CN112899788A - Preliminary screening method and device for silicon carbide crystal ingot - Google Patents
Preliminary screening method and device for silicon carbide crystal ingot Download PDFInfo
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- CN112899788A CN112899788A CN202110050329.9A CN202110050329A CN112899788A CN 112899788 A CN112899788 A CN 112899788A CN 202110050329 A CN202110050329 A CN 202110050329A CN 112899788 A CN112899788 A CN 112899788A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07C—POSTAL SORTING; SORTING INDIVIDUAL ARTICLES, OR BULK MATERIAL FIT TO BE SORTED PIECE-MEAL, e.g. BY PICKING
- B07C5/00—Sorting according to a characteristic or feature of the articles or material being sorted, e.g. by control effected by devices which detect or measure such characteristic or feature; Sorting by manually actuated devices, e.g. switches
- B07C5/34—Sorting according to other particular properties
- B07C5/3416—Sorting according to other particular properties according to radiation transmissivity, e.g. for light, x-rays, particle radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B19/00—Single-purpose machines or devices for particular grinding operations not covered by any other main group
- B24B19/22—Single-purpose machines or devices for particular grinding operations not covered by any other main group characterised by a special design with respect to properties of the material of non-metallic articles to be ground
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
- B28D5/02—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by rotary tools, e.g. drills
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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Abstract
The invention provides a preliminary screening method and a device of a silicon carbide crystal ingot, wherein the method comprises the following steps: (1) polishing or cutting the surface of the silicon carbide crystal ingot to obtain a transparent or semitransparent silicon carbide crystal ingot; (2) irradiating the silicon carbide crystal ingot by using an ultraviolet light source to obtain a light transmission wavelength of the silicon carbide crystal ingot, comparing the light transmission wavelength with a standard color wavelength range to judge whether the density of the microtubes or the density of inclusions is qualified, screening to obtain the silicon carbide crystal ingot with qualified microtubes or inclusions, and carrying out the next operation; the standard color wavelength is the range of the light-transmitting color wavelength of the standard silicon carbide crystal ingot with qualified density of the microtube and the inclusion after the standard silicon carbide crystal ingot is irradiated by the same ultraviolet light source. After the silicon carbide crystal ingot is polished and cut, the visualization degree is improved, and the silicon carbide crystal ingot with qualified microtubule density or inclusion density is obtained by screening through ultraviolet irradiation, so that the accuracy of primary screening is improved, and the working strength of subsequent processing and detection is reduced.
Description
Technical Field
The application relates to a preliminary screening method and a preliminary screening device for a silicon carbide crystal ingot, and belongs to the technical field of semiconductor material processing equipment.
Background
After the silicon carbide crystal ingot is prepared, subsequent steps of processing, quality detection and the like are needed, and the product with qualified detection quality can be further applied. Because the ingot needs to be sliced during processing, the workload is large; and if the defective goods are unqualified in the subsequent quality detection, the whole utilization of the defective goods is limited because the defective goods are sliced.
The silicon carbide crystal ingot can be manually judged after the furnace is started, primary screening is carried out, obviously unqualified products are removed, and the workload of subsequent processing and quality detection can be reduced. However, the silicon carbide ingot is low in visibility, and is difficult to judge artificially, and judgment errors are liable to occur. The existing method needs to process and slice the silicon carbide crystal ingot, all the obtained wafers are subjected to quality detection, unqualified products are removed, qualified products are reserved, and the working strength is high.
Disclosure of Invention
In order to solve the problems, the application provides a preliminary screening method and a preliminary screening device for silicon carbide crystal ingots, the visualization degree is improved after the silicon carbide crystal ingots are polished and cut, the silicon carbide crystal ingots with qualified microtubule density or inclusion density are obtained by screening through ultraviolet irradiation, the accuracy of preliminary screening is improved, and the working strength of subsequent processing and detection is reduced.
According to an aspect of the present application, there is provided a preliminary screening method of a silicon carbide ingot, the method including the steps of:
(1) polishing or cutting the surface of the silicon carbide crystal ingot to obtain a transparent or semitransparent silicon carbide crystal ingot;
(2) irradiating the silicon carbide crystal ingot obtained in the step (1) by using an ultraviolet light source to obtain a light transmission wavelength of the silicon carbide crystal ingot, comparing the light transmission wavelength with a standard color wavelength threshold value to judge whether the density of the microtubes or the density of the inclusions is qualified, screening to obtain the silicon carbide crystal ingot with qualified microtubes or inclusions, and carrying out the next operation; the standard color wavelength is the range of the light-transmitting color wavelength of the standard silicon carbide crystal ingot with qualified density of the microtube and the inclusion after the standard silicon carbide crystal ingot is irradiated by the same ultraviolet light source.
Further, in the step (2), a crystal plane diagram of the silicon carbide crystal ingot is obtained by using a microscope, the position area of the micropipe or the inclusion on the crystal plane diagram is determined, and whether the density of the micropipe or the inclusion is qualified or not is judged according to the light transmission wavelengths corresponding to different areas;
preferably, when the transmission wavelength is 393-400 nm, determining that the density of the microtubes is unqualified; when the transmission wavelength is 365-375 nm, determining that the density of the inclusion is unqualified; and when the transmission wavelength is more than 375nm and less than 393nm, determining that the densities of the microtube and the inclusion are qualified.
