WO2013005095A1 - Procédé pour déterminer la qualité du cristal d'une couche de semi-conducteur iii-v - Google Patents

Procédé pour déterminer la qualité du cristal d'une couche de semi-conducteur iii-v Download PDF

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Publication number
WO2013005095A1
WO2013005095A1 PCT/IB2012/001311 IB2012001311W WO2013005095A1 WO 2013005095 A1 WO2013005095 A1 WO 2013005095A1 IB 2012001311 W IB2012001311 W IB 2012001311W WO 2013005095 A1 WO2013005095 A1 WO 2013005095A1
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etching
inp
lll
substrate
semiconductor layer
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PCT/IB2012/001311
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English (en)
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Alexandra Abbadie
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Soitec
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32—Polishing; Etching

Definitions

  • the invention relates to a method for determining the crystalline quality of a lll-V semiconductor layer.
  • Ill-V semiconductor substrates are becoming more and more popular in optoelectronic applications, but they are still rather difficult to fabricate in large scales.
  • One particular sensitive parameter is the crystalline quality, which directly affects the electronic characteristics of the substrate.
  • the stoichiometry of the crystal, the presence of impurities or dopants like for example zinc (Zn), iron (Fe), sulfur (S) or tin (Sn) in Ill-V semiconductors, or in non-intentionally doped Ill-V materials, and the dislocation mobility are all known to affect the crystalline quality.
  • dislocations in the substrate also affect the surface topology after epitaxial growth, which can have adverse effects on the structural and electronic characteristics of the epitaxial layers. Therefore, reducing the dislocation density is a critical step in the crystal pulling technology.
  • Indium phosphide is one example of a Ill-V semiconductor material with zincblende crystalline structure, which is conventionally grown by the so called Liquid Encapsulated Czocralski (LEC) pulling technique, and commonly used for a variety of optoelectronic applications.
  • LEC Liquid Encapsulated Czocralski
  • the techniques for the inspection and follow-up of InP that are known from the prior art, like US 4 316 765, are based on the etch pit method and use chemical solutions, that are either toxic or aggressive, hardly reproducible, and sometimes not even authorized any longer by official regulations on chemicals and their safe use (REACH).
  • the solutions of the art are ; known as the A-B etch (a solution based on chromium, in particular chromium trioxide Cr0 3 ), and the Hubert etch (a solution based on bromic acid HBr0 3 ).
  • Less noxious alternatives using solutions based on hydrochloric acid (HCI) and nitric acid (HN0 3 ) have also been reported and are used for etching crystallographic defects and planes.
  • the inventive method for determining the crystalline quality of a lll-V semiconductor layer comprises the steps of : a) performing a first etching of a surface of the lll-V semiconductor layer to obtain a first etched surface under first etching conditions, and b) performing a second etching of the first etched surface to obtain a second etched surface under second etching conditions, wherein the first etching conditions and the second etching conditions are different.
  • the inventive method couples two etching steps with different purposes.
  • Step a) of the inventive method enables the initiation of the reaction by starting the etching and revealing at least partially surface defects that are already present, without degrading the surface which could lead to the formation of etch pits. Such unwanted etch pits would appear as pre- existing defects and thus form defect artifacts.
  • the second conditions of step b) of the inventive method can then be chosen such that the defects of the first etched surface become enlarged to make sure that they can be distinguished and identified.
  • the first etched surface comprises at least one revealed defect
  • the second etched surface comprises at least one revealed and/or enlarged defect.
  • the inventive method can further comprise the step of: c) inspecting (he second etched surface optically, in particular using an optical microscopy means.
  • c) inspecting he second etched surface optically, in particular using an optical microscopy means.
  • the lll-V semiconductor layer can be a lll-V semiconductor bulk substrate or a recycled substrate, or a lll-V semiconductor layer provided on a layer stack.
  • the inventive method can be used for determining the crystalline quality of a bulk substrate at the beginning of a given procedure, for example upon reception of a manufacturer.
