CN114347277B - InSb wafer preparation method - Google Patents
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- CN114347277B CN114347277B CN202111445494.0A CN202111445494A CN114347277B CN 114347277 B CN114347277 B CN 114347277B CN 202111445494 A CN202111445494 A CN 202111445494A CN 114347277 B CN114347277 B CN 114347277B
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- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 148
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- 238000009825 accumulation Methods 0.000 abstract 1
- 238000009828 non-uniform distribution Methods 0.000 abstract 1
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of an InSb wafer, which comprises the following steps: after the ingot is fixed according to a fixed reference, cutting the ingot perpendicular to the axis of the ingot to cut out a first InSb wafer; determining the crystal orientation of a first InSb wafer, adjusting the cutting angle, and continuously cutting out the end face of a first target crystal orientation on the cut ingot; maintaining a cutter blade angle, rotating the ingot by a target angle based on the fixed reference, performing cutting to obtain an end face of a second target crystal orientation; marking the end face of the second target crystal orientation, and cutting out a required seed crystal based on the marked end face; and performing crystal growth and cutting based on the cut seed crystal to obtain the target InSb wafer. The method solves the technical problem of nonuniform distribution of electrical parameters caused by accumulation of Te elements in the central area of the wafer after crystal growth, thereby improving the uniformity of the electrical parameters in the range of the effective area of the large-size InSb wafer and the effective use area of the wafer.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a preparation method of an InSb wafer.
Background
InSb is used as a III-V compound semiconductor material, has extremely high electron mobility, extremely narrow forbidden bandwidth, extremely small effective electron quality and other unique semiconductor properties, and is widely applied to the infrared detection field because an infrared device prepared from the InSb material is intrinsically absorbed in a medium-wave infrared band of 3-5 mu m and has extremely high quantum efficiency and response rate. Infrared detectors based on InSb materials have been developed from single-dimensional, multi-dimensional to one-dimensional arrays and two-dimensional focal plane arrays so far, with the ever increasing number of detector pixels, the ever decreasing pixel size, making the demand for high quality InSb wafers with high electrical uniformity, low defects increasingly urgent and enormous. In order to meet the requirements of InSb material electrical parameters on the preparation of infrared focal plane detectors, te element doping is required to be carried out on intrinsic InSb crystals. In a semiconductor, trace impurity elements can obviously influence the electrical properties of the semiconductor, and as a substrate material for an infrared detector, the electrical parameters of InSb must be strictly controlled so as to meet the preparation requirements of the infrared detector device.
Through the electrical parameter test research of the crystal grown by the traditional method, the phenomenon that the carrier concentration is obviously higher than that of other areas exists in the central area of the radial section of the crystal, namely Te element doping is accumulated in the area. Te element gathers in the center of wafer diameter direction, and is very unfavorable to the manufacturing of follow-up device, and the inhomogeneous region of electrical parameter falls into the device, and the device performance is probably seriously influenced, especially infrared focal plane array device of big area array. In addition, the concentration of Te elements in the central area of the wafer in the diameter direction also reduces the effective use area of the wafer and the core yield of the wafer.
Disclosure of Invention
The embodiment of the invention provides a preparation method of an InSb wafer with high electrical uniformity, which solves the technical problem of nonuniform electrical parameter distribution caused by Te element aggregation in the central area of the wafer after crystal growth, thereby improving the uniformity of electrical parameters in the effective area range of a large-size InSb wafer and the effective use area of the wafer.
The present disclosure proposes a method for preparing an InSb wafer, comprising:
after fixing the ingot according to a fixed reference, cutting the ingot perpendicular to the axis of the ingot to cut out a first InSb wafer;
Determining the crystal orientation of the first InSb wafer, adjusting the cutting angle based on the crystal orientation of the first InSb wafer, and continuously cutting out the end face of the first target crystal orientation on the cut ingot according to the adjusted cutting angle;
Maintaining a cutter blade angle, rotating the ingot by a target angle based on the fixed reference, and performing cutting to obtain an end face of a second target crystal orientation;
marking the end face of the second target crystal orientation, and cutting out a required seed crystal based on the marked end face;
And performing crystal growth and cutting based on the seed crystal obtained by cutting to obtain the target InSb wafer.
