CN1078264C - Microwave plasma chemical vapor deposition synthesis of crystalline phase carbon nitrogen film - Google Patents
Microwave plasma chemical vapor deposition synthesis of crystalline phase carbon nitrogen film Download PDFInfo
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- CN1078264C CN1078264C CN97121868A CN97121868A CN1078264C CN 1078264 C CN1078264 C CN 1078264C CN 97121868 A CN97121868 A CN 97121868A CN 97121868 A CN97121868 A CN 97121868A CN 1078264 C CN1078264 C CN 1078264C
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Abstract
本发明涉及用微波等离子体化学气相沉积法合成碳氮薄膜及装置。将基片经过预处理后，置于工作腔内，按一定比例通入工作气体，然后将微波通入工作腔内，使气体放电产生等离子体从而沉积薄膜。用这种方法合成的氮化碳薄膜均匀、致密，无杂质，成分和成键符合要求，膜中含有α、β和p相的C3N4。该方法工艺稳定、可靠，重复性好，适合工业化生产。The invention relates to a carbon-nitrogen thin film synthesized by a microwave plasma chemical vapor deposition method and a device. After the substrate is pretreated, it is placed in the working chamber, and the working gas is passed into the working chamber at a certain ratio, and then the microwave is passed into the working chamber to make the gas discharge generate plasma to deposit the film. The carbon nitride thin film synthesized by this method is uniform, dense, free of impurities, and its composition and bonding meet the requirements. The film contains C 3 N 4 in α, β and p phases. The process of the method is stable, reliable and repeatable, and is suitable for industrial production.
Description
The present invention relates to prepare the superhard material field, particularly with the synthetic crystalline phase carbon nitrogen (C of microwave plasma CVD with chemical vapour deposition technique
3N
4) method of thin-film material.
Professor such as U.S. M.L.Cohen in 1989 calculates according to first principle and confirms β-C
3N
4Young's modulus and diamond are suitable, caused the concern of material educational circles and solid educational circles, so far existing 10 countries, more than 50 research group participated in this work sutdy, nearly hundred pieces of articles have been delivered, but from the academic paper of having delivered, progress situation in this respect is at present: film forming density is poor, and is impure; Composition does not reach the requirement of N/C=1.33, has indivedual groups to reach, but cannot take out structured data; The structured data that has obtained still can not be identified a cenotype.
Situation about applying for a patent is as follows, the patented invention (Japanese Patent J03240959) of SUME SUMITPMO ELEC IND KK adds negative bias on the norbide substrate, add voltage of alternating current to the mixed gas that contains carbon, hydrogen, Sauerstoffatom then and make its discharge generation plasma body, the deposit carbon nitrogen film, but only claim and synthesized carbon-nitrogen film, not carbonitride (the C of synthetic crystalline phase
3N
4) film, the b-C of the synthetic crystalline phase of distance
3N
4Film is far in addition.
People's such as Chen Yan and king's grace brother invention " crystalline alpha mutually with beta-phase carbon nitride thin film material and preparation method thereof " (Chinese patent CN1151386A) is with the synthetic Crystalline Carbon Nitride Films of the auxiliary hot filament CVD of negative bias.Because this method adopts the tungsten filament heating, impurity is inevitable, and purity is difficult to guarantee.And the ionization level of the plasma body that utilization heating and direct-current discharge produce is not high, and nitrogen ionic concentration wherein is not high, is unfavorable for forming fine and close film.In addition, the tungsten filament that is used for heating in this method is running stores, and often replacing has also caused the unstable of growth conditions.
The objective of the invention is in order to overcome the existing methods deficiency, one, the pollution of heated filament in the device improves the purity of crystalline phase carbon-nitrogen film; Its two, nitrogen ionic concentration and electronic temp are very high in the plasma body, improve the nitrogen content of institute's synthetic film greatly; Its three, in order to improve process repeatability, the invention provides a kind of employing microwave and produce plasma body, the method for the crystalline phase carbon-nitrogen film material of the synthetic even compact of chemical vapour deposition.
