CN105568220B - A kind of method that magnetron sputtering prepares cubic boron nitride thick film - Google Patents
A kind of method that magnetron sputtering prepares cubic boron nitride thick film Download PDFInfo
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- CN105568220B CN105568220B CN201610027359.7A CN201610027359A CN105568220B CN 105568220 B CN105568220 B CN 105568220B CN 201610027359 A CN201610027359 A CN 201610027359A CN 105568220 B CN105568220 B CN 105568220B
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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
- C23C14/0641—Nitrides
- C23C14/0647—Boron nitride
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0063—Reactive sputtering characterised by means for introducing or removing gases
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The method that a kind of magnetron sputtering of the present invention prepares cubic boron nitride thick film, belong to the technical field of superhard material and its preparation.Using silicon chip as substrate, using h BN or pure boron target as sputtering target material, c BN thick films are prepared using two step sedimentations.In Ar/N2First layer boron nitride film is first sputtered under mixed-gas atmosphere, then is passed through H2, by mass flowmenter H2Dosage is the 4%~15% of total gas flow rate, keeps underlayer temperature, regulation substrate DC bias sputtering second layer boron nitride film.The method of the present invention is without using transition zone plus H2Measure it is less under conditions of, directly on a silicon substrate obtain cubic phase content more than 75%, even more than 95% c BN thick films, up to more than 4 μm, its stability is significantly improved thickness.
Description
Technical field
The invention belongs to superhard material and its technical field of preparation.More particularly to magnetron sputtering means prepare a cube nitridation
The technical field of boron (c-BN) thick film.Appropriate amount of hydrogen is introduced in traditional nitrogen, argon gas hybrid working gas, by controlling not
With hydrogen gas flow-rate ratio, underlayer temperature and substrate DC bias, in no metal, alloy cpd, boron carbide and diamond etc.
In the case of transition zone, directly on a silicon substrate obtain c-BN thick film of the cubic phase content more than 75% method.
Technical background
C-BN is a kind of superhard material with zincblende lattce structure, similar with diamond, has good physics and chemistry
Property, especially superpower oxidation resistance and chemical stability at high temperature, do not react with iron group metal, can win extensively
Appoint machining, cutting element and the grinding tool of the substantially any material including the material of iron group metal.Except excellent machinery
Performance, c-BN are wide bandgap semiconductors, it is easy to accomplish n-type and p-type doping, have negative electron affinity (NEA).Therefore, c-BN is in height
Temperature, high frequency, high-power electronic device and high speed, efficient, high-accuracy machining etc. have very big application potential.
Application industrial at present is generally with polycrystalline cubic boron nitride (polycrystalline cubic boron
Nitride, PCBN) based on.The bonding agent used in PCBN making can substantially reduce c-BN performance.Therefore directly in knife
The BN thick films that high cubic phase content is deposited on the substrate instrument such as tool, grinding tool mean a great for modern manufacturing industry.It is it is well known that vertical
The key that side is mutually nucleated is the surface of load energy particle constant bombardment film in film forming procedure, causes the film of sputtering sedimentation
Residual stress is all very big, and easily explosion, causes the thickness of film typically not over 200nm.Although current preparation means are
The c- of high Emission in Cubic can be obtained by the multiple means including chemical vapor deposition (CVD) and physical vapour deposition (PVD) (PVD)
BN films, but wanting the thick film of acquisition quality preferably, stable still has certain technical difficulty.Magnetron sputtering method can avoid
The poisonous working gas used in CVD, reduces the unintentional impurity that introduces in sample, and it is cheap, manipulation is simple, splashes
Rate height, steady performance are penetrated, is the preferred option of industrial plated film.There is minority to synthesize the μ of thickness 1 using magnetically controlled sputter method
M or so c-BN films, then it is by adding appropriate oxygen in reacting gas, and employs metal, alloy cpd or carbonization
The coatings such as boron are used as transition zone redeposition c-BN films in advance.
