CN110468378A - A kind of preparation method of densification five oxidation two tantalum film - Google Patents
A kind of preparation method of densification five oxidation two tantalum film Download PDFInfo
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- CN110468378A CN110468378A CN201910864226.9A CN201910864226A CN110468378A CN 110468378 A CN110468378 A CN 110468378A CN 201910864226 A CN201910864226 A CN 201910864226A CN 110468378 A CN110468378 A CN 110468378A
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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
- C23C14/083—Oxides of refractory metals or yttrium
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
Abstract
The invention discloses a kind of preparation methods of fine and close five oxidation two tantalum film, under a high vacuum, accelerated on the tantalum pentoxide particle from the electron focusing that tungsten wire emits into copper crucible by e type electron gun, gasified, deposition growing goes out five oxidation two tantalum film on a silicon substrate, the annealing that different temperatures is finally carried out to it, prepares the thin-film material that pattern is uniform and smooth and consistency is high.The method of the present invention is compared to magnetron sputtering method, gained film crystal unity is high, voidage and hole are few, stability is good, it is fast, high-efficient relative to anodizing rate of film build, have the ability of commercial production, provides support to prepare fine and close five oxidation two tantalum film later.
Description
Technical field
The invention belongs to the preparation of material and optical film technology fields, and in particular to a kind of densification five oxidation two tantalum film
Preparation method.
Background technique
Five oxidation two tantalum film has good optical property, electrical properties and structural property, in recent years in optical thin film
Material, dielectric material and schemochrome Material Field are widely used.In terms of optical film materials, tantalum pentoxide can be saturating
Near infrared light and visible light are crossed, and in visible spectrum, five oxidation two tantalum film has lower absorptivity, and it belongs to
In high-index material, transmitted spectrum wider range (0.3~10 μm), so five oxidation two tantalum film material can be widely applied
In components such as anti-reflection film, photoelectric material, laser resonant cavity chip, solar wafer and liquid crystal displays.In electricity material
Aspect, tantalum pentoxide dielectric constant with higher (30~35), preferable thermal stability, and chemical property are stablized, can be with
The manufacturing process matching of semiconductor material, large scale integrated circuit component, it is considered to be most opened in microelectronic circuit arts
The non-silicon dielectric material for sending out potentiality, promises to be the capacitance material of next-generation multi-chip module and dynamic random reservoir, separately
Outer tantalum pentoxide also has application in certain heat engine parts surface coatings and positive electrode material surface coating.In structural property side
Face, five oxidation two tantalum film structure uniformly, good compactness, high mechanical strength, wearability are good, and it is thin can be widely used as types of functionality
The protective film of film, and can be used as schemochrome and be coated on all kinds of ornaments extensively, the material easy to fall off such as substitution pigment is environmentally protective,
Service life is long.
Summary of the invention
It is an object of the present invention to provide a kind of methods that fine and close five oxidation two tantalum film is prepared by electron beam evaporation method.This
Inventive technique scheme is: under vacuum conditions, being heated with high-power electron beam to tantalum pentoxide particle, in silicon chip
The identical film of upper deposition two layers of thickness, is finally made annealing treatment in 300 ~ 900 DEG C of air atmosphere, obtains five oxidations two
Tantalum films.
The detailed process of above-mentioned five oxidation two tantalum film material preparation method is:
S1, the high purity silicon substrate cleaned is placed in apparatus for electron beam evaporation, the tantalum pentoxide particle of high-purity is put
Enter in copper crucible；
S2, starting vacuum pump system, make chamber vacuum degree be down to 1 × 10-3Pa is hereinafter, be heated to 300 DEG C simultaneously to silicon chip simultaneously
Maintain constant temperature；
S3, the high-power electron beam manually emitted using e type electron gun carry out tantalum pentoxide particle to melt processing in advance；
S4, plasma processing, intracavitary residual gas during cleaning is melted in advance are carried out；
S5, setting coating process parameter, making the deposition rate of monofilm is 0.2~0.4nm/s, starts plated film；
S6, the annealing that sample is carried out to 300~900 DEG C in air, obtain five oxidation two tantalum film.
The purity of the tantalum pentoxide particle is 99.99% or more.
The silicon chip is cleaned by ultrasonic 15 minutes in acetone respectively, is then cleaned by ultrasonic 15 minutes in dehydrated alcohol,
Finally it is cleaned by ultrasonic 15 minutes in deionized water.
The electron gun filament electric current is 300~320 mA.
