WO2012166298A1 - Low-temperature methods for spontaneous material spalling - Google Patents

Low-temperature methods for spontaneous material spalling Download PDF

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Publication number
WO2012166298A1
WO2012166298A1 PCT/US2012/036860 US2012036860W WO2012166298A1 WO 2012166298 A1 WO2012166298 A1 WO 2012166298A1 US 2012036860 W US2012036860 W US 2012036860W WO 2012166298 A1 WO2012166298 A1 WO 2012166298A1
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WO
WIPO (PCT)
Prior art keywords
layer
temperature
base substrate
stressor
stressor layer
Prior art date
Application number
PCT/US2012/036860
Other languages
French (fr)
Inventor
Maha M. Khayyat
Norma E. Sosa Cortes
Katherine L. Saenger
Stephen W. Bedell
Devendra K. Sadana
Original Assignee
International Business Machines Corporation
King Abdulaziz City For Science And Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by International Business Machines Corporation, King Abdulaziz City For Science And Technology filed Critical International Business Machines Corporation
Priority to GB1318741.4A priority Critical patent/GB2503851B/en
Priority to CN201280026784.4A priority patent/CN103582934A/en
Priority to DE112012002305.6T priority patent/DE112012002305T5/en
Publication of WO2012166298A1 publication Critical patent/WO2012166298A1/en

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture 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
    • H01L21/18Manufacture 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
    • H01L21/185Joining of semiconductor bodies for junction formation
    • H01L21/187Joining of semiconductor bodies for junction formation by direct bonding
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture 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
    • H01L21/18Manufacture 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
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26

Definitions

  • the present disclosure relates to semiconductor device manufacturing, and more particularly, to methods for controlling the removal of a surface layer from a base substrate utilizing low-temperature spontaneous spalling.
  • Efforts to (i) create thin-film substrates from bulk materials (i.e., semiconductors) and (ii) form thin-film device layers by removing device layers from the underlying bulk substrates on which they were formed are ongoing.
  • the controlled surface layer removal required for such applications has been successfully demonstrated using a process known as spalling; see U.S. Patent Application Publication No. 2010/0311250 to Bedell et al.
  • Spalling includes depositing a stressor layer on a substrate, placing an optional handle substrate on the stressor layer, and inducing a crack and its propagation below the substrate/stressor interface. This process, which is performed at room temperature, removes a thin layer of the base substrate below the stressor layer.
  • thin it is meant that the layer thickness is typically less than 100 microns, with a layer thickness of less than 50 microns being more typical.
  • the depth of at which the crack propagates is dictated by the thickness of the stressor layer, the inherent tensile stress of the stressor layer, and the fracture toughness of the base substrate being exfoliated (spalled).
  • control of the initiation of the release layer process (crack initiation and propagation) and uniformity in the thickness of the spalled material are difficult to achieve utilizing prior art spalling processes.
  • the present disclosure provides methods to (i) introduce additional control into a material spalling process, thus improving both the crack initiation and propagation, and (ii) increase the range of selectable spalling depths.
  • the methods of the present disclosure are spontaneous spalling processes which are performed below room temperature, not mechanical spalling processes which are performed at room temperature as disclosed, for example, in U.S. Patent Application Publication No. 2010/0311250 to Bedell et al.
  • spontaneous it is meant that the removal of a thin material layer from a base substrate occurs without the need to employ any manual means to initiate crack formation and propagation for breaking apart the thin material layer from the base substrate.
  • room temperature it is meant a temperature from 15°C to 40°C.
  • low-temperature spalling it is meant the removal of a material layer from a base substrate at a temperature below room temperature.
  • the method of the present disclosure includes providing a stressor layer on a surface of a base substrate at a first temperature which is room temperature; bringing the base substrate including the stressor layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
  • the method includes providing a stressor layer on a surface of a base substrate at a first temperature which is room temperature; bringing the base substrate including the stressor layer to a second temperature of less than 206 Kelvin (K); spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
  • K 206 Kelvin
  • the method includes providing a spall inducing tape layer on a surface of a base substrate at a first temperature which at approximately room temperature or slightly above (e.g., from 15°C to 60°C); bringing the base substrate including the spall inducing tape layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
  • the method of the present disclosure includes providing a two-part stressor layer on a surface of a base substrate, wherein a lower part of the two-part stressor layer is formed at a first temperature which at approximately room temperature or slightly above (e.g., from 15°C to 60°C), wherein an upper part of the two-part stressor layer comprises a spall inducing tape layer at an auxiliary temperature which is room temperature; bringing the base substrate including the two-part stressor layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
  • a first temperature which at approximately room temperature or slightly above (e.g., from 15°C to 60°C)
  • an upper part of the two-part stressor layer comprises a spall inducing tape layer at an auxiliary temperature which is room temperature
  • bringing the base substrate including the two-part stressor layer to a second temperature which is less than room temperature
  • the effective stress that induces material spalling is modified owing to differential thermal expansion, crystal structure changes at the crack front, fracture toughness value differences at lower-than-room temperatures, to reach a stress regime necessary for spalling-type fracture that would not be reached using the room temperature spalling technique disclosed in U.S. Patent Application Publication No.
  • One advantage of the aforementioned spalling methods of the present disclosure is that the layer release process is spontaneous at all stages of the process, from spall initiation through spall completion. Another advantage of the present methods is that the component of stressor layer stress due to thermal expansion mismatch stress is reversible and will disappear upon warming back to room temperature, thus providing a spalled stressor layer/spalled film couple that is flatter at room temperature than at the temperature at which it was spalled. Yet another advantage of the present methods is that they widen the process window for controlled, spontaneous spalling: base substrates including stressor layers having thickness/stress values lower than the threshold required for spalling at room temperature can be safely stored at room temperature until spontaneous spalling is deliberately introduced by a temperature reduction.
  • FIG. 1 is a pictorial representation (through a cross sectional view) illustrating a base substrate that can be employed in one embodiment of the present disclosure.
