CN102912449A - Bonding method for improving bonding force and optical properties of bonding crystal - Google Patents
Bonding method for improving bonding force and optical properties of bonding crystal Download PDFInfo
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- CN102912449A CN102912449A CN2012103879609A CN201210387960A CN102912449A CN 102912449 A CN102912449 A CN 102912449A CN 2012103879609 A CN2012103879609 A CN 2012103879609A CN 201210387960 A CN201210387960 A CN 201210387960A CN 102912449 A CN102912449 A CN 102912449A
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Abstract
The invention relates to a bonding method for improving the bonding force and the optical properties of a bonding crystal, which can be applied to preparing a quasi-phase-matched nonlinear crystal, belongs to the field of nonlinear optical crystals and mainly solves the problems that the quasi-phase-matched crystal obtained through conventional bonding is large in optical loss and small in bonding force. According to the bonding method, a gallium arsenide crystal is selected as a bonding material, ultrahigh vacuum ion source cleaning equipment is utilized, and the loss of a bonding interface is reduced and the bonding force of the bonding crystal is improved by solution cleaning, ion cleaning, ultrahigh vacuum low-temperature bonding, low-pressure heat treatment and other technologies. The bonding method for improving the bonding force and the optical properties of the bonding crystal is mainly used for preparing the quasi-phase-matched gallium arsenide crystal with nonlinear frequency conversion in an infrared band.
Description
Technical field
The present invention relates to a kind of bonding method that improves bonding crystal bonding power and optical characteristics, can be used for preparing accurate phase matching non-linear crystal, belong to the non-linear optic crystal field.
Background technology
Wafer bonding techniques is through surface cleaning and activation treatment with the homogeneity of two cleaning surfaces, atomic roughness or dissimilar materials, do not use any adhesive substance, directly fitting under certain condition is integral, and two crystal are by Van der Waals force, molecular force, even atomic power combines.Wafer bonding techniques has great superiority, and the interface that obtains by this technology has firm, level and smooth, optically transparent advantage, and this interface has very important significance for the innovation of optical device.Accurate phase matched is a kind of effective optical nonlinearity frequency inverted mode that grew up in recent years, quasi-phase-matching crystals internal polarization direction needs the cycle to change, utilize two wafer bondings that wafer bonding can be opposite with direction of polarization together, reach the purpose of phase matched, this material infrared band of gallium arsenide transmitance is high, be fit to the infrared band nonlinear frequency transformation, also have the damage threshold height simultaneously, nonlinear factor is large, the thermal conductivity high.As far back as 1976, the people such as Thompson of U.S. Luo Keweier international corporation just provide the theoretical explanation that gallium arsenide is used for accurate phase matched, because this material is not ferroelectric material, can't puncture period polarized with electrode, main method is epitaxy at present, but epitaxially grown quasi-phase-matching crystals clear aperature is little, can not bring into play the advantage of crystal, and the quasi-phase-matching crystals clear aperature for preparing with the bonding mode is large, is easy to surpass 1cm
2Yet there is zone of oxidation in the gallium arsenide surface, not only can reduce second order nonlinear effect, affects the efficient of frequency inverted, and oxide compound has stronger absorption to infrared band, and is larger on the frequency translation impact.
The existence of zone of oxidation makes the poor effect of the accurate phase matched device of gallium arsenide, therefore the application that obtains accurate phase matched device with the bonding mode is restricted, the diffusion interlinked research work of gallium arsenide mainly concentrates on eighties of last century nineties, up to the present this diffusion interlinked gallium arsenide still is not used widely, and the accurate phase matched device of gallium arsenide mainly still adopts epitaxially grown mode to obtain.In order to remove oxide compound, reduce the optical loss of diffusion interlinked gallium arsenide, people study discovery, the oxide compound of gallium arsenide begins volatilization in 500 ℃, temperature during greater than 850 ℃ oxide compound effectively volatilize, (document 1, Wu YS, Feigelson RS, Route RK, Zheng D, Gordon LA, Fejer MM, Byer RL.Improved GaAs bonding process for quasi-phase-matched second harmonic generation, Journal of the Electrochemical Society, 1998,145 (1): 366 ~ 371).Adopt the diffusion interlinked of high temperature evaporation oxide compound, evaporative process is to carry out in pre-bonding process, cause the evaporation of crystal interface oxide compound not exclusively, the crystal edge transmitance is higher than the germ nucleus, and gallium is different from the oxide content of arsenic, volatilization causes the surface component imbalance, have a strong impact on frequency-doubling conversion efficiency (document 2, E. Lallier, M. Brevignon, and J. Lehoux. Efficient second-harmonic generation of a CO2 laser with a quasi-phase-matched GaAs crystal, 1998,23 (19): 1511 ~ 1513).