It is document Surface＆Coatings Technology 380-383 534 with the immediate prior art of the present invention
(2013).Document report uses non-balance magnetically controlled sputter method, and a large amount of hydrogen are passed through in argon gas and nitrogen mixture that (content surpasses
Cross more than 25%), it is prepared for the c-BN films that cubic phase content is only 60% on a silicon substrate using Nano diamond as transition zone, its
Maximum gauge is 2 μm so that many excellent properties of c-BN films cannot play well.Also, in view of current semiconductor work
Skill is based on silicon substrate, and Direct precipitation can make in c-BN preferably integrated technology fields till now on a silicon substrate.Make
Certain limitation is had in practical application to grow c-BN films with diamond substrate, while cost can also be significantly increased
Cost.Therefore, Direct precipitation c-BN films would is that more preferable selection on silicon substrate.
The content of the invention
The technical problem to be solved in the present invention is, using two step sedimentations, to utilize industrially conventional rf magnetron sputtering
Means, appropriate amount of hydrogen is introduced in nitrogen and argon gas gaseous mixture, directly on a silicon substrate, without being grown under conditions of other transition zones
C-BN thick films, it is set to be applied on industrial coating.
The present invention keeps radio-frequency power (that is, sputtering power), operating air pressure and nitrogen/argon by radio-frequency magnetron sputter method
Gas is than in the case of constant, changing hydrogen gas flow, substrate DC bias and underlayer temperature, determining BN Growth phase diagram, obtain
The optimum growh window of high cubic phase content.Hydrogen gas flow, substrate DC bias and underlayer temperature are studied simultaneously to high cube
The influence of the sedimentation rate of phase c-BN films.With reference to both, the cubic phase content more than 4 μm is directly obtained on a silicon substrate 95%
C-BN thick films above.
The present invention concrete technical scheme be：
A kind of method that magnetron sputtering prepares c-BN thick films, using silicon chip as substrate, with hexagonal boron nitride (h-BN) or simple substance
Boron target is sputtering target material, first cleans up substrate；Cleaned silicon chip is placed on the sample stage of magnetron sputtering vacuum chamber, target
Base spacing is 4~5cm, 50~100W of radio-frequency power；Characterized in that, prepare c-BN thick films using two step sedimentations；
First step deposition is that the back end vacuum of vacuum chamber is evacuated into 1.0 × 10-3More than Pa, introduce Ar/N2Mixed gas reaches
To operating air pressure 2.0Pa, N2/ Ar mass flow ratios are 1: 2~6；Under 300~500 DEG C of underlayer temperature, substrate DC bias 150V
Start to sputter first layer boron nitride film, 1~2h of growth time；
Second step deposition is to be passed through appropriate H on the basis of first step deposition2, H is controlled with mass flowmenter2Dosage is gas
The 4%~15% of total flow, keep underlayer temperature to 300~500 DEG C, regulation substrate DC bias be 0~150V, start sputtering the
Two layers of boron nitride film, growth time are 2~15h.
Described substrate cleaning, method that can be routinely are carried out；Preferably carried out by following processes：The silicon chip that will first cut
Wiped clean, it is put into petroleum ether and boils, then cleaned with acetone, then uses deionized water rinsing；Silicon chip is put into boiling again
Soak in the ammoniacal liquor risen, hydrogen peroxide, deionized water mixed solution, rinsed well after taking-up with deionized water；Silicon chip is inserted again
The hydrochloric acid of boiling, hydrogen peroxide, deionized water mixed liquor in soak, rinsed well again with deionized water after taking-up；It is finally putting into
Soak in hydrofluoric acid solution, cleaned up after taking-up, vacuum chamber is put into after being dried up with nitrogen.The time length soaked three times has no
Hinder greatly.
Currently preferred sedimentary condition is：400 DEG C of underlayer temperature, substrate DC bias 150V, life in first step deposition
Long-time 1h；Mass flowmenter H is pressed in second step deposition2Dosage is the 5.4%~11% of total gas flow rate, keeps underlayer temperature
