CN1834288A - Low temp chemical gaseous deposition for preparing silicon nitride thin film - Google Patents
Low temp chemical gaseous deposition for preparing silicon nitride thin film Download PDFInfo
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- CN1834288A CN1834288A CN 200610025537 CN200610025537A CN1834288A CN 1834288 A CN1834288 A CN 1834288A CN 200610025537 CN200610025537 CN 200610025537 CN 200610025537 A CN200610025537 A CN 200610025537A CN 1834288 A CN1834288 A CN 1834288A
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Abstract
This invention relates to a chemical vapor deposition method for manufacturing silicon nitride (SiNx) thin films. The method uses NH3 as nitrogen source, and organic silicon precursor (R1R2N) nSi (R3)4-n as silicon source, wherein R1, R2 = H, CH3, C2H5, C3H7 or C4H9, R3 = H or Cl, and n = 2, 3 or 4. With optimized conditions, the low-pressure chemical vapor deposition method can manufacture uniform, low H and C content and near stoichiometric SiNx thin films at a relatively low reaction temperature. SiNx (x = 1.28-1.33) thin films can be used in semiconductor industry and silicon-based solar cells.
Description
Technical field
The present invention relates to a kind of employing chemical vapor deposition (CVD) and prepare SiN at low temperatures
xThe method of film is more precisely with NH
3Being nitrogenous source, is the silicon source with organosilicon source presoma, adopts low-pressure chemical vapor deposition (LPCVD) technology to prepare SiN at low temperatures
xThe method of film belongs to the semiconductor film field.
Background technology
In semiconductor integrated circuit, be used between the device and wiring between the insulating film of electrical isolation be very important.For improving the stability and the reliability of device performance; must keep apart device and surrounding environment atmosphere; with the blocking capability that enhance device is stain foreign ion, the characteristic on control and stabilization of semiconductor surface, the interconnection of protection device inside and prevent that device is subjected to machinery and chemical damage.Because with Si substrate good interface consistency and preparation easily, SiO
2Film becomes the surface protecting material of using the earliest in unicircuit.With SiO
2Film is compared, SiN
xFilm in anti-diffusion of contaminants (as Na
+) and water vapor permeable ability aspect have remarkable advantages, have simultaneously high disruptive strength, high chemical stability, excellent mechanical property again, thereby become surface passivation material the most excellent in the semiconductor integrated circuit.In addition, in silica-based solar cell, SiN
xFilm can be used as antireflective coating, plays the effect of passivation in surface passivation and the body simultaneously, thereby improves the efficiency of conversion of solar cell.
SiN
xFilm usually can be by chemical vapor deposition (CVD) and two kinds of method preparations of plasma enhanced CVD (PECVD).Wherein the PECVD depositing temperature is low, thereby has obtained significant progress at recent two decades.But the sedimentary SiN of PECVD method
xFilm is normally non-stoichiometric, often contains a large amount of impurity elements, thereby electrical property is not too satisfactory.Along with the develop rapidly of microelectronics, to SiN
xThe electrical property of film is had higher requirement, thereby the hot CVD legal system is equipped with SiN
xFilm comes into one's own again.LPCVD is one of hot CVD method of extensively adopting of semi-conductor industry, and it is big with the load capacity, and particle pollution is little, and homogeneity is high and enjoy favor, becomes preparation SiN
xOne of main method of film.At present, the industrial NH that generally adopts
3-SiH
2Cl
2System is by LPCVD prepared SiN
xFilm, but the deposition reaction temperature is generally more than 750 ℃.Too high temperature of reaction tend to cause lattice imperfection in the Si sheet growth, spread the distribution again with impurity, and be heated stress and produce serious warpage etc., therefore carrying out cryogenic hot CVD technology prepares SiN
xFilm has crucial meaning.