  • the inventive method can be used for determining the crystalline quality of a recycled lll-V semiconductor substrate obtained after the detachment of a layer of the lll-V semiconductor material, in particular in a layer transfer process.
  • the lll-V semiconductor layer can be a lll-V semiconductor layer that has been transferred from a donor substrate to a handle substrate before carrying out steps a) to b) or steps a) to c), in particular by a layer transfer process.
  • the inventive method can be used for determining the crystalline quality at any time in the process of a lll-V semiconductor material.
  • the lll-V semiconductor substrate can be indium phosphide (InP) or any N-based lll-V material.
  • InP is commonly used for a variety of optoelectronic applications.
  • the inventive method can be used for determining the crystalline quality of an InP bulk substrate, an InP layer transferred from a donor substrate to a handle substrate, in particular by layer transfer process, or also a recycled InP product obtained after the detachment of the InP layer during a layer transfer process.
  • the inventive method can be used for determining the crystalline quality of In layers at any step of a layer transfer process by Smart CutTM technology.
  • the inventive method can also be used for determining the crystalline quality of an InP layer provided on a layer stack, e.g. by epitaxial growth.
  • the handle substrate consists of or comprises sapphire, and/or silicon, and/or quartz, and/or a metallic substrate.
  • Sapphire like silicon, is commonly used as a handle substrate in optoelectronic applications.
  • an InP layer can be deposited on a handle substrate comprising sapphire by a layer transfer process, for example by Smart CutTM technology, to form an InP on sapphire structure, which is also called InPOS.
  • the inventive method can be used for determining the crystalline quality of InP of any other lll-V semiconductor layer at any time in the layer transfer process.
  • the etch rate of the first etching can be superior to the etch rate of the second etching.
  • the duration of step a) and step b) depends essentially on the efficiency of step a) as it initiates the etching reaction.
  • a high etch rate in step a) is advantageous in order to ensure defect decoration.
  • the duration between step b) and step a) can be optimized, thus reducing the characterization time for the lll-V semiconductor.
  • the duration of the first etching step is comprised between 30 and 60 seconds
  • the duration of the second etching step is comprised between 10 and 20 seconds.
  • the timing between the two steps should be limited as far as possible in order to avoid the degradation of the etching solution and surface passivation (oxidation for instance) while the substrate is waiting for the second etching step.
  • the timing should preferably be below 30 minutes.
  • the first etching can be performed using a mixture of hydrochloric acid and phosphoric acid (HCI / H 3 P0 ). Using this solution allows to perform the first etching and to reveal at least partially defects without degrading the surface, and prevents the formation of artifacts due to the etching technique itself.
  • the roughness of an etched surface can be kept similar to that of the initial surface before etching, typically with rms values inferior to 5 A at the center of the layer in the case of InP and InPOS layers.
  • the inventive method is performed on a rougher initial surface like on a recycled semiconductor substrate obtained after the detachment of a layer of the l ll-V semiconductor material, in particular in a layer transfer process, the first etching can furthermore reduce the roughness within the same step.
  • the phosphoric acid can be in a concentration at least equal or superior to that of hydrochloric acid. For such ratios, optimized properties of the treated surface have been observed.
  • the solution can comprise hydrochloric acid in a volume of 1 to 2 and said phosphoric acid in a volume of 1 to 4.
  • the mixture ol hydrochloric acid and phosphoric acid can be diluted with water (H 2 0). The addition of water allows an optimized control of the etch rate of the HCI / H 3 P0 solution used in step a) for the first etching.
  • the ratio by volume of water can be from 0.1 to 10.
  • optimized properties have been observed for InP and InPOS layers.
  • the second etching can be performed using a mixture of hydrochloric acid, nitric acid, and water (HCI / HN0 3 / H 2 0).
  • This solution finalizes the etching by enlarging the defects of the first etched surface to make sure that they can be better distinguished and identified.