400 DEG C, substrate DC bias 100V.
Experiment shows, by change it is different obtain the growth window that Emission in Cubic and hexagonal phase BN are respectively present into film parameters,
Hexagonal phase and Emission in Cubic BN sedimentation rate are also can obtain simultaneously with the change of hydrogen flowing quantity ratio and underlayer temperature.Work as underlayer temperature
More than 400 DEG C, the condition of Emission in Cubic growth is optimal, in the case of keeping other membrance casting conditions constant, with sputter gas hydrogen
The increase of throughput, Emission in Cubic BN sedimentation rate is reducing, and the content of Emission in Cubic is gradually increasing in BN films, and this is abundant
Hexagonal phase can be etched away by illustrating the introducing of hydrogen, and contribute to nucleation and the growth of Emission in Cubic.If only using traditional
The mixed gas of reacting gas argon gas and nitrogen, by changing substrate DC bias, it is found that with the increase of substrate bias,
Emission in Cubic starts to be nucleated, and its content is gradually increasing, and illustrates that substrate DC bias has certain influence for the nucleation of Emission in Cubic, simultaneously
Will also result in the aggregation of film internal stress, be c-BN films it is unstable the main reason for.After introducing appropriate amount of hydrogen, Emission in Cubic can be reduced
The substrate DC bias threshold value of nucleation.Being introduced into for hydrogen can reduce in Emission in Cubic nucleation process due to load energy particle in the present invention
The surface of constant bombardment film and caused by residual stress, make the surface of film be not easy to burst, it is thick to grow stable c-BN
Film.
The present invention only introduces appropriate amount of hydrogen in traditional nitrogen, argon gas hybrid working gas, by controlling different hydrogen
Gas flow ratio, underlayer temperature and substrate DC bias, in transition zones such as no metal, alloy cpd, boron carbide and diamonds
In the case of, thickness c-BN thick film more than 4 μm of the cubic phase content more than more than 75% is directly obtained on a silicon substrate.In view of
Semiconductor technology is based on silicon substrate at present, and it is existing that Direct precipitation of the present invention can make c-BN preferably be integrated on a silicon substrate
Technology field in.
In a word, the present invention is by two step sedimentations, without using transition zone plus H2Measure it is less under conditions of, directly in silicon
On substrate obtain cubic phase content more than 75%, after optimization be even more than 95% c-BN thick films, thickness up to more than 4 μm, its
Stability is significantly improved.
Brief description of the drawings：
Fig. 1 is rf magnetron sputtering Principle of plating figure.
Phasor when Fig. 2 is the content and underlayer temperature that embodiment 2 changes working gas hydrogen.
Fig. 3 is the timing of 3 underlayer temperature of embodiment one, changes the phase when content and substrate DC bias of working gas hydrogen
Figure.
Fig. 4 is the three-dimensional relationship figure between the hydrogen usage, sedimentation rate and underlayer temperature of embodiment 4.
Fig. 5 is the graph of a relation of the timing of 5 underlayer temperature of embodiment one, sedimentation rate and different hydrogen dosage.
Fig. 6 is SEM (SEM) low power figure of c-BN thick films prepared by embodiment 1.
Fig. 7 is SEM (SEM) high power figure of c-BN thick films prepared by embodiment 1.
Fig. 8 is SEM (SEM) cross-sectional view of c-BN thick films prepared by embodiment 1.
Fig. 9 is FTIR spectrum (FTIR) figure of c-BN thick films prepared by embodiment 1.
Embodiment
Rf magnetron sputtering Principle of plating using r. f. magnetron sputtering equipment as shown in figure 1, prepare cubic phase content
High c-BN thick films.In Fig. 1,1 is is placed on the silicon substrate on substrate table, and 2 be air inlet, and 3 be sputtering target material, and 4 be gas outlet；Figure
In 1, target h-BN, substrate is Si, and reacting gas is Ar, H2And N2.Following examples are all the purity using silicon as substrate
99.9% h-BN is that target grows c-BN films.Target in each embodiment can also be replaced by pure boron target, now suitably carry
High N2Addition, but the N also provided in the present invention2, in the range of Ar usage ratios.
Embodiment 1
The first step deposits：After being cleaned to substrate by the cleaning process of the present invention, in the vacuum chamber of magnetic control sputtering device
The mixed gas for being re-filled with argon gas and nitrogen is vacuumized, to operating air pressure 2Pa, regulation target base spacing is 4~5cm, radio-frequency power
For 80W；The mass flow ratio of nitrogen and argon gas is maintained at 1: 2,400 DEG C, substrate DC bias 150V of underlayer temperature, grows 1h.
This stage is nucleation stage.
Second step deposits：In the operating air pressure 2Pa of first step deposition, regulation target base spacing is 4~5cm, radio-frequency power is
80W, in the case of 400 DEG C of underlayer temperature is constant, regulation substrate DC bias to 100V；It is filled with H2, H2Dosage is calculated as gas by mass flow
The 5.4% of body total flow or 11%；Remove baffle plate and start sputtering sedimentation 14h.This stage is growth phase.
