CN105648417B - A kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition technology - Google Patents
A kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition technology Download PDFInfo
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- CN105648417B CN105648417B CN201610144655.5A CN201610144655A CN105648417B CN 105648417 B CN105648417 B CN 105648417B CN 201610144655 A CN201610144655 A CN 201610144655A CN 105648417 B CN105648417 B CN 105648417B
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/505—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges
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Abstract
The invention discloses a kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition technology, this method comprises the following steps：(1) monocrystalline silicon piece is cleaned；(2) cleaned silicon chip is put into the high quartz annealing furnace filled with oxygen and carries out thermal oxidation, its surface is formed one layer of silicon oxide film；(3) using methane as reacting gas, using plasma strengthens silicon oxide film depositing amorphous carbon film on surface of the chemical vapour deposition technique formed in step (2).Prepared amorphous carbon film has the advantages that technique is simple, uniformity is good, resistivity is low and prepared by suitable large area in aforementioned manners, and this technique is mutually compatible with existing semiconductor process technique, is advantageous to the application of amorphous carbon film.
Description
Technical field
The present invention relates to thin-film material preparation method, and in particular to a kind of using plasma strengthens chemical vapour deposition technique
The method for preparing amorphous carbon film.
Background technology
Amorphous carbon film is due to good wear resistance, low-friction coefficient, good thermal conductance and translucency, band
The features such as gap adjustability, high rigidity and chemical property are stable, the application in fields such as optics, semiconductor and machinings is more next
More it is taken seriously.At present, preparing the method for amorphous carbon film mainly has micromechanics stripping method, organic synthesis method, carborundum pyrolysis
Epitaxial growth method, chemical stripping method and chemical vapour deposition technique etc..Though micromechanics stripping method can prepare high quality amorphous carbon film,
But controllability is relatively low, it is difficult to realizes extensive prepare；Organic synthesis method reactions steps are more, and aromatic ring system area dissolves when larger
Property be deteriorated, and with more side reaction, while catalyst amount is more, reaction time length；Carborundum thermal decomposition epitaxy growth method is difficult to
Realize prepared by the large area of amorphous carbon film, film forming is uneven, and condition is harsh, and high temperature and ultrahigh vacuum cost are high；Chemical stripping
Amorphous carbon film performance and stability deficiency prepared by method.Chemical vapour deposition technique is the important side in current thin film technology of preparing
One of method, common chemical vapour deposition technique have photoinduction chemical vapour deposition technique, heated filament catalytic chemical vapor deposition technique with
And the preparation method such as plasma glow discharge.Photoinduction chemical vapour deposition technique has mercury pollution, and film deposits on substrate
While can also be deposited on window.It is bad that heated filament catalytic chemical vapor deposition technique prepares amorphous carbon film uniformity, heated filament
Life-span is not high, adds cost, and heater strip may also produce pollution to the amorphous carbon film of deposition.
The content of the invention
, should it is an object of the invention to provide a kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition method
Amorphous carbon film prepared by method has film-forming process is simple, uniformity is good, resistivity is small and prepared by suitable large area etc.
Advantage.It is provided by the present invention it is a kind of using low temperature chemical vapor deposition method prepare the method for amorphous carbon film mainly include it is following
Step：
(1) monocrystalline silicon piece is cleaned；
(2) cleaned monocrystalline silicon piece is put into the quartzy annealing furnace filled with high purity oxygen gas and carries out thermal oxidation, made
Its surface forms one layer of silicon oxide film.The mode of monocrystalline silicon piece thermal oxidation is：Before heating, by cleaned monocrystalline silicon piece
High purity oxygen gas is passed through into quartzy tube annealing furnace while being put into quartzy tube annealing furnace and is kept for 15~25 minutes, then by stone
English tube annealing furnace is slowly heated to 600~900 DEG C and kept for 20~35 minutes, afterwards, disconnects heating power supply, takes out monocrystalline silicon piece,
Now monocrystalline silicon surface just forms one layer of silicon oxide film；
(3) monocrystalline of the chemical vapour deposition technique after thermal oxidation is strengthened by reacting gas using plasma of methane
Depositing amorphous carbon film on silicon chip.Preparation technology parameter is：100~150W of radio-frequency power, rf frequency 13.56MHz, substrate temperature
200~250 DEG C, 100~140Pa of chamber pressure of degree, purity are the CH of (percent by volume) 99.999%4Gas 10~
20sccm, plated film time 30~60 minutes.
A kind of low temperature chemical vapor deposition method is will pass through by above step amorphous carbon film material successfully to prepare.
