CN103427019B - Magneto-resistor film and preparation method thereof - Google Patents
Magneto-resistor film and preparation method thereof Download PDFInfo
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Abstract
The manufacture method of a kind of magneto-resistor film, is included in substrate formation insulation material layer；Groove is formed in insulation material layer；In the bottom of groove, the surface of sidewall and described insulation material layer form the first barrier layer；Forming the second barrier layer on the first barrier layer, the thickness on described second barrier layer is less than the thickness on described first barrier layer；Described second barrier layer is formed magnetic material layer；Described magnetic material layer is made annealing treatment, to form described magneto-resistor film.In addition present invention also offers a kind of magneto-resistor film, including: first, second barrier layer set fluted insulation material layer, being successively set on insulation material layer and magnetic material layer.Technical scheme has the advantage that the second barrier layer surface is the most smooth, be conducive to the formation of follow-up magnetic material layer, the crystal grain making described magnetic material layer arranges more rule, and then improves the anisotropic magnetoresistance relative change rate of described magneto-resistor film.
Description
Technical field
The present invention relates to magnetic sensor field, be specifically related to a kind of magneto-resistor film and preparation method thereof.
Background technology
Magneto-resistor film is widely used in all kinds of random access memory, reading magnetic head and magnetic sensor
In the middle of equipment.In such devices, information storage density depends on described magneto-resistor to a great extent
The performance of thin film.
Magneto-resistance effect (Magneto Resistance, MR) refers to resistance the changing along with externally-applied magnetic field of material
The phenomenon become and change.The magneto-resistor film of the most modal employing magneto-resistance effect is mainly huge magnetoelectricity
Resistance (Giant Magneto Resistance, GMR) and anisotropic magnetoresistance (Anisotropic Magneto
Resistance,AMR).But, the information storing device made due to described giant magnet resistance film exists
The problem of less stable, the information storing device that relatively conventional anisotropic magnetoresistance thin film is made is still
So in occupation of mainstream market.
Anisotropic magnetoresistance refers to the quasi-resistance device that resistance sizes changes along with electric current and the direction of magnetization
Part.It is little, low in energy consumption, highly sensitive that magneto-resistance device based on anisotropic magnetoresistance formation has volume
And the feature that capacity of resisting disturbance is strong.
Owing to the size of anisotropic magnetoresistance relative change rate and the performance of magneto-resistance device are directly related,
Magneto-resistor relative change rate is the biggest for anisotropic, then the performance of magneto-resistance device is the best, therefore, how to carry
High anisotropy magneto-resistor relative change rate is one of those skilled in the art's problem demanding prompt solution.
Summary of the invention
The problem that the present invention solves is to provide a kind of magneto-resistor film and preparation method thereof, improves magneto-resistor thin
The anisotropic magnetoresistance relative change rate of film.
For solving the problems referred to above, the present invention provides the manufacture method of a kind of magneto-resistor film, including:
Substrate is formed insulation material layer；
Groove is formed in described insulation material layer；
In the bottom of described groove, the surface of sidewall and described insulation material layer form the first barrier layer；
Forming the second barrier layer on described first barrier layer, the thickness on described second barrier layer is less than described
The thickness on the first barrier layer；
Described second barrier layer is formed magnetic material layer；
Described magnetic material layer is made annealing treatment, to form described magneto-resistor film.
Optional:
In the step forming the first barrier layer, the thickness on described first barrier layer is at 1600～2000 angstroms
In the range of；
In the step forming the second barrier layer, the thickness on described second barrier layer is at the model of 200～400 angstroms
In enclosing.
Optionally, using plasma strengthen chemical gaseous phase deposition mode formed described first barrier layer and
At least one of described second barrier layer.
Optionally, the deposition pressure of plasma enhanced chemical vapor deposition in the range of 2.47～2.73 torr,
Temperature is maintained in the range of 361～399 degrees Celsius.
Optionally, formed described first barrier layer step after, formed the second barrier layer step it
Before, described manufacture method also includes: described first barrier layer being pointed to described insulation material layer surface is entered
Row chemical mechanical polish process.
Optionally, described first barrier layer and described second barrier layer all use silicon nitride material.
Optionally, the step forming magnetic material layer includes: form nickel successively on described second barrier layer
Iron layer and titanium nitride layer.