The purging method with hydrogen ion bombardment plane of crystal that the present invention proposes is removed oxide on surface, can reduce the optical loss of bonding crystal, bombardment does not increase surfaceness, behind the pre-bonding crystal is annealed, the arrangement of bonded interface atom is recombinated, form firmly covalent, increase linkage force.
Summary of the invention
The object of the invention is to overcome the problem that present diffusion interlinked gallium arsenide linkage force is little, optical loss is large, propose a kind of hydrogen ion and remove oxide on surface, the pre-bonding of ultrahigh vacuum(HHV), the method of high-temperature heat treatment, increase the linkage force of the diffusion interlinked crystal of gallium arsenide, reduce the bonded interface optical loss.
A kind of bonding method that improves bonding crystal bonding power and optical characteristics is characterized in that: the arsenide gallium monocrystal of twin polishing, remove surface organic matter impurity with chemical solvents, and use afterwards deionized water rinsing; Place the vacuum effects on surface to carry out the H rays bombardment processing wafer, the vacuum tightness during bombardment processing is less than 5*10
-5Pa, ion beam current energy are 300-500eV, ion beam current density 2-10 μ A/cm
2, bombardment time is 15-25 minute under the room temperature, is heated to 150 ℃, bombards 5 minutes; Ingress of air does not move to vacuum tightness less than 10
-7Pre-bonding in the vacuum chamber of Pa, wafer integral body evenly is warmed to 150-200 ℃ in the pre-bonding process, and wafer surface evenly applies 10kg/cm
2-15kg/cm
2Pressure, kept 1-2 hour; At last wafer is placed Ar compression ring border to heat-treat, be warmed up to 650-800 ℃ by room temperature, apply simultaneously 20 kg/cm
2-60 kg/cm
2Pressure, be incubated 2-3 hour, naturally cool to room temperature.
With the arsenide gallium monocrystal of twin polishing as the bonding crystal, remove surface organic matter impurity with chemical solvents, afterwards through deionized water rinsing, place the vacuum effects on surface to carry out the H rays bombardment processing wafer, ingress of air does not move to pre-bonding in the high vacuum, at last wafer is placed Ar compression ring border to heat-treat.
Do not remove the bonding method of gallium arsenide surface oxide compound, optical loss is excessive, can't be applied to optical nonlinearity frequency transformation field; And high temperature is removed the method for oxide compound, can exist volatilization not exclusively, the shortcoming of surface component imbalance, and optical loss is large; The method that the present invention adopts hydrogen ion to clean can effectively be removed oxide on surface, does not increase the plane of crystal roughness simultaneously.Hydrogen ion can also increase surperficial dangling bonds quantity when cleaning, and is conducive to increase bonding area, and the combination that improves crystal interface can, be bonded in advance in the high vacuum and carry out, can avoid the residual of bonded interface gas, anneal behind the pre-bonding, annealing process can improve the linkage force of crystal.
The present invention has substantial characteristics and marked improvement, and method of the present invention has following advantage with respect to the diffusion interlinked method of present routine:
Effectively eliminate oxide on surface, improve the optical property of bonding crystal;
Increase surperficial dangling bonds quantity, improved bonding area and linkage force;
Pre-bonding is avoided the entrap bubble problem between the bonded interface in the high vacuum;
The method of annealing can improve the linkage force of crystal.
Description of drawings
Fig. 1 is the used ultrahigh vacuum(HHV) hydrogen ion washing unit of bonding.
Fig. 2 is the Ga3d(A that does not clean gallium arsenide through hydrogen ion) and As3d(B) spectral line photoelectron collection of illustrative plates.
Fig. 3 is the Ga3d(A of gallium arsenide after hydrogen ion cleans) and As3d(B) spectral line photoelectron collection of illustrative plates.
Fig. 4 is the high-resolution-ration transmission electric-lens image of bonded interface.
Fig. 5 is the diffraction pattern of bonding crystal section.