The present invention promotes monocrystalline silicon substrate surface to form one layer of silicon oxide film, this oxidation using thermal oxide mode first
Silicon thin film can not only reduce amorphous carbon film caused stress in growth course, and be advantageous to improve amorphous carbon film
With the adhesion of monocrystalline silicon substrate, then using plasma enhancing chemical vapour deposition technique low temperature preparation amorphous carbon film,
Amorphous carbon film technique prepared by this method is simple, cost is low, uniformity is good, resistivity is small, is adapted to large area to prepare, and this
Technique is mutually compatible with existing semiconductor process technique, is advantageous to amorphous carbon film application.
Embodiment
Following case study on implementation is not used in the limitation present invention to illustrate the present invention.
Embodiment 1
A kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition method, this method are comprised the following steps：
(1) monocrystalline silicon piece is cleaned；
(2) cleaned monocrystalline silicon piece is put into the quartzy annealing furnace filled with high purity oxygen gas and carries out thermal oxidation, made
Its surface forms one layer of silicon oxide film.Monocrystalline silicon piece carry out thermal oxidation mode be：Before heating, by cleaned monocrystalline
High purity oxygen gas is passed through into quartzy tube annealing furnace while silicon chip is put into quartzy tube annealing furnace and is kept for 15 minutes, then by stone
English tube annealing furnace is slowly heated to 600 DEG C and kept for 35 minutes, afterwards, disconnects heating power supply, takes out monocrystalline silicon piece, now monocrystalline silicon
Surface just forms one layer of silicon oxide film；
(3) monocrystalline of the chemical vapour deposition technique after thermal oxidation is strengthened by reacting gas using plasma of methane
Depositing amorphous carbon film on silicon chip.Preparation technology parameter is：Radio-frequency power 100W, rf frequency 13.56MHz, substrate temperature 200
DEG C, chamber pressure 100Pa, purity is the CH of (percent by volume) 99.999%4Gas 10sccm, plated film time 30 minutes.
A kind of low temperature chemical vapor deposition method is will pass through by above step amorphous carbon film material successfully to prepare, its resistance
Rate is less than 6.0 × 10-3Ω·cm。
Embodiment 2
A kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition method, this method are comprised the following steps：
(1) monocrystalline silicon piece is cleaned；
(2) cleaned monocrystalline silicon piece is put into the quartzy annealing furnace filled with high purity oxygen gas and carries out thermal oxidation, made
Its surface forms one layer of silicon oxide film.Monocrystalline silicon piece carry out thermal oxidation mode be：Before heating, by cleaned monocrystalline
High purity oxygen gas is passed through into quartzy tube annealing furnace while silicon chip is put into quartzy tube annealing furnace and is kept for 17 minutes, then by stone
English tube annealing furnace is slowly heated to 750 DEG C and kept for 30 minutes, afterwards, disconnects heating power supply, takes out monocrystalline silicon piece, now monocrystalline silicon
Surface just forms one layer of silicon oxide film；
(3) monocrystalline of the chemical vapour deposition technique after thermal oxidation is strengthened by reacting gas using plasma of methane
Depositing amorphous carbon film on silicon chip.Preparation technology parameter is：Radio-frequency power 120W, rf frequency 13.56MHz, substrate temperature 220
DEG C, chamber pressure 120Pa, purity is the CH of (percent by volume) 99.999%4Gas 15sccm, plated film time 45 minutes.
A kind of low temperature chemical vapor deposition method is will pass through by above step amorphous carbon film material successfully to prepare, its resistance
Rate is less than 7.0 × 10-3Ω·cm。
Embodiment 3
A kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition method, this method are comprised the following steps：
(1) monocrystalline silicon piece is cleaned；
(2) cleaned monocrystalline silicon piece is put into the quartzy annealing furnace filled with high purity oxygen gas and carries out thermal oxidation, made
Its surface forms one layer of silicon oxide film.Monocrystalline silicon piece carry out thermal oxidation mode be：Before heating, by cleaned monocrystalline
High purity oxygen gas is passed through into quartzy tube annealing furnace while silicon chip is put into quartzy tube annealing furnace and is kept for 20 minutes, then by stone
English tube annealing furnace is slowly heated to 850 DEG C and kept for 25 minutes, afterwards, disconnects heating power supply, takes out monocrystalline silicon piece, now monocrystalline silicon
Surface just forms one layer of silicon oxide film；
(3) monocrystalline of the chemical vapour deposition technique after thermal oxidation is strengthened by reacting gas using plasma of methane
Depositing amorphous carbon film on silicon chip.Preparation technology parameter is：Radio-frequency power 130W, rf frequency 13.56MHz, substrate temperature 230
DEG C, chamber pressure 110Pa, purity is the CH of (percent by volume) 99.999%4Gas 17sccm, plated film time 50 minutes.
