CN103436847B - The reaction sputtering system controlled based on vibrating type reacting gas - Google Patents
The reaction sputtering system controlled based on vibrating type reacting gas Download PDFInfo
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- CN103436847B CN103436847B CN201310312221.8A CN201310312221A CN103436847B CN 103436847 B CN103436847 B CN 103436847B CN 201310312221 A CN201310312221 A CN 201310312221A CN 103436847 B CN103436847 B CN 103436847B
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- 238000004544 sputter deposition Methods 0.000 title claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 65
- 239000012495 reaction gas Substances 0.000 claims abstract description 33
- 239000012159 carrier gas Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 13
- 230000009514 concussion Effects 0.000 claims abstract description 5
- 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 10
- 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
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 3
- 239000010409 thin film Substances 0.000 description 15
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 10
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 10
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 8
- 239000010408 film Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 150000002736 metal compounds Chemical class 0.000 description 5
- 238000005546 reactive sputtering Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000005684 electric field Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910021645 metal ion Inorganic materials 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
- 239000000376 reactant Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002294 plasma sputter deposition Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of reaction sputtering system controlled based on vibrating type reacting gas, including vacuum chamber and reaction gas pipeline and gas-carrier pipeline, in described vacuum chamber, be provided with relative anode wafer carrier and cathode targets；Described reaction sputtering system also includes gas Flowrate Control System, described gas Flowrate Control System includes that computer, flow controller, reacting gas mass flowmenter and carrier gas mass flowmenter, described reacting gas mass flowmenter and described carrier gas mass flowmenter are separately positioned in described reaction gas pipeline and described gas-carrier pipeline；Described computer controls described reacting gas mass flowmenter by described flow controller, and the reaction gas flow making the described vacuum chamber of entrance is periodically concussion flow.The present invention is by the reaction gas flow periodically shaken so that whole sputter procedure achieves dynamic stable, and and then stablizes the metallic compound composition required for obtaining.
Description
Technical field
The present invention relates to use physical sputtering method to prepare the technology of metal compound film, specifically one
Plant the reaction sputtering system controlled based on vibrating type reacting gas.
Background technology
Reactive sputtering method is a kind of conventional method preparing metal compound film, its operation principle be
Certain density reacting gas it is passed through so that metal ion is during sputtering and reacts during sputtering
Gas reaction, thus the compound required for obtaining.
Traditional reaction sputtering system structure includes: vacuum chamber, shielding power supply, vacuum pump group system, crystalline substance
Circle transmission system, gas circuit and control system etc..Wafer carrier it is provided with sputtered for placing in vacuum chamber
Wafer.Be provided with target device at the top of vacuum chamber, this target device include place target pedestal,
The strong magnet array of the rotation required for the cathode targets being connected on pedestal and magnetic control sputtering system.Sputtering
Technique is carried out under certain vacuum environment, when being passed through a certain amount of argon in vacuum chamber, and at negative electrode and
Plus voltage between anode, then can produce gas self-excited discharge, this charged gas ion adding at electric field
The lower bombarding cathode target of speed so that target metal ionization to be deposited on anode by electric field acceleration (to be sputtered
Wafer) on.If period is passed through reacting gas such as O2、N2Deng, these gases will be at plasma
Become ion under bombardment, thus react with metal ion, wafer is formed required metal compound
Thing thin film.The composition of the metal compound film that reactive sputtering is generated is divided by the reacting gas in vacuum chamber
Pressure (i.e. the concentration of reacting gas) determines, especially some is had the metallic compound of multiple valence state, its
Topmost valence state is dependent on being passed through the uninterrupted of reacting gas.
There is a problem the biggest in existing this reaction sputtering system, it may be assumed that for some electric conductivity ratios
Poor compound-material, along with the increase of reacting gas, on a part of compound meeting backwash to target, shape
Become the thin film that one layer of electric conductivity is poor, this reduce sputtering current, reduce sputtering rate.Sputtering electricity
The reduction of stream promotes reacting gas dividing potential drop to increase further, thus the compound that result in more conduction difference is thin
Film is formed on target, so that sputtering current reduces further, forms vicious cycle, ultimately results in sputtering
Technique stops.So using traditional reaction sputtering system to have sizable limitation, even cannot obtain
The thin film of required metal state composition.