Optionally, in the step forming magnetic material layer, the thickness of described nifesphere is at 100～300 angstroms
In the range of, the thickness of described titanium nitride layer is in the range of 500～900 angstroms.
Optionally, the step forming magnetic material layer includes, forms institute by the way of physical vapour deposition (PVD)
Stating magnetic material layer, wherein deposition pressure is in the range of 4～6 millitorrs.
The present invention also provides for a kind of magneto-resistor film, including:
Insulation material layer, is provided with groove in described insulation material layer；
It is arranged on the first barrier layer on described channel bottom, sidewall and insulation material layer surface；
Being arranged on the second barrier layer on described first barrier layer, the thickness on described second barrier layer is less than institute
State the thickness on the first barrier layer；
Magnetic material layer, is arranged on described second barrier layer.
Compared with prior art, technical scheme has the advantage that
The first thicker barrier layer is additionally formed the second relatively thin barrier layer, so that arrive
Second barrier layer surface is the most smooth, the formation of follow-up magnetic material layer so that described magnetic
The crystal grain of material layer arranges more rule, and then improves the anisotropic magnetoresistance phase of described magneto-resistor film
To rate of change.
It addition, the crystal grain arrangement that annealing steps can make magnetic material layer is more neat, thus improve each to
Opposite sex magneto-resistor relative change rate.
Further, the thickness on the second barrier layer is in the range of 200～400 angstroms, and described second barrier layer can
To form the surface of more flat smooth, the crystal grain of magnetic material layer can be made further to arrange regularly.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the manufacture method embodiment of magneto-resistor film of the present invention；
Fig. 2 to Fig. 6 is that manufacture method one embodiment of magneto-resistor film of the present invention forms magneto-resistor film
Schematic diagram；
Fig. 7 is the experimental data figure of manufacture method one embodiment of magneto-resistor film of the present invention；
Fig. 8 is the experiment effect comparison diagram of manufacture method one embodiment of magneto-resistor film of the present invention.
Detailed description of the invention
The anisotropic magnetoresistance relative change rate of existing magneto-resistor film is relatively low, by described respectively to
In opposite sex magneto-resistor, magnetic material layer formation process carries out research discovery, crystal grain arrangement in magnetic material layer
Neat degree is relevant with the degree of roughness of magnetic material layer growing surface:
The growing surface of magnetic material layer is the most coarse, and the crystal grain arrangement of magnetic material layer is the most irregular.And magnetic
The arrangement of property material layer is the most irregular, the most easily reduces anisotropic magnetoresistance relative of magnetic material layer
Rate of change.
Therefore, the degree of roughness reducing magnetic material layer growing surface is conducive to crystal grain in magnetic material layer
Aligned transfer, and then the relative change rate of the anisotropic magnetoresistance of magnetic material layer can be improved.
To this end, the present invention provides the manufacture method of a kind of magneto-resistor film.With reference to Fig. 1, it is shown that the present invention
The schematic flow sheet of the manufacture method embodiment of magneto-resistor film.The manufacture method bag of described magneto-resistor film
Include:
Step S1, forms insulation material layer in substrate；
Step S2, forms groove in described insulation material layer；
Step S3, in the bottom of described groove, the surface of sidewall and described insulation material layer form first
Barrier layer；
Step S4, forms the second barrier layer, the thickness on described second barrier layer on described first barrier layer
Thickness less than described first barrier layer；
Step S5, forms magnetic material layer on described second barrier layer；
Step S6, makes annealing treatment described magnetic material layer, to form described magneto-resistor film.
The second barrier layer that the present embodiment is less by forming thickness, can make the table on described second barrier layer
Mask has relatively low degree of roughness, therefore, the crystalline substance of the magnetic material layer formed on described second barrier layer
Grain can arrange more regularly, and the relative change rate of the anisotropic magnetoresistance of magnetic material layer also will
Higher.
Below in conjunction with the accompanying drawings the technical scheme of each step is described in detail.
Perform step S1, substrate is formed insulation material layer.In the present embodiment, described insulant
The material of layer uses silicon dioxide.
