CN115440574A - Method for preparing single crystal substrate slice by dividing indium phosphide defective crystal bar - Google Patents
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- CN115440574A CN115440574A CN202211029141.7A CN202211029141A CN115440574A CN 115440574 A CN115440574 A CN 115440574A CN 202211029141 A CN202211029141 A CN 202211029141A CN 115440574 A CN115440574 A CN 115440574A
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Abstract
The invention discloses a method for preparing a single crystal substrate slice by dividing an indium phosphide defective crystal bar, which comprises the following steps: making angles at the head and the tail of the cutting, marking positioning edges, cutting, avoiding defects, scribing and edging. The method can reasonably utilize the effective area of each wafer through sorting the wafers after cutting, improves the utilization rate of single crystals, avoids the problem that the defects of the cut wafers cannot be avoided after picking and qualifying, and reduces the risk of uncontrollable factors; the method is flexible, and can screen and scribe according to different effective areas, thereby reducing the phenomenon of wafer scrap and improving the value of single wafers; laser cutting is adopted, and compared with the 1.5mm loss of a bar, the material loss is saved by about 94 percent, and time and materials are saved; the crystal orientation angle quality is obviously improved.
Description
Technical Field
The invention relates to a method for preparing a single crystal substrate slice by dividing an indium phosphide defective crystal bar, belonging to the technical field of processing of the indium phosphide defective crystal bar.
Background
Indium phosphide (InP) is one of important group iii-v compound semiconductor materials, and is a new-generation electronic functional material following Si and GaAs. Indium phosphide has many advantages such as a direct transition type energy band structure, high photoelectric conversion efficiency and electron mobility, easiness in making a semi-insulating sheet material, suitability for making high-frequency microwave devices and circuits, high operating temperature, strong radiation resistance, high conversion efficiency as a solar cell material, and the like. The characteristics determine that the light-emitting diode has wide application in civil and military fields such as solid light emitting, microwave communication, optical fiber communication, guidance/navigation, satellites and the like.
Indium phosphide (InP) has the advantages of high electron mobility, good radiation resistance, large forbidden band width and the like, and has key advantages in two application fields, namely (1) the photon field, namely the emission and detection capability with the wavelength of more than 1000 nm; (2) High speed and low noise performance in high frequency RF applications. Currently, the real driving force in the InP wafer market is in photonic applications.
At present, the main specifications of indium phosphide comprise 2 inch 3 inch specifications and 4 inch specifications, crystals mainly grow on 4 inch crystals, a plurality of Twin line (Twin line) defects are found in the existing processing process of the crystals, the defects are cut into one extremely fine line on the rear surface of a substrate sheet, the length of the line is 1-100 mm, even goldenrain tree crystal lines penetrate through the whole crystal bar, most goldenrain tree lines have inclination angles, and the Twin line positions are randomly generated in the edge inner part or the central area of the crystal plate in the crystal production process and are extremely difficult to find. The traditional processing method comprises the following steps: the method comprises the steps of head and tail cutting, bar drawing, angle making, excircle rolling, edge grinding, edge cutting and edge grinding, wherein cutting adjustment cannot be performed on the basis due to fixed bar drawing positions, a round bar is further reduced, the appearance of defects inside crystals is unknown, the possibly drawn region contains polycrystal or Luan Jing (Twin line) defects, so that wrong drawing or misjudgment is easily caused, inclined Luan Jingxian also causes that single crystals cannot be made, or a considerable part of wafers contain 3532 defects in a small region after the cut bar is cut, so that the wafers are scrapped, namely the defects cannot be avoided in the traditional process for processing, therefore, a large number of scrapped wafers are generated due to the defects in the processing process, which causes high production cost, and in order to solve the problem, the inventor develops a new process and solves the problem, and solves the problem of a cutting method for avoiding 3425 xzft 3425.
