CN102534472B - Double ion beam reaction sputtering deposition equipment and method for preparing vanadium oxide film - Google Patents
Double ion beam reaction sputtering deposition equipment and method for preparing vanadium oxide film Download PDFInfo
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Abstract
The invention relates to improved double ion beam reaction sputtering deposition equipment. A multichannel closed-loop control system and a relative gain array (RGA) feedback control device are arranged in the equipment, the flow control accuracy of reaction gas is improved, the partial pressure of the reaction gas oxygen is stabilized, and the stability and repeatability of parameters such as square resistance, thickness, temperature coefficient of resistance (TCR) of the deposited vanadium oxide (VOx) film are ensured; and moreover, the oxygen is introduced from an auxiliary source of a chamber, a risk of target poisoning caused by reaction of the target and the oxygen is eliminated, the service life of the target is prolonged and the utilization rate of the equipment is improved. The invention also relates to a method for preparing a vanadium oxide film by using the equipment. The method comprises the following steps of: performing ion beam milling on a substrate wafer; and preparing the vanadium oxide film by using an improved double ion beam reaction sputtering deposition method.
Description
Technical field
The present invention relates to technical field of electronic materials, relate in particular to a kind of improved double-ion beam reactive sputtering equipment and use the method that this equipment prepares vanadium oxide film.
Background technology
Since finding that vanadium oxide has high resistance-temperature characteristic, people just never stopped the research of vanadium oxide film.Especially recent two decades comes, the develop rapidly of non-refrigerated infrared detector technology, and one of its core technology is exactly selection and the improvement in performance of thermal sensitive resistance material.Vanadium oxide film is a kind of good electronic functional material, has good sensitive characteristic, at infrared acquisition and thermal imaging field wide application is arranged.When being subjected to extraneous illuminated with infrared radiation, absorption layer and medium layer absorb ir radiation, cause the temperature of vanadium oxide thermo-sensitive material to change, thereby cause the resistance of vanadium oxide thermo-sensitive material to change.Can be converted to electrical signal to the infrared radiation signal in the external world thus, be applied to infrared acquisition and thermal imaging.Vanadium oxide (VOx) film is because it has high temperature coefficient of resistance (TCR, Temperature Coefficient of Resistance), and thin film preparation process and ic process compatibility.At present, nearly 70% non-refrigerated infrared detector uses the VOx film as thermo-sensitive material.
Along with the widespread use of miniature bolometer in the military and civilian field, also more and more higher to the requirement of VOx film quality.Not only to have high TCR, also will have suitable square resistance, fine and close microcosmic phase structure, stable machining reproducibility and level and smooth resistance-temperature characteristic curve.But because vanadium presents multiple stable chemical valence state, its oxide compound has nearly 13 kinds of different phase structures at occurring in nature, the vanadium oxide of semiconductor property (VOx) thin film deposition processes window is very narrow, and property of thin film is easy to change between metal-semiconductor-dielectric.Therefore to prepare that to have repeatability high, good stability, the vanadium oxide film that the satisfies certain TCR difficulty very that just becomes.Ion beam sputter depositing technology (IBSD, Ion Beam Sputter Deposition) is the common method of preparation high quality thin film, and it has certain advantage with respect to traditional magnetron sputtering technique.The ion of bombardment target material surface causes the cascade collision of target upper layer atom when shifting self-contained energy or momentum, make target atom break away from the surface and form sputtered atom.If in the sputtered atom flux, substrate is set, the sputtered atom that then carries certain energy is deposited on substrate surface, along with continuing of sputter and deposition process, deposition and atomic through nucleation and grain growing, forms and grows into film in modes such as island mode, laminated form or unordered atomic reactors at substrate surface.
Existing technology is mostly used single ion source sputter, and the vanadium target is as sputtering target material, bombarding gas Ar and reactant gases O
2Become Ar+ and O by the ion source ionization
2+, accelerating back bombardment vanadium metal target by accelerating grid, and generate VOx in the surface reaction of vanadium metal target, VOx is splashed on the substrate again, forms the ion beam reactive sputtering deposition.This method is fairly simple, but the film density of deposition is lower, is not easy control, repeatability and stable poor." target poisoning " phenomenon takes place in the easier over oxidation that causes the vanadium metal target.