  • the inventive method can thus prevent or at least reduce a degradation of the surface, in particular the roughness, so that the second etched surface maintains a surface topology as close as possible to the one after the first etching step of the lll-V semiconductor layer. Optimized properties have been observed when this solution is used in combination with a first etching performed using the HCI / H3PO 4 solution.
  • said hydrochloric acid, nitric acid, and water can be in the ratio by volume of 1 / 6 / 6.
  • optimized etching properties have been observed when performing step b) of the inventive method for InP and InPOS.
  • the temperature of at least one of the two etching steps can be in the range of 15°C to 100°C, preferably 15 °C to 40 °C. Optimized properties have been observed for both etchings in this temperature range, in particular when treating InP or InPOS surfaces.
  • both etching steps a) and b) are carried out in this temperature range.
  • the temperature range of the etching solution HCI / H 3 P0 used in step a) can be in the range 15°C to 80 "C, in particular for use on other lll-V materials such as N-based materials.
  • the step of inspecting the second etched surface optically can be accompanied by an optical profilometer.
  • the optical profilometer can comprise an optical interferometer.
  • large surfaces can be inspected at once, and different dopants can be observed in the lll-V semiconductor.
  • the surface topologies are different depending on the nature of the dopants, in particular when the lil-V semiconductor is InP, hence dopants can indirectly be identified based on bulk defects delineation.
  • the object of the invention is also achieved with the method according to claim 18.
  • the method for determining the crystalline quality of a lll-V semiconductor layer comprises the step of performing an etching of a surface of the lll-V semiconductor layer to obtain an etched surface, characterized in that the etching is performed using a mixture of hydrochloric acid and phosphoric acid (HCI / H 3 PO*).
  • the etching step of the inventive method allows to reveal surface defects at least partially without creating etch artifacts.
  • the process parameters are such that the surface essentially keeps or improves the roughness of the initial surface of the lll-V semiconductor layer before performing the first etching, except for the locations of surface defects. Between positions of etched defects, the surface can be considered as "mirror polished" even after the etching step. This smooth surface is an attractive feature because the creation of etch pits is avoided that could be considered as pre-existing defects (defects artifacts).
  • the. lll-V semiconductor can be indium phosphide (InP). Surprisingly, it was found that the HCI / H 3 P0 4 solution is efficient for revealing defects in InP.
  • the roughness of an etched surface is kept similar to that of the initial surface before etching, typically with rms values inferior to 5 A at the center of the InP layer or can be even used to smoothen rougher surfaces following a layer transfer process as described above.
  • the inventive method can be used for determining the crystalline quality of an InP layer at any time in the industrial process of an InP material.
  • the inventive method can be used for determining the crystalline quality of an InP bulk substrate, an InP layer transferred from a donor substrate to a handle substrate, in particular by layer transfer process, or also a recycled InP product obtained after the detachment of the InP layer during a layer transfer process.
  • the inventive method can be used for revealing defects and thus determining the crystalline quality of InP layers at any step of a layer transfer process by Smart CutTM technology.
  • the handle substrate can consist of or comprise sapphire, and/or silicon, and/or quartz, and/or a metallic substrate.
  • the inventive method can also be used determining the crystalline quality of an InP layer provided on a layer stack, e.g. by epitaxial growth.
  • the phosphoric acid can be in a concentration at least equal or superior to that of hydrochloric acid.
  • optimized properties of the treated surface have been observed.
  • the hydrochloric acid can be in the ratio by volume of t to 2, and said phosphoric acid is in a ratio by volume of 1 to 4.
  • optimized properties have been observed when performing the etching of the inventive method for In P layers.
  • the mixture of hydrochloric acid and phosphoric acid can be diluted with water (H 2 0).
  • water H 2 0
  • the addition of water allows an optimized control of the etch rate of the HCI / H 3 P0 4 solution used in step a) for the first etching.
  • the ratio by volume of water can be of 0.1 to 10.
