CN101078105A - Automatic controlling method for increasing AIN medium film reaction direct current sputtering speed - Google Patents
Automatic controlling method for increasing AIN medium film reaction direct current sputtering speed Download PDFInfo
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- CN101078105A CN101078105A CN 200710118133 CN200710118133A CN101078105A CN 101078105 A CN101078105 A CN 101078105A CN 200710118133 CN200710118133 CN 200710118133 CN 200710118133 A CN200710118133 A CN 200710118133A CN 101078105 A CN101078105 A CN 101078105A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 44
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims description 25
- 230000001276 controlling effect Effects 0.000 claims description 6
- 238000005546 reactive sputtering Methods 0.000 claims description 5
- 239000013077 target material Substances 0.000 claims description 4
- 238000005755 formation reaction Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 239000012495 reaction gas Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000005477 sputtering target Methods 0.000 claims description 2
- 238000006557 surface reaction Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 2
- 230000002950 deficient Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 33
- 229910052757 nitrogen Inorganic materials 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000002184 metal Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000376 reactant Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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Abstract
An automatic control method for improving the reaction dc sputtering speed of AIN medium film, which belongs to vacuum solid film facture technology field. During sputtering process, N2 reacts with Al butt surface to generate AlN, a control system sets the dividing voltage value PN of N2 of the reaction chamber, the control system also measures the air pressure PAr of the reaction chamber which only allows Ar plasm pass through, and N2 is pumped into the chamber to implement reaction sputtering; to adjust N2 input flow amount based on the setting N2 dividing voltage, when the actual air pressure P of the reaction chamber is above to the sum of PN and PAr, N2 is excessive, a controller reduces N2 input flow; when the air pressure P of the reaction chamber is below to the sum of PN and PAr, N2 is deficient, the controller increases N2 input flow. The present invention also provides a automatic control system which improves the reaction dc sputtering speed of AIN medium film based on N2 dividing voltage control. The present invention makes the dividing voltage PN of the remainder N2 steady with a relative low value, which ensures the AlN purity in the film, also possesses a higher sputtering speed.
Description
Technical field
A kind of autocontrol method that improves AlN dielectric film reaction d.c. sputtering speed belongs to vacuum solid film manufacture technology field, especially the solar selectively absorbing coating manufacture technology field.
Background technology
The AlN dielectric thin-film material has higher thermostability and chemical stability, and solar spectrum is had higher transmittance, is used widely at solar energy heat utilization field.Such as, middle low-temperature solar energy heat collector extensively adopts the Al-AlN coating for selective absorption, needs the anti-reflection film (Yin Zhiqiang of AlN dielectric film as this coating, " sputtered coating absorbing solar energy selectively ", Chinese patent, applying unit: Tsing-Hua University, application number: 85100142).In high-temp solar heat collector, the metal-dielectric film coating for selective absorption that refractory metal and AlN medium are formed is expected to obtain widespread use (Q.-C.Zhang, D.R.Mills, and A.Monger, " Thin-film solar selective surface coating ", Australia Patent, Applicant:The University of Sydney, Application number:AU9220346).
In solar energy heat utilization field, adopt the method for sputter to make the AlN film usually.Sputter is meant the specific gas of input under vacuum condition, produces plasma body under the effect in electric field, magnetic field, and ion bombardment target surface makes target atom and atomic group overflow from the surface, thereby attached to the vacuum coating technology of matrix surface.According to the difference of applied field, sputter can be divided into two kinds of d.c. sputtering and radio-frequency sputterings.Wherein d.c. sputtering generally with metal as target, reaction chamber input rare gas element is generally Ar, produces plasma body under the effect of DC electric field, the mode by physical bombardment sputters atoms metal, can be used for making metallic film.For general medium target,, can only adopt radio-frequency sputtering because d.c. sputtering can produce the electric charge accumulation on target.Relative d.c. sputtering, the radio-frequency sputtering cost of manufacture is higher.For some metallic compound dielectric materials, as AlN, Al
2O
3Deng, also can make by the method for reaction d.c. sputtering metal targets.Promptly in rare gas element, add N
2, O
2Isoreactivity gas, under the vacuum plasma concrete conditions in the establishment of a specific crime, on the one hand, N, the atoms metal of O isoreactivity gas atom and target material surface (as Al) reaction generation metal oxynitride medium (as AlN, Al
2O
3); Simultaneously, and the metal oxynitride molecule of target material surface (as AlN, Al
2O
3) under the bombardment of inert gas ions such as Ar, sputtered out, thereby form the metallic compound dielectric film at substrate surface.
