CN101104925A - Method for chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma - Google Patents
Method for chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma Download PDFInfo
- Publication number
- CN101104925A CN101104925A CNA2007100185188A CN200710018518A CN101104925A CN 101104925 A CN101104925 A CN 101104925A CN A2007100185188 A CNA2007100185188 A CN A2007100185188A CN 200710018518 A CN200710018518 A CN 200710018518A CN 101104925 A CN101104925 A CN 101104925A
- Authority
- CN
- China
- Prior art keywords
- gas
- source gas
- chamber
- silicon nitride
- nitride film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a low-temperature manufacturing method of silicon nitride film used in passivation layer of an integrated circuit. The silicon nitride film grows on a substrate positioned inside a deposition chamber. The method comprises cleaning the substrate and placing inside the working chamber, vacuumizing the working chamber and presetting working conditions, introducing a mixed gas composed of silicon source gas and nitride source gas into the working chamber, performing ionization and decomposition of the mixed gas with the action of energy absorbed from a microwave source upon electron cyclotron resonance effect, transferring active charged particles produced by the ionization and decomposition to the surface of the substrate with the action of permanent magnetic field, and depositing silicon nitride film on the substrate. The working conditions are as follows: working chamber pressure: 0.1-5Pa, microwave power: 600-2000W, deposition temperature: room temperature to 300 DEG C, total gas flow: 50-300sccm, flow ratio of silicon source gas to nitride source gas: 1:6 to 1:12, and substrate rotation speed: 60 r/min. The inventive method can rapidly and uniformly deposit the low-hydrogen silicon nitride film (6 inch thickness) at low temperature (below 300 DEG C), which is used as a material for passivation layer of integrated circuit or optical devices.
Description
Technical field
The invention belongs to microelectronics technology, relate to the semiconductor integrated circuit manufacturing, particularly a kind of nonthermal plasma chemistry gas-phase deposition method that relates to the silicon nitride film that is used for the unicircuit passivation layer.
Background technology
Silicon nitride material is one of dielectric material of widespread use in the Micrometer-Nanometer Processing Technology.Silicon nitride has higher dielectric constant and specific refractory power, can be used as the gate medium of Metal-oxide-semicondutor MOS device or is applied in the development or manufacturing process of optics; Silicon nitride also has higher density simultaneously, can effectively stop the pollution of tramp material, can be used as diffusion impervious layer and device passivation layer in integrated circuit technology.
Silicon nitride film in the unicircuit is to use known technology to form as chemical vapour deposition CVD.In CVD technology, the reactant gases and the carrier gas of given composition and flow are introduced in the reaction chamber by air-path control system.Gas molecule transports to substrate, and is attracted to substrate surface, through behind surface transport and the film forming chemical reaction on substrate deposition film, for example silicon nitride.The reactant gases by product then also finally is drawn out of reaction chamber by band from substrate surface.The motivating force of film forming chemical reaction can be supplied with by several method usually, for example heat, light, radio frequency, catalyzer or plasma body.Conventional CVD system generally includes gas source, gas circuit, gas flow controller, reaction chamber, temperature sensor vacuum measuring device, power source, substrate bias, heating and swivel arrangement etc.Existing chemical vapor shallow lake method mainly contain following several in:
1. low pressure chemical vapor deposition LPCVD method.This method is usually used in the dielectric film deposit of front end production technique, and it uses silane SiH
4With ammonia NH
3Be precursor gas, can the good silicon nitride film of processability under 800 ℃～900 ℃ temperature, but this technology can't satisfy in integrated circuit back-end technology and some photoelectric device and other device technologies high technology temperature is no more than 450 ℃, promptly is lower than the fusing point of aluminium, even lower requirement.Simultaneously, LPCVD prepares temperature too high in the silicon nitride film process can produce higher stress, may cause the degeneration of the device reliability that is caused by stress, as phenomenons such as medium layer peel off.In addition, high temperature also can cause the secondary diffusion of impurity, thereby influence is to the isoparametric accurate control of transistor junction depth.More than these aspects all limited the application that the LPCVD method prepares silicon nitride film.
2. Chang Gui plasma reinforced chemical vapor deposition PECVD method.This method prepares silicon nitride film under 300 ℃～400 ℃ temperature.But owing to be difficult to ionization N
2Deng not hydrogenous source gas in nitridation, generally use SiH
4And NH
3As precursor gas, the film hydrogen richness of deposit is about 9%～30%, and deposition rate is lower, generally is lower than 100nm/min, and interface state density is higher, causes the degeneration of device performance and reliability easily.