Disclosure of Invention
The invention provides a method for preparing a single crystal substrate slice by dividing an indium phosphide defect crystal bar, which can effectively avoid the defect of the crystal bar, improve the effective utilization rate of the single crystal and reduce the cost by improving the method.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for preparing a single crystal substrate slice by dividing an indium phosphide defective crystal bar comprises the following steps:
1) Cutting off the head and the tail of the crystal bar, and making an angle on the end surface of the head (100) of the crystal bar according to requirements;
2) Sawing a sample wafer with the thickness OF 0.5-1.5 mm from the head OF the crystal bar, corroding for 2-5 min by hydrochloric acid, flushing with water, drying, observing the crystal cell direction under a 10X objective lens by using a microscope, determining the crystal orientation OF [0-1-1] OF the crystal cell, and grinding an OF positioning flat edge with the width OF 5-10 mm at the edge position OF the crystal orientation OF [0-1-1] OF the crystal bar by using a flat grinder as a mark;
3) Positioning and slicing the processed crystal bar on a multi-wire cutting machine, and cutting into wafers with uniform thickness;
4) Inspecting all wafers, avoiding defects, marking the appearance of a defect-free qualified wafer, contrasting the marks in the step 2), and performing cleavage to obtain a cleaved flat edge;
5) Taking the cleavage flat edge as a positioning edge, scribing and cutting the marked qualified area of the wafer into blank wafers of 2 inches, 3 inches or 4 inches by using a laser scribing machine;
6) And edging the InP blank wafer to obtain a qualified 2-inch, 3-inch or 4-inch wafer.
In the step 1), the angle is made according to the requirement of a client, and the precision range required by the client is usually about 0.01-0.2 degrees.
In the step 2), when the sample wafer is sawed, the direction of the saw blade is vertical to the height direction of the crystal bar.
The indium phosphide segmentation preparation method can effectively avoid single crystal defects.
As a general knowledge, the [100] plane is the surface OF the wafer, the OF flat side is the large side, and the OF flat side direction is the [0-1-1] direction.
The design steps of the invention are as follows: the method can obtain 2-inch, 3-inch or 4-inch flawless substrate slices by cutting the head and the tail, marking the positioning edge, slicing, avoiding the defect, scribing and edging the edge so as to obtain 4-inch flawed wafers. According to the invention, after the crystal bar is divided by evaluating the effective area OF the wafer through the surface OF the single crystal, bar drawing and excircle processing are cancelled, the multi-line cutting mode is directly adopted for slicing, defects can be avoided through measuring the position OF the effective area, 2-inch, 3-inch or 4-inch cutting areas are marked, and then the OF flat edge is cut by cleavage according to the lining mark, so that the Luan Jing (Twin line) defect can be perfectly avoided, and the processing OF the lossless single crystal is realized.
Indium phosphide polycrystal or Luan Jing (Twin wire) defect in the prior art, the following 2 cases resulted in scrap: 1) Scrapping of crystal bar defects: the large-angle inclined Luan Jing (Twin line) or a plurality of Luan Jing defects have more defects, the defects account for about 60 percent of crystals, the crystal bars cannot completely utilize an effective area to manufacture qualified substrates in a bar drawing mode, and only a part of the effective area can be drawn for utilization. 2) And (3) scrapping of wafer defects: after the crystal bar is processed into a shape, the shape of the wafer cannot be adjusted to avoid defects, and the wafer is scrapped due to the existence of partially invisible Luan Jing (Twin wire) or internal fine polycrystal after being cut into the wafer. The invention can utilize the single crystal containing partial defects to process the effective area of the single crystal rod into a single crystal wafer to the maximum extent.
In order to further improve the utilization rate of the crystal bar, in the step 1), when the head and the tail are cut off, the rotating speed of the blade is 500-5000 r/min, the cutting speed is 1-20 mm/min, the cutting depth is 50-120 mm, and the flow rate of water is 100-600 ml/min. When the head and the tail are cut off, no requirement is made on the temperature.
