CN103590013B - Method for predicting components by analytical process to prepare Fe-Ga alloy film - Google Patents

Abstract

The invention provides a method for predicting components by an analytical process to prepare an Fe-Ga alloy film. JZCK-600F type multifunctional coating equipment is adopted, an alloy single target is utilized for magnetron sputtering, the alloy target is composed of Fe75Ga25, a round alloy target with a diameter of 60mm and a thickness of 3mm is installed on a target seat, and the target-substrate distance is 100mm. The method includes the steps of: selecting a substrate and performing pretreatment; conducting film component prediction calculation; determining a required sheet iron area; carrying out sputtering coating; performing sampling: taking out a well prepared sample when the film and substrate cool to room temperature, and placing the sample into a drying vessel to prevent the structure and properties of the film from changing in the air; employing EDS (energy disperse spectroscopy) or x-ray fluorescence analysis (XRF) to detect components, conducting comparison with predicted values, and calculating the error so as to adjust the sheet iron area for correction during next sputtering. The method provided by the invention solves the difficulty of hard preparation of an alloy film from the low-melting-point metal gallium by elemental target multi-target co-sputtering, and is also convenient for film component control at the same time.

Description

A kind of method of analysis prediction composition prepares the method for Fe-Ga alloy firm

Technical field

The present invention relates to a kind of method adopting magnetron sputtering method to prepare Fe-Ga alloy firm, belong to the functional materials technology of preparing of materials processing engineering field.

Background technology

At present, in the manufacture field of integrated magnetostriction apparatus, Fe-Ga alloy firm is subject to people's attention day by day.Film micro element develops the preparation that most crucial technology is exactly film.The performances such as the mechanics of film and physical chemistry depend on the weave construction of film, and the weave construction of film is closely related with the composition of film.

Magnetron sputtered deposition technology prepares the conventional method of metal and alloy firm, is also that current giant magnetostrictive thin film prepares the most frequently used technology.Magnetron sputtered deposition technology generally adopts simple substance target or alloys target to prepare alloy firm.

But, because gallium fusing point is very low, simple substance target co-sputtering technology cannot be adopted to prepare.Prepare film with alloys target magnetron sputtering and will expect that the film of what composition must smelt the target of tie element, and the composition of target also has difference with the thin film composition sputtered, think to obtain required composition exactly not only difficult, cost is also very high.

Adopting alloys target mount technology (mosaic target) to prepare Fe-Ga film is a kind of simple and easy to do method.But mount technology just rests on the experimental study stage, also do not have document to mention at present and calculate design Fe-Ga alloy firm composition accurately by a kind of theoretical formula, the Fe-Ga alloy firm wanting conveniently, prepare accurately heterogeneity also has difficulties.Therefore, when preparing Fe-Ga alloy firm, if its ingredient prediction Controlling model can be built, its composition being predicted, and then instructing the preparation of Fe-Ga film theoretically, there is very great meaning.

The present invention mainly establishes the predictive model of preparation technology and Fe-Ga alloy firm composition relation, propose a kind of can the preparation method of prediction and calculation composition.

Through By consulting literatures, when the people such as Byelorussian D.A.Golosov have studied mosaic target magnetic control sputtering, film elemental composition calculates.They utilize sputtering raste derivation on target surface, propose the analysis formula of a kind of alloy firm elemental composition calculating.Concrete scheme is that the Zr right cylinder of diameter 12mm and the Pb right cylinder of diameter 10.5mm are embedded in 5mm is thick, on the Ti target of diameter 80mm, Ti-Zr-Pb alloy firm is prepared through magnetron sputtering, the thin film composition of actual preparation is analyzed by isotope X-ray fluorescence analysis method (XRF), again according to area and the position of compact land, the formulae discovery checking alloy firm composition of deriving with them.