3. electron cyclotron resonace ecr plasma chemical vapour deposition.This method is a kind of Special Circumstances of CVD technology, when equaling electron gyro-frequency, the microwave frequency of input resonates, microwave energy is coupled to electronics, the electron ionization neutral gas molecule that obtains energy forms plasma discharge, and makes the high reactivity composition in the plasma body form thin-film deposition at substrate surface.When microwave frequency is 2.45 * 10
9During hertz, reach magnetic induction density B=0.0875 tesla of electron cyclotron resonace.It is low that ecr plasma has an operating air pressure, the density height, the ionization level height, big area is even, processing unit is simple, but steady running and parameter are easy to advantages such as control, can realize the free of contamination surface treatment of efficient cryogenic, at thin-film deposition, huge application potential is arranged in the IC manufacturing process such as plasma etching, but because the normal ammonia of easy ionization that adopts of existing ecr plasma chemical gaseous phase deposition of silicon nitride passive film is as precursor gas, the film hydrogen content of deposit is higher, influenced the performance of film, and the more difficult ionization of not hydrogenous source gas in nitridation causes the deposition rate of film low, far below 100nm/min; When the chip area increase, deposit homogeneity and repeatability are difficult to guarantee; And ECR equipment also mostly is current coil type magnetic field, and it is higher to consume energy; Ecr plasma chemical gaseous phase deposition of silicon nitride film processing method is still waiting to improve at present.
The content of invention
The method that the purpose of this invention is to provide a kind of chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma, existing silicon nitride film high temperature preparation, deposition rate are low to overcome, large-area uniformity difference and the higher defective of hydrogen richness, are implemented in the integrated circuit technology grown silicon nitride film as diffusion impervious layer and device passivation layer or be applied to some optics manufacturing process.
The technical scheme that realizes the object of the invention is to utilize electron cyclotron resonace ecr plasma chemical vapor deposition apparatus ECRCVD to form silicon nitride film on the substrate of deposition chamber, and specific embodiment is as follows:
To be placed in the chamber after the substrate cleaning;
Chamber is vacuumized;
Set processing condition, promptly
The pressure of chamber: remain on 0.1Pa～5Pa;
Microwave power: be controlled at 600W～2000W;
Deposition temperature: be controlled at room temperature～300 ℃ scope;
Total gas flow rate: 50～300sccm;
The throughput ratio of silicon source gas and source gas in nitridation: 1: 6～1: 12;
Speed of rotation remains 60 rev/mins.
Silicon source gas and source gas in nitridation are mixed the back mutually to feed in the chamber;
Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb carries out the ionization decomposition to mixed silicon source gas and source gas in nitridation, and the effect by permanent magnetic field of active charged particle that the back produced is decomposed in ionization be transported to substrate surface, deposition silicon nitride film on substrate.
The preferred technical solution of the present invention comprises following process:
To be placed in the chamber after the substrate cleaning;
Chamber is vacuumized;
Set processing condition, promptly
The total pressure of chamber: 1Pa;
Microwave power: 1200W;
Deposition temperature: 200 ℃;
Total gas flow rate: 150sccm;
The throughput ratio of silicon source gas and source gas in nitridation: 1: 8;
Speed of rotation remains 60 rev/mins.
Silicon source gas and source gas in nitridation are mixed the back mutually to feed in the chamber;
Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb carries out the ionization decomposition to mixed silicon source gas and source gas in nitridation, and the effect by permanent magnetic field of active charged particle that the back produced is decomposed in ionization be transported to substrate surface, deposition silicon nitride film on substrate.
The method of above-mentioned chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma, wherein silicon source gas is elected as with 95% the Ar gas SiH as carrier gases dilute
4Source gas in nitridation is elected N as
2
The present invention has following advantage:
(1) to compare deposition temperature low for the present invention and existing LPCVD method, i.e. deposition silicon nitride film at room temperature;
(2) compare with the ECRCVD method with existing PECVD, the present invention is owing to adopt not hydrogenous N
2As precursor gas and adopt microwave power input more than the 600W to make SiH
4The abundant ionization of gas, so the silicon nitride film of deposit do not contain hydrogen substantially, promptly hydrogen richness can't detect under NEXUS 750 infrared spectrometer detection sensitivities;
(3) the silicon nitride film specific refractory power of deposit of the present invention and chemical structure approach to adopt the silicon nitride film of LPCVD method deposit;
(4) thin-film deposition speed of the present invention can reach 140nm/min, and homogeneity and repeatability are better than 95%.
Below by accompanying drawing purpose of the present invention and embodiment are described in further detail.
