CN103436847A - Reaction sputtering system based on oscillation-type reaction gas control - Google Patents
Reaction sputtering system based on oscillation-type reaction gas control Download PDFInfo
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- CN103436847A CN103436847A CN2013103122218A CN201310312221A CN103436847A CN 103436847 A CN103436847 A CN 103436847A CN 2013103122218 A CN2013103122218 A CN 2013103122218A CN 201310312221 A CN201310312221 A CN 201310312221A CN 103436847 A CN103436847 A CN 103436847A
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- mass flowmeter
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- 239000012495 reaction gas Substances 0.000 title claims abstract description 40
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 61
- 239000012159 carrier gas Substances 0.000 claims abstract description 21
- 239000000376 reactant Substances 0.000 claims description 42
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 229910052720 vanadium Inorganic materials 0.000 claims description 11
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 13
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 4
- 230000000737 periodic effect Effects 0.000 abstract description 3
- 230000010355 oscillation Effects 0.000 abstract 2
- 230000006641 stabilisation Effects 0.000 abstract 1
- 238000011105 stabilization Methods 0.000 abstract 1
- 239000013077 target material Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 21
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 5
- 150000002736 metal compounds Chemical class 0.000 description 5
- 238000005546 reactive sputtering Methods 0.000 description 5
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 2
- 230000009514 concussion Effects 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000002294 plasma sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- -1 vanadium oxide compound Chemical class 0.000 description 1
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Abstract
The invention relates to a reaction sputtering system based on oscillation-type reaction gas control. The reaction sputtering system comprises a vacuum chamber, a reaction gas pipeline and a carrier gas pipeline; an anode wafer carrying platform and a cathode target material which face with each other are disposed in the vacuum chamber; the reaction sputtering system also comprises a gas flow control system, and the gas flow control system comprises a computer, a flow controller, a reaction gas mass flowmeter and a carrier gas mass flowmeter; the reaction gas mass flowmeter and the carrier gas mass flowmeter are respectively disposed in the reaction gas pipeline and the carrier gas pipeline; and the computer is used to control the reaction gas mass flowmeter via the flow controller and enable the reaction gas flow entering into the vacuum chamber to be a periodic oscillation flow. By employing the reaction gas flow with periodic oscillation, the reaction sputtering system helps to realize dynamic stabilization of a whole sputter process, and further to realize stable obtaining of needed metallic compound components.
Description
Technical field
The present invention relates to adopt the physical sputtering method to prepare the technology of metal compound film, specifically a kind of reaction sputtering system of controlling based on the vibrating type reactant gases.
Background technology
Reactive sputtering method is a kind of method for preparing metal compound film of commonly using, its principle of work is to pass into certain density reactant gases in the process of sputter, make the process neutralization reaction gas reaction of metal ion in sputter, thereby obtain needed compound.
Traditional reaction sputtering system structure comprises: vacuum chamber, shielding power supply, vacuum pump group system, wafer transfer system, gas circuit and Controlling System etc.Be provided with the wafer that wafer carrier is sputtered for placement in vacuum chamber.Top at vacuum chamber is provided with target device, and this target device comprises the pedestal of placing target, be connected to cathode targets on pedestal and the strong magnet array of the needed rotation of magnetic control sputtering system.Sputtering technology is carried out under certain vacuum environment, pass into a certain amount of argon gas in vacuum chamber, and add voltage between negative electrode and anode, can produce the gas self-excited discharge, this charged gaseous ion bombarding cathode target under the acceleration of electric field, make the target metal ion and be deposited on anode (treating the wafer of sputter) by electric field acceleration.If pass into during this time reactant gases as O
2, N
2deng, these gases will become ion under the bombardment of plasma body, thereby react with metal ion, form needed metal compound film on wafer.The composition of the metal compound film that reactive sputtering generates is determined by the reactant gases dividing potential drop in vacuum chamber (being the concentration of reactant gases), especially some are had the metallic compound of multiple valence state, its topmost valence state just depends on the uninterrupted that passes into reactant gases.
There is a very large problem in existing this reaction sputtering system, that is: the poor compound-material for some conductivities, increase along with reactant gases, part compound meeting backwash is to target, form the poor film of one deck conductivity, this has reduced sputtering current, has reduced sputtering rate.The reducing of sputtering current further impels the reactant gases dividing potential drop to increase, thereby caused more conduction, poor compound film is formed on target, thereby sputtering current is further reduced, and forms vicious cycle, finally causes sputtering technology to stop.So adopt traditional reaction sputtering system to there is sizable limitation, even can't obtain the film of needed metal valence state composition.
