CN110660655A - Bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method - Google Patents
Bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method Download PDFInfo
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
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Abstract
The invention relates to a bubble-free and threading dislocation-free Ge/Si low-temperature bonding method which comprises the steps of processing Si and Ge substrate materials, crystallizing a Ge film, polishing and bonding Ge/Si. The method utilizes the loose structure of the polycrystalline Ge and the characteristic of existence of a crystal boundary to absorb and transfer bubbles of a Ge/Si bonding interface, and realizes the Ge/Si bonding interface without bubbles. And secondly, the Ge and Si single crystals are isolated by utilizing the disordered crystal orientation property of the polycrystalline Ge, so that the lattice mismatch between the Ge and the Si is relieved, the nucleation of threading dislocation can be effectively limited, and the further reduction of the threading dislocation density is realized.
Description
Technical Field
The invention relates to a novel bubble-free and threading dislocation-free Ge/Si low-temperature bonding method, in particular to a novel bubble-free and threading dislocation-free Ge/Si low-temperature bonding method realized by using the material properties of loose polycrystalline Ge, existence of crystal boundaries and no specific crystal orientation.
Background
In recent years, the preparation of high-temperature Si-based Ge thin films dominated by epitaxial techniques cannot further reduce the threading dislocation density in Ge thin films to 10 due to the inability to break through the technical limitations of lattice mismatch, low temperature growth, and the like6cm-2The following[1-3]. Although researchers have proposed many improved Ge/Si epitaxy techniques[4-7]However, the limiting mechanism of threading dislocation of the methods is to restrict the propagation and interaction of threading dislocation in the Ge thin film, and the limitation of threading dislocation nucleation in the Ge thin film is still inexperienced because the Ge thin film always makes direct contact with the Si substrate during epitaxy, and 4.2% lattice mismatch between Ge and Si is always unavoidable.
To further reduce threading dislocation density in Si-based Ge films, researchers turned their attention to Ge/Si heterobonding[8-13]. Kanbe et al[8,9]The Ge/Si wet hydrophilic bonding is researched by high-temperature annealing, namely, a Si sheet and a Ge sheet with hydrophilic surfaces after cleaning are bonded in deionized water and subjected to H bonding at 880 DEG C2And annealing for 90min in the atmosphere to realize Ge/Si bonding. Research shows that a transition layer with the thickness of tens of nanometers exists at a Ge/Si bonding interface, and severe interdiffusion and high-density threading dislocation exist in the transition layer. This indicates that high temperature Ge/Si bonding can form threading dislocations in the Ge layer, mainly because high temperature Ge/Si bonding cannot avoid forming dislocations in the Ge thin film due to not only lattice mismatch but also severe thermal mismatch between Ge and Si.
In recent years, Byun et al[10,11]And Gity et al[12,13]The system researches the application of plasma free radical activation in low-temperature Ge/Si bonding. Firstly, the surfaces of a cleaned Si wafer and a cleaned Ge wafer are processed by adopting different plasma free radicals (O and N), and then the two wafers are attached together and are hot-pressed in a bonding machine to realize Ge/Si bonding at the low temperature of 300 ℃. Although an oxide layer with the thickness of about 2nm is introduced into the Ge/Si bonding interface in this way to dredge bubbles formed at the bonding interface, the bubble density of the bonding interface is reduced, but the bubble density of the bonding interface is reducedIn this way, the bubbles at the bonding interface can not be removed effectively. On the other hand, the direct bonding of Ge/Si cannot effectively limit the lattice mismatch of the bonding interface and still cannot avoid the nucleation of dislocation because no other intermediate layer is arranged between Ge/Si to isolate two single crystals.