  • FIG. 2 is a pictorial representation (through a cross sectional view) illustrating the base substrate of FIG. 1 after forming an optional metal-containing adhesion layer on a surface of the base substrate.
  • FIG. 3 is a pictorial representation (through a cross sectional view) illustrating the structure of FIG. 2 after forming a stressor layer and/or spall inducing tape layer on a surface of the optional adhesion layer.
  • FIG. 4 is a pictorial representation (through a cross sectional view) illustrating the structure of FIG. 3 after forming an optional handle substrate atop the stressor layer.
  • FIG. 5 is a pictorial representation (through a cross sectional view) illustrating the structure of FIG. 4 after removing an upper portion of the base substrate by utilizing a low- temperature spontaneous spalling method of the present disclosure.
  • FIGS. 1-5 illustrate the basic processing steps of the method of the present disclosure which spalls, i.e., exfoliates, a material layer from a base substrate in a controlled manner.
  • the material layer that is spalled is thin and may or may not include one of more devices thereon.
  • the term "thin" is used to denote that the material layer that is spalled has a thickness that is typically less than 100 microns, with a thickness of less than 50 microns being more typical.
  • FIGS. 1 -5 illustrate a low-temperature spontaneous spalling method that includes providing a stressor layer on a surface of a base substrate at a first temperature which is at room temperature; bringing the base substrate including the stressor layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature, e.g., the first temperature.
  • the base substrate 10 having an upper surface 12 that can be employed in the present disclosure.
  • the base substrate 10 employed in the present disclosure may comprise a semiconductor material, a glass, a ceramic, or any another material whose fracture toughness is less than that of the stressor layer to be subsequently formed.
  • Fracture toughness is a property which describes the ability of a material containing a crack to resist fracture. Fracture toughness is denoted K lc . The subscript Ic denotes mode I crack opening under a normal tensile stress perpendicular to the crack, and c signifies that it is a critical value. Mode I fracture toughness is typically the most important value because spalling mode fracture usually occurs at a location in the substrate where mode II stress (shearing) is zero, and mode III stress (tearing) is generally absent from the loading conditions. Fracture toughness is a quantitative way of expressing a material's resistance to brittle fracture when a crack is present.
  • the base substrate 10 comprises a semiconductor material
  • the semiconductor material may include, but is not limited to, Si, Ge, SiGe, SiGeC, SiC, Ge alloys, GaSb, GaP, GaAs, InAs, InP, and all other III-V or II-VI compound semiconductors.
  • the base substrate 10 is a bulk semiconductor material.
  • the base substrate 10 may comprise a layered semiconductor material such as, for example, a semiconductor-on- insulator or a semiconductor on a polymeric substrate. Illustrated examples of semiconductor- on-insulator substrates that can be employed as base substrate 10 include silicon-on-insulators and silicon-germanium-on-insulators .
  • the semiconductor material can be doped, undoped or contain doped regions and undoped regions.
  • the semiconductor material that can be employed as the base substrate 10 can be single crystalline (i.e., a material in which the crystal lattice of the entire sample is continuous and unbroken to the edges of the sample, with no grain boundaries).
  • the semiconductor material that can be employed as the base substrate 10 can be a polycrystalline (i.e., a material that is composed of many crystallites of varying size and orientation; the variation in direction can be random (called random texture) or directed, possibly due to growth and processing conditions). It is noted that when the semiconductor material is a polycrystalline material the spalling process of the present disclosure spalls certain grains, while leaving certain grains unspalled.
  • spalling of polycrystalline semiconductor material using the low-temperature spalling process of the present disclosure may produce a non- continuous spalled material layer.
  • the semiconductor material that can be employed as the base substrate 10 can be amorphous (i.e., a non-crystalline material that lacks the long-range order characteristic of a crystal).
  • the semiconductor material that can be employed as the base substrate 10 is a single crystalline material.
  • the glass can be an Si0 2 -based glass which may be undoped or doped with an appropriate dopant.
  • doped Si0 2 -based glasses that can be employed as the base substrate 10 include undoped silicate glass, borosilicate glass, phosphosilicate glass, fluorosilicate glass, and borophosphosilicate glass.
  • the ceramic is any inorganic, non- metallic solid such as, for example, an oxide including, but not limited to, alumina, beryllia, ceria and zirconia, a non-oxide including, but not limited to, a carbide, a boride, a nitride or a silicide; or composites that include combinations of oxides and non-oxides.
  • one or more devices including, but not limited to, transistors, capacitors, diodes, BiCMOS, resistors, etc. can be processed on and/or within the upper surface 12 of the base substrate 10 utilizing techniques well known to those skilled in the art. The upper portion of the base substrate that includes the one or more devices can be removed utilizing the spalling methods of the present disclosure.
  • the upper surface 12 of the base substrate 10 can be cleaned prior to further processing to remove surface oxides and/or other contaminants therefrom.
  • the base substrate 10 is cleaned by applying to the base substrate 10 a solvent such as, for example, acetone and isopropanol, which is capable of removing contaminates and/or surface oxides from the upper surface 12 of the base substrate 10.
  • FIG. 2 there is illustrated the base substrate 10 of FIG. 1 after forming an optional metal-containing adhesion layer 14 on upper surface 12.
  • the optional metal- containing adhesion layer 14 is employed in embodiments in which the stressor layer to be subsequently formed has poor adhesion to upper surface 12 of base substrate 10.
  • the metal-containing adhesion layer 14 is employed when a stressor layer comprised of a metal is employed.
  • the optional metal-containing adhesion layer 14 employed in the present disclosure includes any metal adhesion material such as, but not limited to, Ti/W, Ti, Cr, Ni or any combination thereof.
  • the optional metal-containing adhesion layer 14 may comprise a single layer or it may include a multilayered structure comprising at least two layers of different metal adhesion materials.