In some embodiments, the fixed reference is determined based on a growth ridge of the ingot.
In some embodiments, determining the crystal orientation of the first InSb wafer and adjusting the dicing angle based on the crystal orientation of the first InSb wafer comprises: performing crystal orientation test on the first InSb wafer; and determining an adjusted cutting angle based on the deviation of the crystal orientation of the first InSb wafer and the first target crystal orientation.
In some embodiments, the InSb wafer fabrication method further comprises, prior to dicing the end face of the second target crystal orientation: the cut surfaces were marked by dislocation etching.
In some embodiments, marking the end face of the second target crystal orientation comprises: marking the end face of the second target crystal orientation according to the grid line.
In some embodiments, the InSb wafer preparation method further comprises, prior to crystal growth and dicing based on the dicing obtained seed crystal: and grinding, mechanically polishing, cleaning and chemically polishing the seed crystal obtained by cutting.
In some embodiments, performing crystal growth and dicing based on the dicing-obtained seed crystal to obtain a target InSb wafer comprises: cutting the crystal grown based on the seed crystal, and removing the edge area of the cut wafer to obtain the target InSb wafer.
According to the embodiment of the invention, the crystal orientation of the first InSb wafer is determined, then the required end face is cut, and the angle is adjusted, so that the end face of the second crystal direction can be cut at the end face, the seed crystal is cut on the basis of the end face of the second crystal direction, then the crystal is grown and cut, and the Te element gathering area originally positioned at the central position can be adjusted to the edge position in the mode, so that the InSb wafer with high electrical uniformity can be obtained only by removing the edge of the wafer in subsequent processing.
The foregoing description is only an overview of the present invention, and is intended to be implemented in accordance with the teachings of the present invention in order that the same may be more clearly understood and to make the same and other objects, features and advantages of the present invention more readily apparent.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to designate like parts throughout the figures. In the drawings:
FIG. 1 is a basic flow chart of the InSb wafer manufacturing method of the present disclosure;
FIG. 2 is a schematic diagram of a Te element aggregation region of a first target crystal orientation of the present disclosure;
FIG. 3 is an end view schematic of an ingot of the present disclosure;
FIG. 4 is an example of a marking of an end face of a second target crystal orientation of the present disclosure;
FIG. 5 is a tetragonal seed crystal example of a second target crystal orientation of the present disclosure;
FIG. 6 is a schematic view of a wafer Te element aggregation region cut with a seed grown crystal of the present disclosure;
Fig. 7 is an example of a processing path of a high electrical uniformity InSb wafer of the present disclosure.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The present disclosure proposes a method for preparing an InSb wafer with high electrical uniformity, as shown in fig. 1, including:
In step S101, after the ingot is fixed in accordance with a fixed reference, a cut is made perpendicular to the axis of the ingot to cut out a first InSb wafer. The InSb wafer preparation method according to the present disclosure plays an important role in terms of fixed reference fixation, on which the subsequent dicing and angle adjustment are performed. After the ingot is fixed in a fixed reference, a cut is made perpendicular to the axis of the ingot, so that a first InSb wafer for orientation can be obtained.
In step S102, determining a crystal orientation of the first InSb wafer, and adjusting a cutting angle based on the crystal orientation of the first InSb wafer, so as to continuously cut an end face of the first target crystal orientation at the sliced ingot according to the adjusted cutting angle. Since the crystal orientation of the wafer from which the initial ingot was cut is uncertain, the present disclosure further determines the crystal orientation of the first InSb wafer for orienting the ingot currently held by the held reference, and then adjusts the cutting angle so that the end face of the first target crystal orientation is continuously cut at the cut ingot according to the adjusted cutting angle. For example, a first InSb wafer may be placed on an X-ray diffraction orienter for crystal orientation testing to determine the cutter angle, whereby the desired <111> ±0° ingot end face may be cut on a fixed basis. To this step the end face of the base, i.e. <111> + -0 deg. ingot end face, was determined. As shown in fig. 2, in this case, the Te element aggregation region 1 is located in the central region of the end face 2 of the first target crystal orientation, and in order to avoid the problem of aggregation of the Te element aggregation region in the central region, dicing is performed as follows.
