CN111192853A - Epitaxial layer material stripping method based on 3D laminated mask substrate - Google Patents
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- CN111192853A CN111192853A CN202010025960.9A CN202010025960A CN111192853A CN 111192853 A CN111192853 A CN 111192853A CN 202010025960 A CN202010025960 A CN 202010025960A CN 111192853 A CN111192853 A CN 111192853A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/77—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate
- H01L21/78—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices
- H01L21/7806—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices involving the separation of the active layers from a substrate
- H01L21/7813—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices involving the separation of the active layers from a substrate leaving a reusable substrate, e.g. epitaxial lift off
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—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
- 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
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
Abstract
The invention discloses an epitaxial material stripping method based on a 3D laminated mask substrate, which is used for epitaxial growth and stripping of III-V group compound semiconductor materials such as GaN and the like and belongs to the technical field of photoelectrons. The substrate structure comprises a substrate, wherein a bottom mask layer, an intermediate layer and a top mask layer are sequentially arranged on the substrate; wherein the windows of the bottom mask layer and the windows of the top mask layer are staggered. The invention also provides a preparation method of the substrate structure and an epitaxial layer stripping method based on the structure. Compared with the prior art, the invention provides a more optimized stripping method, improves the stripping success rate, shortens the stripping time and has higher use value.
Description
Technical Field
The invention belongs to the technical field of photoelectrons, and particularly relates to an epitaxial layer material stripping method based on a 3D laminated mask substrate, which is used for epitaxial growth and stripping of III-V group compound semiconductor materials such as GaN and the like.
Background
Currently, third generation semiconductor materials, represented by gallium nitride (GaN), have been used in many important fields, such as semiconductor lasers, radar for early warning devices, fast chargers, etc. Due to the lack of a homogeneous substrate, most of the growth of GaN materials is currently epitaxial using a heterogeneous substrate, such as a single crystal substrate of sapphire, silicon carbide, and the like. These foreign substrates have a large lattice mismatch and thermal mismatch with the GaN material and thus accumulate stress. In order to obtain a stress-free GaN material, the GaN material needs to be peeled off from the foreign substrate. In some application scenarios, because the high-power device has a high requirement on heat dissipation performance, for example, when the high-power device is applied to a radio-frequency power device on an early warning radar, the heat conductivity of a conventional substrate cannot meet the heat dissipation requirement, and therefore, the GaN material and the device need to be peeled off from the original heterogeneous substrate and bonded to the diamond heat sink with the highest heat conductivity again. In other applications, the device design of the flip-chip or vertical structure requires the original substrate to be peeled off and re-bonded to a new backplane. In summary, the substrate lift-off technology has become more and more important in the fields of GaN material growth and device fabrication, and the development of the high-efficiency and low-cost substrate lift-off technology will greatly promote the technological progress in the related fields.
Currently, there are several main categories of techniques for peeling GaN from foreign substrates: the first type is a laser lift-off method, in which an interface of GaN and a foreign substrate is vaporized using a laser light of a specific wavelength and a specific energy density, thereby being separated. The second type is a self-lift-off method, in which a thick film GaN is grown using HVPE technology, and a self-lift-off effect is generated using a large mismatch stress between the GaN thick film and a foreign substrate, so that the GaN is separated from the substrate. The third type is wet etching stripping, which is to deposit some easily-corroded materials and structures in advance, then carry out GaN epitaxial growth, and then carry out wet etching by using corrosive liquid. The fourth type is a grinding and polishing method to remove the substrate, which mainly comprises the steps of grinding the substrate to be thin by a mechanical method and then grinding and polishing by a chemical mechanical method (CMP) until the original substrate is removed and a flat surface is obtained.