  • the metal-containing adhesion layer 14 that can be optionally formed on the upper surface 12 of base substrate 12 is formed at room temperature (15°C-40°C) or above. In one embodiment, the optional metal-containing adhesion layer 14 is formed at a temperature which is from 20°C to 180°C. In another embodiment, the optional metal-containing adhesion layer 14 is formed at a temperature which is from 20°C to 60°C.
  • the metal-containing adhesion layer 14, which may be optionally employed, can be formed utilizing deposition techniques that are well known to those skilled in the art.
  • the optional metal-containing adhesion layer 14 can be formed by sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, chemical solution deposition, physical vapor deposition, and plating.
  • the sputter deposition process may further include an in-situ sputter clean process before the deposition.
  • the optional metal-containing adhesion layer 14 When employed, the optional metal-containing adhesion layer 14 typically has a thickness of from 5 nm to 200 nm, with a thickness of from 100 nm to 150 nm being more typical. Other thicknesses for the optional metal-containing adhesion layer 14 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
  • FIG. 3 there is illustrated the structure of FIG. 2 after forming a stressor layer 16 on an upper surface of the optional metal-containing adhesion layer 14.
  • the stressor layer 16 is formed directly on the upper surface 12 of base substrate 10; this particular embodiment is not shown in the drawings, but can readily be deduced from the drawings illustrated in the present application.
  • the stressor layer 16 employed in the present disclosure includes any material that is under tensile stress on base substrate 10 at the spalling temperature.
  • Illustrative examples of such materials that are under tensile stress when applied atop the base substrate 10 include, but are not limited to, a metal, a polymer, such as a spall inducing tape layer, or any combination thereof.
  • the stressor layer 16 may comprise a single stressor layer, or a multilayered stressor structure including at least two layers of different stressor material can be employed.
  • the stressor layer 16 is a metal, and the metal is formed on an upper surface of the optional metal-containing adhesion layer 14.
  • the stressor layer 16 is a spall inducing tape, and the spall inducing tape is applied directly to the upper surface 12 of the base substrate 10.
  • the stressor layer 16 may comprise a two-part stressor layer including a lower part and an upper part. The upper part of the two-part stressor layer can be comprised of a spall inducing tape layer.
  • the metal can include, for example, Ni, Cr, Fe or W. Alloys of these metals can also be employed.
  • the stressor layer 16 includes at least one layer consisting of Ni.
  • the polymer is a large
  • polymers that can be employed as the stressor layer 16 include, but are not limited to, polyimides polyesters, polyolefms, polyacrylates, polyurethane, polyvinyl acetate, and polyvinyl chloride.
  • the spall inducing tape layer includes any pressure sensitive tape that is flexible, soft, and stress free at the first temperature used to form the tape, yet strong, ductile and tensile at the second temperature used during removal of the upper portion of the base substrate.
  • pressure sensitive tape it is meant an adhesive tape that will stick with application of pressure, without the need for solvent, heat, or water for activation.
  • Tensile stress in the tape at the second temperature is primarily due to thermal expansion mismatch between the base substrate 10 (with a lower thermal coefficient of expansion) and the tape (with a higher thermal expansion coefficient).
  • the pressure sensitive tape that is employed in the present disclosure as stressor layer 16 includes at least an adhesive layer and a base layer.
  • Materials for the adhesive layer and the base layer of the pressure sensitive tape include polymeric materials such as, for example, acrylics, polyesters, olefins, and vinyls, with or without suitable plasticizers.
  • Plasticizers are additives that can increase the plasticity of the polymeric material to which they are added.
  • the stressor layer 16 employed in the present disclosure is formed at a first temperature which is at room temperature (15°C-40°C).
  • the tape layer can be formed at a first temperature which is from 15°C to 60°C.
  • the stressor layer 16 is a metal or polymer
  • the stressor layer 16 can be formed utilizing deposition techniques that are well known to those skilled in the art including, for example, dip coating, spin-coating, brush coating, sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, chemical solution deposition, physical vapor deposition, and plating.
  • the tape layer can be applied by hand or by mechanical means to the structure.
  • the spall inducing tape can be formed utilizing techniques well known in the art or they can be commercially purchased from any well known adhesive tape manufacturer.
  • Some examples of spall inducing tapes that can be used in the present disclosure as stressor layer 16 include, for example, Nitto Denko 3193MS thermal release tape, Kapton KPT-1, and Diversified Biotech's CLEAR- 170 (acrylic adhesive, vinyl base).
  • a two-part stressor layer can be formed on a surface of a base substrate, wherein a lower part of the two-part stressor layer is formed at a first temperature which is at room temperature or slight above (e.g., from 15°C to 60°C), wherein an upper part of the two-part stressor layer comprises a spall inducing tape layer at an auxiliary temperature which is at room temperature.
  • the base substrate including the two-part stressor layer is brought to a second temperature which is less than room temperature.
  • the base substrate 10 is then spalled at the second temperature to form a spalled material layer.
  • the spalled material layer is then returned to room temperature.
  • the stressor layer 16 is of a metallic nature, it typically has a thickness of from 3 ⁇ to 50 ⁇ , with a thickness of from 4 ⁇ to 7 ⁇ being more typical. Other thicknesses for the stressor layer 16 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
  • the stressor layer 16 is of a polymeric nature, it typically has a thickness of from 10 ⁇ to 200 ⁇ , with a thickness of from 50 ⁇ to 100 ⁇ being more typical. Other thicknesses for the stressor layer 16 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
  • FIG. 4 there is illustrated the structure of FIG. 3 after forming an optional handle substrate 18 atop the stressor layer 16.
  • the optional handle substrate 18 employed in the present disclosure comprises any flexible material which has a minimum radius of curvature of less than 30 cm.
  • Illustrative examples of flexible materials that can be employed as the optional handle substrate 18 include a metal foil or a polyimide foil.