This patent adopts the polycrystal Ge that has loose structure and has the grain boundary to the hydrophilic H that reacts formation of bonding interface2O and H2And absorbing and transferring to realize the Ge/Si bonding without interface bubbles. On the other hand, the characteristic that the polycrystalline Ge has no specific crystal orientation is utilized to separate the Ge and the Si single crystal, so that the formation of lattice mismatch and the nucleation of dislocation are inhibited, and the Si-based Ge thin film material without threading dislocation is obtained.
Cited documents:
[1]Michel,J.,et al.(2010).High-performance Ge-on-Si photodetectors.Nature photonics,4(8),527.
[2]Osmond,J.,et al.(2009).Ultralow dark current Ge/Si(100)photodiodes with low thermal budget.Appliedphysics letters,94(20),201106.
[3]Nakamura,Y.,et al.Epitaxial growth ofhigh quality Ge films on Si(001)substrates by nanocontact epitaxy.Crystal Growth&Design,11(7),3301-3305.
[4]Liu,Z.,et al.(2017).48GHz high-performance Ge-on-SOI photodetector with zero-bias 40Gbps grown by selective epitaxial growth.Journal ofLightwave Technology,35(24),5306-5310.
[5]Chen,C.,et al.(2012).Epitaxial growth of germanium on silicon for light emitters.International Journal ofPhotoenergy,2012,1-8.
[6]Currie,M.T.,et al.(1998).Controlling threading dislocation densities in Ge on Si using graded SiGe layers and chemical-mechanicalpolishing.Applied Physics Letters,72(14),1718-1720.
[7]Li,Q.,Han,et al.(2003).Selective growth ofGe on Si(100)through vias ofSiO2nanotemplate using solid source molecular beam epitaxy.Applied Physics Letters,83(24),5032-5034.
[8]Kanbe,H.,et al.(2007).Analysis of a wafer bonded Ge/Si heterojunction by transmission electron microscopy.Applied Physics Letters,91(14),142119.
[9]Kanbe,H.,et al.(2010).Crystallographic properties of Ge/Si heterojunctions fabricatedby wet waferbonding.Journal ofelectronic materials,39(8),1248-1255.
[10]Byun,K.Y.,et al.(2012).Overview of low temperature hydrophilic Ge to Si direct bonding for heterogeneous integration.MicroelectronicsReliability,52(2),325-330.
[11]Byun,K.Y.,et al.(2011).Comprehensive investigation of Ge-Si bonded interfaces using oxygen radical activation.Journal ofApplied Physics,109(12),123529.
[12]Gity,F.,et al.(2012).Characterization of germanium/silicon p-n junction fabricated by low temperature direct wafer bonding and layerexfoliation.Applied Physics Letters,100(9),092102.
[13]Gity,F.,et al.(2012).Ge/Si pn diode fabricated by direct wafer bonding and layer exfoliation.ECS Transactions,45(6),131-139.
disclosure of Invention
The invention aims to solve the problems that the threading dislocation density in an epitaxial Si-based Ge film cannot be further reduced and bubbles at a Ge/Si heterogeneous bonding interface are difficult to eliminate, and provides a Ge/Si bonding interface which realizes zero bubbles by absorbing and transferring the bubbles at the Ge/Si bonding interface by utilizing the loose structure of polycrystalline Ge and the characteristic of existence of grain boundaries. And secondly, the Ge and Si single crystals are isolated by utilizing the disordered crystal orientation property of the polycrystalline Ge, so that the lattice mismatch between the Ge and the Si is relieved, the nucleation of threading dislocation can be effectively limited, and the further reduction of the threading dislocation density is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method comprises the following steps:
1) respectively and sequentially ultrasonically cleaning a Si sheet and a Ge sheet for 10-15 min by using acetone, ethanol and deionized water, and removing adsorbed particles and organic matters on the surface of a substrate;
2) firstly, the volume ratio of the Si pieces which are cleaned by the organic ultrasonic in the step 1) is H2SO4:H2O2Boiling the solution with the volume ratio of 4:1 for 10-15 min, washing with deionized water for 10-15 times, and then using HF to H to the Si sheet according to the volume ratio2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times;