Description of drawings
Fig. 1 is the ECRCVD device structure synoptic diagram that the present invention is used to form silicon nitride film;
Fig. 2 is the gas circuit structure synoptic diagram of the ECRCVD equipment that uses of the present invention;
Fig. 3 is a process flow sheet of the present invention;
Fig. 4 is the change curve of the deposition rate of silicon nitride film of the present invention with microwave power;
Fig. 5 is the change curve of the deposition rate of silicon nitride film of the present invention with gas flow ratio;
Fig. 6 is the change curve of the specific refractory power of silicon nitride film of the present invention with gas flow ratio;
Fig. 7 is the change curve of the specific refractory power of silicon nitride film of the present invention with microwave power;
Fig. 8 is the change curve of the silicon nitride film specific refractory power of the present invention's deposit under differing temps with gas flow ratio;
Fig. 9 is the change curve of the chemical ingredients of silicon nitride film of the present invention with microwave power and gas flow ratio;
Figure 10 is the chemical structure and the H content infrared analysis figure of the silicon nitride film of deposit of the present invention.
Embodiment
Whole deposition process of the present invention is finished on ECRCVD equipment shown in Figure 1.
With reference to Fig. 1, the ECRCVD equipment of realizing the inventive method by microwave power source and transmission system 21, ecr plasma source 22, chamber 23, pass chip system 24, vacuum system 25, air-channel system 26, microcomputer control system 27 etc. automatically and partly form.Wherein:
Described microwave power source and transmission system 21 provide stable microwave energy for ecr plasma source 22, and microwave frequency is 2.45 * 10
9Hertz, microwave power is adjustable controlled in 0 to 3 kilowatt scope.It partly is made of microwave power source 201, hydrokineter 202, water load 203, resistance dynamometer 204, directional coupler 205, load tuner 206 etc.Microwave power source adopts WY50002-1C type continuous microwave power source.BJ-26 rectangular waveguide 207 is adopted in microwave transmission, by three pin tuners 206 and short-circuit plunger 208 regulating load coupling and reflective powers.The microwave transmission loop comprises a waveguide-coaxial converter 209, coaxial waveguide that is made of the outer conductor of the inner wire of external diameter 21mm and internal diameter 49mm is extended to the coaxial-type resonator 211 that tapered tube 210 and are made of the outer conductor of the inner wire of external diameter 304mm and internal diameter 344mm with 45.2.45 * 10
9Near the Al of the microwave of the hertz transmission loop is incorporated into the resonator opening surface
2O
3On the ceramic window 220.The thick 13.3mm of this ceramic window, diameter 266mm, its lower surface have an O type rubber seal 221, the vacuum-sealing of double as discharge chamber.The ceramic window upper surface has distributed permanent magnet steel system, and this system is made up of magnetism-free stainless steel disk 222, soft iron shielding slab 223 and Nd-Fe-B permanent magnetic steel 224.Permanent magnetic steel 224 is embedded on the magnetism-free stainless steel on the disk 222, is covered by soft iron shielding slab 223 on it.Microwave is transported to the center by the outer rim of ceramic window 220, thereby forms uniform surface-duided wave electric field distribution on ceramic window 220 surfaces of discharge chamber one side, under the effect in this electric field and magnetic field, has formed even heavy caliber ecr plasma in the discharge chamber.
Described ecr plasma source 22 is the microwave electron cyclotron resonance plasma source, and the magnetic field in this plasma body source is distributed permanent magnetic field.
Described chamber 23 is the cavitys that carry out thin-film deposition processing, and its inside comprises process gas ring 231, sample table 232 and other annex etc.Process gas ring 231 inboards are the pore of 0.5mm with 30 ° of equally distributed apertures of angular interval; The maximum finish size of sample table 232 is 6 inches of Φ, the wafer that provides groove to hold 2 inches, 3 inches and 4 inches simultaneously, and required temperature of technology and mechanical support are provided; Reaction chamber water cooling system 233 makes ceramic window 220 remain on the lower temperature; Langmuir probe diagnositc system 234 is measured the plasma discharge parameters, and with quartz plate, quartz tube and grounded bracket as plasma shield so that plasma body be confined to around the print, not shown among Fig. 1; Substrate heating system 235 adopts sealing resistive heating modes that print is heated, and adopts thermopair to carry out temperature survey, carries out the setting and the controlled temperature of temperature with computer, and span of control is room temperature～300 ℃ ± 1 ℃ of precision; Sample table rotation and lifting system 236 adopts no magnetic mode of connection, makes the sample table uniform rotation, controls the height location of sample table in chamber simultaneously.In an one exemplary embodiment, the sample table height be controlled in apart under the ceramic window 3 centimetres to 15 centimeters, be preferably 5 centimeters, the sample table speed of rotation is 60 rpms.
Described automatic biography chip system 24 is a core with the GB3 type vacuum mechanical-arm that U.S. Genmark company produces, can be 10
-6The high vacuum state of handkerchief is work down, and its radial accuracy is 0.05 millimeter, and axially precision is 0.025 millimeter, and angle precision is 0.015 °, and terminal transfer blade length is 345.5 millimeters, 580 millimeters of ranges, the maximum rising 12.5 millimeters.After finishing deposit, the plummer lifting assembly in the sample table is made of the about 3 inches pallet of thin bar and diameter that is threaded, and makes wafer rise to ceramic window below 5 centimeters by ceramic window below 7 centimeters; Open rectangle valve 241 then, transfer blade enters reaction chamber 23 with cantilevered fashion by rectangle valve 241, thereby control plummer lifting assembly descends and makes the wafer on the sample table drop on transfer blade, be ceramic window below 5.2 centimeters, loading finishes the back transfer blade by automatic the biography in the sheet chamber 24 of rectangle valve 241 withdrawals, and rectangle valve 241 cuts out.From automatic biography sheet chamber, get process that new wafer puts into chamber before the deposit in contrast.