With reference to Fig. 2, perform step S2, described insulation material layer 100 forms groove 101, in this reality
Execute in example, form groove 101 and comprise the steps:
Insulation material layer 100 coats photoresist (not shown)；
Photoresist is exposed by having figuratum mask, develops, the pattern of described mask is shifted
To photoresist；
With photoresist as mask, insulation material layer 100 is etched, to obtain with groove 101
Insulation material layer 100, removes photoresist afterwards.
In the present embodiment, the method for etching insulation material layer 100 uses plasma anisotropic etch,
Adopting and be advantageous in that in this way, the sidewall that can make groove 101 is the most neat.But, in reality
Being not limited to this method in application, it is also possible to use other engraving method, this is not made by the present invention
Limit.
With reference to Fig. 3, perform step S3, in the bottom of described groove 101, sidewall and described insulation material
The surface of the bed of material 100 forms the first barrier layer 110；
In the present embodiment, described first barrier layer 110 is injury-free for protective insulator layer 100.
The thickness on the first barrier layer 110, in the range of 1600～2000 angstroms, uses thicker first to stop
Layer 110, can provide enough protections to insulation material layer 100.
Described in the present embodiment, the first barrier layer 110 uses silicon nitride material, forms described first barrier layer
The mode of 110 is plasma enhanced chemical vapor deposition (Plasma Enhanced Chemical Vapor
Deposition, PECVD), described depositional mode has preferable step coverage.
Further, when carrying out plasma enhanced chemical vapor deposition, deposition pressure is maintained at
In the range of 2.47～2.73 torr, depositing temperature is maintained in the range of 361～399 degrees Celsius, with relatively low
At a temperature of form more uniform thin film.
But, the present invention does not make for deposit thickness and the depositional mode on described first barrier layer 110
Limit, in other embodiments, it is also possible to employing such as physical vapour deposition (PVD) (Physical Vapor Deposition,
Etc. PVD) other deposition process.
In the present embodiment, after forming described first barrier layer 110, also include:
The surface on described first barrier layer 110 is chemically-mechanicapolish polished (Chemical Mechanical
Polishing, CMP) process, make to be positioned at the surface on first barrier layer 110 on insulation material layer 100 surface
Become smooth, in order to the formation on the second barrier layer in subsequent step.
With reference to Fig. 4, perform step S4, described first barrier layer 110 form the second barrier layer 120,
The thickness on described second barrier layer 120 is less than described first barrier layer 110.
Described second barrier layer 120, for protective insulator layer 100, is additionally operable to the magnetic for being subsequently formed
Material layer provides growing surface.
It has been investigated that, when depositing device carries out depositing operation, the rough surface of the material layer eventually formed
Degree is directly related with deposit thickness, when deposit thickness is relatively big (such as: deposit thickness is probably at 400 angstroms
Time above) surface roughness of material that obtains of deposition significantly increases, obtains through experiment, deposit thickness
Time in the range of 200～400 angstroms, the surface roughness of the deposition material obtained is minimum.
Owing to the thickness on described second barrier layer 120 is less relative to the first barrier layer 110, formation of deposits
The surface roughness on the second barrier layer 120 will reduce a lot relative to the first barrier layer 110, slightly
The surface that rough degree is low is that magnetic material layer provides the most smooth growing surface, beneficially magnetic material
The neat arrangement of layer crystal grain, and then the relative change of the anisotropic magnetoresistance of magneto-resistor film can be improved
Rate.
In the present embodiment, the second barrier layer 120 uses the material identical with described first barrier layer 110,
But the invention is not limited in this regard, in other embodiments, described second barrier layer 120 can also be adopted
With the material different from described first barrier layer 110.
Specifically, the material on described second barrier layer 120 is silicon nitride, can strengthen with using plasma
The mode of chemical gaseous phase deposition (Plasma Enhanced Chemical Vapor Deposition, PECVD)
Form described silicon nitride.Specifically, deposition pressure is in the range of 2.47～2.73 torr, and depositing temperature exists
In the range of 361～399 degrees Celsius.
Due in the present embodiment, described second barrier layer 120 and the first barrier layer 110 use identical
Material, can reduce material cost.Additionally, in a particular application, the first barrier layer 110 can formed
After first pass through stop or stop depositing device, then restarted by programme-control depositing device,
With the second barrier layer 120 described in formation of deposits.As such, it is possible to complete the first stop in same depositing device
Layer 110 and the deposition on the second barrier layer 120, simplify step.