In order to further improve the utilization rate of the crystal bar, in the step 1), when an angle is formed, the environment temperature is 15-28 ℃, the rotating speed of a blade is 500-5000 r/min, the cutting speed is 1-20 mm/min, the cutting depth is 50-120 mm, the cutting precision is 0.01-0.5 degrees, and the flow rate of water is 100-600 ml/min.
In order to further improve the utilization rate of the crystal bar, in the step 2), when marking is carried out, the environmental temperature is 15-28 ℃, the rotating speed of the blade is 500-5000 r/min, the cutting speed is 0.01-0.1 mm/min, the cutting depth is 0.1-2 mm, the cutting precision is 0.1-0.5 degrees, and the flow rate of water is 100-600 ml/min.
In order to further improve the efficiency, in the step 3), the environmental temperature is 20-26 ℃ during slicing, and the mass ratio of the silicon carbide powder to the cutting fluid is (1.1-2): 1, the rotating speed of a blade is 200-1000 r/min, the cutting speed is 1-10 mm/min, the cutting depth is 50-120 mm, the cutting precision is 0.01-0.5 degrees, and the flow of cutting fluid is 300-3000 ml/min.
In order to further improve the product quality, in the step 4), the environment temperature is 15-28 ℃, the rotating speed of the blade is 1-5 r/min, the cutting speed is 1-50 times/min, and the cutting depth is 0.1-1 mm during cleavage.
In order to further consider the efficiency and the quality, in the step 5), during laser scribing, the laser instantaneous temperature is high, the wafer is cracked and cracked due to the excessively low environmental temperature, the environmental temperature is set to be 20-26 ℃, the frequency is 20-100 HZ, the cutting speed is 10-500 times/min, and the cutting depth is 0.3-1 mm.
In step 6), during edging, the ambient temperature is 15-28 ℃, the rotating speed of a blade is 500-5000 r/min, the cutting speed is 1-10 mm/min, the cutting depth is 0.2-2 mm, the cutting precision is 0.01-0.5 degrees, and the flow rate of water is 100-1000 ml/min.
The invention relates to a method for preparing a single crystal substrate slice by dividing an indium phosphide defect crystal bar, which comprises the steps of estimating the effective area of a wafer through the surface of the single crystal, dividing the crystal bar, canceling bar drawing and excircle processing, slicing in a direct multi-line cutting mode, then effectively marking and cutting a lining, obtaining a blank slice by marking the position by adopting a laser scribing method, then obtaining a finished product of the indium phosphide wafer in an edging mode, and perfectly avoiding the Luan Jing (Twin line) defect to realize processing of a lossless single crystal.
The prior art is referred to in the art for techniques not mentioned in the present invention.
The method for preparing the single crystal substrate slice by dividing the indium phosphide defective crystal bar reduces the steps of bar digging and excircle processing on the basis of the prior art, introduces a new technical process route of sorting, piece checking, marking and cutting and laser scribing, and has the following beneficial effects compared with the traditional processing technology: 1. the effective area of each wafer can be reasonably utilized through sorting the cut wafers, the utilization rate of single crystals is improved, the problem that the defects of the cut wafers cannot be avoided after bar picking and qualification are avoided, and the risk of uncontrollable factors is reduced; 2. the method is flexible, the scribing can be respectively screened according to different effective areas, the phenomenon of wafer scrap is reduced, the value of the wafer is high when the size of the wafer is larger, the value of 3 inches is larger than 2 inches, the wafer which can be processed by 2 inches or 3 inches is sorted according to the position of a defect, and the value of a single wafer is improved; 3. the laser cutting technology which is mature in the prior art is adopted, the cutting gap of laser cutting is about 0.1mm, and compared with the loss of 1.5mm of a bar, the material loss is saved by about 94%, and time and materials are saved; 4. the crystal orientation angle quality is obviously improved.