(1) Disadvantages of laser lift-off techniques:
a) in the process of laser stripping of the GaN substrate, the damage to the GaN substrate material is difficult to avoid. Patent US7256483 states that GaN after laser lift-off needs to be subjected to Chemical Mechanical Polishing (CMP) to reduce damage. The Chinese patent CN 105006446A adopts a femtosecond laser technology, reduces damage in a cold processing mode, and improves the quality of laser stripping. However, the method has special requirements on the laser light source, and the problem of epitaxial layer damage generated by laser cannot be solved fundamentally at present.
b) The laser lift-off technique is relatively costly. The laser equipment is sold at a price of millions per set, and the domestic supply factories are few, so that the stability of the equipment is to be improved.
c) The stripping efficiency is low. In order to improve the power density, the laser needs to be focused, so that the light spot is small, the point-by-point ablation achieves the stripping effect, and finally the time is long, so that the development of a more efficient and low-cost stripping technology becomes necessary.
d) The laser lift-off yield needs to be improved. Due to the fact that large mismatch stress exists between the substrate and the GaN epitaxial layer, during the stripping process, partial stress is still in the partial region due to partial region stress release, and therefore the GaN epitaxial layer can be cracked due to the non-uniform stress distribution, and the yield of finished products is reduced.
(2) Disadvantages of the self-peeling process:
a) self-lift-off methods typically require the growth of thicker GaN epitaxial layers. Generally, MOCVD and MBE methods are not suitable for growing a thick GaN epitaxial layer due to a slow growth rate, and HVPE methods are generally used to grow a thick GaN epitaxial layer. However, HVPE methods have several drawbacks that have not been overcome by themselves, such as parasitic growth issues, background doping issues, and the like.
b) The self-peeling yield is low. Since self-lift-off requires that the GaN epitaxial layer stress build-up be sufficiently large, during cooling, the stress further builds up due to the difference in the coefficients of thermal expansion of the substrate and GaN epitaxial layer, breaking and separating near the interface. It is possible that the planar GaN epitaxial layers are cracked prior to separation, thereby reducing yield. The larger the wafer size, the lower the self-strip yield.
c) The self-peeling substrate also has a fatal problem of crystal warpage. Because epitaxial GaN is in a strain state on a foreign substrate, partial stress can be gradually relaxed in the growth process, and after self-peeling, although the strain relaxation state in the crystal is not bound by the substrate any more, the strain relaxation state in the crystal is different, so the residual stress can cause the crystal to deform, the crystal is warped, the surface is not a plane any more, even if the surface can be ground flat by a CMP grinding and polishing process, the crystal plane orientation of the surface is not consistent all the time. The non-uniform crystal plane orientation can seriously affect the quality of subsequent epitaxial devices. And the larger the wafer size, the more severe the warpage.
d) As described in patent CN 103779185 a, the sacrificial layer can be preset in advance to control the self-peeling position of GaN, but the sacrificial layer usually reduces the GaN quality of the subsequent epitaxy, which is a method to increase the yield by replacing the crystal quality.
(3) The disadvantages of the wet etching stripping method are:
a) for conventional wet stripping methods, some corrosive material, such as SiO, needs to be deposited first2Then, photolithography is performed to expose the material growth region, a layer of material such as AlN is deposited, and GaN is epitaxially grown on the AlN material. The etching process is divided into two steps, firstly, hydrofluoric acid is used for etching SiO2Etching is carried out, and after the through channel is formed, the AlN layer is etched by KOH. As described in chinese patent CN 101794849B. The disadvantage of this method is that hydrofluoric acid is difficult to etch away SiO quickly without a void channel at the beginning2The etching process will gradually spread from the edge of the wafer to the center of the wafer, so the spreading speed is limited and the production efficiency is limited.
b) In addition, during the etching process using KOH in the second stage, a certain etching effect is generated on the GaN epitaxial layer. Since both the GaN dislocation outcrop region and the N-face contacting the substrate are susceptible to strong base corrosion, the use of KOH during the lift-off process can cause some damage to the GaN material.
(4) The polishing method has the following defects:
a) a certain mechanical stress is generated during the polishing process, and particularly when the material is already in a relatively thin state, the mechanical stress may break the material, resulting in a reduction in yield.
b) Sapphire and silicon carbide are both hard materials, the hardness of the materials is second to that of diamond, therefore, the polishing speed is slow, the used mechanical force is larger, and several hours are needed to complete the polishing of a sapphire substrate, so that the improvement of the production efficiency is not facilitated. Sapphire is a relatively inexpensive substrate that is used in large quantities for industrial production and is not negligible.
Disclosure of Invention
The invention provides an epitaxial layer material stripping method based on a 3D laminated mask substrate aiming at the problems.