Further, the silicon carbide crystal ingot with qualified micropipe density refers to a silicon carbide crystal ingot with the micropipe density of less than or equal to 0.2 pieces/cm 2;
the silicon carbide crystal ingot with qualified inclusion density is a silicon carbide crystal ingot with the inclusion density of less than 20 percent of unit area in unit volume;
preferably, the silicon carbide ingot has a thickness of at least 5mm or more; the silicon carbide crystals are selected from one or two of 4H type silicon carbide and 6H type silicon carbide.
Further, before the step (2), detecting polytype of the silicon carbide crystal ingot to obtain polytype thickness, and if the difference between the thickness of the silicon carbide crystal ingot and the polytype thickness is more than or equal to 4mm, performing the next step of removing the polytype;
and if the difference between the thickness of the silicon carbide crystal ingot and the polytype thickness is less than 4mm, judging the silicon carbide crystal ingot to be unqualified.
Further, a cold light source is used for irradiating one side surface of the silicon carbide crystal ingot, the other side surface of the silicon carbide crystal ingot is marked with a production position of multiple types, and the thickness of the multiple types is measured;
preferably, the positions of the polytypes are marked on the other side surface of the silicon carbide ingot by a marker pen, and the thickness of the polytype is measured by a measuring tool.
Further, the step (2) further includes detecting the resistivity of the silicon carbide ingot, and specifically includes:
irradiating the side surface of the silicon carbide crystal ingot by using a cold light source, detecting the light transmission wavelength of the silicon carbide crystal ingot, comparing the light transmission wavelength with the standard color wavelength range, and judging whether the resistivity is qualified or not according to the comparison result; the standard color wavelength range is a numerical range of light-transmitting color wavelength of a standard silicon carbide crystal ingot with qualified resistivity after being irradiated by the same cold light source.
Further, when the light transmission wavelength is 585-596 nm, judging that the resistivity is qualified; when the light transmission wavelength is less than 575nm or more than or equal to 5978nm, judging that the resistivity is unqualified; and when the transmission wavelength is greater than or equal to 575nm and less than 585nm or equal to 597nm, precisely detecting the resistivity of the silicon carbide crystal ingot and then judging.
Further, in the step (1), the polishing process for the side surface of the silicon carbide ingot comprises: placing a silicon carbide crystal ingot on a placing platform, fixing the silicon carbide crystal ingot, and controlling a polishing rotating shaft to move so that the silicon carbide crystal ingot is positioned in the polishing rotating shaft; controlling the grinding rotating shaft to rotate so that the grinding rotating shaft grinds the side face of the silicon carbide crystal ingot; and/or
In the step (1), the specific operation of removing the seed crystal face of the silicon carbide crystal ingot comprises the following steps: fixing the side surface of the silicon carbide crystal ingot, and controlling a polishing rotating shaft with a polishing plate arranged at the bottom end to move so that the polishing plate is contacted with the seed crystal surface of the silicon carbide crystal ingot; controlling the grinding rotating shaft to rotate so that the grinding plate polishes to remove the seed crystal face; and/or
In the step (1), the specific operation of removing the seed crystal face of the silicon carbide crystal ingot comprises the following steps: the convex surface of the silicon carbide crystal ingot is upward, the side surface of the silicon carbide crystal ingot is fixed, the cutting structure is controlled to move to the position with the required cutting thickness, and the cutting structure is controlled to rotate, so that the cutting structure cuts the convex surface of the crystal ingot.
According to another aspect of the present application, there is provided an apparatus that can implement the preliminary screening method of a silicon carbide ingot of any one of the above, the apparatus including:
the polishing processing unit is used for polishing the side surface of the silicon carbide crystal ingot and removing a seed crystal face and a convex face of the silicon carbide crystal ingot;
the detection unit comprises a microscope, an objective table of the microscope is used for placing the silicon carbide crystal ingot, and an ultraviolet light source is arranged below a light through hole of the objective table; and a scanning imaging device is arranged above the objective table, and an ultraviolet receiving device is arranged in the scanning imaging device.
Furthermore, a cold light source is arranged on one side of the objective table, which is positioned at the light through hole, and a chromatic aberration processing device is arranged on the other side of the light through hole;
preferably, the grinding processing unit includes: a placement platform for placing the ingot; the polishing rotating shaft is arranged above the placing platform and can rotate, a polishing surface is arranged on the inner wall of the polishing rotating shaft and can be in contact with the side surface of the crystal ingot so as to polish the side surface of the crystal ingot, a polishing plate is detachably mounted at the bottom end of the polishing rotating shaft and is used for polishing the seed crystal surface of the crystal ingot; a cutting structure disposed above the placement platform, the cutting structure for cutting a convex surface of the ingot;
preferably, the polishing process unit further comprises a first fixing member disposed above the placing platform, the first fixing member being capable of contacting an upper surface of the ingot and fixing the ingot;
preferably, the first fixing assembly comprises a first telescopic rod and a fixing block, the fixing block is fixed at the bottom end of the first telescopic rod, and the fixing block contacts with the upper surface of the crystal ingot and fixes the crystal ingot; the polishing rotating shaft is connected with the first telescopic rod;
preferably, a second fixing assembly is arranged on the side edge of the placing platform, the second fixing assembly comprises a second telescopic rod and a clamping structure, the clamping structure is arranged at the top end of the second telescopic rod, and the clamping structure is used for fixing the side face of the crystal ingot;
preferably, the sanding processing unit further comprises a third telescopic rod, the bottom end of which is provided with a cutting structure for cutting the convex surface of the ingot.