Summary of the invention
The objective of the invention is provides a kind of improved double-ion beam reactive sputtering equipment at above-mentioned deficiency.
Another object of the present invention has provided a kind of method for preparing vanadium oxide film.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of improved double-ion beam reactive sputtering equipment (as Fig. 1) mainly comprises reaction chamber (1), target stand (2), main source (3), auxilliary source (4), second air intake valve (5), molecular pump (9), wafer (13), dried pump (11), sample table (14) first air intake valve equipment such as (6); Wherein reaction chamber (1) inside mainly is made up of main source (3), auxilliary source (4), sample table (14), wafer (13), target stand (2), and external dried pump (11), the molecular pump (9) of reaction chamber (1) is used for vacuumizing; Wafer (13) is fixed on the sample table (14), and main source (3), auxilliary source (4) are connected with second air intake valve (5), first air intake valve (6) respectively, are used for entering of gas; Wherein said auxilliary source (4) is connected with first mass flowmeter, by first mass flowmeter and multichannel closed loop control system (as Speedflo
TM) connect the control gas flow; Described reaction chamber (1) also is provided with inlet mouth (15), and reaction chamber (1) links to each other with second mass flowmeter by this inlet mouth (15), and second mass flowmeter is connected with RGA (Residual Gas Analyser) feedback control system.
Further, described auxilliary source (4) links to each other with first air intake valve (6), is connected with first mass flowmeter by first air intake valve (6); Main source (3) links to each other with second air intake valve (5), is connected with the 3rd mass flowmeter by second air intake valve (5).
Speedflo
TMBe a kind of multichannel closed loop control system, in reactive sputtering, be used for the quick adjustment flow rate of reactive gas usually.This system uses advanced Digital Control mode, is more suitable for the accuracy control requirement of mass flowmeter (MFC:Mass Flow Controller) with respect to traditional analog pid control.This system works under the control of PC network and watchdog routine, side in process cavity is equipped with independently controller, the control algolithm of system embeds in this controller, can accurately control fast MFC full range flow ± 1% flow accuracy, if use range to be the MFC of 20.0sccm, control accuracy can reach ± 0.2sccm, thereby guarantees the fast and stable of auxilliary source reaction gas flow fluctuation.
By RGA (Residual Gas Analyser) feedback control system device, control process cavity oxygen partial pressure is regulated the gas inlet (15) of oxygen partial pressure.RGA monitors oxygen partial pressure, when fluctuation takes place the partial pressure of monitoring, regulates the oxygen flow of inlet mouth (15) automatically by the closed loop feedback Controlling System, guarantees that oxygen partial pressure is stable.
The beneficial effect that adopts above-mentioned further scheme is to make reaction gas flow fluctuation fast and stable, thereby makes partial pressure more stable, and then can guarantee the stability of technology.
A kind of method for preparing vanadium oxide film, its concrete steps are as follows:
Step 1: the angle of adjusting sample table (14) and target stand (2), wafer (13) is positioned on the right opposite of sputter vanadium atom or vanadium ion passage, reaction chamber (1) is vacuumized, vacuum tightness is reached below the 1E-5Pa, specimen heating holder (14) makes sample temperature control at 150～250 ℃.
Step 2: wafer is carried out ion beam milling: feed Ar gas from auxilliary source (4), flow applies the ion voltage of 50～200V between the scope of 5.0sccm～15.0sccm, make the Ar gas ionization, carries out the ion beam milling of crystal column surface, mill off
Upper layer.
Step 3: the pre-sputter of target: feed Ar gas from main source (3), use the flow of MFC control Ar gas between 10.0～20.0sccm, use the voltage of 800～1200V that the ionization of Ar gas is become the Ar+ ion, vanadium metal target target stand (2) is carried out pre-sputter; Use baffle plate to shelter from wafer before the pre-sputter.