  • optimized properties have been observed for InP layers.
  • the temperature of the etching step can be in the range of 15 °C to 100 °C, preferably 15 °C to 40 °C. Optimized properties have been observed for the etching in this temperature range, in particular when treating InP surfaces.
  • the invention will be described in more detail in the following, based on advantageous embodiments described in conjunction with the following Figures:
  • Figure 1 A schematically illustrates the principles of the method for determining the crystalline quality of a lll-V semiconductor layer of an InP bulk substrate using the HCI / H3PO4 solution in a first embodiment
  • Figure 1 B schematically illustrates the principles of the method lor determining the crystalline quality of a lll-V semiconductor layer of an InP bulk substrate in a second embodiment
  • Figure 2 illustrates optical profiles obtained after selective etching of InP using a chemical solution in two steps
  • Figure 3 schematically illustrates the principles of the method for determining the crystalline quality of an InP layer previously attached to a handle substrate by a layer transfer process in a third embodiment
  • Figure 4 schematically illustrates the principles of the method for determining the crystalline quality of a lll-V semiconductor layer of a residual InP substrate recycled from a first layer transfer process and to be used as donor substrate in a new layer transfer process in a fourth embodiment.
  • the inventive method for determining the crystalline quality of a lll-V semiconductor layer is described in a first embodiment according to claim 13, wherein the III- V semiconductor layer is an InP bulk substrate (101 ).
  • the inventive method could be used for determining the crystalline quality of any other lll-V semiconductor material.
  • an etching step is performed on the surface of an InP bulk substrate ( 101 ) to reveal existing defects, while keeping the surface properties of the etched surface as similar as possible to those of the initial surface before etching which is typically a mirror polished surface.
  • the first embodiment of the method according to the invention as illustrated in Figure 1 A comprises performing a first etching ( 102) on the surface of the InP bulk substrate ( 101 ) to obtain a first etched surface (103) under first etching conditions to reveal at least partially defects already present before the etching step (step I).
  • step I) of the first embodiment as illustrated in Figure 1 A the etching ( 102) performed on the surface of the InP bulk substrate
  • HCI hydrochloric acid
  • H3PO 4 phosphoric acid
  • HCI is used to enable the dissolution of the oxidized defects.
  • the concentration of phosphoric acid is at least equal or superior to that of hydrochloric acid: HCI is in a ratio by volume of 1 - 2, and H 3 P0 is in a ratio by volume of 1 4.
  • the roughness of the etched surface (103) is thereby kept similar to that of the initial surface of the InP bulk substrate (101 ) before etching, with observed values inferior to 5 A rms at the center of the plate.
  • the etch rate of the first etching (102) performed in step I) in the first embodiment of the ' invention is controlled by adding water (H 2 0) to the HCI / H 3 P0 mixture in a ratio by volume of 0.1 to 10. With the combination of these optimized ratios, the etch rate of the first etching
  • the first etching (102) is superior or equal to 5000 A / min, so that the first etching (102) typically lasts from about a few seconds to about one minute.
  • the first embodiment as illustrated in Figure 1A is combined with a second etching step II) (104) performed on the first etched surface (103) to obtain a second etched surface ( 105) under second etching conditions.
  • the second etching step (104) serves to enlarge at least the at least partially revealed defects, wherein the first and second etching conditions are different.
  • the second embodiment of the method according to the invention as illustrated in Figure 1 B further comprises the step of: step III) inspecting the second etched surface ( 105) optically using e.g. an optical microscopy means ( 106).
  • this step is accompanied by an optical profilometer (107) comprising an optical interferometer.
  • the second etching (104) is performed on the first etched surface (103) using a chemical etching solution of hydrochloric acid, nitric acid, and water (HCI / HN0 3 / H 2 0) in the ratios by volume of 1 / 6 / 6.