The beneficial effects of the invention include but are not limited to:
(1) according to the preliminary screening method of the silicon carbide crystal ingot, the visualization degree is improved after the silicon carbide crystal ingot is ground or cut, the silicon carbide crystal ingot with qualified microtubule density or inclusion density is obtained by screening through ultraviolet irradiation, the accuracy of preliminary screening is improved, and the working strength of subsequent processing and detection is reduced.
(2) The preliminary screening method of the silicon carbide crystal ingot further removes unqualified products by detecting the polytype and the resistivity of the silicon carbide crystal ingot, further improves the accuracy of preliminary screening, has simple steps and strong operability, and provides the integral working efficiency.
(3) According to the device, the visualization degree of the surface of the silicon carbide crystal ingot is increased through the polishing processing unit, and then the microtubes, the inclusion bodies and the like are detected by the detection unit, so that the accuracy of primary screening is improved, and the working strength of subsequent processing and detection is reduced.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a cross-sectional view of a sanding process unit to which the present application is directed;
fig. 2 is a sectional view of a sanding process unit according to an embodiment of the present application;
FIG. 3 is a front view of a detection unit according to the present application;
wherein, 1, a platform is placed; 2. polishing the rotating shaft; 3. a first telescopic rod; 4. a fixed block; 5. grinding the plate; 6. a second telescopic rod; 7. a clamping structure; 8. a third telescopic rod; 9. cutting the structure; 10. a slider; 11. a slide rail; 12. an object stage; 13. a light through hole; 14. an objective lens; 15. an ultraviolet light source; 16. scanning an imaging device; 17. a cold light source; 18. and a color difference processing device.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced in other ways than those described herein, and therefore the scope of the present application is not limited by the specific embodiments disclosed below.
In addition, in the description of the present application, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present application.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
In this application, unless expressly stated or limited otherwise, the terms "mounted," "connected," "coupled," and the like are to be construed broadly and include, for example, fixed or removable connections or integral parts; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. In the description herein, reference to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Example 1
Referring to fig. 1, the present embodiment provides a preliminary screening device for a silicon carbide ingot, the device includes a polishing processing unit and a detection unit, the polishing processing unit includes a placing platform 1, a polishing spindle 2 and a cutting structure 9, the placing platform 1 is used for placing the silicon carbide ingot, the polishing spindle 2 is disposed above the placing platform 1, the polishing spindle 2 can rotate, the inner wall of the polishing spindle 2 is provided with a polishing surface, and the polishing surface can contact with the side surface of the silicon carbide ingot to polish the side surface of the silicon carbide ingot. The grinding surface of the grinding rotating shaft is used for grinding the side surface of the silicon carbide crystal ingot; the bottom end of the polishing rotating shaft 2 is detachably provided with a polishing plate 5, and the polishing plate 5 is used for polishing the seed crystal surface of the silicon carbide crystal ingot. The cutting structure 9 is used to cut the convex surface of the silicon carbide ingot. The detection unit comprises a microscope, an object stage 12 of the microscope is used for placing a silicon carbide crystal ingot, and an ultraviolet light source 15 is arranged below a light through hole 13 of the object stage 12; a scanning imaging device 16 is arranged above the objective table, and an ultraviolet receiving device is arranged in the scanning imaging device 16; the ultraviolet light source 15 penetrates through the upper surface or the lower surface of the silicon carbide crystal ingot, the ultraviolet light source 15 penetrates through the silicon carbide crystal ingot and is received by the ultraviolet receiving device, and an ultraviolet absorption photometry graph of the silicon carbide crystal ingot can be obtained through the scanning imaging device 16. The polishing processing unit increases the visualization degree of the surface of the silicon carbide crystal ingot, and then the detection unit is used for detecting the microtube and the inclusion of the silicon carbide crystal ingot, so that the accuracy of primary screening is improved.
Specifically, the surface of the silicon carbide ingot consists of a side surface, a seed crystal surface and a convex surface (here, a long crystal surface), the seed crystal surface and the convex surface are oppositely arranged, and the side surface is arranged between the seed crystal surface and the convex surface; after the silicon carbide ingot is placed on the placing platform, the upper surface of the silicon carbide ingot can be a seed crystal plane or a convex plane of the silicon carbide ingot. The specific structure of the polishing spindle 2 is not limited as long as the polishing surface of the polishing spindle 2 can polish the silicon carbide ingot. The polishing rotating shaft 2 is connected with a driving motor to realize the rotation of the polishing rotating shaft 2. The material of the polishing surface is not particularly limited as long as polishing treatment can be realized; preferably, the grinding surface is made of steel or iron; more preferably, the polishing surface is made of diamond. The detachable mounting manner of the polishing plate 5 and the polishing spindle 2 is not particularly limited, and a detachable connection manner conventional in the art may be adopted. For example, the side wall of the grinding rotating shaft 2 is provided with a bolt hole, and the grinding plate 5 is arranged at the bottom end of the grinding rotating shaft 2 through a bolt; or the side of the polishing plate 5 is provided with a buckle, the inner wall of the polishing rotating shaft 2 is provided with a clamping groove matched with the buckle, and the polishing plate 5 is installed through the matching of the buckle and the clamping groove.