The c-BN thick films grown on this condition, film thickness are 4.5 μm.SEM (SEM) figure of product is shown in
Fig. 6~8, the infrared spectrum (FTIR) of product are shown in Fig. 9.The content 95%~97% of Emission in Cubic in obtained c-BN films.
The present embodiment is that sedimentary condition is optimal, and all very high embodiment of the content and film thickness of product Emission in Cubic, is to pass through
Change it is different into film parameters, inquire into hexagonal phase and Emission in Cubic BN sedimentation rate with the change of hydrogen flowing quantity ratio and underlayer temperature,
The associating of sedimentation rate and cubic phase content, substrate bias starts nucleation on Emission in Cubic and its content it is increased influence, hydrogen
Introduce to growing stable causality of c-BN thick films etc., obtained optimal deposition parameter.
Embodiment 2
The first step deposits：After being cleaned to substrate by the cleaning process of the present invention, in the vacuum chamber of magnetic control sputtering device
The mixed gas for being re-filled with argon gas and nitrogen is vacuumized, to operating air pressure 2Pa, regulation target base spacing is 4~5cm, radio-frequency power
For 80W；The mass flow ratio of nitrogen and argon gas is maintained at 1: 6,300~400 DEG C, substrate DC bias 150V of underlayer temperature is raw
Long 2h.This stage is nucleation stage.
Second step deposits：In the operating air pressure 2Pa of first step deposition, regulation target base spacing is 4~5cm, radio-frequency power is
80W, regulation underlayer temperature room temperature are not added with substrate DC bias to 500 DEG C；It is filled with H2, H2Dosage is calculated as gas by mass flow and always flowed
The 0~6% of amount；Remove baffle plate and start sputtering sedimentation 2h.This stage is growth phase.
Product is in H2Dosage is calculated as 0~6% and underlayer temperature of total gas flow rate in 100~500 DEG C of bars by mass flow
C-BN films Growth phase diagram is shown in Fig. 2 under part.It is 300~400 DEG C particularly in underlayer temperature, H2Dosage is calculated as gas by mass flow
When total flow is 4%~6%, the content of Emission in Cubic is more than 75% (referring to the black circle in Fig. 2) in c-BN films.
Embodiment 3
The first step deposits：After being cleaned to substrate by the cleaning process of the present invention, in the vacuum chamber of magnetic control sputtering device
The mixed gas for being re-filled with argon gas and nitrogen is vacuumized, to operating air pressure 2Pa, regulation target base spacing is 4~5cm, radio-frequency power
For 80W；The mass flow ratio of nitrogen and argon gas is maintained at 1: 2,400 DEG C, substrate DC bias 150V of underlayer temperature, grows 2h.
This stage is nucleation stage.
Second step deposits：In the operating air pressure 2Pa of first step deposition, regulation target base spacing is 4~5cm, radio-frequency power is
80W, in the case of 400 DEG C of underlayer temperature is constant, regulation substrate DC bias to 0~150V；It is filled with H2, H2Dosage presses mass flowmenter
For the 0%~15% of total gas flow rate；Remove baffle plate and start sputtering sedimentation 2h.This stage is growth phase.
The phasor of the cubic phase content of product is shown in Fig. 3.Black circle represents that the content of Emission in Cubic in c-BN films exists in figure
More than 75%.
When second step sedimentary condition is 0~150V of substrate DC bias；By mass flowmenter H2Dosage is total gas flow rate
When 8%, in the c-BN films of preparation the content of Emission in Cubic more than 75% (see 4 filled circles of the horizontally-arranged upper row of number the 3rd in Fig. 3
Point).
When second step sedimentary condition is 0~100V of substrate DC bias；By mass flowmenter H2Dosage is total gas flow rate
When 11%, in the c-BN films of preparation the content of Emission in Cubic more than 75% (see 3 filled circles of horizontally-arranged several second rows in Fig. 3
Point).
When second step sedimentary condition is 100~150V of substrate DC bias；By mass flowmenter H2Dosage is total gas flow rate
4% when, in the c-BN films of preparation the content of Emission in Cubic more than 75% (see 2 filled circles of the horizontally-arranged upper row of number the 4th in Fig. 3
Point).