The object of the present invention is achieved like this: the present invention adopts microwave discharge, and decomposition reaction gas produces plasma body, because be electrodeless discharge, thereby has avoided the pollution of heated filament, can prepare the higher film of purity.Simultaneously, the ionization level of plasma body is greatly improved, and nitrogen ionic concentration and electronic temp are very high in the plasma body, can improve the nitrogen content of institute's synthetic film.In addition, with the method process stabilizing of microwave generation plasma body, reliable, processing condition easily repeat.Method with the synthetic crystalline phase carbon-nitrogen film material of microwave plasma CVD provided by the invention, to place silica tube through cleaning and surface-treated substrate earlier, feed working gas by a certain percentage, then microwave is fed, thereby make geseous discharge produce the plasma body deposit film.
The present invention is suitable at Si, SiO
2, Pt, Ni, semi-conductors such as Ta, Mo, deposit on the substrate of isolator and conductor material, the reactant gases of feeding is made up of two parts, a kind of is carbonaceous gas, as CH
4, CO, C
2H
2Deng, a kind of is nitrogenous gas, as N
2, NH
3Deng, can also feed complementary gas, as Ar, H
2, He etc.
Microwave plasma CVD method of the present invention is synthesized C
3N
4The step of film is as follows: (1) is earlier with the pre-treatment of substrate process.In the preprocessing process of substrate, substrate need polish and matting, in addition, the platinum substrate can also be made anneal earlier in the protectiveness rare gas element, annealing temperature 800-1000 ℃, time 10-30 minute so that the growing up of the crystal grain of platinum substrate, improve the degree of crystallinity of sedimentary crystalline phase carbon-nitrogen film; Silicon substrate can be handled by cut, adds deionized water for ultrasonic at 0.5-1.0 μ m bortz powder and handles, so that increase the nucleation chance, accelerates sedimentation velocity.
(2) substrate of handling well is placed in the quartzy holder, put into the silica tube of isolated plant of the present invention again, make it be in the central position of microwave process.Carbon pipe in the isolated plant silica tube is vacuumized, and vacuum tightness reaches more than 3 handkerchiefs.
(3) feed working gas, reactant gases is respectively through entering the sediment chamber behind the mass rate control meter.A part is 0.2-5 standard cubic centimeter/per minute (SCCM) for the flow of carbonaceous gas, and the flow of a part of nitrogenous gas is 20-100 standard cubic centimeter/per minute (SCCM).Can also comprise adding complementary gas, flow is 0-80 standard cubic centimeter/per minute (SCCM).
(4) state of adjusting plasma body, the dynamic (dynamical) process of control growing is prepared required crystalline phase selectively.Regulate the size of the extraction valve passage between silica tube and the vacuum pump, make the air pressure in the silica tube working chamber remain on the 15-30 holder.Drive microwave source then, power is 750 watts, and the microwave that produces from the magnetron of microwave generator enters waveguide, through hydrokineter, behind the four screw tuners, arrives the substrate place.The microwave that reflects back is gone into water load and is sponged through hydrokineter is laggard.At the water load place one detector is arranged, can survey the intensity of microwave reflection, thereby reflection enters the power of the microwave of silica tube.Regulate the position of the governor lever on the matching box, making the power that enters the microwave in the silica tube is 300-400W.The ionization working gas produces plasma body, deposits carbon-nitrogen film on substrate.
(5) temperature of substrate is measured by speculum by infrared thermometer, and it is relevant with the air pressure in microwave power that enters the sediment chamber and the sediment chamber, can change by the power that adjusting enters the microwave of silica tube.Substrate temperature remains on 700～950 ℃.
Isolated plant of the present invention is made up of following four major parts:
1, microwave system.Microwave system is by microwave generator (comprising power supply and magnetron), hydrokineter and water load, and tuner, working cavity, short-circuit plunger five parts are formed, and provide and regulate and control microwave required in the deposition process of carbon-nitrogen film.
2, airing system.Airing system is by steam line, and mass flowmeter group control enclosure is formed, and provides growth crystalline phase carbon-nitrogen film required working gas, and controls and measure its flow.
3, vacuum system.By mechanical pump, molecular pump, silica tube, pump-line and valve are formed, the air pressure the when work of vacuum environment and balance is provided.