  • a chemical etching solution of hydrochloric acid, nitric acid, and water HCI / HN0 3 / H 2 0
  • the second etched surface ( 105) presents enlarged defects with respect to the first etched surface (103) and the original surface of the InP bulk substrate (101 ), which can be detected and identified using the optical microscopy means (106).
  • ratios only represent one example of how to carry out the inventive method according to claim 1 using two different etching solutions. As long as the etch rates are sufficiently high, the ratios can deviate from these optimized values. In particular, as long as the etch rate of the first etching (102) in step I) remains higher than that of the second etching ( 104) in step I I), so that the second etching ( 104) can be initiated in optimized timing conditions after the first etching (102), the ratios can deviate from these optimized values.
  • the etch rate obtained for the second etching ( 104) step is in the range of 1000 A min '1 to 3000 A min '1 for a temperature in the range of 15 °C to 40 °C, and the duration of the second etching ( 1 04) ranges from about a few seconds to about five minutes.
  • step III) an optical inspection of the second etched surface (105) is done using an optical microscopy means ( 1 06), wherein this step is accompanied by an optical profilometer (107) comprising an optical interferometer.
  • One output of the optical profilometer (107) is an optical profile ( 108) of the observed second etched surface (105) as illustrated in Figure 2. This allows a fast and direct evaluation of the surface topology of the InP bulk substrate ( 101 ), and a visual identification and automated counting of the defects at the surface of the InP bulk substrate ( 101 ).
  • Figure 2 illustrates one output of an optical profilometer ( 107) in form of an optical profile ( 1 08) obtained after the selective two-steps etching of the surface of an InP bulk substrate ( 101 ) according to the second embodiment of the invention as illustrated in Figures 1 A and 1 B.
  • Comparable profiles can be obtained when inspecting the surface of a layer of any other lll-V semiconductor according to the various embodiments of the inventive method.
  • Figure 2 illustrates a plane or two dimensional view (201 ) of the inspected second etched surface ( 1 05) according to the second embodiment described in Figures 1 A and 1 B, two profiles or cross-sections (202, 203) , one along the X or abscissa axis (202) and one along the Y or ordinate axis (203), a quadrant indicating the position of the cursor (204) , and a reconstructed three dimensional view (205) of the defects observed on the second etched surface ( 105). Height and depth measurements of the observed defects can be performed along both the abscissa and the ordinate axes, so that peak-to-valley measurements, etc.
  • defects can be characterized as a function of their shape and their dimension (round, rectangular, elongated, etc.) using the available plane view (201 ), and/or cross-sections (202, 203), and/or cursor measurements (204), and/or three dimensional reconstruction (205).
  • At least dislocations (pits), hillocks, ridges, twinnings, vacancies, for example interstitial defects, can be identified on the second etched surface (105) of the InP bulk substrate (101 ) in the profiles illustrated in Figure 2 and characterized.
  • the optical profiles (201 , 202, 203, 205) reveal that a density of defects equivalent to. 10 5 cm '2 is obtained when the InP bulk substrate (1 01 ) has been doped with iron (Fe).
  • Figure 3 illustrates a third embodiment of the invention.
  • the lll-V semiconductor layer of this embodiment is an InP layer (31 1 ) that has been transferred from an InP donor substrate (301 ) to a handle substrate comprising sapphire (302) by a layer transfer process.
  • the Smart CutTM technology can be used to form an InP on sapphire structure (305, 305'), also called InPOS.
  • the starting substrate is an InP donor substrate (301 ), which can be an InP bulk substrate.
  • the surface of the InP donor substrate (301 ) could also be inspected for crystalline defects according to the second embodiment of the inventive method.
  • the surface of the InP donor substrate (301 ) could also be inspected for crystalline defects according to the second embodiment of the inventive method.
  • it is referred back to Figures 1 A and 1 B and the description above. This could be carried out as an initial step, prior to starling the process described hereafter for the third embodiment.