Below to prepare vanadium dioxide (VO2) further illustrate as a example by thin film and use tradition reaction sputtering system
Limitation.Generally target uses pure vanadium metal target, utilizes argon (Ar) as carrier gas, then is passed through O2Make
For reacting gas.At certain temperature and plasma sputtering environment, reacting gas O2Vanadium with ionic state
In conjunction with, the oxide forming vanadium is deposited on wafer.Tetravalent oxide vanadium dioxide (the VO of vanadium2) in room temperature
Under there is higher resistance coefficient (Temperature Coefficient ofResistivity is called for short TCR) and relatively
Low resistivity, is a kind of splendid material making micrometer bolometer, so the main mesh of usual technique
Be obtain highly purified VO2Thin film.
Fig. 1 illustrates and above-mentioned prepares vanadium dioxide (VO2) schematic diagram of an experimental result of thin film.Experiment
In, according to certain time interval, inject different reaction gas flows in the different time respectively.Just open
The time begun, reacting gas is zero, and the corresponding material sputtered out is pure vanadium metal, corresponding chemical valence
Position is 0 valency；After 10th second, change reaction gas flow, sputter out for monovalence barium oxide, instead
Should result stablize；After 20th second, again changing reaction gas flow, sputter out aoxidizes for bivalent vanadium
Thing, reaction result is stable；By that analogy；But after the 40th second, change reaction gas flow, sputtering
Result is the most stable, and time initial, chemical composition is tetravalent vanadium compound, increases over time, several seconds with
Rear compound just becomes the pentavalent oxide of vanadium, i.e. vanadic anhydride.As can be seen here, traditional sputtering is used
Method can not obtain high-quality tetravalence barium oxide, i.e. VO2Thin film.Therefore, tradition reactive sputtering work
The sputtered film Composition Control difficulty of skill, the even thin film of some special component cannot sputter.
Summary of the invention
The present invention is directed to the problems referred to above, it is provided that a kind of reaction sputtering system controlled based on vibrating type reacting gas,
This reaction sputtering system can sputter the metal compound film of stable components.
According to technical scheme: a kind of reaction sputtering system controlled based on vibrating type reacting gas,
The reaction gas pipeline including vacuum chamber and being connected with described vacuum chamber respectively and gas-carrier pipeline, described
Relative anode wafer carrier and cathode targets it is provided with in vacuum chamber；Described reaction sputtering system also includes
Gas Flowrate Control System, described gas Flowrate Control System includes computer, flow controller, reaction gas
Weight effusion meter and carrier gas mass flowmenter, described reacting gas mass flowmenter and described carrier gas quality stream
Gauge is separately positioned in described reaction gas pipeline and described gas-carrier pipeline, described reacting gas mass flow
Meter and described carrier gas mass flowmenter are connected with described flow controller respectively, and described flow controller is with described
Computer is connected；Described computer controls described reacting gas mass flowmenter by described flow controller,
Making the reaction gas flow entering described vacuum chamber from described reaction gas pipeline is periodically concussion flow.
Described anode wafer carrier is arranged at the bottom of described vacuum chamber, and described cathode targets is arranged at described
The top of vacuum chamber, described reaction gas pipeline and described gas-carrier pipeline are respectively arranged at described vacuum chamber
Sidewall on.
The exit position of described reaction gas pipeline is corresponding with described cathode targets, going out of described gas-carrier pipeline
Mouth position is corresponding with described anode wafer carrier.
Described reacting gas is oxygen, and described carrier gas is argon, and described cathode targets is 5N pure vanadium target.
The method have technical effect that: the present invention is provided with gas Flowrate Control System, make entrance vacuum
The reaction gas flow of chamber is periodically to shake flow, so that whole sputter procedure achieves dynamically
Stable, and and then stablize the metallic compound composition required for obtaining.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that employing tradition reaction sputtering system prepares an experimental result of vanadium dioxide film.
Fig. 2 is the structural representation of the present invention.
Fig. 3 is the schematic diagram using the present invention to control gas flow.
Detailed description of the invention
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is further described.