Drawings
FIG. 1 is a schematic diagram of a VGF produced crystal Luan Jing (Twin line) defect crystal sample;
FIG. 2 is a schematic view of the processing steps of "cutting the head and the tail to make an angle", "making a positioning edge mark", and "slicing" of the ingot of FIG. 1;
FIG. 3 is a schematic view of the processing steps of "defect avoidance, scribing and edge grinding" of the slice obtained in FIG. 2;
FIG. 4 is a schematic view OF a wafer, where 1 is the [100] direction OF the wafer surface, 2 is the OF flat side [0-1-1] direction (alignment side), and 3 is the IF flat side [0-11] direction (minor side);
Detailed Description
For better understanding of the present invention, the following examples are given for further illustration of the present invention, but the present invention is not limited to the following examples.
Example 1
Taking a Luan Jing Twin line defect as an example, because of the inclined penetration of Twin line, the conventional bar drawing process is not suitable for the processing production of indium phosphide with this kind of defect, as shown in fig. 1, the crystal bar is a round blank, the height (length) is about 100mm, the diameter is 103-105 mm, there are two and three Luan Jing (Twin line), the conventional processing method is to draw bar vertically from the cone part to prepare 2 inch (3 inch) specification, because of the requirement of angle surface, the defect cannot be completely avoided, so that the single crystal cannot be well utilized, in this example, the following method is adopted to prepare single crystal substrate slices by dividing:
1) The length of the crystal bar after head and tail cutting of the crystal bar is 72mm, whether a cut surface of the end surface is defective or not is checked, the complete area of the [100] end surface is oriented on an X ray, the orientation precision is controlled to be 0.03 degrees, the cutting speed of a circular saw in MB TS206 is controlled to be 15mm/min for cutting, the angle is 0.07 +/-0.05 degrees, the angle is 31 DEG 39 '45' in the positive crystal direction, 31 DEG 44 '05' in the 111 polarization direction, and the angle is 68mm after head and tail invalid areas are cut in the crystal direction of 0.07 degrees;
2) A sample wafer with the thickness OF 0.8mm is made by circular sawing in an MB TS206 along the head (100) direction OF the crystal bar, and is corroded for 5min by hydrochloric acid (formed by mixing 35% by mass OF hydrochloric acid and water), washed for 2min by water, dried, the direction OF a crystal cell is observed by a microscope under a 10X objective lens, one surface OF the crystal cell is transversely vertical and the other surface is transversely parallel, the (0-1-1) crystal direction OF the crystal cell is determined as an OF positioning flat edge, and a 12mm width is ground at the edge position OF the (0-1-1) crystal direction OF the crystal bar by a plane grinder to be used as an OF positioning flat edge as a mark;
3) Solidifying a processed crystal bar on a crystal puller by using AB adhesive glue, adjusting a (100) plane on a high bird 610SD multi-line slicer to be within the range of 0.01-0.5 degrees, cutting the crystal bar into 480 mu m wafers in a multi-line mode, configuring slurry into 1500-mesh silicon carbide powder and cutting liquid (model JX-8A, petrochemical research institute in Shaanxi province) of Liuhe Gaipu powder company Limited according to the mass ratio of 1.5, degumming and cleaning the surfaces after slicing to obtain 480 mu m 113 wafers, and obtaining the following data through sampling test;
| tablet number | BOW | WARP | TTV | TIR | LTIR | LTV |
| 1 | 0.832 | 17.745 | 2.919 | 2.128 | 0.827 | 1.221 |
| 20 | -2.113 | 19.788 | 2.915 | 2.603 | 1.427 | 0.869 |
4) Checking the defect position on the surface of the wafer for marking, avoiding the defect, marking the shape of a defect-free qualified slice, marking a gap with the length of 2-4 mm at the edge by using a diamond pen at the marking position (0-1-1) to avoid the defect, breaking the gap to obtain a cleavage flat edge, marking 36 slices in 3 inches and 77 slices in 2 inches;
5) Taking the cleavage flat edge as a positioning edge, avoiding the 2-inch mark position of the defect, carrying out scribing and cutting by adopting a Kehanlong laser scribing machine according to the appearance drawn in the step 4), and reserving a machining allowance of 0.2-2 mm during scribing and cutting;
6) The diameter OF the InP blank wafer is measured to be in a qualified range, an edge mold is ground into a finished product on a WGM4200 edge grinding machine by a molding wheel groove with the diameter OF R0.1-R0.5mm to obtain 77 2-inch wafers and 36 3-inch wafers, and the angle measurement precision is better by an X-ray orientation instrument manufactured by Dandong New Oriental Crystal Instrument Limited, the 2-inch OF plain edge measures an angle OF 21 degrees and 45 'and 36', and the IF (0-11) measures: 21 '43' was relatively normal, and 3 inches OF Flat edge crystal orientation was measured OF 31 '45' 42 ", IF (0-11) was measured: 21 ° 44' is in range.