Described vacuum system 25 provides high base vacuum degree, suitable pumping speed and reaction pressure for chamber, air-channel system, biography chip system, be made up of turbomolecular pump 252, oilless vacuum pump 254, gamut vacuumometer 256, plate valve 251, segregaion valve 255, magnetic valve 253, pipeline and biography chip system prechamber and air-channel system 257, its base vacuum degree should reach 1 * 10
-5Handkerchief, the technology dynamic vacuum is 1 * 10
-2In 10 handkerchief scopes.Vacuum measurement system 256 adopts thermocouple rule and ionization gauge bonded method to measure the vacuum tightness of reaction chamber, and useful range is 10
-5Handkerchief is to 10 handkerchiefs.
Described air-channel system 26 is finished the required working gas of processing unit, reactant gases and purge gas, as input, measurement and the control of nitrogen.Air-channel system is established 6 tunnel gas circuits altogether, partly form by reacting gas source 301, reducing valve 302, pressure demonstration 310, magnetic valve 303, electromagnetism 305, electromagnetism 306, electromagnetism 308 and electromagnetism 311, mass flow controller 304, mixed gas tank 307, purge gas source 309 and stainless steel pipeline etc. respectively, as shown in Figure 2.Before the thin-film deposition, reactant gases in the source of the gas 301 is entered in the mixed gas tank 307 by mass flowmeter 304 controls behind decompress(ion) valve 302 decompress(ion)s, and the pressure of gas circuit node is read by pressure display unit 310, this moment, magnetic valve 303 and electromagnetism 305 were opened, and electromagnetism 306, electromagnetism 311 and electromagnetism 308 are closed.Opening magnetic valve 308 during deposit gets final product.Source of the gas 309 is a purge gas source, opens magnetic valve 311 and closes other source of the gas and can clean gas circuit.Other source of the gas and corresponding gas circuit thereof are identical with above-mentioned source of the gas 301 and corresponding gas circuit control mode thereof.
Described microcomputer control system 27 adopts/lower computer network structure control mode.Because the network structure control mode is distributed to different control units with control task, microcomputer and control unit are realized by the RS485 interface.Upper computer is selected for use and is ground magnificent IPC-6811 industrial control computer, and switchboard adopts the RS-485 interface board to constitute.The Controlling System software platform adopts Windows98, and control software adopts the visualized graphs interface of VB exploitation.
The present invention utilizes process that above-mentioned electron cyclotron resonance plasma equipment carries out chemical gaseous phase deposition of silicon nitride film as shown in Figure 3, and according to the difference of setup parameter, the present invention can be listed below different embodiment:
It is that p (100) monocrystalline silicon piece of Φ 150mm is as substrate that the present invention selects substrate for use.
The first step is cleaned substrate and is put into chamber.
With 4: 1 H of silicon chip immersion
2SO
4: H
2O
2Solution cleaned 10 minutes, and solution temperature is 90 ℃; Washed with de-ionized water 5 minutes comprises 6 circulations; With 5: 1: 1 H of silicon chip immersion
2O: H
2O
2: cleaned 10 minutes in the HCl solution, solution temperature is 70 ℃; Washed with de-ionized water comprised 6 circulations in 5 minutes; Silicon chip is immersed in 50: 1 the HF solution 15 to 30 seconds; Washed with de-ionized water comprised 6 circulations in 5 minutes; Rotation under the nitrogen atmosphere protection dries to be handled, promptly 80 seconds washed with de-ionized water, and rotation in 120 seconds dries.Clean the back and obtain the surface by the saturated clean silicon surface of H key.Silicon chip after cleaning is placed on the sample table 232 in the chamber 23.
In second step, chamber is vacuumized.
Open oilless vacuum pump and molecular pump and related valve successively, chamber is vacuumized, make the base vacuum degree reach 1.0 * 10
-5Pa.
In the 3rd step, set processing condition respectively.
1. substrate temperature is set at room temperature;
2. total gas flow rate is 50sccm, and gas flow ratio is 1: 6;
3. the pressure of chamber is set at 0.1Pa;
4. the sample table speed of rotation is 60 rpms;
5. microwave power is 600W, and the microwave discharge time is 10 seconds.
In the 4th step, feed mixed gas.