Step 4: preparation vanadium oxide film: after pre-sputter finishes, continue to feed Ar gas from main source (3), use the flow of MFC control Ar gas between 10.0～20.0sccm, from auxilliary source (4) aerating oxygen, MFC and Speedflo
TMThe flow of multichannel closed loop control system control oxygen feeds auxiliary oxygen from inlet mouth (15) simultaneously at 5.0～15.0sccm, and functional quality under meter and RGA feedback control system are controlled its flow simultaneously between 0.2～5.0sccm; Reactant gases to be fed makes chamber pressure rise to 1E-2Pa～4E-2Pa, after remove baffle plate, wafer (13) is carried out the double-ion beam reactive sputter-deposition of VOx film, the rotating disk that loads wafer simultaneously rotates with 20 rev/mins, after treating that film thickness reaches goal-selling, process ends.
Adopt the beneficial effect of such scheme to be: to improve the vanadium oxide film deposition quality, strengthened the sticking power of vanadium oxide film on crystal column surface, reduced the pollution of impurity to film; Improved the repeated and stable of thin film deposition, made the vanadium oxide film component of deposition controlled, the repeatability of the Vanadium Oxide Thin Film Resistance rate of deposition, thickness, TCR is high, and homogeneity improves, and improves the numerical value of TCR simultaneously; Increase the degree of freedom of technology controlling and process, the feasible quality that can go to improve deposition from a plurality of parameters; Can make the vanadium oxide film of deposition for the manufacturing of non-refrigerated infrared detector and other optics.Simultaneously protect target to a certain extent, prevent " target poisoning " phenomenon, reduced the pre-sputtering time of technology target, the work-ing life of having improved target;
Description of drawings
Fig. 1 is double-ion beam reactive sputter-deposition equipment cavity configuration synoptic diagram;
In the accompanying drawing, the list of parts of each label representative is as follows:
1, reaction chamber, 2, target stand, the vanadium metal target is installed, 3, main source, 4, auxilliary source, 5, second air intake valve, 6, first air intake valve, 7, vent valve, 8, high valve, 9, molecular pump, 10, the level valve, 11, dried pump, 12, dried pump valve door, 13, wafer, 14, sample table, 15, inlet mouth
Embodiment
Below in conjunction with accompanying drawing principle of the present invention and feature are described, institute gives an actual example and only is used for explaining the present invention, is not for limiting scope of the present invention.
The testing method explanation: square resistance uses 4 probes to test, 25 points/sheet, and edge 5mm gets rid of.Heterogeneity method of calculation: 1sigma/mean.
The TCR calculation formula: the relation of semiconductor resistor and temperature can be used the Steinhart-Hart The Representation Equation:
C1 and C2 are temperature independent Steinhart-Hart coefficients, so LnR (T) and 1/T be linear relationship, and slope is 1/C2.
According to above-mentioned Steinhart-Hart equation, the temperature factor of resistance can calculate according to following formula:
Case study on implementation 1:
Step 1: the angle of adjusting sample table (14) and target stand (2), the target stand angle is 27 °, wafer (13) is positioned on the right opposite of sputter vanadium atom or vanadium ion passage, reaction chamber (1) is vacuumized, make base vacuum reach 1E-5Pa, specimen heating holder (14) makes sample temperature control at 200 ℃.
Step 2: wafer is carried out ion beam milling: feed Ar gas from auxilliary source (4), use the flow of MFC control Ar gas at 10.0sccm, apply the voltage of 100V, make the Ar gas ionization, use the ion mill off
Upper layer.
Step 3: the pre-sputter of target: feed Ar gas from main source (3), use the flow of MFC control Ar gas at 15.0sccm, the voltage that adds 1000V becomes the Ar+ ion with the ionization of Ar gas, vanadium metal target target stand (2) is carried out the pre-sputter of 3min; Need to open the preceding baffle plate of wafer (13) before the pre-sputter, shelter from wafer.
Step 4: preparation vanadium oxide film: after pre-sputter finished, feeding the Ar gas flow from main source (3) still was 15.0sccm, from auxilliary source (4) aerating oxygen, used MFC and Speedflo
TMThe flow of multichannel closed loop control system control oxygen feeds auxiliary oxygen from inlet mouth (15) simultaneously at 12.0sccm, uses MFC and RGA feedback control system to control its flow at 3.0sccm; Make reaction chamber (1) pressure rise to 2E-2Pa; Remove baffle plate then, wafer (13) is carried out the double-ion beam reactive sputter-deposition of VOx film, the rotating disk that loads wafer simultaneously rotates with 20 rev/mins, and depositing time is 20min, process ends.