Parameters of the procedures in example 1
Through the adjustment of the scheme, after the rod drawing and rounding process is removed, sorting and defect avoidance are added, a laser cutting technology is introduced, scribing is carried out while avoiding the defects, the position of the defects can be avoided by the sorting method while avoiding the defects, qualified wafers are scribed, and the wafer qualification rate is improved; the slit of laser cutting is about 0.1mm, and the material loss is saved by about 94% compared with the loss of 1.5mm of the bar.
Comparative example 1
The method is characterized in that a defective crystal bar is processed by adopting the existing method, the crystal bar is a round blank, the height (length) of the crystal bar is about 100mm, the diameter of the crystal bar is in a 4-inch specification of 103-105 mm, two and three channels of Luan Jing (Twin lines) are provided, the defect is similar to that in the embodiment 1, and the processing steps comprise: cutting the head and the tail, digging a rod, making an angle, rolling the outer circle, grinding a positioning edge, slicing and edging, digging the rod and rolling the outer circle according to a conventional method, and referring to the parameter requirements of the rest steps in the embodiment 1.
Comparison of yields from example 1 and comparative example 1:
| processing method | Crystal bar numbering | Length of crystal | Producing sheets | 2 |
3 inch slice | Defect sheet | Yield of finished products | |
| Example 1 | IF20032-1 | 68 | 113 | 77 | 36 | 0 | 100.00％ | |
| Comparative example 1 | IS20023 | 65 | 108 | 49 | 0 | 59 | 45.37％ |
Precision comparison of example 1 and comparative example 1
The flat edge OF the wafer OF is not more than 0.05 degrees and is a high-precision crystal orientation, and the quality OF the crystal orientation angle is obviously improved by the above table.
Comparative example 2
The ambient temperature for laser scribing was raised to 30-35 ℃ only, and the remainder was as in example 1, resulting in 75 2 inch wafers and 36 3 inch wafers.
Comparative example 3
The ambient temperature for laser scribing was reduced to 10-15 deg.C only, and the rest was referenced to example 1, resulting in 64 2 inch wafers and 33 3 inch wafers.
Claims (8)
1. A method for preparing a single crystal substrate slice by dividing an indium phosphide defective crystal bar is characterized by comprising the following steps: the method comprises the following steps:
1) Cutting off the head and the tail of the crystal bar, and making an angle on the end surface of the head [100] of the crystal bar according to requirements;
2) Sawing a sample wafer with the thickness OF 0.5-1.5 mm from the head OF the crystal bar, corroding for 2-5 min by hydrochloric acid, flushing with water, drying, observing the crystal cell direction under a 10X objective lens by using a microscope, determining the crystal orientation OF [0-1-1] OF the crystal cell, and grinding an OF positioning flat edge with the width OF 5-10 mm at the edge position OF the crystal orientation OF [0-1-1] OF the crystal bar by using a flat grinder as a mark;
3) Positioning and slicing the processed crystal bar on a multi-wire cutting machine, and cutting into wafers with uniform thickness;
4) Inspecting all wafers, avoiding defects, marking the appearance of a defect-free qualified wafer, contrasting the marks in the step 2), and performing cleavage to obtain a cleaved flat edge;
5) Taking the cleavage flat edge as a positioning edge, scribing and cutting the non-defective qualified wafer along the shape marked by the laser scribing machine into 2-inch, 3-inch or 4-inch blank wafers;
6) And edging the InP blank wafer to obtain a qualified 2-inch, 3-inch or 4-inch wafer.
