull；Hydrogen is passed through, 4 20h are reduced at 300 ~ 400 DEG C, to obtain iron thin film；Ammonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, 0.1 ~ 2T of magnetic field intensity；Cooling cools to room temperature with the furnace, takes out sample, you can obtains iron nitride thin film.This method can directly obtain high α " Fe16N2The iron nitride thin film of content is conducive to the integrated application of thin-film device, in addition using the method for magnetic-field heat treatment, makes to generate crystalline orientation during thin film silicon nitride, the convenient crystallography easy magnetizing axis for controlling film.

Description

A kind of preparation method of iron nitride thin film
Technical field
The present invention relates to a kind of preparation methods of iron nitride thin film, belong to field of material preparation.
Background technology
Magnetic membrane material refers to ferromagnetism of the thickness below 1 micron（Ferromagnetism and ferrimagnetism）Material.Wherein iron Nitrogen thin magnetic film in magnetic thin film devices field due to excellent magnetic property, improved corrosion performance and abrasion resistance properties, having Huge application prospect.The preparation method of ferromagnetic phase mainly has vacuum vapor deposition method, electrodeposition process, sputtering method etc..
With the variation of nitrogen content, nitrided iron has different structure and performance, mainly including interstitial solid solution（Alpha, gamma, ε）, Compound phase（γ´-Fe4N, ε-Fe3N）With steady phase (α '-martensite and the α "-Fe of being situated between16N2).All nitrided irons are all metastable phase, meeting Resolve into Fe and N2.But the dynamic process that it is decomposed below 400 DEG C is very slow, is limited by dynamic process, nitrided iron It can be mutually stabilized in room temperature.α "-Fe among these16N2Saturation magnetization value for 2.83 T, far above other materials, draw Play people's keen interest.
Inventor uses pulsed laser deposition（PLD) method prepares ferromagnetic phase.By introducing reaction in vacuum cavity Gas, PLD technologies are beneficial to the oxide and nitride film that prepare Various Complex, can also obtain some room temperature nonequilibrium state and consolidate Solution or compound.By controlling the sedimentary conditions such as nitrogen partial pressure, single-phase Fe can be prepared4N and Fe3N.But inventor one Directly α "-Fe are not prepared16N2Phase.
In recent years, using Nano-sized Ferric Oxide Powder, using H2Reduction, NH3Nitridation is prepared by extensive concern.But this method one A shortcoming is H2The iron powder activity obtained after reduction is big, mutually reunites serious, hinders nitridation process.In order to overcome nanometer The reunion of grain, the method for many scientists Nano-sized Ferric Oxide Powder outer cladding aluminium oxide or silica, and achieve one Determine effect.But the problem of new, occurs, and aluminium oxide and silica are non magnetic constituent element, reduce the intensity of magnetization of system.
With reference to more than, inventor prepares sull using PLD methods, then using the side of hydro-reduction, low temperature nitride Method prepares high α "-Fe16N2The iron nitride thin film of phase content, and apply magnetic field in nitridation process, the nitrided iron for making acquisition is thin Film has magnetic anisotropy.
The content of the invention
Sull is obtained by PLD methods the object of the present invention is to provide one kind, then using hydro-reduction, cryogenic nitrogen The method of change prepares high α "-Fe16N2The preparation method of the iron nitride thin film of phase content.
The present invention's concretely comprises the following steps：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 20~600 DEG C；Atmosphere is oxygen, Oxygen flux control is in 10~100sccm；Sedimentation time is controlled in 0.3 ~ 3h；
Second step：Reduction
Sull is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, in 300 ~ 400 DEG C of reduction 4-20h, to obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic 0.1 ~ 2T of field intensity；Cooling cools to room temperature with the furnace, takes out sample, you can obtains iron nitride thin film, phase composition is mainly α"-Fe16N2, and include part α-Fe phases；
The magnetic field is generated by electromagnet or permanent magnet；
The permanent magnet include samarium-cobalt magnet, neodymium iron boron magnetic body, ferrimagnet, iron cobalt magnet, alnico magnet and Ferroplatinum magnet.
It is an advantage of the invention that：
1）Directly obtain high α "-Fe16N2The iron nitride thin film of content is conducive to the integrated application of thin-film device；
2）Using the method for magnetic-field heat treatment, make to generate crystalline orientation during thin film silicon nitride, the convenient crystalline substance for controlling film Body easy magnetizing axis.
Specific embodiment
With reference to embodiment, the present invention will be described in detail, so as to more fully understand the purpose of the present invention, feature and Advantage.Although the present invention is described with reference to the specific embodiment, it is not intended that the invention be limited to described Specific embodiment.On the contrary, the embodiment that can be included in the protection domain defined in the claims in the present invention is carried out Replacement, improvement and equivalent embodiment, belong to protection scope of the present invention.For the technological parameter not marked especially, It can routinely technology carry out.
The present invention's concretely comprises the following steps：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 20~600 DEG C；Atmosphere is oxygen, Oxygen flux control is in 10~100sccm；Sedimentation time is controlled in 0.3 ~ 3h；
Second step：Reduction
Iron nitride thin film is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, in 300 ~ 400 DEG C of reduction 4-20h, to obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic 0.1 ~ 2T of field intensity；Cooling cools to room temperature with the furnace, takes out sample, you can obtains iron nitride thin film, phase composition is mainly α"-Fe16N2, and include part α-Fe phases；
The magnetic field is generated by electromagnet or permanent magnet；
The permanent magnet include samarium-cobalt magnet, neodymium iron boron magnetic body, ferrimagnet, iron cobalt magnet, alnico magnet and Ferroplatinum magnet.
The iron nitride thin film of orientation can be prepared by the present invention.
Embodiment 1：
Step is：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 20 DEG C；Atmosphere is oxygen, oxygen Flow control is in 100sccm；Sedimentation time is controlled in 3h；
Second step：Reduction
Iron nitride thin film is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, in 300 DEG C of reductase 12 0h, To obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 30h is nitrogenized at 120 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic field intensity 2T, magnetic field are generated by electromagnet；Cooling cools to room temperature with the furnace, takes out sample.
XRD characterization is carried out to the sample prepared by embodiment 1, detects α "-Fe16N2With α-Fe phases, and two-phase have There is orientation.
Embodiment 2：
Step is：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 80 DEG C；Atmosphere is oxygen, oxygen Flow control is in 80sccm；Sedimentation time is controlled in 2h；
Second step：Reduction
Iron nitride thin film is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, 16h is reduced at 320 DEG C, To obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 16h is nitrogenized at 140 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic field intensity 1T, magnetic field are generated by electromagnet；Cooling cools to room temperature with the furnace, takes out sample.
XRD characterization is carried out to the sample prepared by embodiment 2, detects α "-Fe16N2With α-Fe phases, and two-phase have There is orientation.
Embodiment 3：
Step is：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 160 DEG C；Atmosphere is oxygen, oxygen Flow control is in 60sccm；Sedimentation time is controlled in 1.5h；
Second step：Reduction
Iron nitride thin film is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, 12h is reduced at 340 DEG C, To obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 8h is nitrogenized at 160 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic field intensity 0.8T, magnetic field are generated by electromagnet；Cooling cools to room temperature with the furnace, takes out sample.
XRD characterization is carried out to the sample prepared by embodiment 3, detects α "-Fe16N2With α-Fe phases, and two-phase have There is orientation.
Embodiment 4：
Step is：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 300 DEG C；Atmosphere is oxygen, oxygen Flow control is in 40sccm；Sedimentation time is controlled in 1h；
Second step：Reduction
Iron nitride thin film is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, 8h is reduced at 360 DEG C, with Obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 4h is nitrogenized at 170 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic field intensity 0.4T, magnetic field are generated by Nd-Fe-B permanent magnet；Cooling cools to room temperature with the furnace, takes out sample.
XRD characterization is carried out to the sample prepared by embodiment 4, detects α "-Fe16N2With α-Fe phases, and two-phase have There is orientation.
Embodiment 5：
Step is：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 450 DEG C；Atmosphere is oxygen, oxygen Flow control is in 20sccm；Sedimentation time is controlled in 0.5h；
Second step：Reduction
Iron nitride thin film is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, 6h is reduced at 380 DEG C, with Obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 2h is nitrogenized at 180 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic field intensity 0.2T, magnetic field are generated by iron cobalt permanent magnet；Cooling cools to room temperature with the furnace, takes out sample.
XRD characterization is carried out to the sample prepared by embodiment 5, detects α "-Fe16N2With α-Fe phases, and with taking Tropism.
Embodiment 6：
Step is：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 600 DEG C；Atmosphere is oxygen, oxygen Flow control is in 10sccm；Sedimentation time is controlled in 0.3h；
Second step：Reduction
Iron nitride thin film is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, 4h is reduced at 400 DEG C, with Obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 1h is nitrogenized at 200 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic field intensity 0.1T, magnetic field are provided by samarium cobalt permanent magnet body；Cooling cools to room temperature with the furnace, takes out sample.
XRD characterization is carried out to the sample prepared by embodiment 6, detects α "-Fe16N2With α-Fe phases, and two-phase have There is orientation.