But, the present invention is to how forming the second barrier layer 120 and the first barrier layer 110 limits
System, it is also possible to adopt in other ways, such as: form described second respectively in different depositing devices and stop
Layer the 120, first barrier layer 110.
With reference to Fig. 5 and Fig. 6, perform step S5, described second barrier layer 120 is formed magnetic material
Layer.
In the present embodiment, the step forming magnetic material layer includes: successively on the second barrier layer 120
Form nifesphere 130 and titanium nitride layer 140.
Selecting ferronickel and titanium nitride material to be advantageous in that, both materials have ideal soft magnetism
Can, there is the relative change rate of higher anisotropic magnetoresistance.
But, the material that magnetic material layer is used by the present invention does not limits, it is also possible to be other magnetic
Material, such as: Perminvar, nickel cobalt (alloy) or ferrocobalt etc..
The present embodiment forms specifically comprising the following steps that of nifesphere 130 and titanium nitride layer 140
As it is shown in figure 5, form nifesphere 130 on described second barrier layer 120.In the present embodiment,
The mode forming described nifesphere 130 is physical vapour deposition (PVD), and deposit thickness is 100～300 angstroms, relatively thin
Nifesphere 130 be favorably improved anisotropic magnetoresistance relative change rate.
As shown in Figure 6, nifesphere 130 continues titanium nitride layer 140.Form described titanium nitride layer
The mode of 140 is physical vapour deposition (PVD), and deposit thickness is 500～900 angstroms, both can guarantee that successive process was to magnetic
The requirement of property layer thickness, also will not cause the shunting of signal because of blocked up.
In the present embodiment, when depositing described nifesphere 130 and titanium nitride layer 140, deposition pressure exists
In the range of 4～6 millitorrs, depositing temperature is room temperature.
Perform step S6, described magnetic material layer is made annealing treatment, to form magneto-resistor film.
In the present invention, annealing way specially magnetizes n 2 annealing；Annealing temperature is Celsius in 350～400
In the range of degree.After described magneto-resistor film is annealed, the stress in thin film and between different thin film obtains
Release, the crystal grain rearrangement of magnetic material layer, the arrangement of crystal grain becomes more rule so that described magnetic
The relative change rate of property material layer anisotropic magnetoresistance is promoted further.
With reference to Fig. 7, illustrate the experimental data of manufacture method one embodiment of magneto-resistor film of the present invention
Figure；This experiment is respectively to (After after (Depo) after formation of deposits magnetic material layer and annealing
Anneal) the anisotropic magnetoresistance relative change rate in two stages is measured.In Fig. 7, transverse axis is
Two barrier layers 120 surface roughness (Rq), the longitudinal axis is the anisotropic magnetic of the magnetic material layer being subsequently formed
Resistance relative change rate (dR/R)；After Fig. 7 intermediate cam shape, the point of rhombus represent formation magnetic material layer
Data, square, circular point then represent annealed after data.
Fig. 7 illustrates four groups of data sets 01,02,03 and 06 altogether (it should be noted that often organize number
According to two measured values included under the same conditions, the most often group data comprise two points in the figure 7), its
In:
Data set 01 represents that substep forms the resistance that threeply degree is 850 angstroms on above-mentioned insulation material layer 100
Barrier；
Data set 03 represents that formation thickness is the barrier layer of 2000 angstroms on above-mentioned insulation material layer 100；
Data set 02 is the method applied in the present invention: after forming above-mentioned the first thicker barrier layer, shape
Becoming relatively thin, thickness is second barrier layer of 400 angstroms；
Data set 06 is for directly heating described insulation material layer 100 (in the present embodiment for silicon), to be formed
One layer of oxide skin(coating) (Si oxide)；
It should be noted that the barrier layer in data set 01,02,03 all uses identical material, specifically
Ground, the material on described barrier layer is silicon nitride.
It can be seen from figure 7 that remove data set 06, in data set 01,02,03, barrier layer
Thickness is the least, and surface roughness (Rq) is the lowest, the anisotropy magnetoelectricity of the magnetic material layer being subsequently formed
Resistance relative change rate (dR/R) is the biggest.