4, temp measuring system.Form by speculum and infrared thermometer, measure the temperature of substrate.
Quartzy holder wherein is installed in the silica tube, sample is placed on last, the terminal link molecule pump of silica tube of quartzy holder, molecular pump connects with the valve that has mechanical pump, the silica tube upper lateral part has inlet mouth, and installation mass-flow gas meter, a speculum is installed in outside, silica tube top, gives infrared thermometer with infrared reflection in the silica tube.Silica tube one side is settled the working cavity that has short-circuit plunger, and corresponding opposite side is settled microwave system; Microwave system assembles by common mounting means.
The invention has the advantages that:
1, with the surface topography of carbon-nitrogen film on the scanning electron microscopic observation institute synthetic silicon substrate, the result as shown in Figure 2.From the photo as can be seen, with microwave plasma CVD method synthetic carbon-nitrogen film be by evenly, the fine and close crystalline phase granulometric composition that distributes.It is hexagonal crystal bar that most of crystal grain can be recognized, and length is about 2 microns, thick about 0.3 micron, be arranged on the substrate densely, analyzed the composition of these crystal bars with EDX, found that nitrogen carbon atomic ratio N/C changes the nitrogen carbon atomic ratio N/C=1.33 of the crystal bar of regular shape between 1.0～2.0.Figure 3 shows that the EDX spectrum of carbon-nitrogen film on the typical silicon substrate.Wherein the atomic percent of N, C, Si is 42%, 31% and 27%.Silicon is owing to substrate causes.Be deposited on the on-chip carbon-nitrogen film of Pt, its nitrogen carbon atomic ratio is 1.3.
2, the carbon-nitrogen film on the silicon substrate is analyzed with X-ray diffraction.Fig. 4 is a typical X ray diffraction spectra.Except the strong diffraction peak of silicon substrate itself, also has a series of sharp-pointed diffraction peak.Table 1 has been listed figure and has been gone up the 2 θ peak positions of each diffraction peak and the spacing d value of correspondence.For the ease of analyzing, also listed α-C simultaneously
3N
4With, β-C
3N
4And p-C
3N
4The theoretical value of interplanar distance d of each crystal face.At the on-chip carbon-nitrogen film of Pt α-C is arranged also
3N
4With, β-C
3N
4And p-C
3N
4Each crystalline phase exists.From experimental data and theoretical value relatively, the situation that meets of theoretical prediction and experimental result is extraordinary, illustrates in the carbon-nitrogen film of preparation in this way to contain α-C
3N
4, β-C
3N
4And p-C
3N
4The crystalline phase particle.
3, the carbon-nitrogen film on the silicon substrate has been done the Raman spectrum analysis, as shown in Figure 5.Find out from figure, except being positioned at 520cm
-1Outside the strong peak of silicon substrate at place, also have two to lay respectively at 250 and 302cm
-1The raman characteristic peak at place is with the β-C of theoretical calculation
3N
4Characteristic peak meet, β-C has been described
3N
4The chemical bond of type exists.
4, measured the hardness and the bulk modulus of the carbon-nitrogen film on the silicon substrate with nano impress meter (Nano-indentor), the result is respectively 23.9GPa and 200GPa.Young's modulus at the on-chip carbon-nitrogen film of Pt is 349GPa.
5, this method adopts electrodeless discharge, does not therefore pollute institute's synthetic crystalline phase carbon-nitrogen film purity height in preparation process.
6, the device of this method employing is reliable and stable, stable process conditions, good reproducibility.
From above-mentioned analysis to measure result, this microwave plasma CVD can be prepared fine crystalline phase C
3N
4Film.