Embodiment
The present invention carries out diffusion interlinked with arsenide gallium monocrystal, the device preparation process can be divided into four key steps.The first step need to be carried out twin polishing with gallium arsenide, and removes surface organic matter impurity with chemical solvents, and deionized water rinsing is clean; Second step carries out the hydrogen ion bombardment in a vacuum; The 3rd step is pre-bonding wafer in high vacuum; The 4th step the high temperature anneal.
Embodiment 1:
After wafer is processed through surface finish, wafer surface is carried out chemical solution cleans, cleaning employed solution is: tetracol phenixin, acetone, ethanol, deionized water, be immersed in pending subsequent technique in the deionized water behind the wafer cleaning, and all operations carries out in clean room.
After sample dried up with nitrogen, (CN201010279377.7, ultrahigh vacuum ion source chip cleaning system were authorized day: 2012-05-02) finish and clean and pre-bonding process, as shown in Figure 1 to use ultrahigh vacuum(HHV) hydrogen ion washing unit.Sample is placed on the specimen holder 7, and be put among the sputter vacuum chamber B, treat that vacuum tightness reaches 10
-5During Pa, produce H rays by hydrogen ion source 5, begin that sample to be cleaned 6 is carried out hydrogen ion and clean, ion beam current energy 350eV is set, ion beam current density 10 μ A/cm
2, bombardment 20 min reduce most of oxide compound under the room temperature, and B chamber integral body is heated to 150 ℃, bombard 5 min again, remove residual oxide, and heat and make the reduzate evaporation.
Behind the end of bombardment, utilize the wafer 6 after driven rod 8 will clean to be passed to the A chamber through valve 4, the vacuum tightness of A chamber need reach 5*10 before transmitting
-8Pa, specimen holder 7 and sample 6 together are fixed on the sample table 2, valve-off 4 is evacuated to the vacuum tightness before the setting-out again, B carries out the cleaning of another wafer in the chamber simultaneously, after cleaning end wafer 6 is passed to the A chamber, by locating device two wafer being fit together obtains the two-layer sample 3 for the treatment of bonding, recovers vacuum tightness 5*10
-8Behind the Pa, utilize magnetic force pressurizing device 1 to apply 10 kg/cm
2Pressure, B chamber integral body is heated to 200 ℃, be incubated 1 hour, finish pre-bonding.
Wafer through pre-bonding can better fit together, and in order further to increase linkage force, wafer is installed in the high temperature resistant anchor clamps, is put in the heat treatment furnace that is full of Ar gas, begins to be warming up to 700 ℃ from room temperature, and pressure is 40kg/cm
2, be incubated 2 hours, naturally be cooled to room temperature, finish whole bonding process.
Remove the situation of oxide compound in order to detect hydrogen ion, hydrogen ion bombardment front and rear surfaces is carried out photoelectron spectrum to be detected, Fig. 2, Fig. 3 be respectively hydrogen ion clean before and after the Ga3d(A of gallium arsenide) and As3d(B) spectral line photoelectron collection of illustrative plates, can find to clean rear surface arsenic and Gallium oxide obviously reduces.Use the contourgraph measure surface roughness, the result shows that the r.m.s. roughness of the front sample of bombardment is 0.37nm, the r.m.s. roughness of sample is 0.40nm after the bombardment, and roughness all less than the lattice parameter of gallium arsenide, does not make surfaceness obviously change before and after the bombardment before and after the bombardment.
In order to detect the hydrogen ion cleaning to the impact of optical property and linkage force, pre-bonding wafer has been carried out stretching experiment, the crystal through hydrogen ion cleaning Direct Bonding does not rupture from bonding face, and bonded energy is 0.34J/cm
2Through the crystal of pre-bonding after the hydrogen ion cleaning, stretched experiment crystal has the area more than 50% to rupture from crystals, and bonded energy is 0.55J/cm
2Can further increase bond strength through Overheating Treatment, according to the wafer of embodiment 1 pre-bonding, bonding area can reach 95% after the annealing, and it is 0.85J/cm that stretching experiment records bonded energy
2, near crystal self in conjunction with energy.With the optical property of infrared transmission mensuration crystal, the average optical loss of bonded layer is 0.3% at wavelength 5.3 μ m places, and 10.6 μ m places are 0.2% at wavelength.