Further, although data set 06 is oxide, the system of the magneto-resistor film to be obtained with the present invention
Make unrelated.But, owing to the surface roughness of described oxide skin(coating) is less than in data set 01,02,03
The surface roughness on barrier layer, and, data set 06 the anisotropy magnetoelectricity of the magnetic material layer formed
Resistance relative change rate be also at higher level (be slightly below data set 02 in the formation of deposits magnetic material layer stage,
It is the highest after the annealing process).Therefore, the effect of data set 06 is further to prove rough surface
Spend the lowest, the effect that the anisotropic magnetoresistance relative change rate of the magnetic material layer being subsequently formed is the highest.
See Fig. 8, it is shown that magneto-resistor film forms magnetic material layer (Post Depo) and annealing treatment
The data in reason (Post Anneal) latter two stage, wherein, four groups of data represent respectively according to four kinds of differences
The anisotropic magnetoresistance relative change rate of magneto-resistor film that obtains of manufacture method, wherein:
Data one and data four are the anisotropic magnetic of the magneto-resistor film using existing manufacture method to obtain
Resistance relative change rate (dR/R)；
The anisotropy magnetoelectricity of the magneto-resistor film that data two and the manufacture method that data three are the present invention obtain
Resistance relative change rate, the difference of data two and data three be data three after forming the first barrier layer, first
Described first barrier layer carrying out chemical mechanical polish process, then forms the second barrier layer, data two are in shape
The second barrier layer is directly formed after becoming the first barrier layer.
As can be seen from Figure 8, after annealed process, the anisotropic magnetoresistance of magneto-resistor film
Relative change rate respectively reaches 2.70% and 2.71%, uses the magnetic that existing manufacture method obtains higher than two groups
The anisotropic magnetoresistance relative change rate (respectively 2.56% and 2.54%) of resistance film, therefore,
Use manufacture method of the present invention can make the anisotropic magnetoresistance relative change rate of magneto-resistor film
Promote 0.14%～0.17%.
Additionally, in magneto-resistor film manufacture method of the present invention, relative to directly on the first barrier layer straight
Connect the technical scheme forming the second barrier layer, after the first barrier layer is carried out chemical mechanical polish process,
Form the anisotropic magnetoresistance relative change rate slightly higher of the magneto-resistor film that the second barrier layer obtains again
A bit.
Correspondingly, the present invention also provides for a kind of magneto-resistor film obtained by above-mentioned manufacture method.Continuing with
With reference to Fig. 6, described magneto-resistor film includes:
Insulation material layer 100, is provided with groove 101 in described insulation material layer 100；
Be arranged on bottom described groove 101, the first stop on sidewall and insulation material layer 100 surface
Layer 110；
It is arranged on the second barrier layer 120 on described first barrier layer 110, described second barrier layer 120
Thickness is less than the thickness on described first barrier layer 110；
Magnetic material layer, is arranged on described second barrier layer 120.
The thickness on described second barrier layer 120 is less than the thickness on described first barrier layer, for magnetic material layer
Providing smooth growing surface, this can make the regular arrangement of crystal grain in magnetic material layer, thus can
To increase the anisotropic magnetoresistance relative change rate of magnetic material layer.
In the present embodiment, the thickness on described second barrier layer 120 in the range of 200～400 angstroms, institute
The second barrier layer 120 stated in thickness range has relatively low surface roughness, carries for magnetic material layer
Supply the most smooth growing surface.
When forming magnetic material layer, owing to the growing surface of magnetic material layer is the most smooth,
Magnetic material layer, is arranged on described second barrier layer 120, in the present embodiment, and described magnetic
Material layer includes: be sequentially located at nifesphere 130 and titanium nitride layer 140 on described second barrier layer 120.
Specifically, the thickness of described nifesphere 130 is 200 angstroms, and the thickness of described titanium nitride layer 140 is
600 angstroms.But, the thickness of nifesphere 130 and titanium nitride layer 140 is not limited by the present invention.
It should be noted that magneto-resistor film of the present invention can be obtained by the manufacture method of above-mentioned magneto-resistor film
Arrive, but, the invention is not limited in this regard, described magneto-resistor film can also use other manufacture methods
Formed.