In Fig. 2, including vacuum chamber 1, shielding power supply 2, cathode targets 3, anode wafer carrier 4, anti-
Answer gas piping 5, gas-carrier pipeline 6, computer 7, flow controller 8, reacting gas mass flowmenter 9,
Carrier gas mass flowmenter 10 etc..
As in figure 2 it is shown, the present invention is a kind of reaction sputtering system controlled based on vibrating type reacting gas, bag
Include vacuum chamber 1 and gas Flowrate Control System.
Relative anode wafer carrier 4 and cathode targets 3 it is provided with in vacuum chamber 1.Anode wafer carrier 4
Being arranged at the bottom of vacuum chamber 1, cathode targets 3 is arranged at the top of vacuum chamber 1, cathode targets 3
It is connected with shielding power supply 2.
Coupled logical reaction gas pipeline 5 and gas-carrier pipeline it is respectively arranged with on the sidewall of vacuum chamber 1
6.The exit position of reaction gas pipeline 5 is corresponding with cathode targets 3, the exit position of gas-carrier pipeline 6 with
Anode wafer carrier 4 is corresponding.
Gas Flowrate Control System include computer 7, flow controller 8, reacting gas mass flowmenter 9 and
Carrier gas mass flowmenter 10.Reacting gas mass flowmenter 9 and carrier gas mass flowmenter 10 are separately positioned on instead
Answer in gas piping 5 and gas-carrier pipeline 6, reacting gas mass flowmenter 9 and carrier gas mass flowmenter 10 points
Not being connected with flow controller 8, flow controller 8 is connected with computer 7.Computer 7 is by flow control
Device 8 processed controls reacting gas mass flowmenter 9, makes to enter the reaction of vacuum chamber 1 from reaction gas pipeline 5
Gas flow is periodically to shake flow.
Prepare vanadium dioxide (VO2) thin film time, reacting gas is oxygen, and carrier gas is argon, cathode targets 3
For 5N pure vanadium target.
The technological process that the employing present invention carries out reactive sputtering is as follows:
1, vacuum chamber 1 is first extracted into required base vacuum by vacuum system, such as 10E-7Torr.
2, computer 7 controls carrier gas mass flowmenter 10 by flow controller 8, is passed through the load of certain flow
Gas, such as the argon of 35sccm, and makes the vacuum of vacuum chamber 1 reach required vacuum, as
5E-3Torr。
3, computer 7 controls reacting gas mass flowmenter 9 by flow controller 8, the reaction gas being passed through
Body flow is not a definite value, but at flow F1 and F2 set according to regular hour periodic vibration
Value.The control process of whole reacting gas is as it is shown on figure 3, be described as follows: in the T0 time by reacting gas stream
Amount is set to F1, in the T1 time, reaction gas flow is set to F2, then is set by reaction gas flow in the T2 time
For F1, by that analogy.Wherein the T0-T1 time is initial time, for TBegin；The T1-T2 time is TF2, table
It it is now time during F2 flow；The T2-T3 time is TF1, show as time during F1 flow, by that analogy,
Form concussion.
4, shielding power supply 2 is opened in the T1 time, until it reaches the film thickness of needs.
One important difference of the present invention and traditional reaction sputtering system is the stream of the reacting gas of the present invention
Amount is a flow periodically shaken, and unconventional firm discharge.The present invention can solve the problem that tradition is fixing
The instability problem that reaction gas flow brings, its principles illustrated contained is as follows: when reaction gas flow is
F1, owing to partial reaction thing backwash causes reactant valence state to increase, reactive state tends to unstable；But it is the shortest
In time, gas flow becomes F2, causes reactant valence state to reduce.The conversion of this high-frequency flow makes on the contrary
Obtain whole sputter procedure and achieve dynamic stable.This is just as the wheelbarrow of acrobatics, if wheelbarrow
Motionless, performance people is difficult to maintain and balances: if but perform people and do not stop the most quickly to move, just it is easy to
Realize the balance of wheelbarrow.
Use the present invention reaction sputtering system, by adjust reacting gas two preset value F1 and F2 with
And conversion time cycle TF1And TF2, it becomes possible in reactive sputtering process, stablize the metallization required for obtaining
Polymer component.