The tantalum pentoxide particle is 130~140 cm, tantalum pentoxide particle and electron gun at a distance from silicon chip
The distance of filament is 20~30 mm.
The time of the annealing is 30 minutes.
Two layers of successive sedimentation of the tantalum pentoxide particle film, thickness are 50 nm.
Beneficial effects of the present invention: the present invention utilizes electron beam evaporation method, first passes through the electronics emitted from tungsten wire by e type
Electron gun accelerates and focuses on the tantalum pentoxide particle in copper crucible, and deposition growing goes out metal-oxide film on a silicon substrate
Structure needs the vaporous parameter using higher melt material since tantalum pentoxide fusing point is higher, reduces electron gun facula area
It is allowed to fusing vapor deposition, different temperatures annealing is carried out to it in air later, prepares that pattern is uniform and smooth and consistency
High five oxidation two tantalum film.This method is easy to operate, and agents useful for same and tantalum pentoxide particle are commercially available, utilizes electronics
According to identical tantalum pentoxide evaporation plating parameter, bilayer repeats to be deposited the method for beam evaporation, and thickness ratio 1:1, film forming speed is fast, double-deck
Vapor deposition mode can give sufficient growth time, and crystal grain distribution is more uniform, the fine and close five oxidation two tantalum film formed after annealing
Better crystallinity degree, purity is high, stability is good, and the film repeatability relative to magnetically controlled sputter method preparation is high, good film-forming property, lower
At a temperature of be formed the relatively high fine and close five oxidation two tantalum film of purity, error rate is small between each batch, while this hair
The fine and close five oxidation two tantalum film of bright acquisition can be used for preparing anti-reflection film and optical protection layer.
The present invention is described in further details below with reference to attached drawing.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the fine and close five oxidation two tantalum film prepared.
Fig. 2 is the Raman spectrogram of the fine and close five oxidation two tantalum film prepared.
Fig. 3 is the scanning electron microscope diagram one of the fine and close five oxidation two tantalum film prepared.
Fig. 4 is the scanning electron microscope diagram two of the fine and close five oxidation two tantalum film prepared.
Fig. 5 is the scanning electron microscope diagram three of the fine and close five oxidation two tantalum film prepared.
Fig. 6 is the scanning electron microscope diagram four of the fine and close five oxidation two tantalum film prepared.
Fig. 7 is the scanning electron microscope diagram five of the fine and close five oxidation two tantalum film cross section prepared.
Fig. 8 is the scanning electron microscope diagram six of the fine and close five oxidation two tantalum film cross section prepared.
Fig. 9 is the scanning electron microscope diagram seven of the fine and close five oxidation two tantalum film cross section prepared.
Figure 10 is the scanning electron microscope diagram eight of the fine and close five oxidation two tantalum film cross section prepared.
Specific embodiment
Reach the technical means and efficacy that predetermined purpose is taken for the present invention is further explained, below in conjunction with attached drawing and reality
Example is applied to a specific embodiment of the invention, structure feature and its effect, detailed description are as follows.
Embodiment 1
It present embodiments provides a kind of preparation method such as the fine and close five oxidation two tantalum film material of Fig. 1~10: being steamed using electron beam
Hair method, control electron gun filament electric current are 310 mA or so, and deposition rate is 0.3 nm/s, first with five oxidations of purity 99.99%
Two tantalum particles are the evaporation material five oxidation two tantalum film that deposition a layer thickness is 50nm on a silicon substrate,；Then with identical electronic
The five oxidation two tantalum film that gun filament electric current and deposition rate redeposition a layer thickness are 50nm；Finally in 300 ~ 900 DEG C of sky
Annealing is carried out in gas atmosphere 30 minutes, heating rate is set in annealing process as 5 DEG C/min, obtains fine and close tantalum pentoxide
Film.