As an embodiment of the present application, the inner wall of the polishing rotating shaft 2 is provided with a fine rough surface consisting of a plurality of concave and convex points, and the fine rough surface forms a polishing surface; the diameter of the concave-convex points is 1-100 nm. The fine rough surface can be in contact with the side surface of the silicon carbide crystal ingot for polishing, a carbon layer formed on the side surface of the silicon carbide crystal ingot can be processed, the visualization degree of the side surface of the silicon carbide crystal ingot is improved, the phenomenon of the concentration of the peripheral stress of the silicon carbide crystal ingot can be reduced, and the peripheral stress of the silicon carbide crystal ingot is reduced to a certain degree.
As an embodiment of the present application, sandpaper is attached to an inner wall of the polishing spindle 2, and forms a polishing surface. The sand paper can reduce the damage to the silicon carbide crystal ingot to be extremely low, further reduces the cracking rate of the silicon carbide crystal ingot and improves the accuracy of primary screening.
As an implementation mode of the application, the inner diameter of the grinding rotating shaft 2 is equal to the outer diameter of the silicon carbide crystal ingot, so that the silicon carbide crystal ingot is just sleeved inside the grinding rotating shaft 2, the grinding rotating shaft 2 rotates, the periphery side edges of the silicon carbide crystal ingot are simultaneously ground, and the grinding treatment efficiency is improved.
As an embodiment of the present application, the polishing process unit further includes a first fixing member disposed above the placing platform 1, the first fixing member being capable of contacting an upper surface of the silicon carbide ingot and fixing the silicon carbide ingot; the first fixing assembly comprises a first telescopic rod 3 and a fixing block 4, the fixing block 4 is fixed at the bottom end of the first telescopic rod 3, and the fixing block 4 is in contact with the upper surface of the silicon carbide crystal ingot and is used for fixing the silicon carbide crystal ingot; the polishing rotating shaft 2 is connected with the first telescopic rod 3. The first telescopic rod 3 controls the movement of the fixed block 4 so that the fixed block 4 is contact-fixed or away from the silicon carbide ingot. Through being connected the pivot 2 of polishing with first telescopic link 3, can realize the removal of pivot 2 of polishing to make pivot 2 of polishing contact or keep away from the carborundum ingot.
As an embodiment of the present application, a movable second fixing component is arranged at a side of the placing platform 1; the second fixing assembly comprises a second telescopic rod 6 and a clamping structure 7, wherein the clamping structure 7 is arranged at the top end of the second telescopic rod 6, and the clamping structure 7 is used for fixing the side surface of the silicon carbide crystal ingot. The second telescopic rod 6 controls the movement of the clamping structure 7 so that the clamping structure 7 clamps the silicon carbide ingot fixed or away. When polishing treatment is carried out on the seed crystal face of the silicon carbide crystal ingot, the side face of the silicon carbide crystal ingot needs to be fixed, so that the silicon carbide crystal ingot is prevented from shifting during polishing treatment, and the polishing treatment efficiency is improved.
Specifically, the clamping structure 7 is not particularly limited as long as the fixation of the side surface of the silicon carbide ingot can be achieved. For example, the clamping structure 7 may be a plurality of clamping blocks that clamp and fix the silicon carbide ingot somewhere on the lateral surface thereof.
As an embodiment of the present application, the clamping structure 7 is a circular ring structure, and the circular ring structure is provided with an inflation inlet, and the circular ring structure is used for fixing the periphery of the side surface of the silicon carbide ingot after being inflated. After the circular ring structure is inflated, extrusion force is applied to the side face of the silicon carbide crystal ingot, so that the periphery of the silicon carbide crystal ingot is fixed. The fixing mode is simple and firm.
As an embodiment of the application, the device also comprises a third telescopic rod 8, the bottom end of the third telescopic rod 8 is provided with a cutting structure 9, and the cutting structure 9 is used for cutting the convex surface of the silicon carbide crystal ingot. Furthermore, the cutting structure is connected with a driving motor, and an output shaft of the driving motor is connected with the cutting structure through a rotating shaft. Preferably, the cutting structure 9 is a cutting gear. The third telescopic rod 8 can control the displacement of the cutting structure 9, so that the convex surface of the silicon carbide crystal ingot can be cut under the condition of selecting the thickness.
As an embodiment of the present application, the bottom end of the placing platform 1 is connected with the slide rail 11 through the slide block 10. The placing platform 1 is arranged to be slidable, so that the placing platform 1 can move, polishing treatment on the side surface and the seed crystal surface of the silicon carbide crystal ingot and cutting treatment on the convex surface of the silicon carbide crystal ingot are achieved respectively.
As an embodiment of the present application, in order to reduce damage to the silicon carbide ingot, at least the surface of the placing platform 1 in contact with the silicon carbide ingot is a rubber material. The device further comprises a control system, wherein the control system is respectively connected with the first telescopic rod 3, the second telescopic rod 6, the third telescopic rod 8 and the sliding block 10 and used for controlling the telescopic movement of the first telescopic rod 3, the second telescopic rod 6 and the third telescopic rod 8 and the movement of the sliding block 10.
In one embodiment of the present invention, a cold light source 17 is mounted on one side of the stage 12, which is located at the light-transmitting hole 13, and a color difference processing device 18 is mounted on the other side of the light-transmitting hole. Preferably, the distance from the cold light source to the silicon carbide crystal ingot is controlled to be 8-12 cm, the distance from the silicon carbide crystal ingot on the opposite side of the irradiation position to the silicon carbide crystal ingot is controlled to be 12-18 cm, and the chromatic aberration processing device is connected with the computer to receive the wavelength data. More preferably, the color difference processing device is a color difference meter. Preferably, a scanning imaging device 16 is mounted above the stage 12 at the transducer of the objective lens 14; preferably, the scanning imaging device 16 is a camera.