Claims (1)

1. a kind of preparation method of iron nitride thin film, it is characterised in that this method comprises the following steps：
The first step：It is prepared by sull
Select pure iron target and clean glass substrate；In preparation process, underlayer temperature is 20~600 DEG C；Atmosphere is oxygen, oxygen Flow control is in 10~100sccm；Sedimentation time is controlled in 0.3 ~ 3h；
Second step：Reduction
Sull is taken out, is placed in heat-treatment furnace, hydrogen is passed through with constant rate, 4- is reduced at 300 ~ 400 DEG C 20h, to obtain iron thin film；
3rd step：Nitridation
Ammonia is passed through, 1 ~ 30h is nitrogenized at 120 ~ 200 DEG C；Apply magnetic field in nitridation process, induce the orientation of nitrided iron, magnetic field is strong Spend 0.1 ~ 2T；Cooling cools to room temperature with the furnace, takes out sample, you can obtains iron nitride thin film；
The magnetic field is generated by electromagnet or permanent magnet；
The permanent magnet includes samarium-cobalt magnet, neodymium iron boron magnetic body, ferrimagnet, iron cobalt magnet, alnico magnet and iron platinum Alloy magnet.
CN201610469979.6A 2016-06-26 2016-06-26 A kind of preparation method of iron nitride thin film Active CN106011748B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101552043A (en) * 2009-05-12 2009-10-07 南京大学 Ferromagnetic thin-film wave absorbing material with periodic structure
CN101607701A (en) * 2009-07-24 2009-12-23 东北大学 Nanometer, the two promotion law of high-intensity magnetic field prepare the method and the device of iron nitride material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101552043A (en) * 2009-05-12 2009-10-07 南京大学 Ferromagnetic thin-film wave absorbing material with periodic structure
CN101607701A (en) * 2009-07-24 2009-12-23 东北大学 Nanometer, the two promotion law of high-intensity magnetic field prepare the method and the device of iron nitride material

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