2. A method for producing a single crystal substrate wafer by dividing an indium phosphide-defective ingot as set forth in claim 1, wherein: in the step 1), when the head and the tail are cut off, the rotating speed of the blade is 500-5000 r/min, the cutting speed is 1-20 mm/min, the cutting depth is 50-120 mm, and the flow rate of water is 100-600 ml/min.
3. The method of producing a single crystal substrate wafer by dividing an indium phosphide-defective ingot as set forth in claim 1 or 2, wherein: in the step 1), when the angle is made, the environment temperature is 15-28 ℃, the rotating speed of the blade is 500-5000 r/min, the cutting speed is 1-20 mm/min, the cutting depth is 50-120 mm, the cutting precision is 0.01-0.5 degrees, and the flow rate of water is 100-600 ml/min.
4. The method of producing a single crystal substrate wafer by dividing an indium phosphide-defective ingot as set forth in claim 1 or 2, wherein: in the step 2), when marking is carried out, the environmental temperature is 15-28 ℃, the rotating speed of the blade is 500-5000 r/min, the cutting speed is 0.01-0.1 mm/min, the cutting depth is 0.1-2 mm, the cutting precision is 0.1-0.5 degrees, and the flow rate of water is 100-600 ml/min.
5. The method of producing a single crystal substrate wafer by dividing an indium phosphide-defective ingot as set forth in claim 1 or 2, wherein: in the step 3), during slicing, the ambient temperature is 20-26 ℃, and the mass ratio of the silicon carbide powder to the cutting fluid is (1.1-2): 1, the rotating speed of a blade is 200-1000 r/min, the cutting speed is 1-10 mm/min, the cutting depth is 50-120 mm, the cutting precision is 0.01-0.5 degrees, and the flow of cutting fluid is 300-3000 ml/min.
6. The method of producing a single crystal substrate wafer by dividing an indium phosphide-defective ingot as set forth in claim 1 or 2, wherein: in the step 4), the environment temperature is 15-28 ℃, the rotating speed of the blade is 1-5 r/min, the cutting speed is 1-50 times/min, and the cutting depth is 0.1-1 mm during cleavage.
7. The method of producing a single crystal substrate wafer by dividing an indium phosphide-defective ingot as set forth in claim 1 or 2, wherein: in the step 5), during laser scribing, the environmental temperature is 20-26 ℃, the frequency is 20-100 HZ, the cutting speed is 10-500 times/min, and the cutting depth is 0.3-1 mm.
8. The method of producing a single crystal substrate wafer by dividing an indium phosphide-defective ingot as set forth in claim 1 or 2, wherein: in the step 6), during edging, the environment temperature is 15-28 ℃, the rotating speed of the blade is 500-5000 r/min, the cutting speed is 1-10 mm/min, the cutting depth is 0.2-2 mm, the cutting precision is 0.01-0.5 degrees, and the flow rate of water is 100-1000 ml/min.
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| CN117901281A (en) * | 2023-12-07 | 2024-04-19 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Processing method and application of indium phosphide monocrystal |
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2022
- 2022-08-26 CN CN202211029141.7A patent/CN115440574A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117901281A (en) * | 2023-12-07 | 2024-04-19 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Processing method and application of indium phosphide monocrystal |
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