Below to prepare vanadium dioxide (VO
2) film is that example further illustrates the limitation that adopts traditional reaction sputtering system.Usually target adopts pure vanadium metal target, utilizes argon gas (Ar) as carrier gas, then passes into O
2as reactant gases.Under certain temperature and plasma sputtering environment, reactant gases O
2with the vanadium combination of ionic state, form the oxidate of vanadium on wafer.Tetravalent oxide vanadium dioxide (the VO of vanadium
2) at room temperature there is higher specific resistance (Temperature Coefficient ofResistivity, be called for short TCR) and lower resistivity, a kind of material of splendid making micrometer bolometer, so the main purpose of technique is to obtain highly purified VO usually
2film.
Fig. 1 has meaned the above-mentioned vanadium dioxide (VO for preparing
2) schematic diagram of an experimental result of film.In experiment, according to certain time interval, inject different reaction gas flows in the different time respectively.The incipient time, reactant gases is zero, and the corresponding material sputtered out is pure vanadium metal, and corresponding chemical price is 0 valency; After the 10th second, change reaction gas flow, what sputter out is the monovalence barium oxide, and reaction result is stable; After the 20th second, again change reaction gas flow, what sputter out is the bivalent vanadium oxide compound, and reaction result is stable; By that analogy; But to after the 40th second, change reaction gas flow, the sputter result is no longer stable, and when initial, the compound composition is tetravalent vanadium compound, along with the time increases, after several seconds, compound just becomes the pentavalent oxide of vanadium, i.e. Vanadium Pentoxide in FLAKES.As can be seen here, adopt traditional sputtering method can not obtain high-quality tetravalence barium oxide, i.e. VO
2film.Therefore, the sputtered film Composition Control difficulty of traditional reactive sputtering process, even the film of some special component can't sputter.
Summary of the invention
The present invention is directed to the problems referred to above, a kind of reaction sputtering system of controlling based on the vibrating type reactant gases is provided, this reaction sputtering system can sputter the metal compound film of stable components.
According to technical scheme of the present invention: a kind of reaction sputtering system of controlling based on the vibrating type reactant gases, comprise vacuum chamber and the reaction gas pipeline and the gas-carrier pipeline that are connected with described vacuum chamber respectively, be provided with relative anode wafer carrier and cathode targets in described vacuum chamber; Described reaction sputtering system also comprises gas Flowrate Control System, described gas Flowrate Control System comprises that computer, flow director, reactant gases mass rate take into account the carrier gas mass flowmeter, described reactant gases mass flowmeter and described carrier gas mass flowmeter are separately positioned in described reaction gas pipeline and described gas-carrier pipeline, described reactant gases mass rate is taken into account described carrier gas mass flowmeter and is connected with described flow director respectively, and described flow director is connected with described computer; Described computer is controlled described reactant gases mass flowmeter by described flow director, makes to enter the reaction gas flow of described vacuum chamber for periodically shaking flow from described reaction gas pipeline.
Described anode wafer carrier is arranged at the bottom of described vacuum chamber, and described cathode targets is arranged at the top of described vacuum chamber, and described reaction gas pipeline and described gas-carrier pipeline are arranged at respectively on the sidewall of described vacuum chamber.
The outlet position of described reaction gas pipeline is corresponding with described cathode targets, and the outlet position of described gas-carrier pipeline is corresponding with described anode wafer carrier.
Described reactant gases is oxygen, and described carrier gas is argon gas, and described cathode targets is the pure vanadium target of 5N.
Technique effect of the present invention is: be provided with gas Flowrate Control System in the present invention, make to enter the reaction gas flow of vacuum chamber for periodically shaking flow, thereby it is dynamic stable to make whole sputter procedure realize, and and then the needed metallic compound composition of stable acquisition.
The accompanying drawing explanation
Fig. 1 is for adopting traditional reaction sputtering system to prepare the schematic diagram of an experimental result of vanadium dioxide film.
Fig. 2 is structural representation of the present invention.
Fig. 3 is for adopting the present invention to control the schematic diagram of gas flow.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is further described.
In Fig. 2, comprise vacuum chamber 1, shielding power supply 2, cathode targets 3, anode wafer carrier 4, reaction gas pipeline 5, gas-carrier pipeline 6, computer 7, flow director 8, reactant gases mass flowmeter 9, carrier gas mass flowmeter 10 etc.
As shown in Figure 2, the present invention is a kind of reaction sputtering system of controlling based on the vibrating type reactant gases, comprises vacuum chamber 1 and gas Flowrate Control System.
Be provided with relative anode wafer carrier 4 and cathode targets 3 in vacuum chamber 1.Anode wafer carrier 4 is arranged at the bottom of vacuum chamber 1, and cathode targets 3 is arranged at the top of vacuum chamber 1, and cathode targets 3 is connected with shielding power supply 2.