Silicon sources such as general silane or silicon halogen compounds are difficult to realize SiN being lower than under 800 ℃ the temperature
xDepositing of thin film, this just makes hot CVD be greatly limited in the application in semiconductor microelectronics field.And adopt organic precursor can under relatively low temperature, realize SiN usually
xTherefore depositing of thin film is developed new Si source, N source presoma comes into one's own in recent years.People such as R.G.Gordon (R.G.Gordon, et al., Silicon dimethylamido complexes andammonia as precursors for atmospheric pressure chemical vapor deposition ofsilicon nitride thin films, Chem.Mater., 1990,2:480-482.) with Si[N (CH
3)
2]
nH
4-n(n=2-4) be the Si source, adopt atmospheric pressure cvd (APCVD) technology, prepare the SiN that H content is about 8-10at.% at 750 ℃
xFilm.People such as J.M.Grow (J.M.Grow, et al., Grow kinetics and characterizationof low pressure chemically vapor deposited Si
3N
4Films from (C
4H
9)
2SiH
2And NH
3, Maters Letters, 1995,23:187-193.) reported with (C
4H
9)
2SiH
2Be the Si source, adopt LPCVD technology, under 600-700 ℃ temperature of reaction, prepare SiN
xThe research of film, prepared SiN
xFilm contains the C of 10at.% approximately, in addition, also contains the certain amount of H element in the film.Similarly, people such as R.A.Levy (R.A.Levy, et al., Lowpressure chemical vapor deposition of silicon nitride using the environmentallyfriendly tris (dimethylamino) silane precursor, J.Mater.Res., 1996,11:1483-1488.) reported with [(CH
3)
2N]
3SiH is the Si source, adopts LPCVD technology, prepares SiN under 650-800 ℃ temperature of reaction
xThe research of film, prepared SiN
xFilm contains the C of 5at.% approximately.Adopt the prepared SiN of these methods
xC or H that film all contains in various degree pollute.
Summary of the invention
The object of the present invention is to provide a kind of SiN for preparing at low temperatures
xThe method of film.Preparation SiN provided by the invention
xThe method of film is with NH
3Be the N source, with organosilicon source presoma (R
1R
2N)
nSi (R
3)
4-nBe Si source (R wherein
1, R
2=H, CH
3, C
2H
5, C
3H
7Or C
4H
9R
3=H or Cl; N=2,3 or 4), adopt LPCVD technology, in operating pressure is 20-300Pa, and substrate temperature is under 600-900 ℃ the condition, to pass through process optimization, can be under relatively low temperature of reaction, the Si substrate surface prepare form and thickness uniformly, hang down H and SiN C content, near-stoichiometric
xFilm.
The objective of the invention is specifically to implement by following technological process:
1. the device of Shi Yonging
With the hot wall type tubular diffusion furnace of low pressure reaction system, temperature control precision ± 1 ℃.
2. the raw material of Shi Yonging
With electronic-grade NH
3Be the N source, with organosilicon source presoma (R
1R
2N)
nSi (R
3)
4-nBe Si source (R wherein
1, R
2=H, CH
3, C
2H
5, C
3H
7Or C
4H
9R
3=H, Cl; N=2,3,4), with high-purity N
2, H
2, Ar or He be carrier gas, is used for the diluting reaction raw material, conditioned reaction system total pressure.
3. prepare SiN
xThe processing condition of film
Uprightly be inserted in the silicon chip (silicon single crystal or polysilicon chip) of cleaning on the quartz boat, 50-100 the silicon chip of at every turn can packing into, equidistantly place, pitch of fins 5-20mm, the quartz boat that installs is positioned over the diffusion furnace middle position, is evacuated to below the 0.5Pa, adopt the thermocouple measurement temperature with vacuum pump, substrate temperature is controlled at 600-900 ℃, and the best is 650-800 ℃.For guaranteeing the homogeneity of deposit film, make diffusion furnace radially produce a thermograde, temperature gradient is 10-30 ℃, the best is 15-25 ℃.N, Si source raw material are introduced reaction system respectively from the inlet end of reactor, and wherein the source bottle of organosilicon source presoma and conveying pipe thereof adopt 50-200 ℃ insulation measure, with carrier gas (N
2, H
2, Ar or He) introduce via the exit end of diffusion furnace, in order to the total pressure of conditioned reaction system.The flow of all raw materials is regulated by mass flowmeter, and reaction system is that the total pressure of diffusion furnace is measured by vacuumometer, and the total pressure of reactive system is 20-300Pa, and the best is 50-100Pa.The mol ratio of N, Si source raw material is not less than 3: 1, and the best is 6 ~ 8: 1.