(D.A.Golosov,S.N.Melnikov,and A.P.Dostanko.Calculation of theelemental composition of thin films deposited by magnetron sputteringof mosaic targets.Surface Engineering and AppliedElectrochemistry.2012.Vol.48.No.1.pp.52-59)

But the method that D.A.Golosov is used and the present invention have following some distinguish:

1, mosaic target changes the principle of thin film composition is utilize target material surface Distribution of Magnetic Field uneven, is changed the composition of film by the position changing tesserae.Usually should consider the skewness in magnetic field and the shape of etched recesses, although D.A.Golosov they consider this point, used to inlay right cylinder comparatively large, the about 110mm of sectional area ², and inlay position by boring restriction.Because target surface Distribution of Magnetic Field is uneven, Ar may be caused ⁺the shock of ion pair target is also uneven, the Ar of target etch areas ⁺ionic concn is higher than other regions.If inlay right cylinder meeting more or less to exceed etch areas, and Ar outside etched area ⁺ionic concn is thinner, to inlaying cylindrical shock amount not as the shock amount in etched area, thus the second amount of substance in actual film being reduced to some extent, thus may cause predicated error.

And the present invention's mosaic target used is enough little by adsorption area, about 4mm ²-50mm ²small iron plate, and all iron plates are nearly all in target etch areas, then the impact that sputters iron plate of the skewness in magnetic field and the out-of-shape of etched recesses is very little, thus the composition of prediction film just more accurately facilitates.The present invention and the method for D.A.Golosov predict that the principle of composition is different.

2, the Computing Principle of the method prediction thin film composition of D.A.Golosov is that target surface is divided into three circle ring areas according to radius size, inlaying right cylinder is second annular regions, Definite Integral Calculation is carried out to the sputtering yield of the difference of different zones, finally draws the calculating composition of element in film.

The model that the present invention builds also combines two target magnetic control sputtering principle based on mosaic target sputtering principle and obtains, and be iron plate is regarded as a miniature little target, and rest part regards a Fe-Ga target in irregular shape as.And two target areas this factor that affects on thin film composition is dissolved among model, ingeniously utilize the rule that on same target stand, power is equal, what establish two target area comparison thin film compositions affects model, and the parameter in model can be determined by test conditions again, and thus accuracy is higher.

3, the method for D.A.Golosov is embedded in target by the second material right cylinder, first target will dig a hole by this method, again the second material right cylinder is inlayed into, the portion extrusion distortion that right cylinder contacts with target, there is very complicated contact area, inlay region can have an impact to sputtering, do not have paster method convenient, be not suitable for this Ferromagnetic target of Fe-Ga alloy.Iron plate is not embedded in target by the present invention's mosaic target used, but utilize the ferromegnetism of iron plate to be directly adsorbed on target, be suitable for Ferromagnetic target, arbitrarily can change the position of the second material very easily, facilitate the composition of control forecasting sputtered film.

4, they comprise target itself by mosaic target used and tesserae is all only applicable to simple substance, if there is a kind of element fusing point lower in film, cannot use.And the mosaic target that the present invention uses overcomes this shortcoming, the alloys target that available fusing point is higher replaces the simple substance target that fusing point is lower.

The technology of what comprehensive analysis had been announced prepare iron gallium alloy film is learnt, existing technology exists the following shortcoming being difficult to overcome:

● inlay right cylinder not aspect reversing of position, the accuracy of the impact prediction that is bound to.

● mosaic target comprises target itself and tesserae is all only applicable to simple substance, if there is a kind of element fusing point lower in film, cannot use.

Summary of the invention

The object of the invention is to overcome the deficiencies in the prior art, propose the method that a kind of method of analysis prediction composition prepares Fe-Ga alloy firm.The process employs a kind of analytic formula, can the thin film composition prepared of computational prediction magnetron sputtering according to paster metallic area and alloys target area ratio, the shortcoming that traditional multi-target magnetic control sputtering preparation method is difficult to prepare low melting point gallium metal alloy firm can be solved.