The technical scheme adopted by the invention is as follows:
an epitaxial layer material stripping method based on a 3D laminated mask substrate comprises the following steps:
growing an epitaxial layer material on the 3D laminated mask substrate; the 3D laminated mask substrate comprises a bottom layer mask layer, a top layer mask layer and a middle layer positioned between the bottom layer mask layer and the top layer mask layer, and a window of the bottom layer mask layer is staggered from a window of the top layer mask layer by a certain distance; forming a gap between the epitaxial layer material which is bent and grown in the channel and the intermediate layer;
and corroding the 3D laminated mask substrate containing the grown epitaxial layer material in a corrosion solution to obtain the stripped epitaxial layer material.
Further, after the epitaxial layer material is grown and before the etching, a back plate bonding operation is performed on the epitaxial layer material.
Further, the back plate is a back plate for supporting, or a back plate circuit, or a back plate with high thermal conductivity.
Further, the etching solution is hydrofluoric acid solution or a mixture of hydrofluoric acid and other chemical agents.
Further, the process of corrosion includes:
the etching solution enters the gap between the epitaxial layer material and the intermediate layer to etch off SiO2An intermediate layer;
without the support of the middle layer, the epitaxial layer material between the window on the bottom mask and the window on the top mask is subjected to a twisting force and is broken, so that the stripped epitaxial layer material is obtained.
Further, the epitaxial layer is made of a III-V compound semiconductor material.
Further, the 3D stacked mask substrate is prepared by the steps of:
depositing an underlying mask layer on a substrate;
etching a window on the bottom mask layer;
depositing an intermediate layer on the underlying mask layer;
depositing a top mask layer on the intermediate layer;
preparing a window with the same pattern as the bottom mask layer on the top mask layer, and staggering a certain distance from the window on the bottom mask layer;
and etching the middle layer by using an etching solution to expose the window of the bottom mask layer.
Further, the bottom mask layer and the top mask layer are made of silicon nitride, and the middle layer is made of silicon dioxide.
Further, the etching is directly performed after the epitaxial layer material is grown; alternatively, the device is first fabricated on the epitaxial layer material and then the etching is performed.
The invention has the following beneficial effects:
1. compared with a laser stripping technology, the method has the advantages of low cost, higher efficiency, higher yield and less damage to materials.
2. The thickness of the GaN epitaxial layer is lower than that required by the self-stripping technology, so that shorter growth time is required, the efficiency can be improved, and the cost can be saved. And the stripping success rate is higher, and the stripped material has no problems of warping and the like.
3. Compared with the existing wet etching stripping technology, the method has fewer process steps, so that the efficiency can be improved, and the cost can be reduced. And can avoid damage to GaN caused by KOH corrosion. On the other hand, by adopting the 3D laminated mask substrate technology, the quality of the epitaxially grown GaN crystal is higher, and the level of the epitaxy of a homogeneous substrate can be almost achieved.
4. Compared with the grinding and polishing technology, the mechanical damage is less, and the period is shorter. Polishing is relatively time consuming.
Drawings
Fig. 1.3D stacked substrate fabrication process step flow diagram, shown as a cross-sectional view.
FIG. 2 is a structural diagram of a grown GaN layer, in which (a) is a schematic cross-sectional structure of the grown GaN layer, and (b) is a scanning electron microscope image of the actual structure, in which the structures of the two are completely corresponding.
FIG. 3 is a schematic diagram of a bonded backplane.
Fig. 4 is a schematic diagram of a fracture site.
FIG. 5 is a schematic diagram of the structure of the peeled sample.
In the figure: 1-a substrate; 2-a bottom mask layer; 3-an intermediate layer; 4-top mask layer; 5-epitaxial GaN layer, 6-void; 7-backplane, 8-bonding layer; 9-location of fracture by distortion.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, the present invention shall be described in further detail with reference to the following detailed description and accompanying drawings.
The key point of the technical scheme of the invention is the combination of the structure design of the pattern substrate and the wet etching process. In the aspect of substrate structure design, a novel 3D laminated substrate technology is mainly adopted, the technology is that the pattern positions of an upper mask layer and a lower mask layer are mutually deviated, and after a corrosion process, the connection of an upper mask layer window and a lower mask layer window is opened, so that GaN can meander from a bottom layer window to grow, and finally, GaN can drill out from a top layer window. As shown in fig. 1, the method specifically comprises the following steps:
1) an underlying mask layer 2 (first layer mask) is deposited on a substrate 1 as shown in fig. 1 (a). The substrate may be a sapphire, silicon carbide, or the like substrate, and the underlying mask layer may be a silicon nitride or the like material.