  • Figure 3 illustrates the Smart CutTM layer transfer process that transfers an InP layer from an InP donor substrate (301 ) to a handle substrate comprising sapphire (302), followed by a crystalline quality inspection of the transferred InP layer (31 1 ) of the hereby formed InPOS structure (305, 305') according to the third embodiment of the invention.
  • the layer transfer by Smart CutTM comprises the steps of: step I) performing a surface oxidation of a surface of the InP donor substrate (301 ) to obtain an insulating surface layer (303) on the InP donor substrate (301 ), step II) performing an ion implantation in the InP donor substrate (301 ) below the insulating surface layer (303) to obtain an in-depth layer (304) forming a predetermined splitting area, step III) flipping the InP donor substrate (301 ) with the insulating surface layer (303) and the in-depth layer (304) and attaching the insulating surface layer (303) to the handle substrate comprising sapphire (302), e.g.
  • step IV detaching the InP donor substrate (301 ) at the level of the in- depth layer (304) to obtain an InP on sapphire (InPOS) structure (305) with a transferred InP layer (31 1 ) and a residual InP substrate (301 ').
  • InPOS InP on sapphire
  • the layer transfer process can also comprise the steps of: step V) recycling the residual InP substrate (301 ') and its use as the donor substrate in a new layer transfer process, and/or step VI) cutting the InPOS structure (305) to a desired thickness to obtain a thinner InPOS structure (305') with a transferred InP layer (31 1 ) and a thinner handle substrate comprising sapphire (302") and a residual handle substrate comprising sapphire (302'), and/or step VII) recycling the residual handle substrate comprising sapphire (302') to use it as the handle substrate in a new layer transfer process.
  • the crystalline quality of the transferred InP layer (31 1 ) of the InPOS structure (305, 305') is then determined using the inventive method after steps IV) or VI) of the layer transfer process described above have been carried out.
  • the procedure follows essentially the procedure already described for Figure 1 : a two-steps etching is performed on the surface of the transferred InP layer (31 1 ) of the InPOS structure (305, 305') to reveal and/or enlarge existing defects, while keeping the etched surface properties close to those of the initial surface before etching.
  • the third embodiment of the inventive method as illustrated in Figure 3 thus comprises the steps of: step VIII) performing a first etching (312) on the surface of the transferred InP layer (31 1 ) of the InPOS structure (305, 305') to obtain a first etched surface (313) under first etching conditions, revealing at least partially present defects, and step IX) performing a second etching (314) of the first etched surface (313) to obtain a second etched surface
  • the third embodiment illustrated in Figure 3 further comprises the step of: step X) inspecting the second etched surface (315) optically using an optical microscopy means
  • this step is accompanied by an optical profilometer (31 7) comprising an optical interferometer, like in the second embodiment.
  • the ratios by volume of the two chemicaJ solutions used to perform respectively the first etching (312) and the second etching (314) of the transferred InP layer (31 1 ) of the InPOS structure (305, 305 * ) in steps VIII) and IX) , the resulting roughness of the first etched surface (313), the temperature range for performing the etchings, and the etch rates of the first etching (312) and of the second etching (314) have been reported in the description of the first and second embodiments illustrated in Figures 1 A and 1 B.
  • step X) in the third embodiment illustrated In Figure 3 comprises an optical inspection of the defects of the second etched surface (315) of the transferred InP layer (31 1 ) of the InPOS structure (305, 305') using an optical microscopy means (316), wherein this step is accompanied by a an optical profilometer (317) comprising an optical interferometer.
  • the analysis of the optical profile (318) shows that the inventive method not only allows to detect a high density of defects (10 5 cm 2 ), but it also keeps a high sensitivity for smaller densities (10 4 cm “2 ).
  • Figure 4 illustrates a fourth embodiment of the invention.
  • the lll-V semiconductor layer of this embodiment is a residual InP substrate (401 ') obtained from a layer transfer process, e.g. the residual InP substrate (301 ') obtained after step iv) in Figure 3, to be recycled as donor substrate in a new layer transfer process.