By transmission electron microscope observing bonded interface pattern, as shown in Figure 4, bonded interface is not observed amorphous layer, illustrates that oxide compound is effectively removed, dislocation does not appear in crystals, because pre-bonding process carries out in high vacuum environment, bonded interface is not observed bubble, and the interface crystal lattice marshalling runs through bonded interface, para-linkage layer integral body is carried out diffraction imaging, as shown in Figure 5, integral body is single crystal structure behind the diffraction pattern demonstration bonding, and the in high quality combination of two-layer gallium arsenide wafer is described.
Embodiment 2:
After wafer is processed through surface finish, wafer surface is carried out chemical solution cleans, cleaning employed solution is: tetracol phenixin, acetone, ethanol, deionized water, be immersed in pending subsequent technique in the deionized water behind the wafer cleaning, and all operations carries out in clean room.
Sample places sample on the specimen holder 7 after drying up with nitrogen, and is put among the sputter vacuum chamber B, treats that vacuum tightness reaches 10
-5During Pa, produce H rays by hydrogen ion source 5, begin that sample to be cleaned 6 is carried out hydrogen ion and clean, ion beam current energy 500eV is set, ion beam current density 5 μ A/cm
2, bombardment 15 min reduce most of oxide compound under the room temperature, and B chamber integral body is heated to 150 ℃, bombard 5 min again.
Behind the end of bombardment, utilize the wafer 6 after driven rod 8 will clean to be passed to the A chamber through valve 4, the vacuum tightness of A chamber need reach 5*10 before transmitting
-8Pa, specimen holder 7 and sample 6 together are fixed on the sample table 2, valve-off 4 is evacuated to the vacuum tightness before the setting-out again, B carries out the cleaning of another wafer in the chamber simultaneously, after cleaning end wafer 6 is passed to the A chamber, by locating device two wafer being fit together obtains the two-layer sample 3 for the treatment of bonding, recovers vacuum tightness 5*10
-8Behind the Pa, utilize magnetic force pressurizing device 1 to apply 10 kg/cm
2Pressure, B chamber integral body is heated to 150 ℃, be incubated 1 hour, finish pre-bonding.
Wafer is installed in the high temperature resistant anchor clamps, is put in the heat treatment furnace that is full of Ar gas, begin to be warming up to 650 ℃ from room temperature, pressure is 20kg/cm
2, be incubated 2 hours, naturally be cooled to room temperature, finish bonding process.
Measuring bonding area after the annealing is 92%, and it is 0.82J/cm that stretching experiment records bonded energy
2, near crystal self in conjunction with energy.With the optical property of infrared transmission mensuration crystal, the average optical loss of bonded layer is 0.2% at wavelength 5.3 μ m places, and 10.6 μ m places are 0.1% at wavelength.
Embodiment 3:
After wafer is processed through surface finish, wafer surface is carried out chemical solution cleans, cleaning employed solution is: tetracol phenixin, acetone, ethanol, deionized water, be immersed in pending subsequent technique in the deionized water behind the wafer cleaning, and all operations carries out in clean room.
Sample places sample on the specimen holder 7 after drying up with nitrogen, and is put among the sputter vacuum chamber B, treats that vacuum tightness reaches 10
-5During Pa, produce H rays by hydrogen ion source 5, begin that sample to be cleaned 6 is carried out hydrogen ion and clean, ion beam current energy 300eV is set, ion beam current density 10 μ A/cm
2, bombardment 15 min reduce most of oxide compound under the room temperature, and B chamber integral body is heated to 150 ℃, bombard 5 min again.
Behind the end of bombardment, utilize the wafer 6 after driven rod 8 will clean to be passed to the A chamber through valve 4, the vacuum tightness of A chamber need reach 5*10 before transmitting
-8Pa, specimen holder 7 and sample 6 together are fixed on the sample table 2, valve-off 4 is evacuated to the vacuum tightness before the setting-out again, B carries out the cleaning of another wafer in the chamber simultaneously, after cleaning end wafer 6 is passed to the A chamber, by locating device two wafer being fit together obtains the two-layer sample 3 for the treatment of bonding, recovers vacuum tightness 5*10
-8Behind the Pa, utilize magnetic force pressurizing device 1 to apply 15kg/cm
2Pressure, B chamber integral body is heated to 200 ℃, be incubated 2 hours, finish pre-bonding.