Close the magnetic valve that mixes gas tank and chamber junction, open each source of the gas respectively and lead to magnetic valve and the under meter that mixes in the gas tank gas circuit branch, silicon source gas and source gas in nitridation are flowed into simultaneously mix mixes more than 5 seconds in the gas tank after, first in feeding mixed gas in chamber 23 silicon source gas is mixed mutually with source gas in nitridation.
The 5th step, deposition silicon nitride film on substrate.
Open rotation control, make the substrate uniform rotation; Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb decomposes mixed silicon source gas and source gas in nitridation, and the effect by permanent magnetic field of active charged particle that the back produced is decomposed in ionization be transported to substrate surface, deposition silicon nitride film on substrate, but controlled microwave goes out the silicon nitride film that thickness is 100 dusts deposit in 10 seconds discharge time.
The 6th step, the purification process chamber.
After deposit is finished, close source gas, feed nitrogen pipeline and chamber 23 are purified.
Embodiment 2
It is that p (100) monocrystalline silicon piece of Φ 150mm is as substrate that the present invention selects substrate for use.
The first step is cleaned substrate and is put into chamber.
With 4: 1 H of silicon chip immersion
2SO
4: H
2O
2Solution cleaned 10 minutes, and solution temperature is 90 ℃; Washed with de-ionized water 5 minutes comprises 6 circulations; With 5: 1: 1 H of silicon chip immersion
2O: H
2O
2: cleaned 10 minutes in the HCl solution, solution temperature is 70 ℃; Washed with de-ionized water comprised 6 circulations in 5 minutes; Silicon chip is immersed in 50: 1 the HF solution 15 to 30 seconds; Washed with de-ionized water comprised 6 circulations in 5 minutes; Rotation under the nitrogen atmosphere protection dries to be handled, promptly 80 seconds washed with de-ionized water, and rotation in 120 seconds dries.Clean the back and obtain the surface by the saturated clean silicon surface of H key.Silicon chip after cleaning is placed on the sample table 232 in the chamber 23.
In second step, chamber is vacuumized.
Open oilless vacuum pump and molecular pump and related valve successively, chamber is vacuumized, make the base vacuum degree reach 1.0 * 10
-5Pa.
In the 3rd step, set processing condition respectively.
1. substrate temperature is set at 300 ℃;
2. total gas flow rate is 300sccm, and gas flow ratio is 1: 12;
3. the pressure of chamber is set at 5Pa;
4. the sample table speed of rotation is 60 rpms;
5. microwave power is 2000W, and the microwave discharge time is 10 seconds.
In the 4th step, feed mixed gas.
Close the magnetic valve that mixes gas tank and chamber junction, open each source of the gas respectively and lead to magnetic valve and the under meter that mixes in the gas tank gas circuit branch, silicon source gas and source gas in nitridation are flowed into simultaneously mix mixes more than 5 seconds in the gas tank after, first in feeding mixed gas in chamber 23 silicon source gas is mixed mutually with source gas in nitridation.
The 5th step, deposition silicon nitride film on substrate.
Open rotation control, make the substrate uniform rotation; Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb decomposes mixed silicon source gas and source gas in nitridation, and the effect by permanent magnetic field of active charged particle that the back produced is decomposed in ionization be transported to substrate surface, deposition silicon nitride film on substrate, but controlled microwave goes out the silicon nitride film that thickness is 290 dusts deposit in 10 seconds discharge time.
The 6th step, the purification process chamber.
After deposit is finished, close source gas, feed nitrogen pipeline and chamber 23 are purified.
Embodiment 3
It is that the quartz plate of Φ 10mm is as substrate that the present invention selects substrate for use.
The first step is cleaned substrate and is put into chamber.
Quartz plate was cleaned 20 minutes with acetone tide sound; Comprised 6 circulations in 5 minutes with washed with de-ionized water; Rotation under the nitrogen atmosphere protection dries to be handled, promptly 80 seconds washed with de-ionized water, and rotation in 120 seconds dries.Quartz plate after cleaning is placed on the sample table 232 in the chamber 23.
In second step, chamber is vacuumized.
Open oilless vacuum pump and molecular pump and related valve successively, chamber is vacuumized, make the base vacuum degree reach 1.0 * 10
-5Pa.
In the 3rd step, set processing condition respectively.
1. substrate temperature is set at 200 ℃;
2. total gas flow rate is 150sccm, and gas flow ratio is 1: 8;
3. the pressure of chamber is set at 1Pa;
4. the sample table speed of rotation is 60 rpms;
5. microwave power is 1200W, and the microwave discharge time is 10 seconds.
In the 4th step, feed mixed gas.
Close the magnetic valve that mixes gas tank and chamber junction, open each source of the gas respectively and lead to magnetic valve and the under meter that mixes in the gas tank gas circuit branch, silicon source gas and source gas in nitridation are flowed into simultaneously mix mixes more than 5 seconds in the gas tank after, first in feeding mixed gas in chamber 23 silicon source gas is mixed mutually with source gas in nitridation.