  • the optional handle substrate 18 can be used to provide better fracture control and more versatility in handling the spalled portion of the base substrate 10. Moreover, the optional handle substrate 18 can be used to guide the crack propagation during the spontaneous spalling process of the present disclosure.
  • the optional handle substrate 18 of the present disclosure is typically, but not necessarily, formed at a first temperature which is at room temperature (15°C-40°C).
  • the optional handle substrate 18 can be formed utilizing deposition techniques that are well known to those skilled in the art including, for example, dip coating, spin-coating, brush coating, sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, chemical solution deposition, physical vapor deposition, and plating.
  • the optional handle substrate 18 typical has a thickness of from 1 ⁇ to few mm, with a thickness of from 70 ⁇ to 120 ⁇ being more typical. Other thicknesses for the optional handle substrate 18 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
  • FIG. 5 there is illustrated the structure of FIG. 4 after removing an upper portion 10" of the base substrate 10 by spontaneous spalling.
  • reference numeral 10' denotes the remaining base substrate 10 that is not spalled
  • reference numeral 10" denotes the spalled portion of the base substrate which can include one or more device thereon.
  • the spontaneous spalling process includes crack formation and propagation which are initiated at a second temperature that is less than room temperature.
  • the spontaneous spalling occurs at a second temperature of 77 K or less.
  • the spontaneous spalling occurs at a second temperature of less than 206 K.
  • the second temperature e.g., the spontaneous spalling temperature, is from 175 K to 130 K.
  • the second temperature used in the present disclosure for spalling can be achieved by cooling the structure shown in FIG. 4 down below room temperature utilizing any cooling means.
  • cooling can be achieved by placing the structure in a liquid nitrogen bath, a liquid helium bath, an ice bath, a dry ice bath, a supercritical fluid bath, or any cryogenic environment liquid or gas.
  • the spalled material layer 10" that is removed from the base substrate 10 by the spontaneous spalling process mentioned above typically has a thickness of from 1000 nm to tens of ⁇ , with a thickness of from 5 ⁇ to 50 ⁇ being more typical. The thickness of the spalled material layer 10" correlates to the depth of crack initiation and propagation. [0060] After the spalling process, the spalled material layer 10" is returned to the first temperature (i.e., room temperature). This can be performed by allowing the spalled material layer 10" to slowly cool up to the first temperature by allowing the same to stand at room temperature. Alternatively, the spalled material layer 10" can be heated up to room temperature utilizing any heating means.
  • the first temperature i.e., room temperature
  • the optional handle substrate 18, the stressor layer 16 and the optional metal-containing adhesion layer 14 can be removed from the spalled material layer 10".
  • the optional handle substrate 18, stressor layer 16 and the optional metal-containing adhesion layer 14 are removed from the spalled material layer 10"
  • the removal of those layers can be achieved utilizing conventional techniques well known to those skilled in the art.
  • aqua regia HN0 3 /HC1
  • the present disclosure can be used in fabricating various types of thin-film devices including, but not limited to, semiconductor devices, and photovoltaic devices.

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Abstract

Method to (i) introduce additional control into a material spalling process, thus improving both the crack initiation and propagation, and (ii) increase the range of selectable spalling depths are provided. In one embodiment, the method includes providing a stressor layer on a surface of a base substrate at a first temperature which is room temperature. Next, the base substrate including the stressor layer is brought to a second temperature which is less than room temperature. The base substrate is spalled at the second temperature to form a spalled material layer. Thereafter, the spalled material layer is returned to room temperature, i.e., the first temperature.

Description

LOW-TEMPERATURE METHODS FOR SPONTANEOUS MATERIAL SPALLING
BACKGROUND
[0001] The present disclosure relates to semiconductor device manufacturing, and more particularly, to methods for controlling the removal of a surface layer from a base substrate utilizing low-temperature spontaneous spalling.
[0002] Devices that can be produced in thin-film form have three clear advantages over their bulk counterparts. First, by virtue of less material used, thin-film devices ameliorate the materials cost associated with device production. Second, low device weight is a definite advantage that motivates industrial-level effort for a wide range of thin-film applications. Third, if dimensions are small enough, devices can exhibit mechanical flexibility in their thin-film form. Furthermore, if a device layer is removed from a substrate that can be reused, additional fabrication cost reduction can be achieved.
[0003] Efforts to (i) create thin-film substrates from bulk materials (i.e., semiconductors) and (ii) form thin-film device layers by removing device layers from the underlying bulk substrates on which they were formed are ongoing. The controlled surface layer removal required for such applications has been successfully demonstrated using a process known as spalling; see U.S. Patent Application Publication No. 2010/0311250 to Bedell et al. Spalling includes depositing a stressor layer on a substrate, placing an optional handle substrate on the stressor layer, and inducing a crack and its propagation below the substrate/stressor interface. This process, which is performed at room temperature, removes a thin layer of the base substrate below the stressor layer. By thin, it is meant that the layer thickness is typically less than 100 microns, with a layer thickness of less than 50 microns being more typical.
[0004] The depth of at which the crack propagates is dictated by the thickness of the stressor layer, the inherent tensile stress of the stressor layer, and the fracture toughness of the base substrate being exfoliated (spalled). However, control of the initiation of the release layer process (crack initiation and propagation) and uniformity in the thickness of the spalled material are difficult to achieve utilizing prior art spalling processes.
SUMMARY
[0005] The present disclosure provides methods to (i) introduce additional control into a material spalling process, thus improving both the crack initiation and propagation, and (ii) increase the range of selectable spalling depths. The methods of the present disclosure are spontaneous spalling processes which are performed below room temperature, not mechanical spalling processes which are performed at room temperature as disclosed, for example, in U.S. Patent Application Publication No. 2010/0311250 to Bedell et al.
[0006] By "spontaneous," it is meant that the removal of a thin material layer from a base substrate occurs without the need to employ any manual means to initiate crack formation and propagation for breaking apart the thin material layer from the base substrate. By "room temperature," it is meant a temperature from 15°C to 40°C. By "low-temperature spalling," it is meant the removal of a material layer from a base substrate at a temperature below room temperature.