Wafer is installed in the high temperature resistant anchor clamps, is put in the heat treatment furnace that is full of Ar gas, begin to be warming up to 800 ℃ from room temperature, pressure is 60kg/cm
2, be incubated 3 hours, naturally be cooled to room temperature, finish bonding process.
Measuring bonding area after the annealing is 98%, and it is 0.86J/cm that stretching experiment records bonded energy
2With the optical property of infrared transmission mensuration crystal, the average optical loss of bonded layer is 0.6% at wavelength 5.3 μ m places, and 10.6 μ m places are 0.4% at wavelength.
Claims (1)
1. bonding method that improves bonding crystal bonding power and optical characteristics is characterized in that: the arsenide gallium monocrystal of twin polishing, remove surface organic matter impurity with chemical solvents, and use afterwards deionized water rinsing; Place the vacuum effects on surface to carry out the H rays bombardment processing wafer, the vacuum tightness during bombardment processing is less than 5*10
-5Pa, ion beam current energy are 300-500eV, ion beam current density 2-10 μ A/cm
2, bombardment time is 15-25 minute under the room temperature, is heated to 150 ℃, bombards 5 minutes; Ingress of air does not move to vacuum tightness less than 10
-7Pre-bonding in the vacuum chamber of Pa, wafer integral body evenly is warmed to 150-200 ℃ in the pre-bonding process, and wafer surface evenly applies 10kg/cm
2-15kg/cm
2Pressure, kept 1-2 hour; At last wafer is placed Ar compression ring border to heat-treat, be warmed up to 650-800 ℃ by room temperature, apply simultaneously 20 kg/cm
2-60 kg/cm
2Pressure, be incubated 2-3 hour, naturally cool to room temperature.
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| CN103643302A (en) * | 2013-11-26 | 2014-03-19 | 浙江上城科技有限公司 | Thermal sapphire compounding method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102570276A (en) * | 2012-01-09 | 2012-07-11 | 北京工业大学 | Preparation method of quasi-phase matching crystals for improving CO2 laser frequency multiplication efficiency |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102570276A (en) * | 2012-01-09 | 2012-07-11 | 北京工业大学 | Preparation method of quasi-phase matching crystals for improving CO2 laser frequency multiplication efficiency |
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| CN103643302A (en) * | 2013-11-26 | 2014-03-19 | 浙江上城科技有限公司 | Thermal sapphire compounding method |
| CN103643302B (en) * | 2013-11-26 | 2017-01-25 | 浙江上城科技有限公司 | Thermal sapphire compounding method |
| CN108493321A (en) * | 2018-03-26 | 2018-09-04 | 华灿光电（浙江）有限公司 | A kind of light-emitting diode chip for backlight unit and preparation method thereof |
| CN108823639A (en) * | 2018-07-09 | 2018-11-16 | 北京工业大学 | 1.5 micron wave length hot keys of one kind and laser cooling preparation method |
| CN109942209A (en) * | 2019-04-25 | 2019-06-28 | 北京工业大学 | A kind of Yb codoped phosphate glass is bonded the preparation method of slab guide with magnesium fluoride crystal |
| WO2021208365A1 (en) * | 2020-04-17 | 2021-10-21 | 中国电子科技南湖研究院 | Method for preparing large-size single crystal |
| WO2021208363A1 (en) * | 2020-04-17 | 2021-10-21 | 中国电子科技南湖研究院 | Device for preparing large-size single crystal |
| WO2021208364A1 (en) * | 2020-04-17 | 2021-10-21 | 中国电子科技南湖研究院 | Hot isostatic pressing bonding method for high-purity semiconductor single crystal |
| CN112921402A (en) * | 2021-01-16 | 2021-06-08 | 北京工业大学 | Improve CO2Method for frequency doubling efficiency of laser |
| CN115161770A (en) * | 2021-04-06 | 2022-10-11 | 中国科学院福建物质结构研究所 | Rare earth ion doped gallium tetraborate crystal, bonded crystal, and preparation method and application of crystal |
| CN115182047A (en) * | 2021-04-06 | 2022-10-14 | 中国科学院福建物质结构研究所 | Self-activated gallium tetraborate crystal, bonded crystal, and preparation method and application of crystal |
| CN115308939A (en) * | 2022-10-12 | 2022-11-08 | 光奥科技（武汉）有限公司 | Acousto-optic deflector adopting novel relaxor ferroelectric single crystal and preparation method thereof |
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