For reducing the cost of manufacture of solar selectively absorbing coating, wish to adopt the method for d.c. sputtering to make metal, the AlN dielectric film usually.Wherein metallic film adopts the non-reaction d.c. sputtering of Ar, and the AlN dielectric film adopts Ar, N
2The reaction d.c. sputtering.Under traditional processing condition, the sputter rate of AlN dielectric film becomes the bottleneck of the production of coating for selective absorption much smaller than the sputter rate of metallic film.Production process with low temperature AI in certain-AlN solar selective coat is an example, needs the Al metallic film that sputter 100nm is thick successively, the AlN dielectric film that Al-AlN metal-dielectric film that 150nm is thick and 100nm are thick in substrate of glass.Constant in other condition, only change N
2Under the flow rate condition, when the sputter rate of metal A l was 20nm/min, the sputter rate of metal-dielectric Al-AlN was 10nm/min, and the sputter rate of pure AlN medium only has 2nm/min.Splash-proofing sputtering metal Al, the time of metal-dielectric Al-AlN and medium A lN was respectively 5,15 and 50 minutes, and the sputter reaction chamber vacuumizes in addition needs about 30 minutes clock times, and the time of sputter medium A lN accounts for the over half of whole sputter procedure.Therefore improve the sputter rate of AlN medium, the production efficiency that improves solar selectively absorbing coating is had very important significance.
The processing parameter of AlN film reaction d.c. sputtering has: sputtering current I, Ar flow, N
2Flow, Al target bias voltage U, reaction chamber air pressure P.The measure that improves AlN film reaction d.c. sputtering has: improve sputtering current I, control Ar flow, N
2Flow, control Al target bias voltage.On the one hand, improve the reactive sputtering speed that sputtering current can effectively improve the AlN film, but the size of electric current is subjected to the restriction of sputtering system power supply.On the other hand, Ar, N
2Flow has bigger influence for the thin film composition and the sputter rate of the sputter of Al target response.Under the constant situation of other condition, work as N
2Flow hour, Ar, N
2Sputter Al target produces Al-AlN metal-dielectric film.Along with N
2The increase of flow, the ratio of AlN increases gradually in the Al-AlN film, and sputter rate descends gradually.Work as N
2Flow surpasses certain threshold value N
Th1The time, will sputtering pure AlN dielectric film, sputter rate also will occur one and fall suddenly.And reduce N this moment
2Flow, sputter rate does not go up at once, still sputters pure AlN dielectric film.Work as N
2Flow reduces to certain threshold value N
Th2The time (N
Th2＜N
Th1), sputter rate sharply gos up, and sputters Al-AlN metal-dielectric film.This phenomenon is called as the hesitation that AlN reacts d.c. sputtering.
The existence of hesitation makes people can not adopt the mode of traditional pre-set gas flow to improve the reaction d.c. sputtering speed of AlN dielectric film, need be to gas flow especially reactive gas N
2Flow is controlled in real time.By discovering nitrogen partial pressure P
N, Al target bias voltage U and reactive gas N
2Also there is tangible hesitation between the flow.As shown in Figure 1, under the situation of only logical Ar plasma glow start, N
2Dividing potential drop approaches 0, the higher (U～400V) of Al target bias voltage.Work as N
2Flow is when 0 raises gradually, and Al target bias voltage descends gradually, and N
2Dividing potential drop still approaches 0.Work as N
2Flow is elevated to threshold value N
Th1After, Al target bias voltage descends fast, and N
2Dividing potential drop sharply rises.
As seen from Figure 1, Al target bias voltage is high more, and film deposition rate is high more, and the control N of people by Al target bias voltage arranged for this reason
2Flow.Concrete feedback system is: the bias voltage U that sets an Al target the best in Controlling System
0, as Al target bias voltage U＜U
0The time, think N
2Excessive, reduce N
2Flow; As Al target bias voltage U＞U
0The time, think N
2Deficiency improves N
2Flow.By target voltage being stabilized in the optimum position, thereby improve the sedimentation rate of AlN medium with upper type.