When second step sedimentary condition is 100~150V of substrate DC bias；By mass flowmenter H2Dosage is total gas flow rate
14.4% when, in the c-BN films of preparation the content of Emission in Cubic more than 75% (see in Fig. 3 on the right of horizontally-arranged several first rows 2
Individual black circle).
The present embodiment also illustrates that most preferred sedimentary condition is 400 DEG C of underlayer temperature, substrate DC bias when second step deposits
100V, by mass flowmenter H2Dosage is the 8%~11% of total gas flow rate.
Embodiment 4
Growth conditions in embodiment 1 is constant, it have studied hydrogen and influence of the temperature to c-BN layer-growth rates.Reaction
Argon gas and nitrogen ratios are maintained at 1: 6 in gas, and hydrogen accounts for the ratio of total gas in 0~5.4% change, and underlayer temperature is from room temperature
(RT) 500 DEG C are progressively increased to, radio-frequency power keeps 80W, pressure 2.0Pa, growth time 2h.It can obtain the growth rate of film
Raised with the rise of underlayer temperature, reach highest when temperature is 200 DEG C and 300 DEG C, then reduction, that is, obtain cube
The mutually critical value of growth.The substrate minimum temperature of Emission in Cubic growth can be determined at 300 DEG C, the growth speed of film during more than 300 DEG C
Rate reduces the growth for being advantageous to Emission in Cubic BN.
Three-dimensional relationship between the growth rate of product, hydrogen usage and temperature is shown in Fig. 4.
Embodiment 5
The first step deposits：It is 1: 6 only to change the argon gas in embodiment 1 and nitrogen ratios.
Second step deposits：Using 400 DEG C of optimum growth temp in embodiment 1 as growth temperature, optimal substrate DC bias
100V biases as growth, changes H2Dosage can obtain deposition speed to be calculated as the 0~15% of total gas flow rate by mass flow
Relation between rate and hydrogen usage, sedimentation rate are gradually being reduced with the increase of hydrogen, substantially remained in after more than 4%
No longer change under low deposition rate.The sedimentation rate of product and the graph of a relation of hydrogen usage are referring to Fig. 5.
Claims (3)
1. a kind of method that magnetron sputtering prepares cubic boron nitride thick film, using silicon chip as substrate, with hexagonal boron nitride or pure boron
Target is sputtering target material, first cleans up substrate；Cleaned silicon chip is placed on the sample stage of magnetron sputtering vacuum chamber, target base
Spacing is 4~5cm, 50~100W of radio-frequency power；It is characterized in that prepare c-BN thick films using two step sedimentations；
First step deposition is that the back end vacuum of vacuum chamber is evacuated into 1.0 × 10-3More than Pa, introduce Ar/N2Mixed gas reaches work
Make air pressure 2.0Pa, N2/ Ar mass flow ratios are 1: 2~6；Start under 300~500 DEG C of underlayer temperature, substrate DC bias 150V
Sputter first layer boron nitride film, 1~2h of growth time；
Second step deposition is to be passed through H on the basis of first step deposition2, by mass flowmenter H2Dosage for total gas flow rate 4%~
15%, keep underlayer temperature to 300~500 DEG C, regulation substrate DC bias be 0~150V, start sputtering second layer boron nitride film,
Growth time is 2~15h.
2. the method that magnetron sputtering according to claim 1 prepares cubic boron nitride thick film, it is characterized in that, described substrate
Cleaning, is the silicon chip wiped clean that will be cut, is put into petroleum ether and boils, then cleaned with acetone, then use deionized water
Rinse；Then silicon chip is put into the ammoniacal liquor, hydrogen peroxide, deionized water mixed solution of boiling and soaked, taking-up is rushed with deionized water
Wash clean；Again by silicon chip insert the hydrochloric acid of boiling, hydrogen peroxide, deionized water mixed liquor in soak, taking-up is rushed with deionized water
Wash clean；Place into hydrofluoric acid solution and soak, wash clean after taking-up, vacuum chamber is put into after being dried up with nitrogen.
3. the method that magnetron sputtering according to claim 1 or 2 prepares cubic boron nitride thick film, it is characterized in that, the first step
400 DEG C of underlayer temperature, substrate DC bias 150V, growth time 1h in deposition；Mass flowmenter H is pressed in second step deposition2With
Measure 5.4%~11% for total gas flow rate, keep 400 DEG C of underlayer temperature, substrate DC bias 100V.
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