It it is below comparative experimental example
Use the Endura5500 model vacuum sputtering system of Applied Materials (Applied Materials) company
During system sputtered film, as a example by sputtering power DC600W.The target used in experiment is 5N pure vanadium target,
Carrier gas is Ar, flow 35sccm, and reacting gas is oxygen, and target product is tetravalence barium oxide VO2。
When oxygen flow is less than critical point 5.5sccm when, such as during 5.4sccm, the thin film composition sputtered out
Predominantly two valency barium oxide VO.After tested, its thin film specific insulation is of about 0.001 Ω cm.Work as oxygen
When throughput equals or exceeds critical point 5.5sccm, even if oxygen flow is highly stable, sputtering current also can be anxious
Falling sharply low, the thin film specific insulation finally sputtered out is more than 1000 Ω cm, through material composition analysis, its
It is mainly composed of V2O5.Test result indicate that, if this vacuum sputter system is not transformed, be to sputter
Go out the oxide VO of the vanadium of+4 valencys2, volume resistance is the thin film of 1 Ω about cm.
According to the present invention, the vacuum sputter system of this Endura5500 model is transformed, adds this
The gas Flowrate Control System of the cuff computer in bright.By computer programming, reaction gas flow is set
Switch between 7.0sccm and 1.5sccm, cycle TF1And TF2It is respectively 1 second and 1.4 seconds, sputtering power
For 600W, total time is 400 seconds.Through measuring, its sputtering thickness isSpeed is substantially
It is mainly composed of VO2, specific insulation, at 1.53 Ω cm, at room temperature has a TCR that comparison is high, and about-2.0%
(negative sign represents that its resistivity increases with temperature and diminishes), property of thin film reaches to use requirement.
Claims (2)
1. the reaction sputtering system controlled based on vibrating type reacting gas, including vacuum chamber (1) and
The reaction gas pipeline (5) being connected with described vacuum chamber (1) respectively and gas-carrier pipeline (6), described
Relative anode wafer carrier (4) and cathode targets (3) it is provided with in vacuum chamber (1)；It is characterized in that:
Described reaction sputtering system also includes that gas Flowrate Control System, described gas Flowrate Control System include calculating
Machine (7), flow controller (8), reacting gas mass flowmenter (9) and carrier gas mass flowmenter (10),
Described reacting gas mass flowmenter (9) and described carrier gas mass flowmenter (10) be separately positioned on described instead
Answer in gas piping (5) and described gas-carrier pipeline (6), described reacting gas mass flowmenter (9) and institute
State carrier gas mass flowmenter (10) to be connected with described flow controller (8) respectively, described flow controller (8)
It is connected with described computer (7)；Described computer (7) controls described by described flow controller (8)
Reacting gas mass flowmenter (9), makes to enter described vacuum chamber (1) from described reaction gas pipeline (5)
Reaction gas flow be periodically concussion flow；
The control process of reacting gas is as follows: in the T0 time, reaction gas flow is set to F1, in the T1 time
Reaction gas flow is set to F2, then in the T2 time, reaction gas flow is set to F1, by that analogy；Its
The middle T0-T1 time is initial time, for TBegin；The T1-T2 time is TF2, show as time during F2 flow；
The T2-T3 time is TF1, show as time during F1 flow, by that analogy, forming concussion；
Described anode wafer carrier (4) is arranged at the bottom of described vacuum chamber (1), described cathode targets
(3) top of described vacuum chamber (1), described reaction gas pipeline (5) and described carrier gas pipe it are arranged at
Road (6) is respectively arranged on the sidewall of described vacuum chamber (1)；
The exit position of described reaction gas pipeline (5) is corresponding with described cathode targets (3), described load
The exit position of air pipe (6) is corresponding with described anode wafer carrier (4).
2., according to the reaction sputtering system controlled based on vibrating type reacting gas described in claim 1, it is special
Levying and be: described reacting gas is oxygen, described carrier gas is argon, and described cathode targets (3) is the pure vanadium of 5N
Target.
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| 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 |
| CN107034443B (en) * | 2017-03-23 | 2019-03-29 | 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (2)
| 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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