[0007] In one embodiment, the method of the present disclosure includes providing a stressor layer on a surface of a base substrate at a first temperature which is room temperature; bringing the base substrate including the stressor layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
[0008] In another embodiment, the method includes providing a stressor layer on a surface of a base substrate at a first temperature which is room temperature; bringing the base substrate including the stressor layer to a second temperature of less than 206 Kelvin (K); spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature. [0009] In yet another embodiment, the method includes providing a spall inducing tape layer on a surface of a base substrate at a first temperature which at approximately room temperature or slightly above (e.g., from 15°C to 60°C); bringing the base substrate including the spall inducing tape layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
[0010] In yet a further embodiment, the method of the present disclosure includes providing a two-part stressor layer on a surface of a base substrate, wherein a lower part of the two-part stressor layer is formed at a first temperature which at approximately room temperature or slightly above (e.g., from 15°C to 60°C), wherein an upper part of the two-part stressor layer comprises a spall inducing tape layer at an auxiliary temperature which is room temperature; bringing the base substrate including the two-part stressor layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
[0011] By using one of the aforementioned methods, the effective stress that induces material spalling is modified owing to differential thermal expansion, crystal structure changes at the crack front, fracture toughness value differences at lower-than-room temperatures, to reach a stress regime necessary for spalling-type fracture that would not be reached using the room temperature spalling technique disclosed in U.S. Patent Application Publication No.
2010/031 1250.
[0012] One advantage of the aforementioned spalling methods of the present disclosure is that the layer release process is spontaneous at all stages of the process, from spall initiation through spall completion. Another advantage of the present methods is that the component of stressor layer stress due to thermal expansion mismatch stress is reversible and will disappear upon warming back to room temperature, thus providing a spalled stressor layer/spalled film couple that is flatter at room temperature than at the temperature at which it was spalled. Yet another advantage of the present methods is that they widen the process window for controlled, spontaneous spalling: base substrates including stressor layers having thickness/stress values lower than the threshold required for spalling at room temperature can be safely stored at room temperature until spontaneous spalling is deliberately introduced by a temperature reduction.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a pictorial representation (through a cross sectional view) illustrating a base substrate that can be employed in one embodiment of the present disclosure.
[0014] FIG. 2 is a pictorial representation (through a cross sectional view) illustrating the base substrate of FIG. 1 after forming an optional metal-containing adhesion layer on a surface of the base substrate.
[0015] FIG. 3 is a pictorial representation (through a cross sectional view) illustrating the structure of FIG. 2 after forming a stressor layer and/or spall inducing tape layer on a surface of the optional adhesion layer.
[0016] FIG. 4 is a pictorial representation (through a cross sectional view) illustrating the structure of FIG. 3 after forming an optional handle substrate atop the stressor layer.
[0017] FIG. 5 is a pictorial representation (through a cross sectional view) illustrating the structure of FIG. 4 after removing an upper portion of the base substrate by utilizing a low- temperature spontaneous spalling method of the present disclosure.
DETAILED DESCRIPTION
[0018] The present disclosure, which relates to methods to (i) introduce additional control into a material spalling process, thus improving both the crack initiation and propagation, and (ii) increase the range of selectable spalling depths, will now be described in greater detail by referring to the following discussion and drawings that accompany the present application. It is noted that the drawings of the present application are provided for illustrative purposes and, as such, they are not drawn to scale.
[0019] In the following description, numerous specific details are set forth, such as particular structures, components, materials, dimensions, processing steps and techniques, in order to provide a thorough understanding of the present invention. However, it will be appreciated by one of ordinary skill in the art that the present disclosure may be practiced with viable alternative process options without these specific details. In other instances, well-known structures or processing steps have not been described in detail in order to avoid obscuring the various embodiments of the present disclosure.
[0020] It will be understood that when an element as a layer, region, or substrate is referred to as being "on" or "over" another element, it can be directly on the other element or intervening elements may also be present. In contrast, when an element is referred to as being "directly on" or "directly over" another element, there are no intervening elements present. It will also be understood that when an element is referred to as being "beneath" or "under" another element, it can be directly beneath or under the other element, or intervening elements may be present. In contrast, when an element is referred to as being "directly beneath" or "directly under" another element, there are no intervening elements present.
[0021] Reference is now made to FIGS. 1-5 which illustrate the basic processing steps of the method of the present disclosure which spalls, i.e., exfoliates, a material layer from a base substrate in a controlled manner. The material layer that is spalled is thin and may or may not include one of more devices thereon. The term "thin" is used to denote that the material layer that is spalled has a thickness that is typically less than 100 microns, with a thickness of less than 50 microns being more typical.
[0022] Specifically, FIGS. 1 -5 illustrate a low-temperature spontaneous spalling method that includes providing a stressor layer on a surface of a base substrate at a first temperature which is at room temperature; bringing the base substrate including the stressor layer to a second temperature which is less than room temperature; spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature, e.g., the first temperature.
[0023] Referring first to FIG. 1 there is illustrated a base substrate 10 having an upper surface 12 that can be employed in the present disclosure. The base substrate 10 employed in the present disclosure may comprise a semiconductor material, a glass, a ceramic, or any another material whose fracture toughness is less than that of the stressor layer to be subsequently formed.
[0024] Fracture toughness is a property which describes the ability of a material containing a crack to resist fracture. Fracture toughness is denoted Klc. The subscript Ic denotes mode I crack opening under a normal tensile stress perpendicular to the crack, and c signifies that it is a critical value. Mode I fracture toughness is typically the most important value because spalling mode fracture usually occurs at a location in the substrate where mode II stress (shearing) is zero, and mode III stress (tearing) is generally absent from the loading conditions. Fracture toughness is a quantitative way of expressing a material's resistance to brittle fracture when a crack is present.