Be respectively arranged with coupled logical reaction gas pipeline 5 and gas-carrier pipeline 6 on the sidewall of vacuum chamber 1.The outlet position of reaction gas pipeline 5 is corresponding with cathode targets 3, and the outlet position of gas-carrier pipeline 6 is corresponding with anode wafer carrier 4.
Gas Flowrate Control System comprises computer 7, flow director 8, reactant gases mass flowmeter 9 and carrier gas mass flowmeter 10.Reactant gases mass flowmeter 9 is separately positioned in reaction gas pipeline 5 and gas-carrier pipeline 6 with carrier gas mass flowmeter 10, and reactant gases mass flowmeter 9 and carrier gas mass flowmeter 10 are connected with flow director 8 respectively, and flow director 8 is connected with computer 7.Computer 7 is controlled reactant gases mass flowmeter 9 by flow director 8, makes to enter the reaction gas flow of vacuum chamber 1 for periodically shaking flow from reaction gas pipeline 5.
Prepare vanadium dioxide (VO
2) during film, reactant gases is oxygen, carrier gas is argon gas, cathode targets 3 is the pure vanadium target of 5N.
Adopt the present invention to carry out the technical process of reactive sputtering as follows:
1, vacuum system first is extracted into needed base vacuum by vacuum chamber 1, as 10E-7Torr.
2, computer 7 is controlled carrier gas mass flowmeter 10 by flow director 8, passes into the carrier gas of certain flow, as the argon gas of 35sccm, and makes the vacuum of vacuum chamber 1 reach needed vacuum tightness, as 5E-3Torr.
3, computer 7 is controlled reactant gases mass flowmeters 9 by flow director 8, and the reaction gas flow passed into is not a definite value, but at the flow F1 set and F2 the value according to the regular hour periodic vibration.The control process of whole reactant gases as shown in Figure 3, is described as follows: in the T0 time, reaction gas flow is made as to F1, in the T1 time, reaction gas flow is made as to F2, then in the T2 time, reaction gas flow is made as to F1, by that analogy.Wherein the T0-T1 time is time of origin, is T
begin; The T1-T2 time is T
f2, the time while showing as the F2 flow; The T2-T3 time is T
f1, the time while showing as the F1 flow, by that analogy, form concussion.
4, open shielding power supply 2 in the T1 time, until reach the film thickness needed.
The flow that the flow that an important difference of the present invention and traditional reaction sputtering system is reactant gases of the present invention is the one-period concussion, and unconventional base runoff.The present invention can solve the instability problem that traditional fixation reaction gas flow brings, and its principles illustrated contained is as follows: when reaction gas flow is F1, because partial reaction thing backwash causes the reactant valence state, increase, it is unstable that response behaviour is tending towards; But in very short time, gas flow becomes F2, cause the reactant valence state to reduce.It is dynamic stable that this high-frequency flow conversion makes whole sputter procedure realize on the contrary.This is just as the wheelbarrow of acrobatics, if wheelbarrow is motionless, the performance people is difficult to maintain balance: if but the performance people does not stop one in front and one in back quick travel, just be easy to realize the balance of wheelbarrow.
Use reaction sputtering system of the present invention, by two preset value F1 and F2 and the conversion time cycle T of adjusting reactant gases
f1and T
f2, just can in reactive sputtering process, stablize and obtain needed metallic compound composition.
It is below comparative experimental example
While using the Endura5500 model vacuum sputter system sputtered film of company of Applied Materials (Applied Materials), take sputtering power DC600W as example.The target used in experiment is the pure vanadium target of 5N, and carrier gas is Ar, flow 35sccm, and reactant gases is oxygen, the target resultant is tetravalence barium oxide VO
2.When oxygen flow, lower than stagnation point 5.5sccm the time, during such as 5.4sccm, the thin film composition sputtered out is mainly two valency barium oxide VO.After tested, its film volume specific resistance is about 0.001 Ω cm.When oxygen flow equals or exceeds stagnation point 5.5sccm, even oxygen flow is highly stable, sputtering current also can sharply reduce, and the film volume specific resistance finally sputtered out is greater than 1000 Ω cm, and through the material composition analysis, its main component is V
2o
5.Experimental result shows, if this vacuum sputter system is not done transformation, is the oxide compound VO of the vanadium of can't sputter+4 valencys
2, the film that volume resistance is 1 Ω cm left and right.
According to the present invention, the vacuum sputter system of this Endura5500 model is transformed, increased the gas Flowrate Control System of the cuff computer in the present invention.By computer programming, reaction gas flow is set and switches between 7.0sccm and 1.5sccm, cycle T
f1and T
f2be respectively 1 second and 1.4 seconds, sputtering power is 600W, and total time is 400 seconds.Through measuring, its sputter thickness is
speed is roughly
main component is VO
2, volume specific resistance, at 1.53 Ω cm, at room temperature has higher TCR, and approximately-2.0% (negative sign means that its resistivity increases and diminishes with temperature), property of thin film reaches service requirements.