2) A first photolithography process is performed to etch a window in the underlying mask layer 2, as shown in fig. 1 (b).
3) An intermediate layer 3 having a support effect and a corrosion-prone feature is deposited on the underlying mask layer 2, as shown in fig. 1 (c). The intermediate layer 3 may be SiO2Materials, and the like.
4) A top mask layer 4 (second layer mask) is deposited on the intermediate layer 3, in the same process as the bottom mask, as shown in fig. 1 (d).
5) The top mask layer 4 is patterned with windows in the same pattern as the bottom mask 2, but the two are shifted by a certain distance (so that the vertical projections of the upper and lower windows do not overlap), as shown in fig. 1 (e).
6) The intermediate layer 3 is etched using hydrofluoric acid to expose the window of the underlying mask layer 2, as shown in fig. 1 (f), so that GaN material can be grown on the lowermost substrate through the curved channel space in the future.
And growing a GaN epitaxial material on the prepared 3D substrate by adopting an MOCVD method. With appropriate growth parameters, GaN can be grown from the channel and folded over the second layer of mask material into a GaN epitaxial layer covering the entire wafer. The preparation of various devices on the epitaxial layer can be continuously carried out and then the stripping can be carried out, and the stripping operation can also be directly carried out without preparing any device. The schematic structure of the grown GaN material is shown in fig. 2, where 5 is an epitaxial GaN layer and 6 is a void, which facilitates entry of etching solution during stripping.
The preparation stripping process is to perform a back-plate bonding operation to prevent the GaN epitaxial layer from being torn due to the thinness of the GaN epitaxial layer after stripping. As shown in fig. 3, where 7 is a backplane and 8 is a bonding layer. For backplanes with different functional requirements, there are different bonding processes. For example, a back plate which has a supporting function, a common flat sapphire substrate can be selected as the supporting back plate because the supporting back plate is cheap and easy to obtain, and a back plate with high thermal conductivity, such as diamond, SiC or high thermal conductivity metal, can be bonded. The bonding material can be selected from paraffin or PDMS. And uniformly coating a bonding material on the surface of the sample to be stripped, and bonding the back plate and the upper surface of the sample by heating or vacuum pumping and other operations. If flip-chip packaging is required on the backplane circuit, silicon or other materials can be selected as the backplane, and metals with ohmic contacts, such as Al/Ni/Ti/Au, can be selected as the bonding materials. And after the bonding metal is deposited on the backboard according to the circuit requirement, the backboard is bonded with the circuit of the backboard through a flip chip bonding technology.
After the back plates are bonded, putting a sample into the sample with the mass concentration of 30-4%And corroding for 3-5 min in 0% hydrofluoric acid solution. As the gaps in the structure form channels, HF solution can easily invade the whole gap pipeline system under the capillary action, and SiO is quickly corroded2An intermediate layer. Under the support of the middle layer, due to the direct mismatch stress of the GaN layer and the substrate, the GaN bent in the original channel can be subjected to twisting force and is broken at the weakest turning part, and the position where the GaN is twisted and broken is shown as 9 in fig. 4, so that the upper GaN epitaxial layer is separated from the original substrate. The stripping is followed by a cleaning and then the next process flow can be entered.
The first key point of the invention is that: this is a lift-off method for 3D stacked masks, that is, a set of methods for matching 3D stacked substrates with lift-off process parameters. The purpose is to obtain a peeled GaN epitaxial material conveniently at low cost. In the present invention, the 3D stacked substrate is one of the key points, and its key roles include:
the first key effect is that after the GaN epitaxial layer grows, gaps can be automatically left, the gap networks can enable corrosive liquid to rapidly enter the center of the wafer, the corrosion process is accelerated, the corrosion time is shortened, and due to the fact that the middle part and the edge are basically corroded synchronously, stress is released uniformly, and the GaN epitaxial layer is prevented from cracking in the stress nonuniform release process.