Table 1No. 2 θ d () (hkl)/d ()
α-C
3N
4 β-C
3N
4 p-C
3N
4 β-Si
3N
4 Si1 9.76 9.1 (001)/9.42 18.52 4.79 (001)/4.713 19.00 4.67 (002)/4.704 21.12 4.20 (100)/4.175 22.72 3.91 (101)/3.816 23.44 3.79 (110)/3.807 27.32 3.26 (110)/3.23 (200)/3.298 28.20 3.16 (111)/3.209 28.96 3.08 (003)/3.1310 33.28 2.69 (111)/2.67 (200)/2.7711 35.60 2.52 (103)/2.50 (210)/2.4912 36.60 2.45 (201)/2.1113 37.92 2.37 (002)/2.3514 39.04 2.31 (004)/2.35 (111)/2.3115 41.08 2.20 (102)/2.1716 41.84 2.157 (101)/2.2117 42.72 2.12 (210)/2.12 (200)/2.1118 44.36 2.04 (210)/2.1019 46.56 1.95 (211)/1.9320 47.04 1.93 (111)/1.92 (202)/1.9121 48.04 1.89 (112)/1.90 (005)/1.88 (220)/1.9022 51.64 1.77 (301)/1.7323 53.56 1.71 (114)/1.6824 56.32 1.63 (220)/1.6225 57.04 1.61 (220)/1.60 (221)/1.5926 58.92 1.57 (212)/1.57 (211)/1.2727 60.12 1.54 (310)/1.55 (310)/1.5428 60.72 1.52 (103)/1.51 (320)/1.5129 62.76 1.479 (311)/1.47530 64.24 1.449 (302)/1.463 (301)/1.465 (106)/1.465 (410)/1.43731 65.36 1.427 (113)/1.412 (401)/1.43332 66.36 1.407 (400)/1.400 (213)/1.40933 69.44 1.352 (400)/1.35734 72.72 1.299 (312)/1.297 (311)/1.29535 75.60 1.257 (213)/1.261 (320)/1.272 (303)/1.271 (330)/1.26736 76.64 1.242 (321)/1.23937 77.52 1.230 (410)/1.222 (410)
21038 94.44 1.049 (403)/1.045 (212)/1.043 (009)/1.043
Below in conjunction with drawings and Examples the present invention is described in further detail:
Description of drawings is as follows: accompanying drawing 1 microwave plasma CVD system and device figure.The C that accompanying drawing 2 is grown on the Si substrate
3N
4The C that the shape appearance figure accompanying drawing 3 of crystalline film is grown on the Si substrate
3N
4The C that the EDX spectrum accompanying drawing 4 of crystalline film is grown on the Si substrate
3N
4The C that one typical X-ray diffraction spectra accompanying drawing 5 of crystalline film is grown on the Si substrate
3N
4One typical Raman spectra caption of crystalline film is as follows: the quartzy holder of 1-microwave generator 2-circulator and water load 3-tuner 4-working cavity 5-short-circuit plunger 6-mass flowmenter 7-quartz ampoule 8-9-vacuum pipe 10-molecular pump 11-valve 12-mechanical pump 13-speculum 14-infrared radiation thermometer
Embodiment 1:
Polishing Si (100) substrate of thick 0.5mm added the deionized water supersound process 20 minutes with bortz powder, with acetone supersound process 10 minutes, placed in the quartz holder of microwave working cavity of isolated plant of the present invention, fed CH
4And N
2, flow is respectively 1.5SCCM and 100 SCCM.Air pressure in the silica tube remains on 20 holders, opens microwave source, and microwave power is at 750W, makes that microwave power is 350W in the silica tube, the ionization working gas produces plasma body, deposit carbon nitrogen film on substrate, substrate temperature remains on 810 ℃, deposits 2 hours, obtains the crystalline phase carbon-nitrogen film.
Embodiment 2:
Preparation process is with embodiment 1, the actual conditions that it changed such as following.Thick 0.5mm, the Pt substrate of 8 * 12mm2 through grinding and polishing, is used acetone supersound process 10 minutes, places the microwave working cavity, feeds CH
4And N
2, flow is respectively 0.7SCCM and 100 SCCM, and the air pressure in the silica tube remains on 20 holders, and substrate temperature remains on 830 ℃, deposits 2 hours, obtains the carbon-nitrogen film of crystalline phase.