[0025] When the base substrate 10 comprises a semiconductor material, the semiconductor material may include, but is not limited to, Si, Ge, SiGe, SiGeC, SiC, Ge alloys, GaSb, GaP, GaAs, InAs, InP, and all other III-V or II-VI compound semiconductors. In some embodiments, the base substrate 10 is a bulk semiconductor material. In other embodiments, the base substrate 10 may comprise a layered semiconductor material such as, for example, a semiconductor-on- insulator or a semiconductor on a polymeric substrate. Illustrated examples of semiconductor- on-insulator substrates that can be employed as base substrate 10 include silicon-on-insulators and silicon-germanium-on-insulators . [0026] When the base substrate 10 comprises a semiconductor material, the semiconductor material can be doped, undoped or contain doped regions and undoped regions.
[0027] In one embodiment, the semiconductor material that can be employed as the base substrate 10 can be single crystalline (i.e., a material in which the crystal lattice of the entire sample is continuous and unbroken to the edges of the sample, with no grain boundaries). In another embodiment, the semiconductor material that can be employed as the base substrate 10 can be a polycrystalline (i.e., a material that is composed of many crystallites of varying size and orientation; the variation in direction can be random (called random texture) or directed, possibly due to growth and processing conditions). It is noted that when the semiconductor material is a polycrystalline material the spalling process of the present disclosure spalls certain grains, while leaving certain grains unspalled. As such, spalling of polycrystalline semiconductor material using the low-temperature spalling process of the present disclosure may produce a non- continuous spalled material layer. In yet another embodiment of the present disclosure, the semiconductor material that can be employed as the base substrate 10 can be amorphous (i.e., a non-crystalline material that lacks the long-range order characteristic of a crystal). Typically, the semiconductor material that can be employed as the base substrate 10 is a single crystalline material.
[0028] When the base substrate 10 comprises a glass, the glass can be an Si02-based glass which may be undoped or doped with an appropriate dopant. Examples of doped Si02-based glasses that can be employed as the base substrate 10 include undoped silicate glass, borosilicate glass, phosphosilicate glass, fluorosilicate glass, and borophosphosilicate glass.
[0029] When the base substrate 10 comprises a ceramic, the ceramic is any inorganic, non- metallic solid such as, for example, an oxide including, but not limited to, alumina, beryllia, ceria and zirconia, a non-oxide including, but not limited to, a carbide, a boride, a nitride or a silicide; or composites that include combinations of oxides and non-oxides. [0030] In some embodiments of the present disclosure, one or more devices including, but not limited to, transistors, capacitors, diodes, BiCMOS, resistors, etc. can be processed on and/or within the upper surface 12 of the base substrate 10 utilizing techniques well known to those skilled in the art. The upper portion of the base substrate that includes the one or more devices can be removed utilizing the spalling methods of the present disclosure.
[0031] In some embodiments of the present disclosure, the upper surface 12 of the base substrate 10 can be cleaned prior to further processing to remove surface oxides and/or other contaminants therefrom. In one embodiment of the present disclosure, the base substrate 10 is cleaned by applying to the base substrate 10 a solvent such as, for example, acetone and isopropanol, which is capable of removing contaminates and/or surface oxides from the upper surface 12 of the base substrate 10.
[0032] Referring now to FIG. 2, there is illustrated the base substrate 10 of FIG. 1 after forming an optional metal-containing adhesion layer 14 on upper surface 12. The optional metal- containing adhesion layer 14 is employed in embodiments in which the stressor layer to be subsequently formed has poor adhesion to upper surface 12 of base substrate 10. Typically, the metal-containing adhesion layer 14 is employed when a stressor layer comprised of a metal is employed.
[0033] The optional metal-containing adhesion layer 14 employed in the present disclosure includes any metal adhesion material such as, but not limited to, Ti/W, Ti, Cr, Ni or any combination thereof. The optional metal-containing adhesion layer 14 may comprise a single layer or it may include a multilayered structure comprising at least two layers of different metal adhesion materials.
[0034] The metal-containing adhesion layer 14 that can be optionally formed on the upper surface 12 of base substrate 12 is formed at room temperature (15°C-40°C) or above. In one embodiment, the optional metal-containing adhesion layer 14 is formed at a temperature which is from 20°C to 180°C. In another embodiment, the optional metal-containing adhesion layer 14 is formed at a temperature which is from 20°C to 60°C.
[0035] The metal-containing adhesion layer 14, which may be optionally employed, can be formed utilizing deposition techniques that are well known to those skilled in the art. For example, the optional metal-containing adhesion layer 14 can be formed by sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, chemical solution deposition, physical vapor deposition, and plating. When sputter deposition is employed, the sputter deposition process may further include an in-situ sputter clean process before the deposition.
[0036] When employed, the optional metal-containing adhesion layer 14 typically has a thickness of from 5 nm to 200 nm, with a thickness of from 100 nm to 150 nm being more typical. Other thicknesses for the optional metal-containing adhesion layer 14 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
[0037] Referring now to FIG. 3, there is illustrated the structure of FIG. 2 after forming a stressor layer 16 on an upper surface of the optional metal-containing adhesion layer 14. In some embodiments in which the optional metal-containing adhesion layer 14 is not present, the stressor layer 16 is formed directly on the upper surface 12 of base substrate 10; this particular embodiment is not shown in the drawings, but can readily be deduced from the drawings illustrated in the present application.
[0038] The stressor layer 16 employed in the present disclosure includes any material that is under tensile stress on base substrate 10 at the spalling temperature. Illustrative examples of such materials that are under tensile stress when applied atop the base substrate 10 include, but are not limited to, a metal, a polymer, such as a spall inducing tape layer, or any combination thereof. The stressor layer 16 may comprise a single stressor layer, or a multilayered stressor structure including at least two layers of different stressor material can be employed. [0039] In one embodiment, the stressor layer 16 is a metal, and the metal is formed on an upper surface of the optional metal-containing adhesion layer 14. In another embodiment, the stressor layer 16 is a spall inducing tape, and the spall inducing tape is applied directly to the upper surface 12 of the base substrate 10. In another embodiment, for example, the stressor layer 16 may comprise a two-part stressor layer including a lower part and an upper part. The upper part of the two-part stressor layer can be comprised of a spall inducing tape layer.