The 5th step, deposition silicon nitride film on substrate.
Open rotation control, make the substrate uniform rotation; Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb decomposes mixed silicon source gas and source gas in nitridation, and the effect by permanent magnetic field of active charged particle that the back produced is decomposed in ionization be transported to substrate surface, deposition silicon nitride film on substrate, but controlled microwave goes out the silicon nitride film that thickness is 150 dusts deposit in 10 seconds discharge time.
The 6th step, the purification process chamber.
After deposit is finished, close source gas, feed nitrogen pipeline and chamber 23 are purified.
Embodiment 4
It is that the NaCl sheet of Φ 10mm is as substrate that the present invention selects substrate for use.
The first step is cleaned substrate and is put into chamber.
The NaCl sheet was cleaned 20 minutes with acetone tide sound; Rotation under the nitrogen atmosphere protection dried and handles in 120 seconds.Silicon chip after cleaning is placed on the sample table 232 in the chamber 23.
In second step, chamber is vacuumized.
Open oilless vacuum pump and molecular pump and related valve successively, chamber is vacuumized, make the base vacuum degree reach 1.0 * 10
-5Pa.
In the 3rd step, set processing condition respectively.
1. substrate temperature is set at 80 ℃;
2. total gas flow rate is 110sccm, and gas flow ratio is 1: 8;
3. the pressure of chamber is set at 1.5Pa;
4. the sample table speed of rotation is 60 rpms;
5. microwave power is 1200W, and the microwave discharge time is 10 seconds.
In the 4th step, feed mixed gas.
Close the magnetic valve that mixes gas tank and chamber junction, open each source of the gas respectively and lead to magnetic valve and the under meter that mixes in the gas tank gas circuit branch, silicon source gas and source gas in nitridation are flowed into simultaneously mix mixes more than 5 seconds in the gas tank after, first in feeding mixed gas in chamber 23 silicon source gas is mixed mutually with source gas in nitridation.
The 5th step, deposition silicon nitride film on substrate.
Open rotation control, make the substrate uniform rotation; Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb decomposes mixed silicon source gas and source gas in nitridation, and the effect by permanent magnetic field of active charged particle that the back produced is decomposed in ionization be transported to substrate surface, deposition silicon nitride film on substrate, but controlled microwave goes out the silicon nitride film that thickness is 130 dusts deposit in 10 seconds discharge time.
The 6th step, the purification process chamber.
After deposit is finished, close source gas, feed nitrogen pipeline and chamber 23 are purified.
Performance of the present invention can describe in detail by following test data and curve.
Change microwave power, make it to increase to 2000W from 650W, measure the thickness of institute's deposition film and be divided by and obtain as shown in Figure 4 deposition rate with the variation relation curve of microwave power with corresponding deposition time, 1001 lines from Fig. 4 as seen, along with the increase of microwave power of the present invention, thin-film deposition speed rises to 140nm/min from 110nm/min.
Test 2
Change gas flow ratio, make it to increase to 12 from 6, measure the thickness of institute's deposition film and be divided by and obtain as shown in Figure 5 deposition rate with the variation relation curve of gas flow ratio with corresponding deposition time, 1002 lines from Fig. 5 as seen, along with the increase of gas flow ratio of the present invention, thin-film deposition speed rises to 95nm/min from 60nm/min.
Test 3
Change gas flow ratio, make it from 6 to increase to 12, the specific refractory power of measuring institute's deposition film obtains that specific refractory power is with the variation relation curve of gas flow ratio as shown in Figure 6, and 1003 lines from Fig. 6 as seen, along with the increase of gas flow ratio of the present invention, film refractive index rises to 2.1 from 1.8.
Test 4
Change microwave power, make it to increase to 2000W from 650W, the specific refractory power of measuring institute's deposition film obtains that specific refractory power is with the variation relation curve of microwave power as shown in Figure 7, and 1004 lines from Fig. 7 as seen, along with the increase of microwave power of the present invention, specific refractory power is reduced to 1.82 from 2.03.
Test 5
Change technological temperature, the specific refractory power of having tested the silicon nitride film of deposit under the gas with various throughput ratio condition as shown in Figure 8.Wherein, 1005 lines are the refraction index test result of 80 ℃ of following deposition silicon nitride films, and 1006 lines are the refraction index test result of deposition silicon nitride film under the room temperature.As seen, along with the increase of technological temperature, the specific refractory power of silicon nitride film rises.
Change microwave power, make it to increase to 2000W from 650W, the ratio of measuring the contained Si element of institute's deposition film and N element obtains as shown in Figure 9 film Si/N than the variation relation curve with microwave power, 1007 lines from Fig. 9 as seen, along with the increase of microwave power of the present invention, film Si/N is than dropping to 0.72 from 0.78.