The present invention is achieved through the following technical solutions: adopt the Fe-Ga giantmagnetostrictive alloy target that containing metal gallium content is higher, and the pure iron sheet that area does not wait is attached to diameter 60mm respectively, in the circular alloys target of thickness 3mm, utilize vacuum magnetic-control sputtering equipment, the Fe-Ga alloy firm of composition needed for Slag coating.By changing the area ratio of iron plate area and alloys target area on target, the object controlling thin film composition can be reached, make the chemical element composition of prepared Fe-Ga alloy firm precisely controlled.

The principle of calculation formula of the present invention and derivation are:

The composition relative content (At%) of Fe-Ga film can be expressed as:

$M_{\mathrm{Fe}}\%=\frac{k_{\mathrm{Fe}}{A}_{\mathrm{Fe}}+k_{\mathrm{Fe}-\mathrm{Ga}}{A}_{\mathrm{Fe}-\mathrm{Ga}}\·m_{\mathrm{Fe}}\%}{k_{\mathrm{Fe}}{A}_{\mathrm{Fe}}+k_{\mathrm{Fe}-\mathrm{Ga}}{A}_{\mathrm{Fe}-\mathrm{Ga}}}---\left(1\right)$

$M_{\mathrm{Ga}}\%=\frac{k_{\mathrm{Fe}-\mathrm{Ga}}{A}_{\mathrm{Fe}-\mathrm{Ga}}\·m_{\mathrm{Ga}}\%}{k_{\mathrm{Fe}}{A}_{\mathrm{Fe}}+k_{\mathrm{Fe}-\mathrm{Ga}}{A}_{\mathrm{Fe}-\mathrm{Ga}}}---\left(2\right)$

In the document about Fe-Ga film preparation, think the composition of most of magnetron sputtering alloys target and thin film composition basically identical.And in the experiment carried out in the present invention, when not pasting iron plate, the thin film composition obtained and target material composition are also very close.Therefore, the m in formula _fe%, m _gathe content of Fe, Ga in the value of % and Fe-Ga alloy target material, adopting energy spectrometer EDS or X-ray fluorescence method (XRF) to detect target composition can obtain.And have

A _fe-Ga=A _target-A _fe(3)

α=A _fe/ A _target(4)

So obtain

$M_{\mathrm{Fe}}\%=\frac{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})m_{\mathrm{Fe}}\%}{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})}---\left(5\right)$

$M_{\mathrm{Ga}}\%=\frac{k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})m_{\mathrm{Ga}}\%}{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})}---\left(6\right)$

Wherein M _fe% is the Fe constituent content of the sputtering rear film that prediction and calculation goes out; M _ga% is the Ga constituent content of the sputtering rear film that prediction and calculation goes out; α is iron plate area and target area ratio; m _fe% is the content of ferro element in target, m _ga% is the content of Ga element in target.In formula, all elements content is atomic ratio content;

K in formula _fe, k _fe-Gafor the coefficient relevant to sputtering condition, be a constant when sputtering condition is identical, directly can substitute in formula and calculate.This two constants defining method is: after Slag coating one cluster film sample, energy spectrometer EDS or X-ray fluorescence method (XRF) is adopted to detect thin film composition, test one group of experimental data, the actual experimental data recorded substituted into respectively in formula (5), (6), row linear equation in two unknowns group obtains the relation conefficient k often organized _fe, k _fe-Ga.Averaged is by simplified formula again.The relation finally obtaining area ratio α and thin film composition is as follows:

M _Fe％≈0.98α+m _Fe％ (7)

Wherein M _fe% is the iron level of sputtering rear film reality; α is iron plate area and target area ratio; m _fe% is the content of ferro element in target.

This model not only can be used for carrying out Forecast and control to the composition of film determining in iron plate area and experiment condition situation, instruct the preparation of heterogeneity film, and required iron plate area can be gone out by inverse when determining target component and experiment condition.