The second key effect is represented by the self-stripping process after etching. Since the misalignment of the upper and lower windows of the 3D stacked substrate causes GaN to grow in the curved channel, the bent corner regions are relatively weak regions, which are regions with concentrated defects, have low material strength, and are prone to fracture. After etching SiO with HF acid2After the middle layer is removed from support, the GaN at the bent part of the channel is subjected to large torsion and is broken, and self-separation is realized. The process saves the step of etching by using hot KOH solution, not only saves the time of the process step (including the time of secondary cleaning), but also effectively protects the GaN epitaxial layer from being etched by KOH and avoids reducing the performance of the GaN epitaxial layer.
A third key role is that the 3D stacked mask substrate has a great benefit on the improvement of the crystal quality of the GaN epitaxial layers. On the basis of an ELOG (epitaxial lateral growth) technology, by arranging a bent channel, misfit dislocation in the growth process of the GaN is filtered more effectively, and the crystal quality is greatly improved.
The second key point of the invention is that: in the corrosion stripping process, only one corrosion process is needed, namely, only HF acid is needed for 3-5 min. The process of usually needing KOH corrosion is omitted.
The etching solution in the invention can be hydrofluoric acid solution, and can also be a mixture of hydrofluoric acid and other chemical reagents.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and a person skilled in the art can modify the technical solution of the present invention or substitute the same without departing from the principle and scope of the present invention, and the scope of the present invention should be determined by the claims.
Claims (10)
1. A3D laminated mask substrate-based epitaxial layer material stripping method is characterized by comprising the following steps:
growing an epitaxial layer material on the 3D laminated mask substrate; the 3D laminated mask substrate comprises a bottom layer mask layer, a top layer mask layer and a middle layer positioned between the bottom layer mask layer and the top layer mask layer, and a window of the bottom layer mask layer is staggered from a window of the top layer mask layer by a certain distance; forming a gap between the epitaxial layer material which is bent and grown in the channel and the intermediate layer;
and corroding the 3D laminated mask substrate containing the grown epitaxial layer material in a corrosion solution to obtain the stripped epitaxial layer material.
2. The method of claim 1, wherein the epitaxial layer material is subjected to a back-plate bonding operation after the epitaxial layer material is grown and before the etching.
3. The method of claim 2, wherein the backplane is a supportive backplane, or a backplane circuit, or a high thermal conductivity backplane.
4. The method of claim 1, wherein the etching solution is a hydrofluoric acid solution or a mixture of hydrofluoric acid and other chemicals.
5. The method according to claim 4, wherein the concentration of the hydrofluoric acid solution is 30% to 40%.
6. The method of claim 1, wherein the process of corrosion comprises:
the etching solution enters the gap between the epitaxial layer material and the intermediate layer to etch off SiO2An intermediate layer;
without the support of the middle layer, the epitaxial layer material between the window on the bottom mask and the window on the top mask is subjected to a twisting force and is broken, so that the stripped epitaxial layer material is obtained.
7. The method of claim 1, wherein the epitaxial layer material is a III-V compound semiconductor material.
8. The method of claim 1, wherein the 3D stacked mask substrate is prepared by:
depositing an underlying mask layer on a substrate;
etching a window on the bottom mask layer;
depositing an intermediate layer on the underlying mask layer;
depositing a top mask layer on the intermediate layer;
preparing a window with the same pattern as the bottom mask layer on the top mask layer, and staggering a certain distance from the window on the bottom mask layer;
and etching the middle layer by using an etching solution to expose the window of the bottom mask layer.
9. The method of claim 1, wherein the bottom and top mask layers are silicon nitride and the middle layer is silicon dioxide.
10. The method according to any one of claims 1 to 9, wherein the etching is performed directly after the growth of the epitaxial layer material; alternatively, the device is first fabricated on the epitaxial layer material and then the etching is performed.
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| CN111785813A (en) * | 2020-06-05 | 2020-10-16 | 北京飓芯科技有限公司 | MicroLED preparation method based on three-dimensional mask substrate |
| CN114318523A (en) * | 2021-12-30 | 2022-04-12 | 吉林大学 | Large-size single crystal diamond epitaxial layer stripping method |
| CN114318527A (en) * | 2021-12-30 | 2022-04-12 | 吉林大学 | Growth and stripping method for large-size monocrystalline diamond film |
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