Change gas flow ratio, make it to increase to 9 from 7, the ratio of measuring the contained Si element of institute's deposition film and N element obtains as shown in Figure 9 film Si/N than the variation relation curve with microwave power, 1008 lines from Fig. 9 as seen, along with the increase of microwave power of the present invention, film Si/N is than rising to 0.79 from 0.73.
With NEXUS 750 infrared spectrometers, adopt the former state direct Detection Method respectively the silicon chip before and after the deposition silicon nitride film to be carried out the Fourier transform infrared spectroscopy analysis as shown in figure 10.As seen, in instrument detecting sensitivity and detectability, do not detect tangible 2160cm
-1Si-H and 3340cm near the wave number
-1Near the wave number N-H key, so the silicon nitride film of institute's deposit contains protium hardly.
Use AUTOEL-IV type ellipsograph to measure the thickness of the film of 4 of the center of circle on 6 inches wafers, 4 of radius and 1/2 radius respectively.The thickness of the silicon nitride film that the monolithic each point measures is as shown in table 1.Calculating thickness mean value is 77.7 nanometers, and the thickness standard deviation is 3.9, and homogeneity is 95% in the diaphragm.
Different time repeats three batches of deposition silicon nitride films with identical deposition conditions, and every day is a collection of, and five every batch, it is as shown in table 2 to obtain each sheet mean thickness, and calculating repeatability is 95%.
More than test as seen, with the inventive method can be under the low temperature below 300 ℃ deposition silicon nitride film, from test 1 and test 2 as seen, thin-film deposition speed is higher, from testing 3～5 as seen, the result that membrane structure and specific refractory power are adjustable and obtain with high-temperature deposition technology is approaching, from testing 6 as seen, film is hydrogeneous hardly, from testing 7 as seen, homogeneity and repeatability are better than 95% in 6 inches silicon wafers, can satisfy unicircuit passivation material performance demands.
Homogeneity in the table 1 silicon nitride film thickness sheet
| The |
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Film thickness (nm) | 81.9 | 80.4 | 80.6 | 80.4 | 81.4 | 74.3 | 73.8 | 72.2 | 74.2 |
Table 2 silicon nitride film depositing technics repeatability
| Film thickness/nanometer | No.1 | No.2 | No.3 | No.4 | No.5 | |
| Batches | ||||||
| 1 batch 2 batches 3 | 82.7 75.9 77.3 | 83.5 81 77 | 87.4 78.8 75.9 | 87.5 76.1 78.3 | 87.8 78.4 80 | 85.8 78 77.7 |
Claims (5)
1. the method for a chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma comprises following process:
To be placed in the chamber after the substrate cleaning;
Chamber is vacuumized;
Set processing condition, promptly
The pressure of chamber: remain on 0.1Pa～5Pa;
Microwave power: be controlled at 600W～2000W;
Deposition temperature: be controlled at room temperature～300 ℃ scope;
Total gas flow rate: 50～300sccm;
The throughput ratio of silicon source gas and source gas in nitridation: 1: 6～1: 12;
Speed of rotation remains 60 rev/mins.
Silicon source gas and source gas in nitridation are mixed the back mutually feed chamber;
Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb carries out the ionization decomposition to mixed silicon source gas and source gas in nitridation, and the effect by permanent magnetic field of active charged particle that the back produced is decomposed in ionization be transported to substrate surface, deposition silicon nitride film on substrate.
2. the method for a chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma comprises following process:
To be placed in the chamber after the substrate cleaning;
Chamber is vacuumized;
Set processing condition, promptly
The total pressure of chamber: 1Pa;
Microwave power: 1200W;
Deposition temperature: 200 ℃;
Total gas flow rate: 150sccm;
The throughput ratio of silicon source gas and source gas in nitridation: 1: 8;
Speed of rotation remains 60 rev/mins.
Silicon source gas and source gas in nitridation are mixed the back mutually to feed in the chamber;
Open microwave source, the microwave source energy that utilizes the electron cyclotron resonace effect to absorb carries out the ionization decomposition to mixed silicon source gas and source gas in nitridation, and the active charged particle that ionization decomposition back is produced is transported to substrate surface by the permanent magnetic field effect, deposition silicon nitride film on substrate.
3. according to claim 1,2 described methods, wherein silicon source gas is elected as with the SiH of Ar gas as carrier gases dilute
4Source gas in nitridation is elected N as
2
4. according to claim 1,2 described methods, wherein with silicon source gas and source gas in nitridation mutually the blended process be: close the magnetic valve that mixes gas tank and chamber junction; Open each source of the gas respectively and lead to magnetic valve and the under meter that mixes in the gas tank gas circuit branch, silicon source gas and source gas in nitridation are flowed into simultaneously mix in the gas tank and mix more than 5 seconds.