Fe-Ga alloy firm preparation method of the present invention comprises following processing step:

Adopt JZCK-600F type Multi-functional coating device, utilize alloy list target to carry out magnetron sputtering, alloys target composition is Fe ₇₅ga ₂₅, by diameter 60mm, the circular alloys target of thickness 3mm is contained on target stand, and target-substrate distance is 100mm;

Coating operation step is:

(1) choosing and pre-treatment to substrate,

Select polished glass or Si sheet as substrate, before sputtering, to the surface acetone of substrate, ethanol, deionized water carries out strict cleaning, deoil, decontamination, deoxidation compound, by ultrasonic cleaning to strengthen cleaning performance, reusable heat source dry for standby after cleaning;

(2) thin film composition prediction and calculation

Choose some amount iron plate, the magnetic force of target stand is utilized to be attracted respectively to be attached within the scope of alloys target etched area by pure iron sheet, by changing the area ratio of iron plate area and alloys target area on target, reach the object controlling thin film composition, the disk of iron plate to be diameter be 2-5mm, thickness 1mm, area 3.14-19.625mm ², quantity 4-10 sheet, is distributed in target etched area according to annular,

Iron plate area and sputtering be after test conditions determines, the iron Fe predicted in sputtering rear film, gallium Ga constituent content can by following formulae discovery:

$M_{\mathrm{Fe}}\%=\frac{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})m_{\mathrm{Fe}}\%}{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})}---\left(5\right)$

$M_{\mathrm{Ga}}\%=\frac{k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})m_{\mathrm{Ga}}\%}{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})}---\left(6\right)$

Wherein M _fe% is the Fe constituent content of the sputtering rear film that prediction and calculation goes out; M _ga% is the Ga constituent content of the sputtering rear film that prediction and calculation goes out; α is iron plate area and target area ratio; m _fe% is the content of ferro element in target, m _ga% is the content of Ga element in target.In formula, all elements content is atomic ratio content;

(3) determination of required iron plate area

If plan wants the thin film composition prepared to determine, i.e. M _fe% is known, and area α needed for iron plate can utilize formula Extrapolation below to draw,

M _Fe％≈0.98α+m _Fe％ (7)

α＝(M _Fe％-m _Fe％)/0.98 (8)

Meanwhile, α=S _fe/ S _target

=n Π r _fe ²/ Π r _target ²(9)

=n r _fe ²/ r _target ²

D _fe=2r _fe=2 × (α/n × r _target ²) ^1/2(10)

Wherein d _fe, r _febe respectively required iron plate diameter and radius; N is iron plate quantity; r _targetfor Fe ₇₅ga ₂₅alloys target diameter; Π is pi.

(4) sputter coating:

A vacuumizes:

Sputtering chamber is vacuumized: after substrate is put into vacuum chamber, be first evacuated to about 3Pa with mechanical pump, then open molecular pump and be about 1 × 10 by being evacuated in vacuum chamber ^-4the vacuum tightness of Pa; The temperature of sputtering is room temperature, and substrate does not heat.

B passes into working gas, adjustment sputtering pressure:

Control high-purity argon gas by gas meter and vacuumometer and enter vacuum chamber, being filled with argon gas to sputtering chamber air pressure is 0.6Pa;

C sets sputtering voltage:

Regulate direct supply, make sputtering power be 90W, wait after stablizing, open baffle plate and carry out thin film deposition, sputtering time is 1.5h;

(5) sample: because during sputtering, energetic particle hits substrate may make substrate temperature raise, sputter rear wait 40 ~ 60Min, the sample prepared can be taken out when temperature Deng film and substrate is down to room temperature and put into drying basin, in case the properity of film changes in atmosphere to some extent;

(6) adopt energy spectrometer EDS or X-ray fluorescence method (XRF) to detect composition, contrast with predictor, miscalculation, so that adjustable iron plate area correction when again sputtering.

The invention has the beneficial effects as follows:

The present invention proposes a kind of new Fe-Ga giantmagnetostrictive alloy thin film composition Forecasting Methodology first, can solve the difficulty that low melting point metal gallium is difficult to prepare with simple substance target More target sputtering together alloy firm, conveniently can control thin film composition simultaneously.