[0040] When a metal is employed as the stressor layer 16, the metal can include, for example, Ni, Cr, Fe or W. Alloys of these metals can also be employed. In one embodiment, the stressor layer 16 includes at least one layer consisting of Ni.
[0041] When a polymer is employed as the stressor layer 16, the polymer is a large
macromolecule composed of repeating structural units. These subunits are typically connected by covalent chemical bonds. Illustrative examples of polymers that can be employed as the stressor layer 16 include, but are not limited to, polyimides polyesters, polyolefms, polyacrylates, polyurethane, polyvinyl acetate, and polyvinyl chloride.
[0042] When a spall inducing tape layer is employed as the stressor layer 16, the spall inducing tape layer includes any pressure sensitive tape that is flexible, soft, and stress free at the first temperature used to form the tape, yet strong, ductile and tensile at the second temperature used during removal of the upper portion of the base substrate. By "pressure sensitive tape," it is meant an adhesive tape that will stick with application of pressure, without the need for solvent, heat, or water for activation. Tensile stress in the tape at the second temperature is primarily due to thermal expansion mismatch between the base substrate 10 (with a lower thermal coefficient of expansion) and the tape (with a higher thermal expansion coefficient).
[0043] Typically, the pressure sensitive tape that is employed in the present disclosure as stressor layer 16 includes at least an adhesive layer and a base layer. Materials for the adhesive layer and the base layer of the pressure sensitive tape include polymeric materials such as, for example, acrylics, polyesters, olefins, and vinyls, with or without suitable plasticizers. Plasticizers are additives that can increase the plasticity of the polymeric material to which they are added.
[0044] In one embodiment, the stressor layer 16 employed in the present disclosure is formed at a first temperature which is at room temperature (15°C-40°C). In another embodiment, when a tape layer is employed, the tape layer can be formed at a first temperature which is from 15°C to 60°C.
[0045] When the stressor layer 16 is a metal or polymer, the stressor layer 16 can be formed utilizing deposition techniques that are well known to those skilled in the art including, for example, dip coating, spin-coating, brush coating, sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, chemical solution deposition, physical vapor deposition, and plating.
[0046] When the stressor layer 16 is a spall inducing tape layer, the tape layer can be applied by hand or by mechanical means to the structure. The spall inducing tape can be formed utilizing techniques well known in the art or they can be commercially purchased from any well known adhesive tape manufacturer. Some examples of spall inducing tapes that can be used in the present disclosure as stressor layer 16 include, for example, Nitto Denko 3193MS thermal release tape, Kapton KPT-1, and Diversified Biotech's CLEAR- 170 (acrylic adhesive, vinyl base).
[0047] In one embodiment, a two-part stressor layer can be formed on a surface of a base substrate, wherein a lower part of the two-part stressor layer is formed at a first temperature which is at room temperature or slight above (e.g., from 15°C to 60°C), wherein an upper part of the two-part stressor layer comprises a spall inducing tape layer at an auxiliary temperature which is at room temperature. Next, the base substrate including the two-part stressor layer is brought to a second temperature which is less than room temperature. The base substrate 10 is then spalled at the second temperature to form a spalled material layer. The spalled material layer is then returned to room temperature. [0048] If the stressor layer 16 is of a metallic nature, it typically has a thickness of from 3 μπι to 50 μηι, with a thickness of from 4 μηι to 7 μπι being more typical. Other thicknesses for the stressor layer 16 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
[0049] If the stressor layer 16 is of a polymeric nature, it typically has a thickness of from 10 μηι to 200 μπι, with a thickness of from 50 μηι to 100 μηι being more typical. Other thicknesses for the stressor layer 16 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
[0050] Referring to FIG. 4, there is illustrated the structure of FIG. 3 after forming an optional handle substrate 18 atop the stressor layer 16. The optional handle substrate 18 employed in the present disclosure comprises any flexible material which has a minimum radius of curvature of less than 30 cm. Illustrative examples of flexible materials that can be employed as the optional handle substrate 18 include a metal foil or a polyimide foil.
[0051] The optional handle substrate 18 can be used to provide better fracture control and more versatility in handling the spalled portion of the base substrate 10. Moreover, the optional handle substrate 18 can be used to guide the crack propagation during the spontaneous spalling process of the present disclosure.
[0052] The optional handle substrate 18 of the present disclosure is typically, but not necessarily, formed at a first temperature which is at room temperature (15°C-40°C).
[0053] The optional handle substrate 18 can be formed utilizing deposition techniques that are well known to those skilled in the art including, for example, dip coating, spin-coating, brush coating, sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, chemical solution deposition, physical vapor deposition, and plating. [0054] The optional handle substrate 18 typical has a thickness of from 1 μηι to few mm, with a thickness of from 70 μηι to 120 μηι being more typical. Other thicknesses for the optional handle substrate 18 that are below and/or above the aforementioned thickness ranges can also be employed in the present disclosure.
[0055] Referring to FIG. 5, there is illustrated the structure of FIG. 4 after removing an upper portion 10" of the base substrate 10 by spontaneous spalling. In FIG. 5, reference numeral 10' denotes the remaining base substrate 10 that is not spalled, while reference numeral 10" denotes the spalled portion of the base substrate which can include one or more device thereon.
[0056] The spontaneous spalling process includes crack formation and propagation which are initiated at a second temperature that is less than room temperature. In one embodiment, the spontaneous spalling occurs at a second temperature of 77 K or less. In another embodiment, the spontaneous spalling occurs at a second temperature of less than 206 K. In yet further embodiment, the second temperature, e.g., the spontaneous spalling temperature, is from 175 K to 130 K.
