CN102360944A - Method for preparing iron-doped titanium nitride ferromagnetic film based on oriented growth - Google Patents
Method for preparing iron-doped titanium nitride ferromagnetic film based on oriented growth Download PDFInfo
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- CN102360944A CN102360944A CN 201110295307 CN201110295307A CN102360944A CN 102360944 A CN102360944 A CN 102360944A CN 201110295307 CN201110295307 CN 201110295307 CN 201110295307 A CN201110295307 A CN 201110295307A CN 102360944 A CN102360944 A CN 102360944A
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Abstract
The invention provides a method for preparing an iron-doped titanium nitride ferromagnetic film based on oriented growth by adopting an ultrahigh vacuum three-target co-deposition magnetron sputtering coating machine. The method comprises the following steps: (1) arranging a pair of titanium (Ti) targets on opposite target heads of the coating machine, and fixing ferrum (Fe) sheets on the surfaces of the Ti targets; (2) arranging a glass substrate on a midperpendicular of a connecting line of the opposite targets; (3) vacuumizing a sputtering chamber; (4) introducing mixed gas of argon (Ar) and nitrogen (N2) into a vacuum chamber; (5) starting a sputtering power supply, and applying current and voltage to the pair of the Ti targets; (6) opening a baffle for sputtering coating; and (7) stopping sputtering after completion of coating, continuously vacuumizing, shutting down a vacuum system, and then filling N2 into the vacuum chamber after the system is cooled so as to finally obtain the target product. The iron-doped titanium nitride ferromagnetic film obtained by the method has room-temperature ferromagnetism and semiconductor properties at the same time, thus achieving potential application value in electronic devices; and the method has the advantages of simple process, high utilization ratio of target materials and low production cost, and is easy to implement, thus being suitable for large-scale popularization and application.
Description
Technical field
The present invention relates to the preparation method of the iron doped titanium nitride ferromagnetic thin film of semi-conducting material technology of preparing, particularly a kind of oriented growth.
Background technology
Nobel Prize in physics in 2007 has been authorized initiator Albert Fert and two professors of Peter Gr ü nberg of spintronics.Now, the electric current that how to obtain high spin-polarization remains one of the hot issue in spintronics field.The way that obtains the high-spin injection mainly contains the electrode material and preparation diluted magnetic semiconductor material of selecting high spinning polarizability.
Dilute magnetic semiconductor is meant the one type of novel semiconductor material that forms by after the nonmagnetic elements in magnetic transiting group metal elements or the thulium part alternative semiconductors.At present, the dilute magnetic semiconductor of broad research mainly comprises: II – VI family dilute magnetic semiconductor, like (Cd, Mn) Te etc.; III – V family dilute magnetic semiconductor is like (Ga, Mn) As and (Ga, Mn) N etc.; The metal oxide dilute magnetic semiconductor is like Mn:ZnO and Co:TiO
2Deng.So because the resistivity of oxide has difficulties in practical application than higher.
The titanium nitride crystal belongs to cubic system, face-centred cubic structure, its lattice constant
a=0.42173 nm.Titanium nitride membrane has excellent machinery, heat, electricity and antiseptic property, because hardness is high, coefficient of friction is low, is widely used as the wear-resisting modified layer of mould, cutter etc.; Because resistance to wear, antiseptic property is good, fusing point is high, high-temperature stability is good, is widely used in Aero-Space parts such as aircraft and rocket; Since conduction, good heat conductivity, the barrier layer of doing commonly used in microelectronic.If magnetic element is doped in the titanium nitride system, if can obtain promptly have the material that magnetic has conduction, will promote the new purposes of titanium nitride material.
Up to now; The people is not through mixing Fe the dilute magnetic semiconductor material that obtains to have room-temperature ferromagnetic in the TiN film, and patent of the present invention adopts the method for magnetron sputtering codeposition to prepare the TiN film of the different orientation of the different Fe content with room-temperature ferromagnetic and characteristic of semiconductor.
Summary of the invention
The objective of the invention is to above-mentioned technical Analysis; A kind of preparation method of iron doped titanium nitride ferromagnetic thin film of oriented growth is provided; Promptly adopt magnetron sputtering method to prepare the iron doped titanium nitride ferromagnetic thin film of doping content regulation and control oriented growth, this thin-film material possesses room-temperature ferromagnetic and two kinds of attributes of semiconductor simultaneously.