In addition, the present invention has following innovation and beneficial effect in process of preparing:

● low melting point metal Ga easily volatilizees, and the Fe-Ga alloys target of the various required composition of melting more difficult, composition is difficult to control.As long as the present invention melts out a kind of Fe-Ga alloy containing high level metal Ga, adopt magnetic controlling target to the magneticaction of iron plate, adopt the method for pasting iron plate to prepare Fe-Ga giantmagnetostrictive alloy film, just can prepare the Fe-Ga alloy firm of multiple different Ga content.

● metal Ga is low melting point metal, is difficult to prepare elemental metals target, and More target sputtering together thus cannot be adopted to prepare Fe-Ga alloy firm.Adopt the present invention can prepare Fe-Ga alloy firm without More target sputtering together technology, and adopt single target sputtering technology namely can prepare the Fe-Ga alloy firm of various gallium content easily.

● the paster of fe can move very easily on target, thus can adjust the position of iron plate on target surface easily, can the Fe-Ga alloy firm composition prepared of prediction and calculation plan very accurately, overcomes the technical disadvantages of existing inlaying process.

Compared with the prior art, the Fe-Ga alloy firm composition prepared by the present invention can look-ahead, convenient and practical.The object of control Fe-Ga alloy firm composition more accurately can be reached by the ratio strictly controlling high purity iron sheet area and Fe-Ga alloys target area.

Embodiment

Be described in detail below in conjunction with the embodiment of the present invention:

Embodiment 1

Adopt JZCK-600F type Multi-functional coating device, utilize alloy list target to carry out magnetron sputtering.Alloys target composition is Fe ₇₅ga ₂₅.By diameter 60mm, the circular alloys target of thickness 3mm is contained on target stand, and target-substrate distance is 100mm.

Film coating sputtering processing parameter and operation steps are:

Choosing and pre-treatment 1, to substrate

Select polished glass or Si sheet as substrate, before sputtering, to the surface acetone of substrate, ethanol, deionized water carries out strict cleaning, deoil, decontamination, deoxidation compound, by ultrasonic cleaning to strengthen cleaning performance, reusable heat source dry for standby after cleaning;

2, thin film composition prediction and calculation

Choosing some amount iron plate, utilize magnetic force to be attracted respectively to be attached within the scope of alloys target etched area by pure iron sheet, by changing the area ratio of iron plate area and alloys target area on target, reaching the object controlling thin film composition.The disk of iron plate to be diameter be 5mm, thickness 1mm, area 19.625mm ², quantity 10.Target etched area is distributed according to annular.

Iron plate area is brought into formula (7) to calculate, in the sputtering rear film of prediction, iron level is:

M _Fe％≈0.98α+m _Fe％

＝0.98×(19.625×10/2826)+0.75

＝0.818

＝81.8％

3, sputter coating:

3.1 vacuumize:

Sputtering chamber is vacuumized: after substrate is put into vacuum chamber, be first evacuated to about 3Pa with mechanical pump, then open molecular pump and be about 1 × 10 by being evacuated in vacuum chamber ^-4the vacuum tightness of Pa.

3.2 pass into working gas, adjustment sputtering pressure:

Control high-purity argon gas by gas meter and vacuumometer and enter vacuum chamber, being filled with argon gas to sputtering chamber air pressure is 0.6Pa.

3.3 setting sputtering voltages:

Regulate direct supply, make sputtering power be 90W, wait after stablizing, open baffle plate and carry out thin film deposition, sputtering time is 1.5h.

4, sample: because during sputtering, energetic particle hits substrate may make substrate temperature raise, sputter rear wait 40 ~ 60Min, the sample prepared can be taken out when temperature Deng film and substrate is down to room temperature and put into drying basin, in case the properity of film changes in atmosphere to some extent;

5, adopt energy spectrometer (EDS) to detect composition, testing iron level in the film recorded is 79.50%.Contrast with predictor, error is 2.8%.