Preparing fine and close five oxidation two tantalum film, detailed process is as follows:
S1, the high purity silicon substrate cleaned is placed in apparatus for electron beam evaporation, the tantalum pentoxide particle of high-purity is put
Enter in copper crucible, prevents the influence in experimentation because of impurity from leading to the failure of an experiment；
S2, starting vacuum pump system, extract gas to chamber, chamber vacuum degree are made to be down to 1 × 10-3Pa is hereinafter, simultaneously to silicon chip
Be heated to 300 DEG C and maintain constant temperature, when preventing lower vacuum degree from evaporation process being caused to fail, while reducing plated film stress because
Element causes film quality poor；
S3, the high-power electron beam manually emitted using e type electron gun melt processing in advance to the progress of tantalum pentoxide particle,
Make it is pre- melt metal surface uniform ground, can be improved more evenly and more stable boil-off gas；
S4, plasma processing is carried out, intracavitary residual gas during cleaning is melted in advance makes experimentation not by the shadow of foreign gas
It rings；
S5, setting coating process parameter, make 0.2~0.4nm/s of its deposition rate, and use crystal oscillator monitoring film deposition of thick
Degree, and so that silicon chip temperature is maintained at 300 DEG C using Resistant heating, start plated film；Detailed process is: by adjusting electron beam
For current density size to control the evaporation rate of tantalum pentoxide particle, adjusting evaporation rate is 0.2~0.4nm/s, is passed through
Be mounted on crystal-vibration-chip above vacuum chamber can with the deposition thickness of the plated film of real-time detection, set each layer of deposition thickness as
50nm, when its deposition thickness reaches set film thickness, film deposition process is automatically stopped；The planetary plate of fixed silicon chip
Surrounding is equipped with after one week resistance wire of vacuum cavity, galvanization planetary plate and the attachment that can uniformly toast uniform rotation
Silicon chip on planetary plate；In evaporation process, the temperature of silicon chip is maintained 300 DEG C using the method for baking, to reduce
Membrane stress improves quality of forming film.
After the completion of S6, film deposition, sample is carried out to 300~900 DEG C of annealing.Sample is made annealing treatment,
Surface and internal atom or molecule can obtain energy, therefore can be redistributed in silicon substrate surface, fill up defect, make thin
More evenly, compactness is more preferable for film quality.
Further, the purity of high-purity tantalum pentoxide particle is 99.99% or more.
Further, high-purity silicon chip is cleaned by ultrasonic 15 minutes in acetone, then ultrasound is clear in dehydrated alcohol
It washes 15 minutes, is finally cleaned by ultrasonic 15 minutes in deionized water, this purpose is the grease stain and indissoluble impurity for removing silicon chip surface,
Prevent it from influencing the growth of film.
Further, the electron gun filament electric current is 300~320 mA, and deposition rate is 0.2~0.4nm/s.Setting
This current value range, it can be ensured that the deposition rate that experiment needs is provided.Because deposition rate can play ratio to the growth of film
More crucial effect, too fast or too slow deposition rate will affect the growth pattern of film, at the same stable deposition rate for
It is vital for preparing the film having good uniformity.
Further, the tantalum pentoxide particle is 130~140 cm, tantalum pentoxide particle at a distance from silicon chip
With at a distance from electron gun filament be 20~30 mm.Tantalum pentoxide particle is to be determined at a distance from electron gun by equipment, cannot
It is adjusted according to different experiments.When with electron beam heat tantalum pentoxide particle when, filament apart from tantalum pentoxide particle compared with
Closely, tantalum pentoxide particle may due in crucible uneven heating it is even and part collapse crucible out, collapse out melting five oxidation two
Tantalum particle drop, which splashes silicon substrate surface, will seriously affect the pattern of film.In addition, filament apart from tantalum pentoxide particle away from
From too close, the climbing speed of gas after uncontrollable tantalum pentoxide particle gasification may cause, to the uniformity of film
It influences.Meanwhile if filament is too far apart from tantalum pentoxide particle, electron beam is difficult to focus, and institute is not achieved in the temperature in crucible
The melting temperature of setting, thus tantalum pentoxide particle cannot be melted or need to use bigger heater current.Work as silicon chip
When with tantalum pentoxide particle distance between 130~140 cm, at this point, the climbing speed of tantalum pentoxide steam and five oxygen
The opposing gas density for changing two tantalum steams can more evenly can play the role of the growth of film advantageous.
Embodiment 2
In the present embodiment, carried out in 500 DEG C of air atmosphere annealing 30 minutes, set in annealing process heating rate as
5 DEG C/min, other steps are same as Example 1, obtain fine and close five oxidation two tantalum film.
Embodiment 3
In the present embodiment, carried out in 700 DEG C of air atmosphere annealing 30 minutes, set in annealing process heating rate as
5 DEG C/min, other steps are same as Example 1, obtain fine and close five oxidation two tantalum film.
Embodiment 4
In the present embodiment, carried out in 900 DEG C of air atmosphere annealing 30 minutes, set in annealing process heating rate as