Embodiment 3:
Preparation process is got the Ni substrate with embodiment 1, through grinding and polishing, pickling, uses acetone supersound process 10 minutes, places the microwave working cavity, passes through CH
4And N
2, flow is respectively 0.7SCCM and 100SCCM.Operating air pressure is 20 holders, and substrate temperature remains on 850 ℃, deposits 2 hours,
Embodiment 4:
Preparation process with embodiment 1, get thick 0.8mm, 4 * 5mm
2The Ta sheet, through polishing,, place the microwave working cavity with acetone supersound process 10 minutes, feed CH
4And N
2, flow is respectively 0.7SCCM and 100SCCM, and the air pressure in the silica tube remains on 25 holders, and substrate temperature remains on 860 ℃, deposits 2 hours, has obtained containing α-C
3N
4, β-C
3N
4, p-C
3N
4Film with TaC.
Embodiment 5:
Preparation process is got thick 0.2mm, 8 * 12mm with embodiment 1
2Polishing Mo sheet, with acetone supersound process 10 minutes, place the microwave working cavity, feed CH
4And N
2, flow is respectively 0.5SCCM and 100SCCM.Air pressure in the silica tube remains on 18 holders, and substrate temperature remains on 850 ℃, deposits 2 hours, has obtained containing α-C
3N
4, β-C
3N
4, p-C
3N
4Film with MoN.
Embodiment 6:
Preparation process is got 0.8mm with embodiment 1,8 * 5mm
2SiO
2Polishing substrate is used acetone supersound process 10 minutes, places the microwave working cavity, feeds CH
4And N
2, flow is respectively 0.7SCCM and 100SCCM.Air pressure in the silica tube remains on 24 holders, and substrate temperature remains on 810 ℃, deposits 5 hours, has obtained containing α-C
3N
4, β-C
3N
4And p-C
3N
4Film.
Embodiment 7:
Preparation process is got thick 0.5mm, 8 * 5mm with embodiment 1
2Si (100) polishing substrate, handle and acetone supersound process 10 minutes through cut, place working chamber, feeding CH
4, N
2And Ar, flow is respectively 0.7SCCM, and 40SCCM and 60SCCM, operating air pressure remain on 20 holders, and substrate temperature remains on 780 ℃, deposits 2 hours, has obtained containing α-C
3N
4, β-C
3N
4And p-C
3N
4Film.
Embodiment 8:
Preparation process is got thick 0.5mm, 8 * 6mm with embodiment 1
2Si (100) polishing substrate, handle and clean through cut, place the microwave working cavity, feed CO and N
2, flow is respectively 2.5SCCM and 100SCCM, and working gas is 20 holders, and substrate temperature remains on 810 ℃, deposits 2 hours, has obtained containing α-C
3N
4, β-C
3N
4And p-C
3N
4Film.
Claims (6)
1. the method for the synthetic crystalline phase carbon-nitrogen film of a microwave plasma CVD is characterized in that: may further comprise the steps:
(1) adopts Si, SiO
2, Pt, Ta, Mo or Ni semiconductor material, insulating material or conduction
Material is cooked substrate, at first the pre-treatment of substrate through matting, polishing;
(2) the good substrate of pre-treatment is put in the quartz holder of isolated plant of the present invention quartzy holder
Put on the central position that silica tube is in the microwave process, seal close good system, vacuumize and make
Its vacuum tightness reaches more than 3 handkerchiefs;
(3) feed working gas then in silica tube, its working gas comprises that a part is carbon containing
Gas, flow are 0.2-5 standard cubic centimeter/per minute and a part of nitrogenous gas, and flow is
20-100 standard cubic centimeter/per minute;
(4) size of the extraction valve passage between adjusting silica tube and the vacuum pump makes gas in the silica tube
Pressure remains on the 15-30 holder, opens microwave source then, and power is 750 watts, and microwave enters ripple
Lead, through hydrokineter, four screw tuners arrive the substrate place again, enter little in the silica tube
Wave power remains on 300-400W, and the ionization working gas produces plasma body, at substrate
Last deposition growing carbon-nitrogen film;
When (5) the ionization working gas produced plasma body, the temperature of substrate remained on
700-950℃。
2. the method for synthesizing the crystalline phase carbon-nitrogen film by the described microwave plasma CVD of claim 1; it is characterized in that: described substrate pre-treatment also comprises: the Pt substrate is anneal in inert protective gas earlier; its annealing temperature is 800-1000 ℃, time 10-30 minute.