Embodiment 2

Adopt JZCK-600F type Multi-functional coating device, utilize alloy list target to carry out magnetron sputtering.Alloys target composition is Fe ₇₅ga ₂₅.By diameter 60mm, the circular alloys target of thickness 3mm is contained on target stand, and target-substrate distance is 100mm.

Film coating sputtering processing parameter and operation steps are:

Choosing and pre-treatment 1, to substrate

Select polished glass or Si sheet as substrate, before sputtering, to the surface acetone of substrate, ethanol, deionized water carries out strict cleaning, deoil, decontamination, deoxidation compound, by ultrasonic cleaning to strengthen cleaning performance, reusable heat source dry for standby after cleaning;

2, thin film composition prediction and calculation

Choosing some amount iron plate, utilize magnetic force to be attracted respectively to be attached within the scope of alloys target etched area by pure iron sheet, by changing the area ratio of iron plate area and alloys target area on target, reaching the object controlling thin film composition.The disk of iron plate to be diameter be 4mm, thickness 1mm, area 12.56mm ², quantity 8.Target etched area is distributed according to annular.

Iron plate area is brought into formula (7) to calculate, in the sputtering rear film of prediction, iron level is:

M _Fe％≈0.98α+m _Fe％

＝0.98×(12.56×8/2826)+0.75

＝0.7848

＝78.48％

3, sputter coating:

3.1 vacuumize:

Sputtering chamber is vacuumized: after substrate is put into vacuum chamber, be first evacuated to about 3Pa with mechanical pump, then open molecular pump and be about 1 × 10 by being evacuated in vacuum chamber ^-4the vacuum tightness of Pa.

3.2 pass into working gas, adjustment sputtering pressure:

Control high-purity argon gas by gas meter and vacuumometer and enter vacuum chamber, being filled with argon gas to sputtering chamber air pressure is 0.6Pa.

3.3 setting sputtering voltages:

Regulate direct supply, make sputtering power be 90W, wait after stablizing, open baffle plate and carry out thin film deposition, sputtering time is 1.5h.

4, sample: the sample prepared can be taken out when waiting the temperature of vacuum chamber to be down to room temperature and put into drying basin, in case the properity of film changes in atmosphere to some extent.

5, adopt energy spectrometer (EDS) to detect composition, testing iron level in the film recorded is 77.30%.Contrast with predictor, error is 1.5%.

Embodiment 3

Adopt JZCK-600F type Multi-functional coating device, utilize alloy list target to carry out magnetron sputtering.Alloys target composition is Fe ₇₅ga ₂₅.By diameter 60mm, the circular alloys target of thickness 3mm is contained on target stand, and target-substrate distance is 100mm.

Film coating sputtering processing parameter and operation steps are:

Choosing and pre-treatment 1, to substrate

Select polished glass or Si sheet as substrate, before sputtering, to the surface acetone of substrate, ethanol, deionized water carries out strict cleaning, deoil, decontamination, deoxidation compound, by ultrasonic cleaning to strengthen cleaning performance, reusable heat source dry for standby after cleaning;

2, thin film composition prediction and calculation

Choosing some amount iron plate, utilize magnetic force to be attracted respectively to be attached within the scope of alloys target etched area by pure iron sheet, by changing the area ratio of iron plate area and alloys target area on target, reaching the object controlling thin film composition.The disk of iron plate to be diameter be 2mm, thickness 1mm, area 3.14mm ², quantity 4.Target etched area is distributed according to annular.

Iron plate area is brought into formula (7) to calculate, in the sputtering rear film of prediction, iron level is:

M _Fe％≈0.98α+m _Fe％

＝0.98×(3.14×4/2826)+0.75

＝0.7544

＝75.44％

3, sputter coating:

3.1 vacuumize:

Sputtering chamber is vacuumized: after substrate is put into vacuum chamber, be first evacuated to about 3Pa with mechanical pump, then open molecular pump and be about 1 × 10 by being evacuated in vacuum chamber ^-4the vacuum tightness of Pa.