3) firstly, using NH as volume ratio to treat the Si sheet treated by the step 2)4OH:H2O2:H2Boiling the solution with the ratio of O to 1:1:4 for 10-15 min, washing with deionized water for 10-15 times, and then using HF to H to the Si sheet according to the volume ratio2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times;
4) the Si sheet processed by the step 3) is firstly processed by HCl to H according to the volume ratio2O2:H2Boiling the solution with the ratio of O to 1:1:4 for 10-15 min, washing with deionized water for 10-15 times, and then using HF to H to the Si sheet according to the volume ratio2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times;
5) spin-drying the Si wafer treated in the step 4) by a glue spreader, putting the wafer into a magnetron sputtering system, and keeping the background vacuum degree of a sputtering chamber to be less than 1 multiplied by 10-4Pa, filling Ar gas with the purity of 5N into the sputtering chamber, and adjusting the flow of the Ar gas to ensure that the pressure in the sputtering chamber is 0.5 Pa;
6) sputtering a layer of amorphous Ge film of 40-90 nm on the surface of a Si sheet at room temperature, and regulating the speed of sputtering the amorphous Ge film by controlling the magnetron sputtering target current and the sample support rotating speed;
7) after the amorphous Ge film is sputtered in the step 6), the Ar gas flow is adjusted to ensure that the air pressure in the sputtering chamber is 0.78Pa, and 50nm SiO is sputtered on the amorphous Ge2As an annealing protection layer.
8) Sputtering the SiO by the step 7) above2The Si sheet is placed in an annealing furnace for high-temperature thermal annealing to change the amorphous Ge film into a polycrystalline Ge film; the thermal annealing is annealing at 600 ℃ for 5 min;
9) the volume ratio of HF to H adopted by the Si sheet after the annealing in the step 8) is2Solution infusion of 1: 20O ═ OSoaking for 5-10 min, washing for 10-15 times by using deionized water, and removing SiO on the surface of the polycrystalline Ge2。
10) Polishing the polycrystalline Ge film by the Si wafer processed in the step 9) through manual chemical mechanical polishing;
11) carrying out ultrasonic cleaning on the polished Si wafer in the step 10) for 10-15 min by adopting acetone, ethanol and deionized water respectively in sequence, washing for 10-15 times by using the deionized water, and removing adsorbed particles on the surface of the polycrystalline Ge;
12) the volume ratio of the Ge sheet cleaned in the step 1) and the Si sheet treated in the step 11) is HF to H2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times;
13) drying the Ge sheet and the Si sheet processed in the step 12) by a glue spreader and then attaching the Ge sheet and the Si sheet together;
14) and (3) putting the Ge/Si laminating sheet obtained in the step 13) into an annealing furnace for low-temperature thermal annealing, and annealing at 300 ℃ for 30h to realize low-temperature Ge/Si bonding.
The invention has the following remarkable advantages:
the invention innovatively provides an effective method for realizing a bubble-free Ge/Si bonding interface by utilizing the characteristics of looseness and existence of crystal boundary of polycrystalline Ge, and realizing the thorough isolation of Ge and Si single crystals by utilizing the characteristic of disordered crystal orientation of the polycrystalline Ge, so as to avoid lattice mismatch and dislocation nucleation, and radically and thoroughly eliminate bubbles of the bonding interface and thoroughly break the nucleation path of the dislocation mismatch.
Drawings
FIG. 1 is a test chart of an ultrasonic microscope for a Ge/Si bonding interface obtained in example 1 of the present invention;
FIG. 2 is a TEM test chart of a Ge/Si bonding interface obtained in example 1 of the present invention;
FIG. 3 is an ultrasonic microscope test chart of the Ge/Si bonding interface obtained in example 2 of the present invention.
Detailed Description
The following examples will further illustrate the present invention with reference to the accompanying drawings.
Example 1
The used equipment is a TRP-450 composite film sputtering deposition system, and two direct current target positions and a radio frequency target position are arranged in a growth chamber. The target material is a high-purity Ge circular target material with 5N (more than 99.999 percent). The Si substrate material used was an N-type single-crystal Si wafer having a crystal orientation of (100) and a single-side polished resistivity of 0.001. omega. cm, and the Ge substrate material used was an N-type single-crystal Ge wafer having a crystal orientation of (100) and a single-side polished resistivity of more than 50. omega. cm.
One, treatment of Si and Ge base materials
1) Selecting a Si and Ge substrate with a crystal orientation of (100), respectively and sequentially ultrasonically cleaning the Si and Ge substrate for 10-15 min by using acetone, ethanol and deionized water, and removing particles and organic matters attached to the surface of the substrate;
2) firstly, the volume ratio of the organic ultrasonically cleaned Si wafer is H2SO4:H2O2Boiling the solution with the volume ratio of 4:1 for 10-15 min, washing with deionized water for 10-15 times, and then using HF to H in the volume ratio2Soaking the mixture in a solution with the ratio of O to O being 1:20 for 2-4 mim, and washing the mixture with deionized water for 10-15 times;
3) followed by a volume ratio of NH4OH:H2O2:H2Boiling the solution with the ratio of O to 1:1:4 for 10-15 min, washing the solution with deionized water for 10-15 times, and then using HF to H in a volume ratio2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times;
4) finally, the volume ratio of HCl to H is2O2:H2Boiling the solution with the ratio of O to 1:1:4 for 10-15 min, washing the solution with deionized water for 10-15 times, and then using HF to H in a volume ratio2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times.
Second, crystallization, polishing and Ge/Si bonding of Ge film
1) Spin-drying the cleaned Si wafer for 30s at 4000 rpm by using a glue spreader, and putting the cleaned Si wafer into a sputtering deposition system until the background vacuum degree of a magnetron sputtering chamber is less than 1 × 10-4Pa, filling Ar gas with the purity of 5N into the sputtering chamber, controlling the pressure in the sputtering chamber by adjusting the gas flow, keeping the pressure in the sputtering chamber at 0.5Pa when the flow of the introduced gas is 6.5sccm, and simultaneously turning on a direct-current sputtering power supply;
2) at room temperature, adjusting the current of a direct-current sputtering power supply to be 0.3A, the voltage to be 406V and the rotating speed of a sample holder to be 10rpm, sputtering an amorphous Ge film with the thickness of 40nm on a Si substrate, and enabling the deposition rate to be 23 nm/min;
3) regulating the flow of Ar gas to 21sccm, keeping the air pressure in the sputtering chamber at 0.78Pa, turning on a magnetron sputtering radio-frequency power supply, regulating the radio-frequency power to 150W, and sputtering 50nm SiO on amorphous Ge2As an annealing protection layer;
4) SiO is sputtered off2Taking out the Si sheet of the film, placing the film in a tubular annealing furnace, adjusting the temperature of the tubular annealing furnace to 600 ℃, and annealing the sample for 5min at the heating rate of 5 ℃/min;
5) taking out the annealed Si wafer by adopting the volume ratio of HF to H2Soaking in a solution with the ratio of O to 1:20 for 5-10 min to remove SiO on the surface2Washing with deionized water for 10-15 times;
6) taking out the washed Si sheet, adhering the back of the Si sheet to a grinding table with the temperature of 70 ℃ on a heating plate by adopting paraffin, and then taking down the grinding table from the heating plate until the paraffin is solidified to ensure that the Si sheet is tightly adhered to the grinding table;
7) the volume ratio of compol80: H is adopted2Carrying out manual chemical mechanical polishing on the polycrystalline Ge film on a polyurethane polishing pad for 5min by using polishing solution with O being 1: 3;
8) after polishing, placing a grinding table on a heating plate at 70 ℃, taking down the Si sheet after paraffin is melted, sequentially ultrasonically cleaning the Si sheet for 10-15 min by using acetone, ethanol and deionized water respectively, washing the Si sheet for 10-15 times by using the deionized water, and removing adsorbed particles on the surfaces of the paraffin and the polycrystalline Ge;
9) the volume ratio of HF to H is adopted for the cleaned Ge sheet and the Si sheet2Soaking in a solution with the ratio of O to O being 1:20 for 2min, and washing with deionized water for 10-15 times;
10) spin-drying the washed Ge sheet and the washed Si sheet by using a glue spreader, then attaching the Ge sheet and the Si sheet together, and applying certain pressure to the attached sample by using fingers, so that the attachment strength of the attached sample is higher while interfacial bubbles are extruded;
11) putting the attached sample into a tubular annealing furnace, and annealing for 30h at 300 ℃, wherein the heating and cooling rate is 0.5 ℃/min;
12) carrying out ultrasonic microscopy on the annealed bonding sampleMirror test and TEM test, as shown in fig. 1 and fig. 2, respectively. As can be seen from fig. 1, few small bubbles formed by the hydrophilic reaction of the interface were observed at the bonding interface except for some large bubbles formed by surface particles and edge tweezer contamination. As can be seen from FIG. 2, the thickness of the bonding interface polycrystalline Ge after polishing is about 30nm, and no threading dislocation is found in the Ge layer at the bonding interface due to the lattice isolation effect of the polycrystalline Ge, which indicates that the threading dislocation density in the bonding Ge is less than 105cm-2。
Example 2
The used equipment is a TRP-450 composite film sputtering deposition system, and two direct current target positions and a radio frequency target position are arranged in a growth chamber. The target material is a high-purity Ge circular target material with 5N (more than 99.999 percent). The Si substrate material used was an N-type single-crystal Si wafer having a crystal orientation of (100) and a single-side polished resistivity of 0.001. omega. cm, and the Ge substrate material used was an N-type single-crystal Ge wafer having a crystal orientation of (100) and a single-side polished resistivity of more than 50. omega. cm.
One, treatment of Si and Ge base materials
1) Selecting a Si and Ge substrate with a crystal orientation of (100), respectively and sequentially ultrasonically cleaning the Si and Ge substrate for 10-15 min by using acetone, ethanol and deionized water, and removing particles and organic matters attached to the surface of the substrate;
2) firstly, the volume ratio of the organic ultrasonically cleaned Si wafer is H2SO4:H2O2Boiling the solution with the volume ratio of 4:1 for 10-15 min, washing with deionized water for 10-15 times, and then using HF to H in the volume ratio2Soaking the mixture in a solution with the ratio of O to O being 1:20 for 2-4 mim, and washing the mixture with deionized water for 10-15 times;
3) followed by a volume ratio of NH4OH:H2O2:H2Boiling the solution with the ratio of O to 1:1:4 for 10-15 min, washing the solution with deionized water for 10-15 times, and then using HF to H in a volume ratio2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times;
4) finally, the volume ratio of HCl to H is2O2:H2Boiling the solution with the ratio of O to 1:1:4 for 10-15 min, washing the solution with deionized water for 10-15 times, and then using HF to H in a volume ratio2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10min15 times.
Second, crystallization, polishing and Ge/Si bonding of Ge film
1) Spin-drying the cleaned Si wafer for 30s at 4000 rpm by using a glue spreader, and putting the cleaned Si wafer into a sputtering deposition system until the background vacuum degree of a magnetron sputtering chamber is less than 1 × 10-4Pa, filling Ar gas with the purity of 5N into the sputtering chamber, controlling the pressure in the sputtering chamber by adjusting the gas flow, keeping the pressure in the sputtering chamber at 0.5Pa when the flow of the introduced gas is 6.5sccm, and simultaneously turning on a direct-current sputtering power supply;
2) at room temperature, adjusting the current of a direct-current sputtering power supply to be 0.3A, the voltage to be 406V and the rotating speed of a sample holder to be 10rpm, sputtering an amorphous Ge film with the thickness of 90nm on a Si substrate, wherein the deposition rate is 23 nm/min;
3) regulating the flow of Ar gas to 21sccm, keeping the air pressure in the sputtering chamber at 0.78Pa, turning on a magnetron sputtering radio-frequency power supply, regulating the radio-frequency power to 150W, and sputtering 50nm SiO on amorphous Ge2As an annealing protection layer.
4) SiO is sputtered off2Taking out the Si sheet of the film, placing the film in a tubular annealing furnace, adjusting the temperature of the tubular annealing furnace to 600 ℃, and annealing the sample for 5min at the heating rate of 5 ℃/min;
5) taking out the annealed Si wafer by adopting the volume ratio of HF to H2Soaking in a solution with the ratio of O to 1:20 for 5-10 min to remove SiO on the surface2Washing with deionized water for 10-15 times;
6) taking out the washed Si sheet, adhering the back of the Si sheet to a grinding table with the temperature of 70 ℃ on a heating plate by adopting paraffin, and then taking down the grinding table from the heating plate until the paraffin is solidified to ensure that the Si sheet is tightly adhered to the grinding table;
7) the volume ratio of compol80: H is adopted2Carrying out manual chemical mechanical polishing on the polycrystalline Ge film on a polyurethane polishing pad for 5min by using polishing solution with O being 1: 3;
8) after polishing, placing a grinding table on a heating plate at 70 ℃, taking down the Si sheet after paraffin is melted, sequentially ultrasonically cleaning the Si sheet for 10-15 min by using acetone, ethanol and deionized water respectively, washing the Si sheet for 10-15 times by using the deionized water, and removing adsorbed particles on the surfaces of the paraffin and the polycrystalline Ge;
9) the volume ratio of HF to H is adopted for the cleaned Ge sheet and the Si sheet2Soaking in a solution with the ratio of O to O being 1:20 for 2-4 min, and washing with deionized water for 10-15 times;
10) spin-drying the washed Ge sheet and the washed Si sheet by using a glue spreader, then attaching the Ge sheet and the Si sheet together, and applying certain pressure to the attached sample by using fingers, so that the attachment strength of the attached sample is higher while interfacial bubbles are extruded;
11) putting the attached sample into a tubular annealing furnace to anneal for 30h at 300 ℃, wherein the heating and cooling rate is 0.5 ℃/min
12) The annealed bonded sample was subjected to ultrasonic microscopy as shown in fig. 3. As can be seen from the figure, few small bubbles formed by the hydrophilic reaction of the interface were observed at the bonding interface except for some large bubbles formed by surface particles and edge tweezer contamination.
Claims (10)
1. A bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method is characterized in that:
the method comprises the steps of processing Si and Ge substrate materials, crystallizing a Ge film, polishing and bonding Ge/Si.
2. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 1, characterized in that: the processing of the Si and Ge base materials specifically comprises the steps of:
s11, respectively and sequentially ultrasonically cleaning the Si sheet and the Ge sheet for 10 ~ 15min by using acetone, ethanol and deionized water, and removing adsorbed particles and organic matters on the surface of the substrate;
step S12, the Si pieces cleaned by the organic ultrasonic wave in the step S11 are firstly cleaned by H2SO4And H2O2Boiling the solution for 10 ~ 15min, washing with deionized water for 10 ~ 15 times, and treating the Si wafer with HF and H2Soaking in O solution for 2 ~ 4min, and washing with deionized water for 10 ~ 15 times;
step S13, the Si wafer processed in step S12 is first treated with NH4OH、H2O2And H2Boiling O solution for 10 ~ 15min, washing with deionized water for 10 ~ 15 times, and mixing with Si piecesWith HF and H2Soaking in O solution for 2 ~ 4min, and washing with deionized water for 10 ~ 15 times;
step S14, the Si pieces processed in step S13 are first treated with HCl and H in volume ratio2O2And H2Boiling O solution for 10 ~ 15min, washing with deionized water for 10 ~ 15 times, and treating Si wafer with HF and H2Soaking in O solution for 2 ~ 4min, and washing with deionized water for 10 ~ 15 times;
step S15, spin-drying the Si wafer processed in the step S14 by a glue spreader, and putting the Si wafer into a magnetron sputtering system until the background vacuum degree of a sputtering chamber is less than 1 multiplied by 10-4And Pa, filling Ar gas with the purity of 5N into the sputtering chamber, and adjusting the flow rate of the Ar gas to ensure that the pressure in the sputtering chamber is 0.5 Pa.
3. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 2, characterized in that: h in step S122SO4And H2O2The volume ratio of the solution is 4: 1; HF and H in step S122The volume ratio of O is: 1: 20; NH in step S134OH、H2O2And H2The volume ratio of O is 1:1: 4; HF and H in step S132The volume ratio of O is 1: 20; HCl and H in step S142O2And H2The volume ratio of O is 1:1: 4; HF and H in step S142The volume ratio of O is 1: 20.
4. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 1, characterized in that: the crystallization of the Ge film is specifically as follows:
step S21, sputtering a layer of amorphous Ge film of 40 ~ 90nm on the surface of the processed Si sheet at room temperature, and adjusting the speed of sputtering the amorphous Ge film by controlling the magnetron sputtering target current and the sample carrier rotating speed;
step S22, after the step S21 finishes sputtering the amorphous Ge film, the Ar gas flow is adjusted to ensure that the air pressure in the sputtering chamber is 0.78Pa, and 50nm SiO is sputtered on the amorphous Ge2As an annealing protective layer;
step S23, sputtering the SiO in the step S222The Si sheet is placed in an annealing furnace to carry out high-temperature thermal annealingThe crystal Ge film is changed into a polycrystal Ge film;
step S24, adopting HF and H for the Si sheet annealed in the step S232Soaking in O solution for 5 ~ 10min, washing with deionized water for 10 ~ 15 times, and removing SiO on the surface of the polycrystalline Ge2。
5. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 4, characterized in that: the thermal annealing in the step S23 is annealing at 600 ℃ for 5 min.
6. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 4, characterized in that: HF and H in step S242The volume ratio of O is 1: 20.
7. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 1, characterized in that: the polishing specifically comprises the following steps:
step S31, polishing the polycrystalline Ge film by the Si sheet after the crystallization treatment of the surface Ge film by adopting manual chemical mechanical polishing;
and S32, respectively and sequentially ultrasonically cleaning the polished Si wafer in the step S31 for 10 ~ 15min by using acetone, ethanol and deionized water, washing the Si wafer for 10 ~ 15 times by using the deionized water, and removing adsorbed particles on the surface of the polycrystalline Ge.
8. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 1, characterized in that: the Ge/Si bonding specifically comprises the following steps:
step S41: the Ge wafer cleaned by the substrate and the polished Si wafer are treated with HF and H2Soaking in O solution for 2 ~ 4min, and washing with deionized water for 10 ~ 15 times;
step S42: the Ge sheet and the Si sheet processed in the step S41 are dried by a glue spreader and then are attached together;
step S43: and (5) placing the Ge/Si laminating sheet obtained in the step (S42) into an annealing furnace for low-temperature thermal annealing to realize low-temperature Ge/Si bonding.
9. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 8, characterized in that: HF and H in step S412The volume ratio of O is 1: 20.
10. The bubble-free and threading dislocation-free Ge/Si heterogeneous hybrid integration method according to claim 8, characterized in that: the thermal annealing in the step S43 is specifically annealing at 300 ℃ for 30 h.
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