3. the method for synthesizing the crystalline phase carbon-nitrogen film by the described microwave plasma CVD of claim 1, it is characterized in that: described substrate pre-treatment also comprises: its silicon substrate cut is handled, and silicon chip is put into 0.5-1.0 μ m bortz powder and added the deionized water for ultrasonic processing.
4. by the synthetic crystalline phase carbon-nitrogen film method of the described microwave plasma CVD of claim 1, it is characterized in that: described carbon containing working gas comprises CH
4, CO or C
2H
2, described nitrogenous working gas comprises N
2Or NH
3
5. by the synthetic crystalline phase carbon-nitrogen film method of the described microwave plasma CVD of claim 1 to 4, it is characterized in that: also comprise adding assist gas Ar, H
2Or He, it feeds flow is 0-80 standard cubic centimeter/per minute.
6. one kind is used for the isolated plant that the described microwave plasma CVD of claim 1 synthesizes crystalline phase carbon-nitrogen film method, it is characterized in that: by microwave system, airing system, vacuum system, temp measuring system is formed, quartzy holder wherein is installed in the silica tube, sample is placed in the quartzy holder, the terminal link molecule pump of silica tube, molecular pump connects with the valve that has mechanical pump, and the silica tube upper lateral part has inlet mouth, and mass-flow gas meter is installed, a speculum is installed in outside, silica tube top, gives infrared thermometer with infrared reflection in the silica tube; Silica tube one side is settled the working cavity that has short-circuit plunger, and corresponding opposite side is settled microwave system; Microwave system assembles by common mounting means.
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| JP2005526359A (en) * | 2002-05-08 | 2005-09-02 | ダナ・コーポレーション | Plasma support processing method and processing apparatus in production line |
| CN102268655A (en) * | 2011-07-28 | 2011-12-07 | 河南大学 | Preparation method and device of nanocrystalline carbon nitride film |
| CN105752953B (en) * | 2016-01-29 | 2017-11-28 | 张家港市东大工业技术研究院 | Preparation method of graphite phase carbon nitride |
| CN105925954B (en) * | 2016-05-27 | 2020-04-14 | 清华大学 | A kind of preparation method of semiconductor carbon nitride film |
| CN107098321B (en) * | 2017-04-12 | 2019-03-19 | 天津大学 | The method that low temperature plasma prepares two-dimensional structure carboritride |
| CN108165952B (en) * | 2017-12-07 | 2019-11-08 | 三峡大学 | A kind of preparation method of light-transmitting hard carbon nitride film |
| CN108546933A (en) * | 2018-04-20 | 2018-09-18 | 长沙新材料产业研究院有限公司 | A kind of MPCVD synthesis devices, control method and synthetic method |
| CN109092227B (en) * | 2018-08-30 | 2021-06-29 | 长沙新材料产业研究院有限公司 | MPCVD synthesis equipment and control method |
| CN110357631B (en) * | 2019-08-14 | 2021-09-17 | 曾杰 | Method and equipment for preparing silicon carbide component by microwave treatment-based chemical vapor conversion process |
| CN115371940B (en) * | 2022-08-09 | 2025-06-10 | 中国科学院力学研究所 | Scour-resistant platinum film heat flow sensor preparation device |
| CN118156187B (en) * | 2024-05-10 | 2024-07-26 | 鸿舸半导体设备(上海)有限公司 | A control method for a gas path system based on a semiconductor reaction chamber |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03240959A (en) * | 1990-02-16 | 1991-10-28 | Sumitomo Electric Ind Ltd | Method for synthesizing carbon nitride thin film |
| JP3240959B2 (en) * | 1997-06-11 | 2001-12-25 | 株式会社大林組 | Fixing tool for belt-shaped PC tendon |
-
1997
- 1997-12-11 CN CN97121868A patent/CN1078264C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03240959A (en) * | 1990-02-16 | 1991-10-28 | Sumitomo Electric Ind Ltd | Method for synthesizing carbon nitride thin film |
| JP3240959B2 (en) * | 1997-06-11 | 2001-12-25 | 株式会社大林組 | Fixing tool for belt-shaped PC tendon |
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