Although present disclosure is as above, but the present invention is not limited to this.Any those skilled in the art,
Without departing from the spirit and scope of the present invention, all can make various changes or modifications, therefore the guarantor of the present invention
The scope of protecting should be as the criterion with claim limited range.
Claims (10)
1. the manufacture method of a magneto-resistor film, it is characterised in that including:
Substrate is formed insulation material layer；
Groove is formed in described insulation material layer；
In the bottom of described groove, the surface of sidewall and described insulation material layer form the first barrier layer；
Forming the second barrier layer on described first barrier layer, the thickness on described second barrier layer is less than described
The thickness on the first barrier layer；
Described second barrier layer is formed magnetic material layer；
Described magnetic material layer is made annealing treatment, to form described magneto-resistor film.
2. manufacture method as claimed in claim 1, it is characterised in that:
In the step forming the first barrier layer, the thickness on described first barrier layer is at 1600～2000 angstroms
In the range of；
In the step forming the second barrier layer, the thickness on described second barrier layer is at the model of 200～400 angstroms
In enclosing.
3. manufacture method as claimed in claim 1, it is characterised in that using plasma strengthens chemistry
The mode of vapour deposition forms at least one of described first barrier layer and described second barrier layer.
4. manufacture method as claimed in claim 3, it is characterised in that PECVD
The deposition pressure of deposition is in the range of 2.47～2.73 torr, and temperature is maintained at the scope of 361～399 degrees Celsius
In.
5. manufacture method as claimed in claim 1, it is characterised in that forming described first barrier layer
Step after, before forming the step on the second barrier layer, described manufacture method also includes: be pointed to institute
Described first barrier layer stating insulation material layer surface carries out chemical mechanical polish process.
6. manufacture method as claimed in claim 1, it is characterised in that described first barrier layer and described
Second barrier layer all uses silicon nitride material.
7. manufacture method as claimed in claim 1, it is characterised in that form the step of magnetic material layer
Including: on described second barrier layer, form nifesphere and titanium nitride layer successively.
8. manufacture method as claimed in claim 7, it is characterised in that in the step forming magnetic material layer
In Zhou, the thickness of described nifesphere is in the range of 100～300 angstroms, and the thickness of described titanium nitride layer exists
In the range of 500～900 angstroms.
9. manufacture method as claimed in claim 1, it is characterised in that form the step of magnetic material layer
Including, by the way of physical vapour deposition (PVD), form described magnetic material layer, wherein deposition pressure is 4～6
In the range of millitorr.
10. a magneto-resistor film, it is characterised in that including:
Insulation material layer, is provided with groove in described insulation material layer；
It is arranged on the first barrier layer on described channel bottom, sidewall and insulation material layer surface；
Being arranged on the second barrier layer on described first barrier layer, the thickness on described second barrier layer is less than institute
State the thickness on the first barrier layer；
Magnetic material layer, is arranged on described second barrier layer.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1171606A (en) * | 1996-07-18 | 1998-01-28 | 三洋电机株式会社 | Magnetoresistive film |
| CN1433093A (en) * | 2002-01-11 | 2003-07-30 | 北京科大天宇微电子材料技术开发有限公司 | Magnetosensitive resistor metal film |
| CN101689599A (en) * | 2007-06-19 | 2010-03-31 | 佳能安内华股份有限公司 | Tunnel magnetoresistive thin film and magnetic multilayer film formation apparatus |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3890893B2 (en) * | 2000-12-28 | 2007-03-07 | 日本電気株式会社 | Spin tunnel magnetoresistive film and element, magnetoresistive sensor using the same, magnetic device, and manufacturing method thereof |
| JP2008309633A (en) * | 2007-06-14 | 2008-12-25 | Yamaha Corp | Magnetic sensor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1171606A (en) * | 1996-07-18 | 1998-01-28 | 三洋电机株式会社 | Magnetoresistive film |
| CN1433093A (en) * | 2002-01-11 | 2003-07-30 | 北京科大天宇微电子材料技术开发有限公司 | Magnetosensitive resistor metal film |
| CN101689599A (en) * | 2007-06-19 | 2010-03-31 | 佳能安内华股份有限公司 | Tunnel magnetoresistive thin film and magnetic multilayer film formation apparatus |
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