Under optimized process conditions, through deposition after a while, can obtain in the sheet and sheet between form and thickness aspect uniformly, hang down H and SiN C content, near-stoichiometric
xFilm.
Preparation SiN provided by the invention
xThe method of film has fairly obvious advantage.Adopting new organic Si source presoma is raw material, by LPCVD technology, can be under relatively low temperature of reaction, and evenly (ununiformity is not more than 10% aspect composition and thickness in the preparation slice and between sheet; Best, be not more than 5%), (H content is not more than 5at.% to low H content; Best, be not more than 3.5%), (C content is not more than 5at.% to low C content; Best, be not more than 2%), near-stoichiometric (x=1.28 ~ 1.33; Best, SiN x=1.30 ~ 1.31)
xFilm.The SiN of preparation
xFilm can be used for the surface encapsulation of various surface passivation protective membranes, insulation layer, diffusion of contaminants mask and semiconductor element in microelectronic material and the device production etc.In addition, can be used as the antireflective coating of silica-based solar cell, to improve the efficiency of conversion of solar cell.
Description of drawings
Fig. 1: the preparation SiN that the present invention uses
xThe LPCVD device of film.
Fig. 2: the SiN that presses embodiment 1 preparation
xThe FTIR collection of illustrative plates of film.
Fig. 3: the SiN that presses embodiment 1 preparation
xThe AES degree of depth composition analysis collection of illustrative plates of film.
Fig. 4: the SiN that presses embodiment 1 preparation
xThe refractive index curve of film.
Fig. 5: the SiN that presses embodiment 1 preparation
xThe atomic force microscope surface topography photo of film.
Embodiment
Below example be in order to further specify the present invention, but limit the present invention by no means.
Embodiment 1
2 inches monocrystalline silicon piece (p types with cleaning, 110) uprightly be inserted on the quartz boat, 80 silicon chips of once packing into, equidistantly place, pitch of fins 8mm, the quartz boat that installs is positioned over the middle position of the described hot wall type tubular type of Fig. 1 quartz reactor, open vacuum pump, be evacuated to below the 0.5Pa, reactor middle position temperature is that substrate temperature is 700 ℃, and for improving the homogeneity of deposit film, making the import of resistance heading furnace (being aforementioned diffusion furnace) and the thermograde of outlet is 20 ℃, temperature controls to ± 1 ℃ after, can begin deposition.With electronic-grade high-purity N H
3For the N source, with [(C
2H
5)
2N]
3SiCl is the Si source, and the two flow is respectively 80,10sccm, adopts high-purity N
2(99.999%) for carrier gas is used for regulation system pressure, the total pressure of reaction system is 80Pa, continues vacuum is evacuated to below the 0.5Pa after deposition finishes, and feeds N
2Can take out sample to normal pressure.Adopt ellipsometer test to measure SiN
xThe thickness of film and specific refractory power, SiN
xDepositing of thin film speed can calculate by the thickness that records.Adopt fourier infrared (FTIR) and Auger photoelectron spectrum (AES) to analyze SiN respectively
xThe chemical constitution of film.Adopt atomic force microscope observation SiN
xThe surface topography of film.
Under above-mentioned processing condition, SiN
xDepositing of thin film speed is about 12 /min.Film thickness measuring shows the SiN that deposits
xUnuniformity in the sheet of film＜5%, ununiformity between sheet＜8%.Prepared SiN
xOnly present very faint N-H stretching vibration (3330cm in the FTIR collection of illustrative plates (Fig. 2) of film
-1) and Si-H stretching vibration absorption (2160cm
-1), show that the H content in the film is very low.Further the method that adopts elastic recoil to survey is come the elastic recoil H atomic spectrum of MEASUREMENTS OF THIN, and the line electric charge of collecting on the sample comes the normalizing power spectrum, is benchmark with standard model (the Si sheet of hydrogeneous 2.7at%), can obtain prepared SiN under these processing condition
xThe content of H is about 3.0at% in the film.At 837cm
-1The strong absorption peak that produces shows the formation of Si-N key, and the peak shape of its broad illustrates that this film is a non-crystalline state.What AES (Fig. 3) depth analysis showed preparation is to form SiN uniform along depth direction, near-stoichiometric
xFilm (x=1.31).Do not occur the characteristic peak of C and O in the AES collection of illustrative plates, show prepared SiN
xDo not contain C and O in the film, perhaps the content of the two all is lower than limit of detection.Refractive index curve (Fig. 4) shows prepared SiN
xThe specific refractory power of film at the 632nm place is 1.935.AFM surface topography photo (Fig. 5) shows prepared SiN
xFilm surface is even, smooth.