Technical scheme of the present invention:
A kind of preparation method of iron doped titanium nitride ferromagnetic thin film of oriented growth adopts the preparation of ultra high vacuum three target codeposition magnetron sputtering coaters, and this step is following:
1) a pair of Ti target is installed on the target head of coating machine subtend, an end is as the N utmost point, and the other end is the S utmost point, and the distance between the fixing Fe sheet on the surface of Ti target, two targets is 100 mm, and the axis of target and the distance between the specimen holder are 100 mm;
2) substrate of glass is carried out sonicated with alcohol after, adopt the mode of hand rubbing that its surface impurity is removed after, put into alcohol and soak, be installed in after drying up on the perpendicular bisector of subtend target line;
3) open subtend target magnetic control sputtering equipment, successively start the one-level mechanical pump and the secondary molecular pump vacuumizes, vacuum degree is 1 * 10 at the bottom of the back of the body of sputtering chamber
– 4Pa;
4) feed Ar and N to vacuum chamber
2Mist, vacuum degree is remained on 1 Pa;
5) open shielding power supply, on a pair of Ti target, apply electric current and voltage, sputter is 20 minutes in advance, waits sputtering current and voltage stable;
6) plate washer of opening on the substrate frame begins sputter coating, and substrate position is fixed in the coating process;
7) the plated film time is 30 minutes, and plated film is closed the plate washer on the substrate frame after finishing, and closes shielding power supply then, stops to feed sputter gas Ar and N
2, open slide valve fully, continue to vacuumize; Close vacuum system then, treat system cools after, charging into purity to vacuum chamber is 99.999% nitrogen; When treating that the air pressure of vacuum type is identical with external atmosphere pressure, open vacuum chamber, open vacuum chamber and take out the target product that makes.
The purity of said Ti target is 99.99%, and the thickness of target is 5 mm, and diameter is 100 mm; The purity of Fe sheet is 99.99%, and the area of Fe sheet is 1-2 cm
2
Said Ar and N
2Mist in, Ar and N
2Purity be 99.999%, Ar and N
2Flow be 15 sccm.
Said sputter DC power supply applies the electric current of 0.3 A and the voltage of 500V on the Ti target.
Advantage of the present invention is: the present invention adopts magnetron sputtering method to prepare the iron doped titanium nitride ferromagnetic thin film of doping content regulation and control oriented growth; This thin-film material possesses room-temperature ferromagnetic and two kinds of attributes of semiconductor simultaneously, on electronics device, has potential using value; This preparation method's technology is simple, easy to implement, and the target utilization rate is high, production cost is low, is suitable for large-scale promotion application.
Description of drawings
Fig. 1 is the scanning electron microscope diagram of the iron doped titanium nitride ferromagnetic thin film of preparation, and wherein Fe content content is respectively (a) 2%, (b) 4%, (c) 9%, (d) 15%, (e) 28%, (f) 43%.
Fig. 2 is the X-ray diffractogram of the iron doped titanium nitride ferromagnetic thin film of preparation.
Fig. 3 is the room temperature magnetic hysteresis loop of the iron doped titanium nitride ferromagnetic thin film of preparation, and wherein Fe content content is respectively (a) 2%, (b) 4%, (c) 9%, (d) 15%, (e) 28%, (f) 43%.
Fig. 4 for the resistivity of iron doped titanium nitride ferromagnetic thin film of preparation with the variation of temperature relation curve.
Embodiment
Embodiment:
The structure and the property analysis that sample prepared among the present invention are carried out according to us; The preferred forms that below subtend target response sputtering method is prepared Fe doped polycrystalline TiN film is at length explained, the DPS-I type ultra high vacuum subtend target magnetic control sputtering coating machine that embodiment adopts scientific instrument development center, Chinese Academy of Sciences Shenyang to produce.