In step S103, maintaining a cutter blade angle, rotating the ingot target angle based on the fixed reference, and performing cutting to obtain an end face of a second target crystal orientation. For example, in some embodiments, the theoretical deviation between the first target crystal orientation <111> ±0.1° and the second target crystal orientation <211> ±0.1° is 19 ° 28', and then the ingot may be rotated by 19 ° 28' directly based on the fixed reference, and the wafer and the end face obtained by cutting may be close to the end face of the second target crystal orientation <211> ±0.1°, and in particular embodiments, the crystal orientation measurement may be performed based on the cut wafer, and then the angle of the ingot may be fixed, and the angle of the cutting machine may be finely tuned to perform cutting until the end face of the second target crystal orientation <211> ±0.1° is obtained by cutting.
In step S104, the end face of the second target crystal orientation is marked, and a desired seed crystal is cut based on the marked end face. The seed crystal cut based on the end face is the desired seed crystal and has a target crystal orientation, for example, the target crystal orientation is <211>, and thus the crystal orientations of the prepared seed crystals are all <211>.
In step S105, crystal growth is performed based on the <211> crystal orientation seed obtained by dicing and dicing is performed to obtain a target InSb wafer. The cut seed crystal is pretreated before growth, and mechanical damage and pollution of surface processing are removed, so that the pretreated seed crystal is used for growth to obtain crystals of Te element aggregation area offset center area, and in the subsequent cutting and processing, the edge is only required to be removed, so that the InSb wafer with high quality and high electrical uniformity can be obtained.
According to the embodiment of the invention, the crystal orientation of the first InSb wafer is determined, then the required end face is cut, and the angle is adjusted, so that the end face of the second crystal direction can be cut at the end face, and the seed crystal is cut on the basis of the end face of the second crystal direction, so that the Te element gathering area originally positioned at the central position can be adjusted to the edge position in the mode, and the high-quality InSb wafer can be obtained only by removing the edge of the wafer in subsequent processing.
In some embodiments, the fixed reference is determined based on a growth ridge of the ingot. In the specific implementation, a section of single crystal ingot with low dislocation density, excellent performance and excellent quality and InSb <111> orientation can be selected. Then, three growing ridges 3 of the ingot are determined, as shown in fig. 3, the end points of the three growing ridges 3 are connected to the tail of the ingot, one side of an equilateral triangle formed by the end points of the three growing ridges 3 is perpendicular to the graphite base, the corner of the equilateral triangle opposite to the side faces to the left, and the crystal is adhered to the graphite base by using adhesive glue, so that the fixation is completed.
In some embodiments, determining the crystal orientation of the first InSb wafer and adjusting the dicing angle based on the crystal orientation of the first InSb wafer comprises: performing crystal orientation test on the first InSb wafer; and determining an adjusted cutting angle based on the deviation of the crystal orientation of the first InSb wafer and the first target crystal orientation. The first InSb wafer cut in the present disclosure is used for orientation use, for example, a crystal orientation test can be performed on an X-ray diffraction orientation machine to confirm the degree of deviation of the crystal orientation of the first InSb wafer from the first target crystal orientation <111>, whereby the angle of the cutter can be adjusted according to the determined deviation, and the cutting can be repeated until the obtained wafer is <111> ±0.1°, at which time the end face of the ingot is also <111> ±0.1°.