And grinding and cutting the silicon carbide crystal ingot to obtain the transparent or semitransparent silicon carbide crystal ingot. The thickness of the polished side surface is 0.8-1 mm, the thickness of the polished seed crystal surface is 1-1.2 mm, and the thickness of the cut convex surface is 1-10 mm, so that the silicon carbide crystal ingot is integrally a transparent or semitransparent solid with a certain thickness, and the visibility is strong; and then, detecting the microtubes, the inclusions, the polytypes and the resistivity by using the detection unit, removing unqualified products, and reserving the products with the microtubes, the inclusions and the polytypes and the resistivity which are qualified for detection for subsequent processing.
Example 2
The present embodiment provides a preliminary screening method of a silicon carbide ingot, the method including the steps of:
1. polishing the side surface of the silicon carbide crystal ingot, and removing a seed crystal face and a convex face of the silicon carbide crystal ingot: placing a silicon carbide crystal ingot on a placing platform, fixing the silicon carbide crystal ingot, and controlling a polishing rotating shaft to move so that the silicon carbide crystal ingot is positioned in the polishing rotating shaft; controlling the grinding rotating shaft to rotate so that the grinding rotating shaft grinds the side face of the silicon carbide crystal ingot; then fixing the side surface of the crystal ingot, and controlling a polishing rotating shaft with a polishing plate arranged at the bottom end to move so that the polishing plate is contacted with the seed crystal surface of the silicon carbide crystal ingot; controlling the grinding rotating shaft to rotate so that the grinding plate polishes to remove the seed crystal face; the convex surface of the silicon carbide crystal ingot is upward, the side surface of the silicon carbide crystal ingot is fixed, the cutting structure is controlled to move to the position with the required cutting thickness, and the cutting structure is controlled to rotate, so that the cutting structure cuts the convex surface of the crystal ingot. The specific operation is as follows:
(1) after the silicon carbide crystal ingot is placed on the placing platform 1, the first telescopic rod 3 drives the first fixing assembly to descend, the first fixing assembly is fixed through downward extrusion force of the first fixing assembly, the polishing plate 5 is not installed at the moment, after the silicon carbide crystal ingot is fixed, the driving motor controls the polishing rotating shaft 2 to rotate, the rotating speed is controlled to be 500-1800 r/min, and the silicon carbide crystal ingot is specifically determined according to the side visibility degree of the silicon carbide crystal ingot; meanwhile, the placing platform 1 can be controlled to rotate, and the silicon carbide crystal ingot is closer to the grinding surface, so that the silicon carbide crystal ingot is ground more smoothly; and finishing the polishing treatment of the side surface of the silicon carbide crystal ingot after the side surface of the silicon carbide crystal ingot shows the visual gloss flatness.
(2) The polishing plate 5 is installed on the polishing rotating shaft 2, the second telescopic rod 6 drives the clamping structure 7 to move upwards, the clamping structure 7 transversely extrudes the silicon carbide crystal ingot, the side face of the silicon carbide crystal ingot is fixed, the stretching amount is controlled according to the thickness of the silicon carbide crystal ingot, the crystal face of the silicon carbide crystal ingot seed is guaranteed to be exposed, the polishing rotating shaft 2 continuously rotates to start polishing the crystal face, and after the luster and flatness is visible to the naked eye, polishing treatment of the crystal face of the silicon carbide crystal ingot seed is finished.
(3) Controlling a second telescopic rod 6 to drive a clamping structure 7 to move downwards, turning the convex surface of a silicon carbide ingot to face upwards, driving the clamping structure 7 to move upwards by the second telescopic rod 6, clamping and fixing the side surface of the silicon carbide ingot by the clamping structure 7, simultaneously controlling a placing platform 1 to move, controlling a third telescopic rod 8 to drive a cutting structure 9 to move downwards, adjusting the cutting thickness by the third telescopic rod 8, performing zero clearing treatment according to the size of the silicon carbide ingot in the implementation process, namely, how much the cutting structure 9 cuts downwards means the thickness of the silicon carbide ingot from the upper part to the lower part layer by layer, performing convex surface cutting on the silicon carbide ingot to facilitate observation, not performing fine processing, after the transverse fixing is completed, after the length control of the third telescopic rod 8 is completed, starting to rotate the cutting structure 9 to cut the silicon carbide ingot, and simultaneously cooling water is used for cutting and polishing in each step, and finishing the primary grinding and cutting treatment of the silicon carbide crystal ingot when the cutting of the convex surface of the silicon carbide crystal ingot is finished.
2. Respectively detecting the polytype, the microtube, the inclusion and the resistivity of the silicon carbide crystal ingot, removing unqualified products, and reserving the qualified products for subsequent processing.
(1) Detection of polytype: irradiating the side surface of the silicon carbide crystal ingot by using a cold light source, marking the output positions of multiple types and the qualified thickness on the other side surface of the silicon carbide crystal ingot by using a vernier caliper and a fine marking pen, wherein the thickness of the silicon carbide crystal ingot is X, the thickness of the multiple types is Y, and unqualified products with the thickness of X-Y <4mm are directly removed; and (4) keeping the product with the X-Y value of more than or equal to 4mm as a qualified product, and carrying out the next step. In order to reduce the detection of polytype to the follow-up microtube and inclusion, polytype is required to be cut and removed, and the polytype is cut and removed by using the cutting structure in the polishing processing unit.