Claims (4)
1. a reaction sputtering system of controlling based on the vibrating type reactant gases, the reaction gas pipeline (5) that comprises vacuum chamber (1) and be connected with described vacuum chamber (1) respectively and gas-carrier pipeline (6), be provided with relative anode wafer carrier (4) and cathode targets (3) in described vacuum chamber (1), it is characterized in that: described reaction sputtering system also comprises gas Flowrate Control System, described gas Flowrate Control System comprises computer (7), flow director (8), reactant gases mass flowmeter (9) and carrier gas mass flowmeter (10), described reactant gases mass flowmeter (9) is separately positioned in described reaction gas pipeline (5) and described gas-carrier pipeline (6) with described carrier gas mass flowmeter (10), described reactant gases mass flowmeter (9) and described carrier gas mass flowmeter (10) are connected with described flow director (8) respectively, described flow director (8) is connected with described computer (7), described computer (7) is controlled described reactant gases mass flowmeter (9) by described flow director (8), makes to enter the reaction gas flow of described vacuum chamber (1) for periodically shaking flow from described reaction gas pipeline (5).
2. according to the reaction sputtering system of controlling based on the vibrating type reactant gases claimed in claim 1, it is characterized in that: described anode wafer carrier (4) is arranged at the bottom of described vacuum chamber (1), described cathode targets (3) is arranged at the top of described vacuum chamber (1), and described reaction gas pipeline (5) is arranged at respectively on the sidewall of described vacuum chamber (1) with described gas-carrier pipeline (6).
3. according to the reaction sputtering system of controlling based on the vibrating type reactant gases claimed in claim 2, it is characterized in that: the outlet position of described reaction gas pipeline (5) is corresponding with described cathode targets (3), and the outlet position of described gas-carrier pipeline (6) is corresponding with described anode wafer carrier (4).
4. according to the reaction sputtering system of controlling based on the vibrating type reactant gases claimed in claim 1, it is characterized in that: described reactant gases is oxygen, and described carrier gas is argon gas, and described cathode targets (3) is the pure vanadium target of 5N.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756865A (en) * | 2016-12-14 | 2017-05-31 | 文晓斌 | A kind of magnetron sputtering reaction atmosphere self feed back control system and its application method |
| CN107034443A (en) * | 2017-03-23 | 2017-08-11 | 江西沃格光电股份有限公司 | The coating apparatus of high resistance film |
| CN113930735A (en) * | 2021-10-15 | 2022-01-14 | 无锡尚积半导体科技有限公司 | Vapor deposition equipment for improving thickness uniformity of vanadium oxide film and vapor deposition method thereof |
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| JPH01278013A (en) * | 1988-04-29 | 1989-11-08 | Nippon Electric Ind Co Ltd | Sputtering apparatus |
| JPH06144991A (en) * | 1992-10-30 | 1994-05-24 | Nec Corp | Method for judging the time for exchanging and replenishing cell of molecular beam epitaxy device |
| US5942089A (en) * | 1996-04-22 | 1999-08-24 | Northwestern University | Method for sputtering compounds on a substrate |
| CN101355010A (en) * | 2007-07-26 | 2009-01-28 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Air-intake installation and reaction chamber |
| CN101864558A (en) * | 2009-04-16 | 2010-10-20 | 北京广微积电科技有限公司 | Reaction sputtering system |
-
2013
- 2013-07-24 CN CN201310312221.8A patent/CN103436847B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01278013A (en) * | 1988-04-29 | 1989-11-08 | Nippon Electric Ind Co Ltd | Sputtering apparatus |
| JPH06144991A (en) * | 1992-10-30 | 1994-05-24 | Nec Corp | Method for judging the time for exchanging and replenishing cell of molecular beam epitaxy device |
| US5942089A (en) * | 1996-04-22 | 1999-08-24 | Northwestern University | Method for sputtering compounds on a substrate |
| CN101355010A (en) * | 2007-07-26 | 2009-01-28 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Air-intake installation and reaction chamber |
| CN101864558A (en) * | 2009-04-16 | 2010-10-20 | 北京广微积电科技有限公司 | Reaction sputtering system |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756865A (en) * | 2016-12-14 | 2017-05-31 | 文晓斌 | A kind of magnetron sputtering reaction atmosphere self feed back control system and its application method |
| CN107034443A (en) * | 2017-03-23 | 2017-08-11 | 江西沃格光电股份有限公司 | The coating apparatus of high resistance film |
| CN113930735A (en) * | 2021-10-15 | 2022-01-14 | 无锡尚积半导体科技有限公司 | Vapor deposition equipment for improving thickness uniformity of vanadium oxide film and vapor deposition method thereof |
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