  • a layer of InP has been deposited from an initial InP donor substrate (401 ) to a handle substrate comprising sapphire (402) by a layer transfer process.
  • the Smart CutTM technology has been used to form an InP on sapphire (InPOS) structure (405, 405').
  • InPOS InP on sapphire
  • sapphire and the Smart CutTM technology other lll-V semiconductor could be used as a donor and/or handle substrates, and any other layer transfer process could be used.
  • the InP donor substrate (401 ) is a recycled residual InP substrate (401 ') obtained from a previous layer transfer process, and which is used as the donor substrate in a new layer transfer process.
  • the surface of the recycled residual InP substrate (401 ') could also be inspected for crystalline defects according to the inventive method. This could be carried out either as an initial step prior to starting a new layer transfer process, or as a part of the routine of the layer transfer process as illustrated in the embodiment of Figure 4.
  • Figure 4 illustrates the Smart CutTM layer transfer process that transfers an InP layer from an InP donor substrate (401 ), to a handle substrate comprising sapphire (402), followed by a crystalline quality inspection of the residual InP substrate (40 ⁇ ) according to an embodiment of the invention.
  • the layer transfer by Smart CutTM according to the fourth embodiment as illustrated in Figure 4 is similar to what is illustrated in Figure 3 and comprises the steps of: step I) performing a surface oxidation of a surface of the InP donor substrate (401 ) to obtain an insulating surface layer (403) on the InP donor substrate (401 ), step II) performing an ion implantation in the InP donor substrate (401 ) below the insulating surface layer (403) to obtain an in-depth layer (404) forming a predetermined splitting area, step III) flipping the InP donor substrate (401 ) with an insulating surface layer (403) and an in-depth weakened layer (404) and attaching the insulating surface layer (403) to the handle substrate comprising sapphire (402), step IV) detaching the InP donor substrate (401 ) at the level of the in-depth layer (404) to obtain an I nP on sapphire structure or InPOS (405) with a transferred InP layer (41 1 ) and a residual InP substrate (401 ').
  • the layer transfer process also comprises the step of: step V) recycling the residual InP substrate (40 ⁇ ) and use it as the donor substrate for a new layer transfer process.
  • the layer transfer process can also comprise the further steps of: step VI) cutting the InPOS structure (405) to a desired thickness to obtain a thinner InPOS structure (405') with a transferred InP layer (41 1 ) and a thinner handle substrate comprising sapphire (402") and a residual handle substrate comprising sapphire (402'), and/or step VII) recycling the residual handle substrate comprising sapphire (402') to use it as the handle substrate in a new layer transfer process.
  • the crystalline quality of the residual InP substrate (401 ') to be recycled is determined using the inventive method in a further step to be carried out after step IV) and before step V) of the layer transfer process described above.
  • the procedure follows essentially the procedures already described for Figure 1 : a two-steps etching is performed on the surface of the residual InP substrate (401 ') to reveal and/or enlarge existing defects.
  • advantage is furthermore taken from the fact that the first etching can be used to reduce surface roughness of the residual InP substrate (40V) .
  • the fourth embodiment of the inventive method as illustrated in Figure 4 thus comprises the following steps: step VII I) performing a first etching (412) on the surface of the residual InP substrate (401 ') to obtain a first etched surface (413) under first etching conditions, thereby revealing at least partially present defects, and step IX) performing a second etching (414) of the first etched surface (413) to obtain a second etched surface (415) under second etching conditions, thereby enlarging at least the at least partially revealed defects, wherein the first and second etching conditions are different.
  • the fourth embodiment illustrated in Figure 4 further comprises the step of: step X) inspecting the second etched surface (415) optically using an optical microscopy means (416).
  • this step is accompanied by an optical profilometer (417) comprising an optical interferometer, like in the second and third embodiments.