The heterogeneity of the square resistance of deposit film is 1.8% (1sigma/mean), and TCR is-2.8% (20 ℃), and the thickness heterogeneity is 1.5% (1sigma/mean).
Case study on implementation 2:
Step 1: the angle of adjusting sample table (14) and target stand (2), the target stand angle is 27 °, wafer (13) is positioned on the tangential face of right opposite of sputter vanadium atom or vanadium ion passage, reaction chamber (1) is vacuumized, base vacuum is reached below the 1E-6Pa, specimen heating holder (14) makes sample temperature control at 250 ℃.
Step 2: wafer is carried out ion beam milling: feed Ar gas from auxilliary source (4), use the flow of MFC control Ar gas at 5.0sccm, apply the voltage of 50V, make the Ar gas ionization, use the ion mill off
Upper layer.
Step 3: the pre-sputter of target: feed Ar gas from main source (3), use the flow of MFC control Ar gas at 10.0sccm, treat that gas stablizes the voltage of after-applied 1200V the ionization of Ar gas is become the Ar+ ion, vanadium metal target target stand (2) is carried out the pre-sputter of 3min; Need to open the preceding baffle plate of wafer (13) before the pre-sputter, shelter from wafer.
Step 4: preparation vanadium oxide film: after pre-sputter finished, feeding the Ar gas flow from main source (3) still was 10.0sccm, from auxilliary source (4) aerating oxygen, used MFC and Speedflo
TMThe flow of multichannel closed loop control system control oxygen feeds auxiliary oxygen from inlet mouth (15) simultaneously at 5.0sccm, and MFC and RGA feedback control system are controlled its flow at 0.2sccm; Make reaction chamber (1) pressure be increased to 1E-2Pa; Remove baffle plate then, wafer (13) is carried out the double-ion beam reactive sputter-deposition of VOx film, the rotating disk that loads wafer simultaneously rotates with 20 rev/mins, and depositing time is 20min, process ends.
The heterogeneity of the square resistance of deposit film is 1.5% (1sigma/mean), and TCR is-2.7% (20 ℃), and the thickness heterogeneity is 1.3% (1sigma/mean).
Case study on implementation 3:
Step 1: the angle of adjusting sample table (14) and target stand (2), the target stand angle is 27 °, wafer (13) is positioned on the tangential face of right opposite of sputter vanadium atom or vanadium ion passage, reaction chamber (1) is vacuumized, make base vacuum reach 1E-6Pa, specimen heating holder (14) makes sample temperature control at 150 ℃.
Step 2: wafer is carried out ion beam milling: feed Ar gas from auxilliary source (4), use the flow of MFC control Ar gas at 15.0sccm, apply the voltage of 200V, make the Ar gas ionization, use the ion mill off
Upper layer.
Step 3: the pre-sputter of target: feed Ar gas from main source (3), use the flow of MFC control Ar gas at 20.0sccm, add that the voltage of 800V becomes the Ar+ ion with the ionization of Ar gas, vanadium metal target target stand (2) is carried out the pre-sputter of 3min; Need to open the baffle plate before the wafer 13 before the pre-sputter, shelter from wafer.
Step 4: preparation vanadium oxide film: after pre-sputter finished, feeding the Ar gas flow from main source (3) still was 20.0sccm, from auxilliary source (4) aerating oxygen, used MFC and Speedflo
TMThe flow of multichannel closed loop control system control oxygen feeds auxiliary oxygen from inlet mouth (15) simultaneously at 15.0sccm, uses MFC and RGA feedback control system to control its flow at 5.0sccm; Make chamber pressure rise to 4E-2Pa; Remove baffle plate then, wafer (13) is carried out the double-ion beam reactive sputter-deposition of VOx film, the rotating disk that loads wafer simultaneously rotates with 20 rev/mins, and depositing time is 22min, process ends.
The heterogeneity of the square resistance of deposit film is 2.0% (1sigma/mean), and TCR is-2.7% (20 ℃), thickness heterogeneity 1.8% (1sigma/mean).