(2) Detection of microtubules and inclusion bodies: the detection unit is arranged in a lightproof darkroom, then an ultraviolet light source is opened to irradiate the lower surface of the crystal, an objective lens is fixed, the focal length is adjusted, at the moment, a scanning imaging device is fixed together with the objective lens, after the fixation, a movable sliding plate on an objective table starts to move clockwise until the whole crystal face appears in an eyepiece, after the fixation, a computer receives data through the scanning imaging device, the scanning imaging device obtains two groups of data, the first group is a crystal face graph, namely the amplified graph of the whole crystal appearing under a microscope can clearly observe the positions of a micropipe and an inclusion, but the second group is an ultraviolet absorption luminosity graph, the ultraviolet light receiving device can obtain crystal face areas with different colors on one crystal face due to different ultraviolet light wavelength intensities, and the graph can only judge the strength of the crystal face position, the absorption type cannot be judged, the change of the ultraviolet light intensity caused by the reason can be judged by combining the first group of graphs and the second group of graphs, and the micro-tube or the wrapping object can be accurately judged, and the judgment on the micro-tube and the wrapping object is finished.
Judging the types of the microtubules and the inclusion: the hollow represents a micro-tube, the solid represents a wrapping object, meanwhile, the crystal plane diagram is divided into a plurality of regions with equal areas, position labeling is facilitated, ultraviolet crystal plane diagram analysis is carried out after the type is determined, the ultraviolet absorption luminosity diagram is divided into a plurality of regions in the same position for analysis and labeling, the position type is convenient to judge, and the specific standard is as follows:
according to statistical data, when the crystal is free from defects, the obtained ultraviolet light with the ultraviolet transmission wavelength of 385 nm; when a certain substance affects ultraviolet light, the wavelength range begins to have floating change in a larger range, and the influence relation between the wavelength of the ultraviolet light and the defect type is observed to find that when the ultraviolet transmission wavelength is 365-375 nm, the crystal plane images of the first group are compared in the same direction, so that the wrapping object in the wavelength range is relatively serious, and the wrapping object in the wavelength range can be seen by naked eyes and has higher density; when the ultraviolet transmission wavelength is 393-400 nm, the ultraviolet transmission is almost nearly not blocked, and the first group of crystal plane images are compared in the same direction, so that the phenomenon of micropipe cavities in the area is obvious, the micropipes are nearly half full-surface between 396 and 400nm, the density of the micropipes is still high between 393 and 396nm, and the micropipe does not reach the qualified standard; when the ultraviolet transmission wavelength is more than 375nm and less than 393nm, a certain degree of defects appear, and the ultraviolet transmission wavelength is qualified through actual detection and can reach the use standard.
Samples were taken for spot inspection in order to characterize the relationship of microtube and inclusion density-qualified samples to the transmission wavelength. Selecting an ingot with a transmission wavelength of 382nm to carry out slicing to obtain 12 wafers, and detecting the density of the microtubes and the inclusions of the 12 wafers by using a precision instrument, wherein the detection result is shown in table 1.
TABLE 1
Selecting an ingot with the transmission wavelength of 398nm to slice the ingot to obtain 11 wafers, and detecting the density of the microtubes and the inclusions of the 11 wafers by using a precision instrument, wherein the detection result is shown in table 2.
TABLE 2
Selecting an ingot with a transmission wavelength of 373nm to slice the ingot to obtain 11 wafers, and detecting the density of the microtubes and the inclusions of the 11 wafers by using a precision instrument, wherein the detection result is shown in Table 3.
TABLE 3
As is clear from the results in Table 1, in the ingot having a transmission wavelength of 382nm, the micropipe density of the wafers numbered 11 and 12 was more than 0.2 roots/cm2Unqualified, the density of the microtubes is unqualified; the inclusion unit area ratio of the wafers 10, 11 and 12 is more than 20%, and the inclusion density is not qualified. If at least one of the plurality of wafers sliced from one silicon carbide crystal ingot is qualified, judging that the silicon carbide crystal ingot is qualified; therefore, the ingot having a transmission wavelength of 382nm was judged as being acceptable. As is clear from the results in Table 2, in the ingot having a transmission wavelength of 398nm, the micropipe density of the wafers numbered 1 to 11 was more than 0.2 counts/cm2The density of the microtubes is unqualified; the inclusion unit area of the wafers of the numbers 10 and 11 is more than 20 percent, and the inclusion density is unqualified; and judging that the density of the silicon carbide crystal ingot micropipes is unqualified. As is clear from the results in Table 3, in the ingot having a transmission wavelength of 373nm, the micropipe density of the wafers numbered 10 and 11 was more than 0.2 roots/cm2The density of the microtubes is unqualified; the inclusion unit area percentage of the wafers with the labels of 1-11 is more than 20%, and the inclusion density is unqualified; and judging that the density of the silicon carbide crystal ingot inclusion is unqualified.
(3) And (3) detection of resistivity: a cold light source is used for irradiating the side surface of the silicon carbide crystal ingot, the chromatic aberration processing device receives wavelength data of the transmitted crystal and displays a numerical value on a computer, whether the resistivity is qualified or not is judged according to the numerical value, and the data accuracy is enhanced when the wavelength range is judged as the silicon carbide crystal ingot is polished and the permeability is enhanced; the wavelength of the adopted cold light source is 560-580 nm.