But there is certain limitation in this method, is in particular in: under the condition that other processing condition change, as sputtering current, Ar flow etc., Al target bias voltage U and N
2Flow F
NRetardant curve will change bias voltage reference mark U
0Also to change.In the making processes of reality, be difficult to guarantee the strict conformance of processing condition, thereby at voltage control point U
0Selection on have certain difficulty.In addition, generally adopt mass rate control meter (Mass Flow Controller, MFC) pilot-gas flow at present.But MFC response speed slow (time of response＞1 second) is difficult to satisfy the needs of control in real time.
We think, the hesitation of AlN reaction d.c. sputtering is by following two factors decision: the 1) chemical reaction of reactive gas and Al target, 2) rare gas element is to the physical bombardment of Al target.As reactive gas N
2During underfed, the physical bombardment of rare gas element is occupied an leading position, and it not only bombards the Al on Al target surface, and reactant gases N is fallen in bombardment
2The AlN that forms on Al target surface, thus sputter Al-AlN metal-dielectric film.And N
2Generated AlN by the capture reaction of Al target surface atom fully, even so N
2Flow increases and N
2Dividing potential drop is constant substantially.When reactant gases was excessive, the chemical reaction of reactant gases was occupied an leading position, reactant gases N
2The AlN that generates with the Al reaction has covered whole Al target surface, and the physical bombardment of rare gas element Ar can only sputter AlN, and unnecessary N
2Then show as the rapid rising of reaction chamber air pressure.
Summary of the invention
Based on above physical phenomenon, the invention provides a kind of based on N
2The branch pressure-controlled improves the autocontrol method of AlN dielectric film reaction d.c. sputtering speed, and wherein sputtering target material adopts Al, and active reaction gas is N
2, in sputter procedure, most of N of input
2Produce AlN with the surface reaction of Al target, remaining N
2Show as the rising of reaction chamber air pressure.The method is characterized in that:
(1) sets the N of reaction chamber by Controlling System
2Partial pressure value P
N
Reaction chamber air pressure P when (2) only leading to the Ar plasma glow start by the Controlling System measurement
Ar
(3) feed N
2Carry out reactive sputtering, based on the N that sets
2Dividing potential drop is regulated N
2Input flow rate.As reaction chamber actual pressure P＞P
N+ P
ArThe time, think N
2Excessive, controller reduces N
2Input flow rate; As reaction chamber air pressure P＜P
N+ P
ArThe time, think N
2Deficiency, controller improves N
2Input flow rate.
It is a kind of based on N that the present invention also provides
2The branch pressure-controlled improves the automatic control system of AlN dielectric film reaction d.c. sputtering speed, described Controlling System, comprise air pressure set with read, draught head comparison process, N
2Three parts of flow control is characterized in that:
Air pressure set and reading section can be before reactive sputtering, set N in the sputter procedure
2Dividing potential drop P
NNumerical value, and will be converted to pseudo-logarithmic voltage signal.
2. air pressure is set and the reaction chamber air pressure P of reading section can read only logical non-active gas sputter in advance the time
Ar, and the setting total gas pressure P=P of the automatic formation reaction chamber of energy
N+ P
Ar, and will be converted to pseudo-logarithmic voltage signal.
3. draught head comparison process part compares actual pressure and setting total gas pressure, is converted into N
2Flow changes required voltage signal.
4.N
2The input flow rate control unit adopts a time of response less than 10 at least
-2The N of second
2Flow director, thus satisfy the needs of control in real time.
By with upper type with remaining N
2Dividing potential drop P
NBe stabilized in a relatively low value, both guaranteed the purity of AlN in the film, have higher sputter rate simultaneously again.
Description of drawings
Fig. 1 .N
2Dividing potential drop, Al target bias voltage is with N
2The change curve of flow.
Fig. 2 .N
2Flow and N
2Dividing potential drop feedback structure synoptic diagram.
Embodiment
Below in conjunction with embodiment the present invention is described.