A kind of low temperature chemical vapor deposition method is will pass through by above step amorphous carbon film material successfully to prepare, its resistance
Rate is less than 8.0 × 10-3Ω·cm。
Embodiment 4
A kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition method, this method are comprised the following steps：
(1) monocrystalline silicon piece is cleaned；
(2) cleaned monocrystalline silicon piece is put into the quartzy annealing furnace filled with high purity oxygen gas and carries out thermal oxidation, made
Its surface forms one layer of silicon oxide film.Monocrystalline silicon piece carry out thermal oxidation mode be：Before heating, by cleaned monocrystalline
High purity oxygen gas is passed through into quartzy tube annealing furnace while silicon chip is put into quartzy tube annealing furnace and is kept for 25 minutes, then by stone
English tube annealing furnace is slowly heated to 900 DEG C and kept for 20 minutes, afterwards, disconnects heating power supply, takes out monocrystalline silicon piece, now monocrystalline silicon
Surface just forms one layer of silicon oxide film；
(3) monocrystalline of the chemical vapour deposition technique after thermal oxidation is strengthened by reacting gas using plasma of methane
Depositing amorphous carbon film on silicon chip.Preparation technology parameter is：Radio-frequency power 150W, rf frequency 13.56MHz, substrate temperature 240
DEG C, chamber pressure 130Pa, purity is the CH of (percent by volume) 99.999%4Gas 20sccm, plated film time 55 minutes.
A kind of low temperature chemical vapor deposition method is will pass through by above step amorphous carbon film material successfully to prepare, its resistance
Rate is less than 6.0 × 10-3Ω·cm。
Embodiment 5
A kind of method that amorphous carbon film is prepared using low temperature chemical vapor deposition method, this method are comprised the following steps：
(1) monocrystalline silicon piece is cleaned；
(2) cleaned monocrystalline silicon piece is put into the quartzy annealing furnace filled with high purity oxygen gas and carries out thermal oxidation, made
Its surface forms one layer of silicon oxide film.Monocrystalline silicon piece carry out thermal oxidation mode be：Before heating, by cleaned monocrystalline
High purity oxygen gas is passed through into quartzy tube annealing furnace while silicon chip is put into quartzy tube annealing furnace and is kept for 23 minutes, then by stone
English tube annealing furnace is slowly heated to 900 DEG C and kept for 18 minutes, afterwards, disconnects heating power supply, takes out monocrystalline silicon piece, now monocrystalline silicon
Surface just forms one layer of silicon oxide film；
(3) monocrystalline of the chemical vapour deposition technique after thermal oxidation is strengthened by reacting gas using plasma of methane
Depositing amorphous carbon film on silicon chip.Preparation technology parameter is：Radio-frequency power 120W, rf frequency 13.56MHz, substrate temperature 250
DEG C, chamber pressure 140Pa, purity is the CH of (percent by volume) 99.999%4Gas 13sccm, plated film time 60 minutes.
A kind of low temperature chemical vapor deposition method is will pass through by above step amorphous carbon film material successfully to prepare, its resistance
Rate is less than 7.0 × 10-3Ω·cm。
Described above is present pre-ferred embodiments, but the present invention should not be limited to disclosed in the embodiment
Content.So every do not depart from the lower equivalent or modification completed of spirit disclosed in this invention, the model that the present invention protects is both fallen within
Enclose.
Claims (1)
- A kind of 1. method that amorphous carbon film is prepared using low temperature chemical vapor deposition method, it is characterised in that under this method includes State step：（1）Clean monocrystalline silicon piece；（2）Cleaned monocrystalline silicon piece is put into the quartzy annealing furnace filled with high purity oxygen gas and carries out thermal oxidation, monocrystalline silicon Piece carry out thermal oxidation mode be：Before heating, while cleaned monocrystalline silicon piece is put into quartzy tube annealing furnace to High purity oxygen gas is passed through in quartzy tube annealing furnace and is kept for 15~25 minutes, quartzy tube annealing furnace is then slowly heated to 600~ 900 DEG C are kept for 20~35 minutes, afterwards, are disconnected heating power supply, are taken out monocrystalline silicon piece, now monocrystalline silicon surface just forms one layer of oxygen SiClx film；（3）Strengthen monocrystalline silicon piece of the chemical vapour deposition technique after thermal oxidation by reacting gas using plasma of methane Upper depositing amorphous carbon film, the technological parameter of depositing amorphous carbon film is on the monocrystalline silicon piece after thermal oxidation：Radio frequency work( 100~150W of rate, rf frequency 13.56MHz, 200~250 DEG C, 100~140Pa of chamber pressure of substrate temperature, purity are The CH of 99.999% percent by volume410~20sccm of gas, plated film time 30~60 minutes.
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Effective date of registration: 20221201 Address after: 314000 Northeast corner, 1st floor, Building 1, No. 333, Jingxing 1st Road, Caoqiao Street, Pinghu City, Jiaxing City, Zhejiang Province Patentee after: Zhejiang Tianji Material Technology Co.,Ltd. Address before: 443002 No. 8, University Road, Yichang, Hubei Patentee before: CHINA THREE GORGES University |