5 DEG C/min, other steps are same as Example 1, obtain fine and close five oxidation two tantalum film.
Embodiment 5
Film prepared by Examples 1 to 4 has been carried out point using scanning electron microscope, X-ray diffractometer, Raman spectrometer
Analysis, the result is shown in Figure 1~10.Fig. 1 is the results show that gained film is five oxidation two tantalum film, but works as temperature and be increased to 900 DEG C
When, Ta2O5It undergoes phase transition, by β-Ta2O5(low form) is transformed into α-Ta2O5(high temperature modification).In Fig. 2 result, by Ta2O5Film exists
306 and 432cm-1Raman peaks vary with temperature curve, qualitative can find out Ta2O5Raman spectrum with annealing temperature variation not
Greatly.Fig. 3~6 is shown: between 300~700 DEG C, Ta2O5With the increase of annealing temperature, particle size obviously becomes smaller film, this
It is the raising due to temperature, surface free energy increases, and increases the surface mobility of atom, the defect for having filled up film surface is made
At, the significant change that 900 DEG C of annealing occurs, it may be possible to since at high temperature, five oxidation two tantalum film occurs from low-temperature phase
It is changed into the phase transformation of high-temperature-phase.The phenomenon has further proved result shown in Fig. 1.Fig. 7~10 are the results show that Ta at 300 DEG C2O5
Film thickness is slightly thicker than other samples, this is because caused by surface defect is more, at 500~900 DEG C, due to the increase of temperature
Mobility is caused to increase, film surface defects are less, so its thickness change is little.
Claims (8)
1. a kind of preparation method of densification five oxidation two tantalum film, it is characterised in that: under vacuum conditions, with high-power electron beam pair
Tantalum pentoxide particle is heated, and deposits five oxidation two tantalum film on a silicon substrate, finally in 300 ~ 900 DEG C of air
It is made annealing treatment in atmosphere, obtains the five oxidation two tantalum film of crystallinity improvement.
2. the preparation method of densification five oxidation two tantalum film as described in claim 1, which is characterized in that preparation densification five aoxidizes
The detailed process of two tantalum films is:
S1, the high purity silicon substrate cleaned is placed in the specimen holder in apparatus for electron beam evaporation, aoxidizes two for the five of high-purity
Tantalum particle is put into copper crucible；
S2, chamber vacuum degree is made to be down to 1 × 10-3Pa is hereinafter, being heated to 300 DEG C to silicon chip simultaneously and maintaining constant temperature；
S3, the high-power electron beam manually emitted using e type electron gun carry out tantalum pentoxide particle to melt processing in advance；
S4, plasma processing, intracavitary residual gas during cleaning is melted in advance are carried out；
S5, setting coating process parameter, make five oxidation two tantalum film 0.2~0.4nm/s of deposition rate, start plated film；
S6, the annealing that sample is carried out to 300~900 DEG C in air obtain the five oxidation two tantalum film of crystallinity improvement.
3. the preparation method of densification five oxidation two tantalum film according to claim 1 or 2, it is characterised in that: five oxygen
The purity for changing two tantalum particles is 99.99% or more.
4. the preparation method of densification five oxidation two tantalum film according to claim 1 or 2, it is characterised in that: the silicon substrate
Piece is cleaned by ultrasonic 15 minutes in acetone, is then cleaned by ultrasonic in dehydrated alcohol 15 minutes, finally ultrasonic in deionized water
Cleaning 15 minutes.
5. the preparation method of densification five oxidation two tantalum film according to claim 2, it is characterised in that: the e type electronics
Gun filament electric current is 300~320 mA.
6. the preparation method of five oxidation two tantalum film according to claim 2, it is characterised in that: the tantalum pentoxide
Grain is 130~140 cm at a distance from silicon chip, and tantalum pentoxide particle is 20~30 mm at a distance from electron gun filament.
7. the preparation method of five oxidation two tantalum film according to claim 1 or 2, it is characterised in that: the annealing
Time be 20~60 minutes.
8. the preparation method of five oxidation two tantalum film according to claim 2, it is characterised in that: the tantalum pentoxide
Two layers of successive sedimentation of film of grain, thickness is 50 nm.
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| CN112592180A (en) * | 2020-12-15 | 2021-04-02 | 海宁拓材科技股份有限公司 | Preparation method of low-fluorine high-purity tantalum pentoxide optical coating material |
| CN114108087A (en) * | 2021-11-23 | 2022-03-01 | 北京工业大学 | Preparation method of orthorhombic phase tantalum pentoxide single crystal film |
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