3.2 pass into working gas, adjustment sputtering pressure:

Control high-purity argon gas by gas meter and vacuumometer and enter vacuum chamber, being filled with argon gas to sputtering chamber air pressure is 0.6Pa.

3.3 setting sputtering voltages:

Regulate direct supply, make sputtering power be 90W, wait after stablizing, open baffle plate and carry out thin film deposition, sputtering time is 1.5h.

4, sample: because during sputtering, energetic particle hits substrate may make substrate temperature raise, sputter rear wait 40 ~ 60Min, the sample prepared can be taken out when temperature Deng film and substrate is down to room temperature and put into drying basin, in case the properity of film changes in atmosphere to some extent;

5, adopt energy spectrometer (EDS) to detect composition, testing iron level in the film recorded is 74.35%.Contrast with predictor, error is 1.5%.

Embodiment 4

Adopt JZCK-600F type Multi-functional coating device, utilize alloy list target to carry out magnetron sputtering.Alloys target composition is Fe ₇₅ga ₂₅.By diameter 60mm, the circular alloys target of thickness 3mm is contained on target stand, and target-substrate distance is 100mm.

Coating operation step is:

Choosing and pre-treatment 1, to substrate

Select polished glass or Si sheet as substrate, before sputtering, to the surface acetone of substrate, ethanol, deionized water carries out strict cleaning, deoil, decontamination, deoxidation compound, by ultrasonic cleaning to strengthen cleaning performance, reusable heat source dry for standby after cleaning;

2, the determination of required iron plate area

Known thin film composition to be prepared is determined, is 81%, and required iron plate area can utilize formula (8) to calculate.

α＝(M _Fe％-m _Fe％)/0.98 (8)

＝(0.81-0.75)/0.98

＝6.1％

Suppose that target diameter is 60mm, if with 10 iron plates, required iron plate diameter d can be calculated by formula (10):

D _fe=2r _fe=2 × (α/n × r _target ²) ^1/2

＝2×(0.061/10×30 ²) ^1/2

＝4.68mm

Namely the required iron plate diameter d of sputtering is that 4.68mm needs 10 altogether.

3, sputter coating:

3.1 vacuumize:

Sputtering chamber is vacuumized: after substrate is put into vacuum chamber, be first evacuated to about 3Pa with mechanical pump, then open molecular pump and be about 1 × 10 by being evacuated in vacuum chamber ^-4the vacuum tightness of Pa.

3.2 pass into working gas, adjustment sputtering pressure:

Control high-purity argon gas by gas meter and vacuumometer and enter vacuum chamber, being filled with argon gas to sputtering chamber air pressure is 0.6Pa.

3.3 setting sputtering voltages:

Regulate direct supply, make sputtering power be 90W, wait after stablizing, open baffle plate and carry out thin film deposition, sputtering time is 1.5h.

4, sample: because during sputtering, energetic particle hits substrate may make substrate temperature raise, sputter rear wait 40 ~ 60Min, the sample prepared can be taken out when temperature Deng film and substrate is down to room temperature and put into drying basin, in case the properity of film changes in atmosphere to some extent;

5, adopt energy spectrometer (EDS) to detect composition, contrast with predictor, miscalculation, so that adjustable iron plate area correction when again sputtering.

Claims (1)

1. prepare a method for Fe-Ga alloy firm with method of analysis prediction composition, it is characterized in that:

Adopt JZCK-600F type Multi-functional coating device, utilize alloy list target to carry out magnetron sputtering, alloys target composition is Fe ₇₅ga ₂₅, by diameter 60mm, the circular alloys target of thickness 3mm is contained on target stand, and target-substrate distance is 100mm;

Coating operation step is:

(1) choosing and pre-treatment to substrate

Select polished glass or Si sheet as substrate, before sputtering, to the surface acetone of substrate, ethanol, deionized water carries out strict cleaning, deoil, decontamination, deoxidation compound, by ultrasonic cleaning to strengthen cleaning performance, reusable heat source dry for standby after cleaning;