In some embodiments, the InSb wafer fabrication method further comprises, prior to dicing the end face of the second target crystal orientation: the cut surfaces were marked by dislocation etching. After the end face of the first target crystal orientation is obtained, the positive direction and the negative direction of growth need to be marked, so that the growth direction is guided by the cut seed crystal at a later stage. For example, the dislocation etching method is used to determine the A-plane ((111) plane) and the B-plane ((-1-1-1) plane) of the sliced wafer, the (111) plane and (-1-1-1) plane referred to in this example are two opposite planes, and after one of the planes is determined, the other plane can also be determined, and similar <211> and < -2-1-1> planes are also two opposite planes. The dislocation corrosive liquid is HF: HNO 3 = 1:1, and the surface on which dislocation etch pits appear can be identified as a surface a, the surface on which no etch pits appear as a surface B, and the surface a can be marked by observing both the front and rear surfaces of the wafer after etching.
In some embodiments, marking the end face of the second target crystal orientation comprises: marking the end face of the second target crystal orientation according to the grid line. As shown in FIG. 4, the grid mark can obtain a seed crystal of a desired specification, for example, according to a 10mm×10mm square mark, and then a cutter is used to cut a 10mm×10mm×60mm square seed crystal based on the grid mark.
In some embodiments, the InSb wafer preparation method further comprises, prior to crystal growth and dicing based on the dicing obtained seed crystal: and grinding, mechanically polishing, cleaning and chemically polishing the seed crystal obtained by cutting. Specifically, the foregoing procedure has cut out a tetragonal seed crystal of the first target crystal orientation as shown in fig. 5.
For each square seed crystal, firstly, polishing and chamfering are carried out on 4 long edges by using 400# abrasive paper to remove edge edges and corners, then, sequentially polishing and mechanically polishing the surfaces of the seed crystals by using 800# abrasive paper, 1000# abrasive paper, 2000# abrasive paper and 5000# abrasive paper, and then, washing the seed crystals by using deionized water.
And (3) chemically polishing and corroding the cleaned seed crystal by utilizing the chemically polished corrosive liquid which is independently developed and prepared by the applicant. The chemical polishing corrosion time is 5-10 s, so that mechanical damage and pollution on the surface are removed, and the defect expansion in the surface damage layer is prevented from extending into the grown Czochralski single crystal InSb. Meanwhile, the impurity metal pollution caused by seed crystals can be reduced by chemical polishing, then the seed crystals are sequentially cleaned by ultrasonic for 5 minutes by trichloroethylene, acetone and absolute ethyl alcohol, the seed crystals are dried in an oven at 110 ℃ after cleaning, finally the seed crystals and the crystal orientation are packaged by using dust-free paper, the seed crystals are marked, and the seed crystals are stored in a nitrogen storage cabinet and are used when the crystal grows.
In some embodiments, the volume ratio of HF and HNO 3 in the chemical polishing slurry is greater than 60%, the remainder of the solution is a buffer solution containing acetic acid, for example, the chemical polishing slurry in one example employs a volume ratio of H 2O：HF：HNO3: hac=2: 5:3: the prepared etching solution can solve the problems that a large amount of gas is separated out in the traditional etching solution chemical etching process, oxidation is easy to cause and the surface state is poor.
In some embodiments, performing crystal growth and dicing based on the dicing-obtained seed crystal to obtain a target InSb wafer comprises: cutting the crystal grown based on the seed crystal, and removing the edge area of the cut wafer to obtain the target InSb wafer.
Specifically, the tetragonal seed crystal with the crystal orientation of < -2-1-1> can be adopted for crystal growth, and a special multi-wire saw can be adopted for wafer cutting after the crystal growth is completed. As shown in FIG. 6, the distribution area of the Te element aggregation area 1 in the InSb crystal growing in the < 2-1-1> crystal orientation is obviously positioned in the edge area, and the distribution area of the Te element aggregation area 1 can be removed according to the path shown in FIG. 7 in the cutting process, so that the standardized high-quality InSb wafer 4 with high electrical uniformity and low defects is prepared.