  • the ratios by volume of the two chemical solutions used to perform the first etching (412) and the second etching (414) of the residual InP substrate (40V) in steps VIM) and IX), the resulting roughness of the first etched surface (413), the temperature range for performing the etchings, and the etch rates of the first etching (412) and of the second etching (414) have been reported in the description of the first and second embodiments illustrated in Figures 1 A and 1 B. It is therefore referred back to the description above.
  • step X) in the fourth embodiment illustrated in Figure 4 comprises an optical inspection of the defects of the second etched surface ( 15) of the residual InP substrate (40 ) using an optical microscopy means (416), wherein this step is accompanied by a an optical profilometer (417) comprising an optical interferometer.
  • This follows essentially the procedure already described for the second embodiment in Figures 1 A, 1 B and 2. It is therefore referred back to Figures 1 - 2 and the description above.
  • the inventive two-steps etching allows to distinguish and identify defects at the surface of a lll-V semiconductor layer by enlarging said defects while keeping or improving the properties of the final etched surface close to those of the initial surface before etching.
  • the creation of etch artifacts can be prevented or at least reduced compared to the prior art.

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Abstract

La présente invention concerne un procédé permettant de déterminer la qualité du cristal d'une couche de semi-conducteur de type III-V. Ce procédé comporte les étapes consistant: a) à réaliser sur la surface de la couche de semi-conducteur III-V (101) une première gravure (102) donnant une surface gravée (103) dans des premières conditions de gravure, et b) à réaliser une seconde gravure (104) de la première surface gravée (103) donnant une deuxième surface gravée (105) dans des deuxièmes conditions de gravure, les premières conditions de gravure (102) étant différentes des deuxièmes conditions de gravure (104). L'invention concerne également un procédé permettant de déterminer la qualité du cristal d'une couche de semi-conducteur III-V. Ce procédé comporte une étape consistant à réaliser une gravure (102) d'une surface de la couche de semi-conducteur III-V (101) de façon à obtenir une surface gravée (103). Pour réaliser cette gravure (102) on utilise un mélange d'acide chlorhydrique et d'acide phosphorique (HCl / H3PO4), en particulier quand le semi-conducteur III-V est InP.
PCT/IB2012/001311 2011-07-06 2012-07-02 Procédé pour déterminer la qualité du cristal d'une couche de semi-conducteur iii-v WO2013005095A1 (fr)

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FR1156136 2011-07-06

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US9873797B2 (en) 2011-10-24 2018-01-23 Aditya Birla Nuvo Limited Process for the production of carbon black
CN110223913A (zh) * 2019-06-03 2019-09-10 云南大学 一种去除InP半导体材料衬底的方法
CN115491203A (zh) * 2022-09-13 2022-12-20 珠海鼎泰芯源晶体有限公司 一种腐蚀液及其制备方法和应用
US11668170B2 (en) 2020-11-24 2023-06-06 Halliburton Energy Services, Inc. Enhanced oil recovery harvesting for fractured reservoirs
US11668169B2 (en) 2020-11-24 2023-06-06 Halliburton Energy Services, Inc. Reactive surfactant flooding at neutral pH

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9873797B2 (en) 2011-10-24 2018-01-23 Aditya Birla Nuvo Limited Process for the production of carbon black
CN110223913A (zh) * 2019-06-03 2019-09-10 云南大学 一种去除InP半导体材料衬底的方法
US11668170B2 (en) 2020-11-24 2023-06-06 Halliburton Energy Services, Inc. Enhanced oil recovery harvesting for fractured reservoirs
US11668169B2 (en) 2020-11-24 2023-06-06 Halliburton Energy Services, Inc. Reactive surfactant flooding at neutral pH
CN115491203A (zh) * 2022-09-13 2022-12-20 珠海鼎泰芯源晶体有限公司 一种腐蚀液及其制备方法和应用
CN115491203B (zh) * 2022-09-13 2024-07-05 珠海鼎泰芯源晶体有限公司 一种腐蚀液及其制备方法和应用

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FR2977711A1 (fr) 2013-01-11

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