5. according to claim 1,2 described methods, wherein substrate material is selected 6 inches silicon wafers or quartz plate or NaCl crystal cut for use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100185188A CN101104925A (en) | 2007-08-21 | 2007-08-21 | Method for chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100185188A CN101104925A (en) | 2007-08-21 | 2007-08-21 | Method for chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101104925A true CN101104925A (en) | 2008-01-16 |
Family
ID=38999003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100185188A Pending CN101104925A (en) | 2007-08-21 | 2007-08-21 | Method for chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101104925A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102610618A (en) * | 2011-01-19 | 2012-07-25 | 三星电子株式会社 | Thin film transistor array panel |
| CN102931143A (en) * | 2011-08-10 | 2013-02-13 | 无锡华润上华科技有限公司 | Method for manufacturing NOR flash device |
| CN103415134A (en) * | 2013-07-18 | 2013-11-27 | 北京东方计量测试研究所 | Double-source ECR plasma source device |
| CN106094446A (en) * | 2016-08-01 | 2016-11-09 | 安徽贝莱电子科技有限公司 | A kind of radar electric controls the processing method of element wafer |
| CN104282656B (en) * | 2013-07-01 | 2017-03-08 | 中芯国际集成电路制造(上海)有限公司 | A kind of semiconductor devices and its manufacture method |
-
2007
- 2007-08-21 CN CNA2007100185188A patent/CN101104925A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102610618A (en) * | 2011-01-19 | 2012-07-25 | 三星电子株式会社 | Thin film transistor array panel |
| CN102931143A (en) * | 2011-08-10 | 2013-02-13 | 无锡华润上华科技有限公司 | Method for manufacturing NOR flash device |
| CN102931143B (en) * | 2011-08-10 | 2015-04-29 | 无锡华润上华科技有限公司 | Method for manufacturing NOR flash device |
| CN104282656B (en) * | 2013-07-01 | 2017-03-08 | 中芯国际集成电路制造(上海)有限公司 | A kind of semiconductor devices and its manufacture method |
| CN103415134A (en) * | 2013-07-18 | 2013-11-27 | 北京东方计量测试研究所 | Double-source ECR plasma source device |
| CN106094446A (en) * | 2016-08-01 | 2016-11-09 | 安徽贝莱电子科技有限公司 | A kind of radar electric controls the processing method of element wafer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100593585C (en) | Microwave electron cyclotron resonance plasma chemistry gas phase sedimentation device | |
| KR100693695B1 (en) | Plasma processing apparatus with a dielectric plate having a thickness based on a wavelength of a microwave introduced into a process chamber through the dielectric plate | |
| US3875068A (en) | Gaseous plasma reaction apparatus | |
| CN101104925A (en) | Method for chemical gaseous phase deposition of silicon nitride film by electron cyclotron resonance plasma | |
| CN102593025A (en) | Multi-zone temperature control for semiconductor wafer | |
| CN100523292C (en) | Method of plasma chemistry vapor depositing fluoridation amorphous carbon membrane and membrane layer structure thereof | |
| CN102428540B (en) | Method for boron doping silicon wafers | |
| CN101256942A (en) | Dosimetry using optical emission spectroscopy/residual gas analyzer in conjunction with ion current | |
| KR20070059036A (en) | Plasma processing method | |
| CN101379214A (en) | Epitaxial deposition process and apparatus | |
| CN203474963U (en) | Chemical vapor deposition equipment for producing silicon carbide epitaxial wafer | |
| US5667701A (en) | Method of measuring the amount of capacitive coupling of RF power in an inductively coupled plasma | |
| CN116254597A (en) | Plasma doped silicon carbide crystal growing furnace | |
| CN100584999C (en) | Chemical vapor depositing method of low dielectric constant silicon oxide membrane | |
| CN109585332A (en) | Clean method, dry cleaning system and the non-transient computer readable media of chamber | |
| US7524745B2 (en) | Method and device for doping, diffusion and oxidation of silicon wafers under reduced pressure | |
| US9598771B2 (en) | Dielectric film defect reduction | |
| CN108277479B (en) | PECVD device capable of controlling air flow uniformly and stably | |
| Jansen | Plasma deposition processes | |
| CN111996514A (en) | Method for monitoring film thickness and uniformity of silicon wafer in LPCVD (low pressure chemical vapor deposition) process | |
| WO2022033178A1 (en) | Semiconductor deposition method and semiconductor deposition system | |
| Lu et al. | Process sensing and metrology in gate oxide growth by rapid thermal chemical vapor deposition from SiH 4 and N 2 O | |
| CN109280905A (en) | Microwave electron cyclotron resonance plasma chemistry gas phase sedimentation device | |
| CN201121209Y (en) | Plasma chemistry vapor deposition apparatus | |
| CN108914086A (en) | Fe2O3 doping diamond dilute magnetic semiconductor and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |