CN104868050A - Method of manufacturing thin film on substrate with different thermal expansion coefficient from original substrate - Google Patents
Method of manufacturing thin film on substrate with different thermal expansion coefficient from original substrate Download PDFInfo
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Abstract
The invention discloses a method of manufacturing a thin film on a substrate with a different thermal expansion coefficient from an original substrate. The method comprises steps: ions are injected on the surface of the original substrate in an ion injection method; the original substrate after ion injection is heated; the substrate is contacted with a thin film layer of the original substrate, the original substrate and the substrate are bonded together by using a wafer bonding method at room temperature, and thus a bonding body is formed, wherein the thermal expansion coefficient of the substrate is different from that of the original substrate; in a condition with temperature lower than 190 DEG C, the bonding body is heated for a preset time, and the thin film layer and a residual layer are separated; and after the thin film layer and the residual layer are separated, annealing treatment is carried out on the thin film layer. Manufacturing of the thin film on the substrate with a different thermal expansion coefficient from the original substrate is realized, and a thin film which has the advantages of large size, nanometer thickness, uniform film thickness, and low defect density can be manufactured.
Description
Technical field
The present invention relates to a kind of method manufacturing film in the substrate different from the thermal coefficient of expansion of original substrate, specifically, relate to the manufacture method of film of a kind of nanometer grade thickness, uniform film thickness, fabricating low-defect-density.
Background technology
LiNbO_3 film and lithium tantalate thin film have been widely used at field tools such as optical signal prosessing, information storage and electronic devices, it can as base material, may be used for making high frequency, high bandwidth, high integration, Large Copacity, the optoelectronics device of low-power consumption and integrated optical device, such as, filter, optical waveguide modulator, optical waveguide switch, spatial light modulator, optical frequency doubler, surface acoustic wave generator, Infrared Detectors and ferroelectric storage etc.Form LiNbO_3 film or lithium tantalate thin film on a silicon substrate, can realize and the production technology of existing silica-base material and production line compatibility, thus machinability and the range of application of LiNbO_3 film or lithium tantalate thin film can be improved.
1992, Bruel proposed a kind of method from stripping film semi-conducting material, and its key step comprises: carry out ion implantation to original substrate; By original substrate and target base plate (that is, substrate) bonding, form bonding body; Bonding body is added thermal release; To techniques such as thin-film surface polishings.This method is widely used in the making of the materials such as silicon-on-insulator (SOI).In this approach, thermal release is a very crucial step, and thermal release has two effects, and first effect is the bonding force (that is, strengthening the bonding force between original substrate and substrate) that can strengthen between bonding wafer; Second effect is the energy that the constraint making the ion be distributed in separating layer obtain being enough to the lattice structure departing from original substrate material disconnects to make the key formed between them, become gas atom (such as, helium), or meet with the injection ion that another departs from, become gas molecule (such as, hydrogen), thus form the bubble that diameter is several nanometer, when the quantity of bubble gets more and more, bubble is connected to each other, and realizes the stripping of film.
Generally, the ion in separating layer forms speed and the temperature exponentially relation of bubble.When heating-up temperature, higher than separation temperature, (separation temperature refers to that the ion be distributed at this temperature in separating layer can form a large amount of bubbles, the stripping of film can be completed after heating certain hour) time can form bubble rapidly, when heating-up temperature is lower than separation temperature, the speed that ion forms bubble can reduce greatly.But, when the thermal coefficient of expansion of original substrate and substrate differs greatly, such as original substrate is lithium niobate crystal chip, when substrate is silicon wafer, the thermal coefficient of expansion of lithium niobate is approximately 2 ~ 8 times of silicon, when the material that these two kinds of thermal coefficient of expansions differ greatly forms bonding body, after heating-up temperature exceedes certain threshold value, because thermal coefficient of expansion is inconsistent, expansion strength and the heating-up temperature of material are linear, the expansion difference of the material that the higher two kinds of thermal coefficient of expansions of heating-up temperature are different is larger, when this difference exceed material bear the limit time, bonding body drawing crack will be drawn broken, this threshold temperature is claimed to be cracked temperature.In addition, when original substrate is lithium niobate crystal chip, when substrate is silicon wafer, the cracked temperature of the bonding body formed is lower than its separation temperature, thus heating-up temperature is reduced under guarantee bonding body is not drawn broken prerequisite by drawing crack, cannot ensure that again thin layer intactly strips down from original substrate.Therefore, said method is utilized in the substrate different from the thermal coefficient of expansion of original substrate, film can not to be made well.
Summary of the invention
One object of the present invention is to provide a kind of method manufacturing film in the substrate different from the thermal coefficient of expansion of original substrate, and described method can produce the film of nanometer grade thickness, uniform film thickness, fabricating low-defect-density.
The invention provides a kind of method manufacturing film, described method comprises: by ion implantation by the surface of ion implantation to original substrate, thus in original substrate, form thin layer, separating layer and remaining matter layer, wherein, thin layer is positioned at the surface of original substrate, separating layer is between thin layer and remaining matter layer, and the ion distribution of injection is in separating layer; Original substrate after ion implantation is heated, obtains to make the ion be distributed in separating layer making ion to form bubble and energy that described bubble can not make the thin layer of original substrate come off or damage; Make the thin film layer of substrate and original substrate, and then at room temperature utilize bonding chip method original substrate and substrate to be bonded together, to form bonding body, wherein, substrate is different from the thermal coefficient of expansion of original substrate; The heating of para-linkage body reaches the scheduled time under lower than the condition of 190 DEG C, and thin layer is separated with remaining matter layer; After thin layer is separated with remaining matter layer, to thin layer heating, to carry out annealing in process.
According to embodiments of the invention, in the step that the original substrate after ion implantation is heated, the original substrate after ion implantation is heated 0.5h ~ 10h under the condition of 200 DEG C ~ 450 DEG C.
According to embodiments of the invention, in the step that the original substrate after ion implantation is heated, the original substrate after ion implantation is heated 3h under the condition of 220 DEG C.
According to embodiments of the invention, in the step of para-linkage body heating, under the condition of 50 DEG C ~ 190 DEG C, heat bonding body reach the scheduled time.
According to embodiments of the invention, the described scheduled time is 1h ~ 150h.
According to embodiments of the invention, in the step that thin layer is heated, under the condition of 250 DEG C ~ 550 DEG C, thin layer is heated to carry out annealing in process.
According to embodiments of the invention, in the step that thin layer is heated, normal pressure or be greater than 1 atmospheric pressure and under being less than 300 atmospheric atmospheric conditions to thin layer heating to carry out annealing in process.
According to embodiments of the invention, under the atmosphere of oxygen or nitrogen, perform the step to thin layer heating.
According to embodiments of the invention, described original substrate is lithium niobate crystal chip or lithium tantalate wafer, and described substrate is silicon wafer or silica wafers.
According to embodiments of the invention, described method also comprises: after the step heated thin layer, carries out surface finish process to thin layer.
Core of the present invention is: the mechanical strength near the separating layer first reducing original substrate, namely, original substrate after ion implantation is heated, with the energy that the quantity making the ion be distributed in separating layer of original substrate obtain to be enough to be formed bubble and these bubbles is not enough to make the thin layer of original substrate to come off or damages, thus make that the structure near separating layer becomes loose, mechanical strength reduction.Afterwards, the bonding body formed is heated certain hour at lower than the cracked temperature (generally lower than 190 DEG C) of bonding body, thin layer is transferred in substrate.With in the process of the heating lower than cracked temperature, the bonding force between original substrate and substrate can be greatly improved; The ion be distributed in separating layer continues to become bubble along with the carrying out of heating, makes the structure near separating layer more loose; Interactional stress is produced between the original substrate causing two kinds of thermal coefficient of expansions different due to heating and substrate; And then under the impact of these three kinds of factors, thin layer is transferred in substrate under the condition lower than cracked temperature, efficiently avoid and occur that bonding body is drawn broken problem by drawing crack, achieve and make film in the substrate different from the thermal coefficient of expansion of original substrate.
The invention has the beneficial effects as follows: the film that large scale, nanometer grade thickness, uniform film thickness, fabricating low-defect-density can be prepared.
Accompanying drawing explanation
By below in conjunction with exemplarily illustrating the description that the accompanying drawing of an example carries out, above and other object of the present invention and feature will become apparent, wherein:
Fig. 1 is the FB(flow block) of the method that manufacture film of the present invention is shown;
Fig. 2 is the schematic diagram that the step being formed thin layer, separating layer and remaining matter layer by ion implantation is shown;
Fig. 3 is the schematic diagram that the step that the original substrate after to ion implantation heats is shown;
Fig. 4 illustrates that the original substrate after by heating and substrate carry out bonding to form the schematic diagram of the step of bonding body;
Fig. 5 is the schematic diagram that the step that para-linkage body carries out heating to make the thin layer of original substrate to peel off is shown;
Fig. 6 is the schematic diagram that film product is shown.
Embodiment
Below in conjunction with accompanying drawing, the method manufacturing film in the substrate different from the thermal coefficient of expansion of original substrate of the present invention is described in detail.
Present inventor finds, when carrying out ion implantation to original substrate, the degree of depth forming separating layer in original substrate can be controlled according to the energy of ion implantation, namely, during, the conditions constant that inject ion certain at the thickness of the original substrate chosen, can be made into homogeneous, the constitutionally stable original substrate of character that ion implantation is crossed.Then, original substrate after ion implantation is heated, the energy that the quantity obtaining being enough to being formed bubble and these bubbles to enable the ion be distributed in separating layer is not enough to make the thin layer of original substrate to come off or damage, thus make that the structure near separating layer becomes loose, mechanical strength reduces, namely by adjustment heating-up temperature with accurately can control thin layer heating time and be in and be separated critical state.At this moment stop heating, by original substrate and substrate bonding, form bonding body.Finally, thin layer can be made by bonding body at a lower temperature to strip down from original substrate, and transfer in substrate, thus form film.
Therefore, the invention provides a kind of method manufacturing film.Fig. 1 shows the flow chart of the method for manufacture film of the present invention.
As shown in Figure 1, the method for manufacture film of the present invention comprises: by ion implantation by the surface imp lantation of ion facing to original substrate, form thin layer, separating layer and remaining matter layer; Original substrate after ion implantation is heated; Bonding is carried out, to form bonding body to the original substrate after heating and substrate; Para-linkage body carries out heating thin layer is separated with remaining matter layer; Annealing in process is carried out to thin layer; And suprabasil thin layer is carried out surface finish process.
The method according to manufacture film of the present invention is described in detail below with reference to Fig. 2 to Fig. 6.Fig. 2 to Fig. 6 is the schematic configuration diagram of the method illustrated according to making film of the present invention.
Fig. 2 is the schematic diagram that the step being formed thin layer, separating layer and remaining matter layer by ion implantation is shown.
As shown in Figure 2, use ion implantation, the upper surface 5 of ion 6 (can be molecular ion) facing to original substrate 1 is injected, form separating layer 3, original substrate 1 is divided into upper and lower Liang Ge district by separating layer 3: a region being the overwhelming majority and injecting the equal process of ion 6, is called thin layer 2; Another be the overwhelming majority inject ion 6 without region, be called remaining matter layer 4.The thickness of thin layer 2 is decided (such as, helium ion energy can be 10keV ~ 2000keV, and the thickness of the thin layer corresponding with this helium ion energy is between 25nm ~ 4500nm) by the energy of ion implantation.Here, ion implantation is injected in the segmentation that ion implantation can comprise conventional ion implanters injection method, plasma soaks ion implantation and different implantation temperature.Wherein, the ion injected in ion implantation can be at least one of hydrogen ion and helium ion.As an embodiment of the invention, when manufacturing LiNbO_3 film or lithium tantalate thin film, original substrate can be lithium niobate crystal chip or lithium tantalate wafer.
The object of execution ion implantation is the top layer in order to a large amount of ions 6 being injected into original substrate 1, ion 6 in separating layer 3 plays pendulum in original substrate 1, ion 6 embeds in lattice defect, produce bulk strain, cause separating layer 3 to become area of stress concentration, thus make the weak mechanical strength of original substrate 1 part near separating layer 3.
Fig. 3 is the schematic diagram that the step that the original substrate after to ion implantation heats is shown.
As shown in Figure 3, original substrate 1 after ion implantation is heated, with the energy that the quantity making the ion 6 in the separating layer 3 of original substrate 1 obtain to be enough to be formed bubble and these bubbles is not enough to make the thin layer 2 of original substrate 1 to come off or damages, thus make that the structure near separating layer 3 becomes loose, mechanical strength reduction.By the temperature and time controlling to heat original substrate 1 in this step, mechanical strength near the separating layer 3 that can reduce original substrate 1 further, make when heating the bonding body of follow-up formation, even if the ion at a lower temperature, in separating layer 3 also can obtain the energy being enough to make thin layer 2 be separated with remaining matter layer 4.
According to the present invention, the original substrate 1 after ion implantation can be heated 0.5h ~ 10h under the condition of 200 DEG C ~ 450 DEG C.In this heating temperature range, the speed that the ion injected in separating layer produces bubble is more moderate, is convenient to the control of working condition (such as, heating time), thus makes thin layer accurately can reach the critical state of separation.Such as, but when heating-up temperature is lower than 200 DEG C, heating time is longer, is unfavorable for the raising of production efficiency, when He isotopic geochemistry dosage is 4 × 10
16ions/cm
2time, at 150 DEG C, heating still can not produce the short texture that enough bubbles make separating layer in 200 hours in separating layer, namely can not reach separation critical condition.When heating-up temperature is higher than 450 DEG C, ion in separating layer can produce a large amount of bubble in the short time makes thin layer come off or cracked, such as, when He isotopic geochemistry dosage is 4 × 10
16ions/cm
2time, at 460 DEG C, heating will make thin layer cracked for 0.3 minute, and heating time is too short, is unfavorable for the control of heating time, thus causes the repeatability produced in batches to decline; In addition, heating time is too short, and Temperature Distribution on wafer can be made to be not easy to reach uniformity, some place on wafer is reached and is separated critical state, and some place does not still reach the critical state that is separated, thus cause the imperfect of follow-up thin layer stripping, affect rate of finished products.
As an embodiment of the invention, original substrate 1 after ion implantation can be heated 1h ~ 5h (preferably under the condition of 200 DEG C ~ 250 DEG C, 3h is heated) under the condition of 220 DEG C, wafer can either be made to be heated evenly under this heating-up temperature with the condition of heating time and wafer can be made to reach to be separated critical condition, thus be conducive to the raising of production efficiency.
Fig. 4 illustrates that the original substrate after by heating and substrate carry out bonding to form the schematic diagram of the step of bonding body.
As shown in Figure 4, utilize bonding chip method, at room temperature make original substrate 1 and substrate 7 be bonded together, form bonding body 8.According to the present invention, bonding chip method can be selected from Direct Bonding method, anode linkage method, low-temperature bonding method, vacuum bonding method, plasma strengthening bonding method and bonding bonding method any one.For Direct Bonding method, have after hydrophilic wafer presses close to mutually at two, the hydroxyl (OH that surface is adhered to naturally
-) van der waals force (intermolecular force) can be relied on to attract each other, form bonding body 8.As an embodiment of the invention, when manufacturing LiNbO_3 film or lithium tantalate thin film, original substrate 1 can be lithium niobate crystal chip or lithium tantalate wafer, and substrate 7 (that is, target base plate) can be silicon wafer or silica wafers.
Fig. 5 illustrates that para-linkage body carries out heating the schematic diagram of the step that thin layer is separated with remaining matter layer.
As shown in Figure 5, bonding body 8 heating under lower than the condition of 190 DEG C is reached the scheduled time.In the process, hydroxyl (-OH) can generate oxygen key (-O-) by chemical reaction, and the bonding force between original substrate and substrate is greatly improved; The ion 6 at separating layer 3 place can continue to become bubble along with the carrying out of heating, makes the structure near separating layer 3 more loose; Interactional stress is produced between the original substrate 1 causing two kinds of thermal coefficient of expansions different due to heating and substrate 7.Under the effect of above-mentioned three kinds of factors, finally realize the stripping of thin layer 2, and thin layer 2 is transferred in substrate 7.Wherein, 1h ~ 150h can be heated under the condition of 50 DEG C ~ 190 DEG C, further preferably, 5h ~ 30h can be heated under the condition of 80 DEG C ~ 110 DEG C, more preferably, 10h can be heated under the condition of 95 DEG C.
Fig. 6 is the schematic diagram that film product is shown.
Film is being carried out in the step of annealing in process, film can carried out annealing in process under the condition of 250 DEG C ~ 550 DEG C, through lattice defect that thin layer 2 inside is formed with the bonding force improved between thin layer 2 and substrate 7 and when eliminating ion implantation.Thickness due to thin layer is nano-scale, this material is made to have higher ductility under nano-scale, therefore, even if higher than cracked temperature, namely under the condition of 250 ~ 500 DEG C, carry out annealing in process, thin layer also can not be made to occur phenomenon that is cracked or that damage.Wherein, except can to except film heating under the atmospheric condition of normal pressure, can also 1 atmospheric pressure be greater than and to film heating under being less than 300 atmospheric atmospheric conditions, to carry out annealing in process.In addition, can according to the demand to film product function, can 1 atmospheric pressure be greater than and pass into oxygen or nitrogen under being less than 300 atmospheric atmospheric conditions to carry out annealing in process, thus obtain the film product of different performance.
Finally, surface finish is carried out to the thin layer 2 in substrate 7, remove the loss layer (that is, separating layer 3) of ion implantation to obtain film product (as shown in Figure 6).
The detailed process that the present invention makes film is described in detail below in conjunction with embodiment.
Embodiment 1
Original substrate is lithium niobate crystal chip, and implantation dosage is 4 × 10
16ions/cm
2helium ion (He
1+), the energy of helium ion is 250keV.Lithium niobate crystal chip after ion implantation is heated 3 hours at 220 DEG C.Substrate is silicon wafer, at room temperature, two plates is carried out bonding, forms bonding body.Bonding body is heated 10 hours at 95 DEG C, realizes the stripping of film.By film annealing in process 5 hours at 400 DEG C.Utilize chemical mechanical polishing method (CMP) that thin layer is polished to target thickness, obtain film product.
Embodiment 2
Original substrate is lithium tantalate wafer, and implantation dosage is 2 × 10
16ions/cm
2helium ion (He
1+), the Implantation Energy of helium ion is 100keV.Lithium tantalate wafer after ion implantation is heated 5 hours at 240 DEG C.Substrate is silicon wafer, at room temperature, lithium tantalate wafer and silicon wafer is carried out bonding, forms bonding body.Bonding body is heated 8 hours at 105 DEG C, realizes the stripping of film.By film annealing in process 5 hours at 400 DEG C.Utilize chemical mechanical polishing method (CMP) that thin layer is polished to target thickness, obtain film product.
Embodiment 3
Original substrate is lithium niobate crystal chip, and implantation dosage is 6 × 10
16ions/cm
2helium ion (He
1+), the Implantation Energy of helium ion is 300keV.Lithium niobate crystal chip after ion implantation is heated 1 hour at 200 DEG C.Substrate is silicon wafer, at room temperature, lithium niobate crystal chip and silicon wafer is carried out bonding, forms bonding body.Bonding body is heated 5 hours at 90 DEG C, realizes the stripping of film.Film is annealed 5 hours at 400 DEG C.Utilize chemical mechanical polishing method (CMP) that thin layer is polished to target thickness, obtain film product.
Embodiment 4
Original substrate is lithium niobate crystal chip, and implantation dosage is 4 × 10
16ions/cm
2helium ion (He
1+), the Implantation Energy of helium ion is 600keV.Lithium niobate crystal chip after ion implantation is heated 5 hours at 220 DEG C.Substrate is silicon wafer, at room temperature, lithium niobate crystal chip and silicon wafer is carried out bonding, forms bonding body.Bonding body is heated 30 hours at 85 DEG C, realizes the stripping of film.Film is annealed 5 hours at 400 DEG C.Utilize chemical mechanical polishing method (CMP) that thin layer is polished to target thickness, obtain film product.
In sum, the method of manufacture film of the present invention, before carrying out bonding by original substrate after ion implantation and substrate, original substrate after ion implantation is heated, the ion be distributed in separating layer is made to obtain certain energy, the mechanical strength near the separating layer namely reducing original substrate; Afterwards, also can ensure that thin layer intactly strips down from original substrate even if heat the bonding body formed at lower temperature (that is, the cracked temperature of bonding body), and transfer in substrate.The present invention is designed cleverly by this, can effectively avoid occurring that bonding body is drawn broken problem by drawing crack, achieves and manufacture monocrystal thin films in the substrate different from the thermal coefficient of expansion of original substrate.
The method of manufacture film of the present invention has that technique is simple, controllable precise, without the need to advantages such as special setting realize.In addition, method of the present invention improves the qualification rate of film product.
The present invention can prepare the film of large scale, nanometer grade thickness, uniform film thickness, fabricating low-defect-density.
More than describe the preferred embodiment of the present invention in detail; but; the present invention is not limited to the detail in above-mentioned execution mode; within the scope of technical conceive of the present invention; can carry out multiple simple variant and combination to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
Claims (10)
1. in the substrate different from the thermal coefficient of expansion of original substrate, manufacture a method for film, described method comprises the steps:
By ion implantation by the surface of ion implantation to original substrate, thus in original substrate, form thin layer, separating layer and remaining matter layer, wherein, thin layer is positioned at the surface of original substrate, separating layer is between thin layer and remaining matter layer, and the ion distribution of injection is in separating layer;
Original substrate after ion implantation is heated, obtains to make the ion be distributed in separating layer making ion to form bubble and energy that described bubble can not make the thin layer of original substrate come off or damage;
Make the thin film layer of substrate and original substrate, and then at room temperature utilize bonding chip method original substrate and substrate to be bonded together, to form bonding body, wherein, the thermal coefficient of expansion of substrate is different from the thermal coefficient of expansion of original substrate;
The heating of para-linkage body reaches the scheduled time under lower than the condition of 190 DEG C, and thin layer is separated with remaining matter layer;
After thin layer is separated with remaining matter layer, to thin layer heating, to carry out annealing in process.
2. method according to claim 1, wherein, in the step heated the original substrate after ion implantation, heats 0.5h ~ 10h by the original substrate after ion implantation under the condition of 200 DEG C ~ 450 DEG C.
3. method according to claim 1 and 2, wherein, in the step heated the original substrate after ion implantation, heats 3h by the original substrate after ion implantation under the condition of 220 DEG C.
4. method according to claim 1, wherein, in the step of para-linkage body heating, heats bonding body and reaches the scheduled time under the condition of 50 DEG C ~ 190 DEG C.
5. the method according to claim 1 or 4, wherein, the described scheduled time is 1h ~ 150h.
6. method according to claim 1, wherein, in the step heated thin layer, heats thin layer to carry out annealing in process under the condition of 250 DEG C ~ 550 DEG C.
7. the method according to claim 1 or 6, wherein, in the step that thin layer is heated, normal pressure or be greater than 1 atmospheric pressure and under being less than 300 atmospheric atmospheric conditions to thin layer heating to carry out annealing in process.
8. method according to claim 7, wherein, performs the step to thin layer heating under the atmosphere of oxygen or nitrogen.
9. method according to claim 1, wherein, described original substrate is lithium niobate crystal chip or lithium tantalate wafer, and described substrate is silicon wafer or silica wafers.
10. method according to claim 1, wherein, described method also comprises: after the step heated thin layer, carries out surface finish process to thin layer.
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| CN112259678B (en) * | 2020-10-19 | 2022-07-19 | 济南晶正电子科技有限公司 | Method for improving burst of thin film layer and thin film material |
| CN112499582A (en) * | 2020-11-25 | 2021-03-16 | 天津津航技术物理研究所 | Preparation method of tunable FP optical filter based on thin film bonding |
| CN112540428A (en) * | 2020-12-09 | 2021-03-23 | 珠海光库科技股份有限公司 | Lithium niobate single crystal thin film chip and manufacturing method thereof |
| CN112540428B (en) * | 2020-12-09 | 2023-02-21 | 珠海光库科技股份有限公司 | Lithium niobate single crystal thin film chip and manufacturing method thereof |
| CN113193109A (en) * | 2021-04-30 | 2021-07-30 | 济南晶正电子科技有限公司 | Preparation method of composite film and composite film |
| CN117096065A (en) * | 2023-10-17 | 2023-11-21 | 天通控股股份有限公司 | Bonding method of large-size ultrathin lithium tantalate wafer |
| CN117096065B (en) * | 2023-10-17 | 2024-01-30 | 天通控股股份有限公司 | Bonding method of large-size ultrathin lithium tantalate wafer |
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