Embodiment 2
With high-purity N H
3For the N source, with (C
2H
5NH)
3SiCl is the Si source, and the two flow is respectively 80,10sccm, and reactor middle position temperature is 680 ℃, and all the other are with embodiment 1.Prepared SiN
xThe content of H is about 4.2at% in the film, the SiN of nearly chemical dose
xDo not contain C and O in the film (x=1.30).
Embodiment 3
With high-purity N H
3For the N source, with [(C
3H
7)
2N]
2SiH
2Be the Si source, the two flow is respectively 80,10sccm, and reactor middle position temperature is 750 ℃, and all the other are with embodiment 1.Prepared SiN
xThe content of H is about 5.3at% in the film (x=1.28), does not contain C and O.
Embodiment 4
With high-purity N H
3For the N source, with [(CH
3)
2N]
4Si is the Si source, and the two flow is respectively 70,10sccm, and reactor middle position temperature is 720 ℃, and all the other are with embodiment 1.Prepared SiN
xThe content of H is about 2.5at% in the film (x=1.31), does not contain C and O.
Claims (10)
1, a kind of low temperature chemical vapor deposition prepares SiN
xThe method of film adopts the hot wall type tubular diffusion furnace with lp system, it is characterized in that with NH
3For the N source, with (R
1R
2N)
nSi (R
3)
4-nThe organosilicon presoma be the Si source, R in the formula
1, R
2=H, CH
3, C
2H
5, C
3H
7, or C
4H
9, R
3Be H or Cl, n=2,3 or 4, with N
2, H
2, a kind of as carrier gas among Ar and the He; Under 20-300pa work total pressure, substrate temperature is under the 600-900 ℃ of condition, prepares the SiN of nearly chemical dose at the Si substrate surface
xFilm.
2, prepare SiN by the described low temperature chemical vapor deposition of claim 1
xThe method of film is characterized in that described Si substrate is a kind of in silicon single crystal or the polysilicon.
3, prepare SiN by claim 1 or 2 described low temperature chemical vapor depositions
xThe method of film is characterized in that the Si substrate uprightly is inserted on the quartz boat, equidistantly places, and a pitch of fins is 5-20mm, again quartz boat is positioned over the diffusion furnace middle position, and the silicon chip number is the 50-100 sheet.
4, prepare SiN by the described low temperature chemical vapor deposition of claim 1
xThe method of film is characterized in that diffusion furnace radially produces one 10-30 ℃ temperature tonsure.
5, prepare SiN by the described low temperature chemical vapor deposition of claim 1
xThe method of film is characterized in that the diffusion furnace total pressure is 50-100Pa.
6, prepare SiN by the described low temperature chemical vapor deposition of claim 1
xThe method of film is characterized in that substrate temperature is 650-800 ℃.
7, prepare SiN by the described low temperature chemical vapor deposition of claim 4
xThe method of film is characterized in that diffusion furnace thermograde radially is 15-25 ℃.
8, prepare SiN by the described low temperature chemical vapor deposition of claim 1
xThe method of film is characterized in that the mol ratio in described N source and Si source is not less than 3: 1.
9, prepare SiN by the described low temperature chemical vapor deposition of claim 8
xThe method of film, the mol ratio that it is characterized in that described N source and SSi source is 6～8: 1.
10, prepare SiN by the described low temperature chemical vapor deposition of claim 1
xThe method of film is characterized in that prepared SiN
xFilm is near stoichiometric, x=1.28～1.33.
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|---|---|---|---|
| CN 200610025537 CN1834288A (en) | 2006-04-07 | 2006-04-07 | Low temp chemical gaseous deposition for preparing silicon nitride thin film |
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|---|---|---|---|
| CN 200610025537 CN1834288A (en) | 2006-04-07 | 2006-04-07 | Low temp chemical gaseous deposition for preparing silicon nitride thin film |
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Family
ID=37002183
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