The method comprises the steps of obtaining 100 silicon carbide crystal ingot samples with the same thickness and purity by adopting a PVT (physical vapor transport) same method and steps, respectively measuring light transmission wavelengths of the 100 silicon carbide crystal ingot samples by adopting the detection method, and counting test results to obtain the light transmission wavelength value of the silicon carbide crystal prepared by adopting the method, wherein the light transmission wavelength value of the silicon carbide crystal is 570-599 nm, randomly selecting one silicon carbide crystal ingot sample at each wavelength point value in the range, sequentially carrying out slicing, circle cutting, grinding and polishing, and then testing the resistivity of the silicon carbide crystal ingot, wherein each silicon ingot sample randomly selects 3 wafers for testing, and when carrying out the resistivity test on the wafers, each point on one crystal face has resistivity and is distributed differently, so that the final resistivity data all take the maximum value of the resistivity on the crystal face, namely the most unqualified value. The results are shown in Table 4.
TABLE 4
From the results of Table 4, it is understood that the range of the wavelength is shortened and refined by polishing the silicon carbide ingot, and that the resistivity is more than 10 at the wavelength less than 575nm-6The film is not qualified; the wavelength is greater than or equal to 575nm and less than 585nm, the resistivity shows that the crystal ingot is qualified and unqualified, and the crystal ingot needs further detection by subsequent processing slices; the specific resistance is less than 10 within the wavelength of 585-596 nm-7The crystal ingot is qualified, the qualified crystal ingot and the unqualified crystal ingot are both qualified when the wavelength is 597nm and further detected, the crystal ingot is unqualified when the wavelength is greater than or equal to 598nm, and all crystal ingots in the unqualified wavelength are screened out.
In the preliminary screening method, the time for polishing and cutting a crystal ingot and detecting polytype, microtubes, inclusion and resistivity is 8-10 min, and the time for processing after preliminary screening is 10-12 min. If one crystal ingot is not subjected to the preliminary screening method, the processing time is 16-18 min. The quality detection time of a processed and sliced ingot is 45-50 min, the time data which is characterized by the quality detection and is detected without any time interval is longer if the flow type detection standard of the wafer downloaded step by step is calculated.
200 samples of silicon carbide ingots with the thickness of 10mm are obtained by the same method and steps of PVT, wherein 100 samples are randomly extracted and subjected to the primary screening method of the application to screen qualified products for subsequent processing and quality detection (operation 1); in addition, in the processing and quality inspection step (operation 2) which is directly performed in 100 cases, since the silicon carbide ingot needs to be sliced at the time of processing, if at least one of the plurality of sliced wafers of the silicon carbide ingot is qualified, the silicon carbide ingot is judged to be qualified. The elapsed time and the number of acceptable products and unacceptable products of runs 1 and 2 were counted, and the results are shown in Table 5.
TABLE 5
As can be seen from the results in Table 5, after the preliminary screening of the application, most even all unqualified samples can be removed by screening, and the screening accuracy is high. In order to further verify the accuracy of the preliminary screening method, 42 unqualified samples removed by the preliminary screening in the operation 1 are subjected to subsequent processing and quality detection, and the 42 samples are detected to be unqualified, and the detection result is completely consistent with the preliminary screening result. After the preliminary screening, the subsequent processing and quality detection time of unqualified samples is saved, and the working strength of the subsequent processing and quality detection is obviously reduced.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above are merely examples of the present application, and the scope of the present application is not limited by these specific examples, but is defined by the claims of the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A method of preliminary screening a silicon carbide ingot, the method comprising the steps of:
(1) polishing or cutting the surface of the silicon carbide crystal ingot to obtain a transparent or semitransparent silicon carbide crystal ingot;
(2) irradiating the silicon carbide crystal ingot obtained in the step (1) by using an ultraviolet light source to obtain a light transmission wavelength of the silicon carbide crystal ingot, comparing the light transmission wavelength with a standard color wavelength threshold value to judge whether the density of the microtubes or the density of the inclusions is qualified, screening to obtain the silicon carbide crystal ingot with qualified microtubes or inclusions, and carrying out the next operation; the standard color wavelength is the range of the light-transmitting color wavelength of the standard silicon carbide crystal ingot with qualified density of the microtube and the inclusion after the standard silicon carbide crystal ingot is irradiated by the same ultraviolet light source.
2. The preliminary screening method of a silicon carbide ingot as set forth in claim 1, wherein in the step (2), a crystal plane map of the silicon carbide ingot is obtained by a microscope, a position region of the micropipes or inclusions on the crystal plane map is determined, and whether the density of the micropipes or inclusions is qualified or not is judged according to light transmission wavelengths corresponding to different regions;
preferably, when the transmission wavelength is 393-400 nm, determining that the density of the microtubes is unqualified; when the transmission wavelength is 365-375 nm, determining that the density of the inclusion is unqualified; and when the transmission wavelength is more than 375nm and less than 393nm, determining that the densities of the microtube and the inclusion are qualified.
3. A preliminary screening method for a silicon carbide ingot as set forth in claim 1 wherein the silicon carbide ingot having a satisfactory micropipe density means that the density of the micropipes is 0.2 pieces/cm or less2A silicon carbide ingot of (a);
the silicon carbide crystal ingot with qualified inclusion density is a silicon carbide crystal ingot with an inclusion unit area ratio of less than 20%;
preferably, the silicon carbide ingot has a thickness of at least 5mm or more; the silicon carbide crystals are selected from one or two of 4H type silicon carbide and 6H type silicon carbide.