Above-mentioned three case study on implementation, the even type of VOx film rectangular resistance of deposition, thickness heterogeneity, repeatability are all less than 3% (1sigma/mean), and all greater than 2.0% (20 ℃), the VOx film of deposition can be used for non-refrigerated infrared detector production to the TCR absolute value.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. method for preparing vanadium oxide film, concrete steps are as follows:
Step 1: adjust the sample table (14) of double-ion beam reactive sputter-deposition equipment and the angle of target stand (2), wafer (13) is positioned on the right opposite of sputter vanadium atom or vanadium ion passage, reaction chamber (1) is vacuumized, and specimen heating holder (14);
Step 2: wafer is carried out ion beam milling: feed Ar gas from auxilliary source (4), the flow of functional quality under meter control Ar gas is between the scope of 5.0sccm～15.0sccm, apply the ion voltage of 50～200V, make the Ar gas ionization, with ionic fluid disk is carried out ion beam milling, ion beam milling stops to feed Ar gas after finishing;
Step 3: the pre-sputter of target: after ion beam milling finishes, feed Ar gas from main source (3), the flow of functional quality under meter control Ar gas uses the voltage of 800～1200V between 10.0～20.0sccm, the ionization of Ar gas is become the Ar ion, vanadium metal target target stand (2) is carried out pre-sputter;
Step 4: preparation vanadium oxide film: after pre-sputter finishes, continue to feed Ar gas from main source (3), the flow of functional quality under meter control Ar gas is between 10.0～20.0sccm, feed reaction oxygen from auxilliary source (4), the flow of mass flowmeter and multichannel closed loop control system control oxygen is at 5.0～15.0sccm, feed auxiliary oxygen from inlet mouth (15) simultaneously, reaction chamber (1) air pressure raises, then wafer (13) is carried out the ion beam reactive sputtering deposition of VOx film, after treating that film thickness reaches goal-selling, finish sputtering sedimentation.
2. method according to claim 1 is characterized in that, refers to that at specimen heating holder described in the step 1 temperature control is at 150～250 ℃.
3. method according to claim 1 is characterized in that, the reaction chamber described in the step 4 (1) air pressure be elevated to 1E ?2Pa～4E ?2Pa.
4. method according to claim 1 is characterized in that, described in the step 2 wafer is being carried out ion beam milling, and mill off crystal column surface layer thickness is
5. according to each described method of claim 1 to 4, it is characterized in that, the described oxygen that feeds from inlet mouth (15) of step 4, flow is between 0.2～5.0sccm.
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| CN103498127B (en) * | 2013-06-13 | 2015-08-26 | 北京航空航天大学 | A kind of method applied double-ion beam coating technique and prepare W-Cr alloy layer in W surface |
| KR20210039825A (en) * | 2019-10-02 | 2021-04-12 | 삼성전자주식회사 | An apparatus for depositing a substrate and a deposition system having the same |
| CN113584442A (en) * | 2021-08-16 | 2021-11-02 | 中科微机电技术（北京）有限公司 | Reactive sputtering apparatus including control system and reactive sputtering method |
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| US6495070B1 (en) * | 1996-12-31 | 2002-12-17 | Honeywell International Inc. | Flexible high performance microbolometer detector material fabricated via controlled ion beam sputter deposition process |
| CN2734774Y (en) * | 2004-07-28 | 2005-10-19 | 雷卫武 | Double-ion-beam co-sputtering deposition atomic-layer nano film device |
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| JPH11279756A (en) * | 1998-03-26 | 1999-10-12 | Okura Ind Co Ltd | Formation of transparent conductive film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6495070B1 (en) * | 1996-12-31 | 2002-12-17 | Honeywell International Inc. | Flexible high performance microbolometer detector material fabricated via controlled ion beam sputter deposition process |
| CN2734774Y (en) * | 2004-07-28 | 2005-10-19 | 雷卫武 | Double-ion-beam co-sputtering deposition atomic-layer nano film device |
Non-Patent Citations (2)
| Title |
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| Reactive gas control of non-stable plasma conditions;V.Bellido-González;《Thin Solid Films》;20060428;第502卷(第1-2期);34-39 * |
| V.Bellido-González.Reactive gas control of non-stable plasma conditions.《Thin Solid Films》.2006,第502卷(第1-2期),34-39. |
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