Embodiment 1
On borosilicate 3.3 glass substrate, adopt Ar, N
2Reaction d.c. sputtering Al target is made the AlN dielectric film.Ar flow 50sccm, sputtering current I=30A.Air pressure P when only leading to the Ar build-up of luminance
Ar=0.4Pa feeds excessive N
2The time nitrogen partial pressure P
N〉=0.12Pa, the about 1.5nm/min of sputter rate; Adopt the present invention, with nitrogen partial pressure P
NBe controlled at 0.03Pa, sputter rate reaches 6nm/min.
Embodiment 2
On at the bottom of the stainless steel lining, adopt Ar, N
2Reaction d.c. sputtering Al target is made the AlN dielectric film.Ar flow 70sccm, sputtering current I=40A.Air pressure P when only leading to the Ar build-up of luminance
Ar=0.6Pa feeds excessive N
2The time nitrogen partial pressure P
N〉=0.1Pa, the about 2nm/min of sputter rate; Adopt the present invention, with nitrogen partial pressure P
NBe controlled at 0.01Pa, sputter rate reaches 8nm/min.
Embodiment 3
On silicon substrate, adopt Ar, N
2Reaction d.c. sputtering Al target is made the AlN dielectric film.Ar flow 50sccm, sputtering current I=20A.Air pressure P when only leading to the Ar build-up of luminance
Ar=0.4Pa feeds excessive N
2The time nitrogen partial pressure P
N〉=0.12Pa, the about 1nm/min of sputter rate; Adopt the present invention, with nitrogen partial pressure P
NBe controlled at 0.02Pa, sputter rate reaches 2nm/min.
Claims (2)
1, improve the autocontrol method of AlN dielectric film reaction d.c. sputtering speed, wherein sputtering target material adopts Al, and active reaction gas is N
2, in sputter procedure, most of N of input
2Produce AlN with the surface reaction of Al target, it is characterized in that this method may further comprise the steps:
(1) sets the N of reaction chamber by Controlling System
2Partial pressure value P
N
Reaction chamber air pressure P when (2) only leading to the Ar plasma glow start by the Controlling System measurement
Ar
(3) feed N
2Carry out reactive sputtering, based on the N that sets
2Dividing potential drop is regulated N
2Input flow rate is as reaction chamber actual pressure P＞P
N+ P
ArThe time, think N
2Excessive, controller reduces N
2Input flow rate; As reaction chamber air pressure P＜P
N+ P
ArThe time, think N
2Deficiency, controller improves N
2Input flow rate.
2, a kind of based on N
2The branch pressure-controlled improves the automatic control system of AlN dielectric film reaction d.c. sputtering speed, it is characterized in that, this system comprise successively air pressure set with read, draught head comparison process, N
2Three parts of flow control,
Air pressure is set and reading section, sets N before reactive sputtering, in the sputter procedure
2Dividing potential drop P
NNumerical value, and will be converted to pseudo-logarithmic voltage signal; Simultaneously, air pressure is set and the reaction chamber air pressure P of reading section when reading only logical non-active gas sputter in advance
Ar, and the setting total gas pressure P=P of the automatic formation reaction chamber of energy
N+ P
Ar, be converted into pseudo-logarithmic voltage signal;
Draught head comparison process part compares actual pressure and setting total gas pressure, is converted into N
2Flow changes required voltage signal;
N
2The flow control part adopts at least one time of response less than 10
-2The N of second
2Flow director is controlled in real time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710118133 CN101078105A (en) | 2007-06-29 | 2007-06-29 | Automatic controlling method for increasing AIN medium film reaction direct current sputtering speed |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710118133 CN101078105A (en) | 2007-06-29 | 2007-06-29 | Automatic controlling method for increasing AIN medium film reaction direct current sputtering speed |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101078105A true CN101078105A (en) | 2007-11-28 |
Family
ID=38905763
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710118133 Pending CN101078105A (en) | 2007-06-29 | 2007-06-29 | Automatic controlling method for increasing AIN medium film reaction direct current sputtering speed |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101078105A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101981221B (en) * | 2008-03-27 | 2012-12-26 | 多摩-技术转让机关株式会社 | Process for production of massive mixture of aluminum nitride and aluminum |
-
2007
- 2007-06-29 CN CN 200710118133 patent/CN101078105A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101981221B (en) * | 2008-03-27 | 2012-12-26 | 多摩-技术转让机关株式会社 | Process for production of massive mixture of aluminum nitride and aluminum |
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