4. The preliminary screening method of a silicon carbide ingot as set forth in claim 1, wherein before the step (2), the method further comprises the steps of detecting polytype of the silicon carbide ingot to obtain polytype thickness, and performing a next polytype cutting operation if the difference between the thickness of the silicon carbide ingot and the polytype thickness is 4mm or more;
and if the difference between the thickness of the silicon carbide crystal ingot and the polytype thickness is less than 4mm, judging the silicon carbide crystal ingot to be unqualified.
5. The preliminary screening method of a silicon carbide ingot as set forth in claim 4, wherein a cold light source is used to irradiate one side surface of the silicon carbide ingot, and a plurality of types of output positions are marked on the other side surface of the silicon carbide ingot, and the thickness of the plurality of types is measured;
preferably, the positions of the polytypes are marked on the other side surface of the silicon carbide ingot by a marker pen, and the thickness of the polytype is measured by a measuring tool.
6. The preliminary screening method of a silicon carbide ingot as set forth in claim 1, wherein the step (2) further comprises detecting the resistivity of the silicon carbide ingot by:
irradiating the side surface of the silicon carbide crystal ingot by using a cold light source, detecting the light transmission wavelength of the silicon carbide crystal ingot, comparing the light transmission wavelength with the standard color wavelength range, and judging whether the resistivity is qualified or not according to the comparison result; the standard color wavelength range is a numerical range of light-transmitting color wavelength of a standard silicon carbide crystal ingot with qualified resistivity after being irradiated by the same cold light source.
7. The preliminary screening method of a silicon carbide ingot as set forth in claim 6, wherein when the transmission wavelength is 585 to 596nm, the resistivity is judged to be acceptable; when the light transmission wavelength is less than 575nm or more than or equal to 598nm, judging that the resistivity is unqualified; and when the transmission wavelength is greater than or equal to 575nm and less than 585nm or equal to 597nm, precisely detecting the resistivity of the silicon carbide crystal ingot and then judging.
8. The preliminary screening method of a silicon carbide ingot as set forth in claim 1, wherein the concrete operation of grinding the lateral surface of the silicon carbide ingot in the step (1) comprises: placing a silicon carbide crystal ingot on a placing platform, fixing the silicon carbide crystal ingot, and controlling a polishing rotating shaft to move so that the silicon carbide crystal ingot is positioned in the polishing rotating shaft; controlling the grinding rotating shaft to rotate so that the grinding rotating shaft grinds the side face of the silicon carbide crystal ingot; and/or
In the step (1), the specific operation of removing the seed crystal face of the silicon carbide crystal ingot comprises the following steps: fixing the side surface of the silicon carbide crystal ingot, and controlling a polishing rotating shaft with a polishing plate arranged at the bottom end to move so that the polishing plate is contacted with the seed crystal surface of the silicon carbide crystal ingot; controlling the grinding rotating shaft to rotate so that the grinding plate polishes to remove the seed crystal face; and/or
In the step (1), the specific operation of removing the seed crystal face of the silicon carbide crystal ingot comprises the following steps: the convex surface of the silicon carbide crystal ingot is upward, the side surface of the silicon carbide crystal ingot is fixed, the cutting structure is controlled to move to the position with the required cutting thickness, and the cutting structure is controlled to rotate, so that the cutting structure cuts the convex surface of the crystal ingot.
9. An apparatus for carrying out the preliminary screening method of a silicon carbide ingot as set forth in any one of claims 1 to 8, characterized by comprising:
the polishing processing unit is used for polishing the side surface of the silicon carbide crystal ingot and removing a seed crystal face and a convex face of the silicon carbide crystal ingot;
the detection unit comprises a microscope, an objective table of the microscope is used for placing the silicon carbide crystal ingot, and an ultraviolet light source is arranged below a light through hole of the objective table; and a scanning imaging device is arranged above the objective table, and an ultraviolet receiving device is arranged in the scanning imaging device.
10. The device of claim 9, wherein a cold light source is installed on one side of the light through hole on the object stage, and a chromatic aberration processing device is installed on the other side of the light through hole;
preferably, the grinding processing unit includes:
a placement platform for placing the ingot;
the polishing rotating shaft is arranged above the placing platform and can rotate, a polishing surface is arranged on the inner wall of the polishing rotating shaft and can be in contact with the side surface of the crystal ingot so as to polish the side surface of the crystal ingot, a polishing plate is detachably mounted at the bottom end of the polishing rotating shaft and is used for polishing the seed crystal surface of the crystal ingot;
a cutting structure disposed above the placement platform, the cutting structure for cutting a convex surface of the ingot;
preferably, the polishing process unit further comprises a first fixing member disposed above the placing platform, the first fixing member being capable of contacting an upper surface of the ingot and fixing the ingot;
preferably, the first fixing assembly comprises a first telescopic rod and a fixing block, the fixing block is fixed at the bottom end of the first telescopic rod, and the fixing block contacts with the upper surface of the crystal ingot and fixes the crystal ingot; the polishing rotating shaft is connected with the first telescopic rod;
preferably, a second fixing assembly is arranged on the side edge of the placing platform, the second fixing assembly comprises a second telescopic rod and a clamping structure, the clamping structure is arranged at the top end of the second telescopic rod, and the clamping structure is used for fixing the side face of the crystal ingot;
preferably, the sanding processing unit further comprises a third telescopic rod, the bottom end of which is provided with a cutting structure for cutting the convex surface of the ingot.
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