A kind of preparation method of iron doped titanium nitride ferromagnetic thin film of oriented growth, this step is following:
1) at ultra high vacuum subtend target magnetic control sputtering coating machine, a pair of purity of installation is 99.99% Ti target on the target head of subtend, a N utmost point as the magnetic line of force, and the other end is the S utmost point; The thickness of target is 5 mm, and diameter is 100 mm; 99.99% pure Fe sheet is fixed on surface at the Ti target; Distance between two targets is 100 mm, and the axis of target and the distance between the specimen holder are 100 mm;
2) glass substrate material is put into the vessel that fill alcohol and carry out sonicated, the mode that adopts hand rubbing is afterwards put into alcohol with sample after cleaning and is soaked after surface impurity is removed, and with hair-dryer sample is dried up at last; Again sample is put on the specimen holder, is installed on the perpendicular bisector of subtend target line;
3) unlatching DPS-I subtend target magnetic control sputtering equipment successively starts the one-level mechanical pump and the secondary molecular pump vacuumizes, and vacuum degree is 1 * 10 at the bottom of the back of the body of sputtering chamber
– 4Pa;
4) feeding purity to vacuum chamber is 99.999% Ar (15 sccm) and N
2The mist of (15 sccm) remains on 1 Pa with vacuum degree;
5) open shielding power supply, at electric current that applies 0.3 A on a pair of Ti target and the direct voltage about 500 V, sputter is 20 minutes in advance, waits sputtering current and voltage stable;
6) plate washer of opening on the substrate frame begins sputter, and substrate position is fixed; In the sputter procedure, substrate is not heated;
7) after sputter finishes, close the plate washer on the substrate frame, close shielding power supply then, stop to feed sputter gas Ar and N
2, open slide valve fully, continue to vacuumize, close vacuum system then; After treating system cools, charging into purity to vacuum chamber is 99.999% nitrogen, opens vacuum chamber and takes out sample and get final product.
For the Fe atom in the preparation film is evenly distributed, the Fe content in the film sample changes through area and the quantity that changes the Fe sheet.According to step identical among the above-mentioned preparation method and condition, the area of Fe sheet is chosen for 1 cm respectively
2, 1.5 cm
2, 2 cm
2When adopting 1 area is 1 cm
2The Fe sheet time, the Fe atom percentage in the sample that obtains preparing through X ray energy dispersion spectrometry is 2%; When adopting 1 area is 1.5 cm
2The Fe sheet time, the Fe atom percentage in the sample is 4%; When adopting 1 area is 2 cm
2The Fe sheet time, the Fe atom percentage in the sample is 9%; When adopting 2 areas is 1.5 cm
2The Fe sheet time, the Fe atom percentage in the sample is 15%; When adopting 1 area simultaneously is 1.5 cm
2Fe sheet and 1 area be 2 cm
2The Fe sheet time, the Fe atom percentage in the sample is 28%; When adopting 2 areas is 2 cm
2The Fe sheet time, the Fe atom percentage in the sample is 43%.
Be the embodiment of confirming that the present invention is best, we have carried out scanning electron microscopy, X-ray diffraction to prepared film of the present invention, the measurement of magnetic property and electronic transport characteristic.
Fig. 1 has provided the scanning electron microscope diagram of the Fe doped polycrystalline TiN film for preparing among the present invention, and wherein Fe content content is respectively (a) 2%, and (b) 4%, (c) 9%, (d) 15%, (e) 28%, (f) 43%.
Fig. 2 has provided the X-ray diffractogram of the Fe doped polycrystalline TiN film of the present invention's preparation, and wherein Fe content is seen among the figure and indicated.As can be seen from the figure, diffraction maximum all comes from the TiN of face-centred cubic structure, explains that Fe mixes the TiN lattice.When the Fe atomic percentage conc less than 4% the time, sample is < 200>oriented growth; When the Fe atomic percentage conc greater than 4% the time, sample is < 111>oriented growth.
Fig. 3 has provided the room temperature magnetic hysteresis loop of the Fe doped polycrystalline TiN film for preparing among the present invention, and wherein Fe content is seen among the figure and indicated.As can be seen from the figure, at room temperature, sample all shows as ferromagnetic characteristic.
Fig. 4 has provided the resistivity of the Fe doped polycrystalline TiN film for preparing among the present invention with the variation of temperature relation curve, and wherein Fe content is seen among the figure and indicated.As can be seen from the figure, the resistivity of sample raises along with the reduction of temperature, shows as to be similar to semi-conductive electrical conductive behavior.
The present invention propose through change the Fe doping content regulate and control < 200>and < 111>oriented growth the preparation method of iron doped titanium nitride ferromagnetic thin film, promptly when the Fe atomic percentage conc less than 4% the time, sample is < 200>oriented growth; When the Fe atomic percentage conc greater than 4% the time, sample is < 111>oriented growth.Be described through embodiment, person skilled obviously can be changed or suitably change and combination content as herein described in not breaking away from content of the present invention, spirit and scope, realizes the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as and are included in spirit of the present invention, scope and the content.