(2) thin film composition prediction and calculation

Choose some amount iron plate, the magnetic force of target stand is utilized to be attracted respectively to be attached within the scope of alloys target etched area by pure iron sheet, by changing the area ratio of iron plate area and alloys target area on target, reach the object controlling thin film composition, the disk of iron plate to be diameter be 2-5mm, thickness 1mm, area 3.14-19.625mm ², quantity 4-10 sheet, is distributed in target etched area according to annular;

Iron plate area and sputtering be after test conditions determines, the iron Fe predicted in sputtering rear film, gallium Ga constituent content can by following formulae discovery:

$M_{\mathrm{Fe}}\%=\frac{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})m_{\mathrm{Fe}}\%}{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})}---\left(5\right)$

$M_{\mathrm{Ga}}\%=\frac{k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})m_{\mathrm{Ga}}\%}{k_{\mathrm{Fe}}\mathrm{\α}+k_{\mathrm{Fe}-\mathrm{Ga}}(1-\mathrm{\α})}---\left(6\right)$

Wherein M _fe% is the Fe constituent content of the sputtering rear film that prediction and calculation goes out; M _ga% is the Ga constituent content of the sputtering rear film that prediction and calculation goes out; α is iron plate area and target area ratio; m _fe% is the content of ferro element in target, m _ga% is the content of Ga element in target; In formula, all elements content is atomic ratio content;

K in formula _fe, k _fe-Gafor the coefficient relevant to sputtering condition, be a constant when sputtering condition is identical, directly can substitute in formula and calculate; This two constants defining method is: after Slag coating one cluster film sample, energy spectrometer EDS or X-ray fluorescence method (XRF) is adopted to detect thin film composition, test one group of experimental data, the actual experimental data recorded substituted into respectively in formula (5), (6), row linear equation in two unknowns group can obtain the relation conefficient k often organized _fe, k _fe-Ga;

(3) determination of required iron plate area

If plan wants the thin film composition prepared to determine, i.e. M _fe% is known, and area α needed for iron plate can utilize formula Extrapolation below to draw,

M _Fe％≈0.98α+m _Fe％ (7)

α＝(M _Fe％-m _Fe％)/0.98 (8)

Meanwhile, α=S _fe/ S _target

=n Π r _fe ²/ Π r _target ²(9)

=n r _fe ²/ r _target ²

D _fe=2r _fe=2 × (α/n × r _target ²) ^1/2(10)

Wherein d _fe, r _febe respectively required iron plate diameter and radius; N is iron plate quantity; r _targetfor Fe ₇₅ga ₂₅alloys target diameter; Π is pi;

(4) sputter coating:

A vacuumizes:

Sputtering chamber is vacuumized: after substrate is put into vacuum chamber, be first evacuated to about 3Pa with mechanical pump, then open molecular pump and be about 1 × 10 by being evacuated in vacuum chamber ^-4the vacuum tightness of Pa; The temperature of sputtering is room temperature, and substrate does not heat;

B passes into working gas, adjustment sputtering pressure:

Control high-purity argon gas by gas meter and vacuumometer and enter vacuum chamber, being filled with argon gas to sputtering chamber air pressure is 0.6Pa;

C sets sputtering voltage:

Regulate direct supply, make sputtering power be 90W, wait after stablizing, open baffle plate and carry out thin film deposition, sputtering time is 1.5h;

(5) sample: because during sputtering, energetic particle hits substrate may make substrate temperature raise, sputter rear wait 40 ~ 60Min, the sample prepared can be taken out when temperature Deng film and substrate is down to room temperature and put into drying basin, in case the properity of film changes in atmosphere to some extent;

(6) adopt energy spectrometer EDS or X-ray fluorescence method (XRF) to detect composition, contrast with predictor, miscalculation, so that adjustable iron plate area correction when again sputtering.