By adopting the InSb seed crystal preparation method, the InSb crystal growth method and the InSb wafer processing method, the technical problem of nonuniform electrical parameter distribution caused by the aggregation of Te elements in the central area of the wafer after crystal growth is solved, and the uniformity of electrical parameters in the range of the effective area of the large-size InSb wafer and the effective use area of the wafer are improved. The method can prepare the high-quality InSb wafer with high electrical uniformity and low defects.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The foregoing embodiment numbers of the present invention are merely for the purpose of description, and do not represent the advantages or disadvantages of the embodiments.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many forms may be made by those having ordinary skill in the art without departing from the spirit of the present invention and the scope of the claims, which are to be protected by the present invention.
Claims (4)
1. A method for preparing an InSb wafer, comprising:
determining a fixed reference based on a growing ridge of the ingot;
after fixing the ingot according to a fixed reference, cutting the ingot perpendicular to the axis of the ingot to cut out a first InSb wafer;
Determining the crystal orientation of the first InSb wafer, adjusting a cutting angle based on the crystal orientation of the first InSb wafer, continuously cutting out an end face of a first target crystal orientation on the cut ingot according to the adjusted cutting angle, and determining that an aggregation area of Te elements is in a central area of the end face of the first target crystal orientation;
Maintaining a cutter blade angle, rotating the ingot by a target angle based on the fixed reference, and performing cutting to obtain an end face of a second target crystal orientation;
marking the end face of the second target crystal orientation, and cutting out a required seed crystal based on the marked end face;
performing crystal growth and cutting based on the seed crystal obtained by cutting to obtain a target InSb wafer;
Determining the crystal orientation of the first InSb wafer, and adjusting the cutting angle based on the crystal orientation of the first InSb wafer comprises:
performing crystal orientation test on the first InSb wafer;
determining an adjusted cutting angle based on a deviation of the crystal orientation of the first InSb wafer from a first target crystal orientation;
performing crystal growth and dicing based on the dicing-obtained seed crystal to obtain a target InSb wafer includes:
Cutting the crystal based on seed crystal growth, wherein the Te element of the InSb crystal is offset from the central area and positioned at the edge position, and removing the edge area of the cut wafer to obtain the target InSb wafer.
2. The InSb wafer fabrication method of claim 1, further comprising, prior to dicing the end face of the second target crystal orientation: the cut surfaces were marked by dislocation etching.
3. The InSb wafer fabrication method of claim 1, wherein marking the end face of the second target crystal orientation comprises: marking the end face of the second target crystal orientation according to the grid line.
4. The InSb wafer preparation method of claim 3, further comprising, before crystal growth and dicing based on the seed crystal obtained by dicing:
and grinding, mechanically polishing, cleaning and chemically polishing the seed crystal obtained by cutting.
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| CN105525350A (en) * | 2015-12-22 | 2016-04-27 | 中国电子科技集团公司第二研究所 | Method for growing large-size and low-defect silicon carbide monocrystal and wafer |
| JP2018104231A (en) * | 2016-12-26 | 2018-07-05 | 昭和電工株式会社 | MANUFACTURING METHOD OF SiC WAFER AND SiC WAFER |
| CN108166060A (en) * | 2017-12-25 | 2018-06-15 | 云南北方昆物光电科技发展有限公司 | A kind of indium antimonide<211>The preparation method of direction monocrystalline |
| CN108417484A (en) * | 2018-04-13 | 2018-08-17 | 中国电子科技集团公司第四十六研究所 | A method of promoting photoelectric sensor silicon epitaxy layer doping concentration uniformity |
| CN111152375A (en) * | 2019-11-05 | 2020-05-15 | 中国电子科技集团公司第十三研究所 | Method for cutting substrate wafer by indium phosphide crystal bar |
| CN111910255A (en) * | 2020-08-04 | 2020-11-10 | 中国电子科技集团公司第十一研究所 | Large-size <111> crystal orientation low dislocation density InSb crystal growth method |
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