Claims (4)
1. the preparation method of the iron doped titanium nitride ferromagnetic thin film of an oriented growth is characterized in that: adopt the preparation of ultra high vacuum three target codeposition magnetron sputtering coaters, this step is following:
1) a pair of Ti target is installed on the target head of coating machine subtend, an end is as the N utmost point, and the other end is the S utmost point, and the distance between the fixing Fe sheet on the surface of Ti target, two targets is 100 mm, and the axis of target and the distance between the specimen holder are 100 mm;
2) substrate of glass is carried out sonicated with alcohol after, adopt the mode of hand rubbing that its surface impurity is removed after, put into alcohol and soak, be installed in after drying up on the perpendicular bisector of subtend target line;
3) open subtend target magnetic control sputtering equipment, successively start the one-level mechanical pump and the secondary molecular pump vacuumizes, vacuum degree is 1 * 10 at the bottom of the back of the body of sputtering chamber
– 4Pa;
4) feed Ar and N to vacuum chamber
2Mist, vacuum degree is remained on 1 Pa;
5) open shielding power supply, on a pair of Ti target, apply electric current and voltage, sputter is 20 minutes in advance, waits sputtering current and voltage stable;
6) plate washer of opening on the substrate frame begins sputter coating, and substrate position is fixed in the coating process;
7) the plated film time is 30 minutes, and plated film is closed the plate washer on the substrate frame after finishing, and closes shielding power supply then, stops to feed sputter gas Ar and N
2, open slide valve fully, continue to vacuumize; Close vacuum system then, treat system cools after, charging into purity to vacuum chamber is 99.999% nitrogen; When treating that the air pressure of vacuum type is identical with external atmosphere pressure, open vacuum chamber, open vacuum chamber and take out the target product that makes.
2. according to the preparation method of the iron doped titanium nitride ferromagnetic thin film of the said oriented growth of claim 1, it is characterized in that: the purity of said Ti target is 99.99%, and the thickness of target is 5 mm, and diameter is 100 mm; The purity of Fe sheet is 99.99%, and the area of Fe sheet is 1-2 cm
2
3. according to the preparation method of the iron doped titanium nitride ferromagnetic thin film of the said oriented growth of claim 1, it is characterized in that: said Ar and N
2Mist in, Ar and N
2Purity be 99.999%, Ar and N
2Flow be 15 sccm.
4. according to the preparation method of the iron doped titanium nitride ferromagnetic thin film of the said oriented growth of claim 1, it is characterized in that: said sputter DC power supply applies the electric current of 0.3 A and the voltage of 500 V on the Ti target.
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|---|---|---|---|
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|---|---|
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6130103A (en) * | 1998-04-17 | 2000-10-10 | Symetrix Corporation | Method for fabricating ferroelectric integrated circuits |
| CN1385397A (en) * | 2002-04-23 | 2002-12-18 | 重庆大学 | Technological method for preparing TiX (X=c,N) compound powder by direct reducing washingtonite |
| CN1986878A (en) * | 2006-12-28 | 2007-06-27 | 复旦大学 | Active atom beam spraying DC discharging process for preparing nano carbon nitride film |
| CN101708959A (en) * | 2009-12-08 | 2010-05-19 | 天津理工大学 | Method for preparing oriented polycrystalline zinc oxide film on glass substrate |
| CN101736303A (en) * | 2009-12-11 | 2010-06-16 | 天津大学 | Preparation method of chromium-doped titanium nitride magnetic semiconductor polycrystal film |
-
2011
- 2011-09-28 CN CN 201110295307 patent/CN102360944A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6130103A (en) * | 1998-04-17 | 2000-10-10 | Symetrix Corporation | Method for fabricating ferroelectric integrated circuits |
| CN1385397A (en) * | 2002-04-23 | 2002-12-18 | 重庆大学 | Technological method for preparing TiX (X=c,N) compound powder by direct reducing washingtonite |
| CN1986878A (en) * | 2006-12-28 | 2007-06-27 | 复旦大学 | Active atom beam spraying DC discharging process for preparing nano carbon nitride film |
| CN101708959A (en) * | 2009-12-08 | 2010-05-19 | 天津理工大学 | Method for preparing oriented polycrystalline zinc oxide film on glass substrate |
| CN101736303A (en) * | 2009-12-11 | 2010-06-16 | 天津大学 | Preparation method of chromium-doped titanium nitride magnetic semiconductor polycrystal film |
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Application publication date: 20120222 |