[0057] Within the second temperature range mentioned above, a crack begins to initiate and propagate spontaneously beneath the upper surface 12 of the base substrate 10.
[0058] The second temperature used in the present disclosure for spalling can be achieved by cooling the structure shown in FIG. 4 down below room temperature utilizing any cooling means. For example, cooling can be achieved by placing the structure in a liquid nitrogen bath, a liquid helium bath, an ice bath, a dry ice bath, a supercritical fluid bath, or any cryogenic environment liquid or gas.
[0059] The spalled material layer 10" that is removed from the base substrate 10 by the spontaneous spalling process mentioned above typically has a thickness of from 1000 nm to tens of μπι, with a thickness of from 5 μηι to 50 μιη being more typical. The thickness of the spalled material layer 10" correlates to the depth of crack initiation and propagation. [0060] After the spalling process, the spalled material layer 10" is returned to the first temperature (i.e., room temperature). This can be performed by allowing the spalled material layer 10" to slowly cool up to the first temperature by allowing the same to stand at room temperature. Alternatively, the spalled material layer 10" can be heated up to room temperature utilizing any heating means.
[0061] In some embodiments of the present disclosure, the optional handle substrate 18, the stressor layer 16 and the optional metal-containing adhesion layer 14 can be removed from the spalled material layer 10". When the optional handle substrate 18, stressor layer 16 and the optional metal-containing adhesion layer 14 are removed from the spalled material layer 10", the removal of those layers can be achieved utilizing conventional techniques well known to those skilled in the art. For example, and in one embodiment, aqua regia (HN03/HC1) can be used for removing the optional handle substrate 18, the stressor layer 16 and the optional metal- containing adhesion layer 14 from the spalled material layer 10" .
[0062] The present disclosure can be used in fabricating various types of thin-film devices including, but not limited to, semiconductor devices, and photovoltaic devices.
[0063] While the present disclosure has been particularly shown and described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that the foregoing and other changes in forms and details may be made without departing from the spirit and scope of the present disclosure. It is therefore intended that the present disclosure not be limited to the exact forms and details described and illustrated, but fall within the scope of the appended claims.

Claims

CLAIMS What is claimed as new is:
1. A method for removing a material layer from a surface of a base substrate, said method comprising:
providing a stressor layer on a surface of a base substrate at a first temperature which is room temperature;
bringing the base substrate including the stressor layer to a second temperature which is less than room temperature;
spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
2. The method of Claim 1, wherein said base substrate has a fracture toughness that is lower than that of the stressor layer.
3. The method of Claim 2, wherein said base substrate comprises a semiconductor material, a glass, or a ceramic.
4. The method of Claim 3, wherein said base substrate is a semiconductor substrate, and said semiconductor substrate is single crystalline.
5. The method of Claim 1 , further comprising forming a metal-containing adhesive layer between said stressor layer and said base substrate.
6. The method of Claim 1 , wherein said stressor layer is a metal, a polymer, a spall inducing tape layer or any combination thereof.
7. The method of Claim 1, wherein said stressor layer is a metal, and said metal comprises Ni, Cr, Fe or W.
8. The method of Claim 1 , wherein said stressor layer is a spall inducing tape layer, and said spall inducing tape layer is a pressure sensitive tape that is flexible and stress free at said first temperature, yet ductile and tensile at the second temperature.
9. The method of Claim 8, wherein said pressure sensitive tape comprises at least an adhesive layer and a base layer.
10. The method of Claim 1, wherein the stressor layer comprises a two-part stressor layer including a lower part and an upper part, said upper part comprising a spall inducing tape layer.
11. The method of Claim 1, further comprising forming a handle substrate atop said stressor layer and at said first temperature.
12. The method of Claim 1, wherein said second temperature is 77 K or less.
13. A method for removing a material layer from a surface of a base substrate, said method comprising:
providing a stressor layer on a surface of a base substrate at a first temperature which is room temperature;
bringing the base substrate including the stressor layer to a second temperature of less than 206 K;
spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
14. The method of Claim 13, further comprising forming a metal-containing adhesive layer between said stressor layer and said base substrate.
15. The method of Claim 13, wherein said stressor layer is a metal, and said metal comprises Ni, Cr, Fe or W.
16. The method of Claim 13, wherein said stressor layer is a spall inducing tape layer, and said spall inducing tape layer is a pressure sensitive tape that is flexible and stress free at said first temperature, yet ductile and tensile at the second temperature.
17. The method of Claim 13, further comprising forming a handle substrate atop said stressor layer and at said first temperature.
18. The method of Claim 13, wherein the stressor layer comprises a two-part stressor layer including a lower part and an upper part, said upper part comprising a spall inducing tape layer.
19. A method for removing a material layer from a surface of a base substrate, said method comprising:
providing a spall inducing tape layer on a surface of a base substrate at a first temperature which is from 15°C to 60°C;
bringing the base substrate including the spall inducing tape layer to a second
temperature which is less than room temperature;
spalling the base substrate at the second temperature to form a spalled material layer; and returning the spalled material layer to room temperature.
20. The method of Claim 19, wherein said spall inducing tape layer is a pressure sensitive tape that is flexible and stress free at said first temperature, yet ductile and tensile at the second temperature.
21. The method of Claim 20, wherein said pressure sensitive tape comprises at least an adhesive layer and a base layer.
22. The method of Claim 19, further comprising forming a handle substrate atop said spall inducing tape layer and at said first temperature.
23. The method of Claim 19, wherein spall inducing tape layer comprises an upper part of a two-part stressor layer.
24. The method of Claim 19, wherein said second temperature is 77 K or less.
25. The method of Claim 19, wherein said second temperature is less than 206 K.
PCT/US2012/036860 2011-06-01 2012-05-08 Low-temperature methods for spontaneous material spalling WO2012166298A1 (en)

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