CN110983435A - Separation method of CVD single crystal diamond seed crystal and growth layer - Google Patents
Separation method of CVD single crystal diamond seed crystal and growth layer Download PDFInfo
- Publication number
- CN110983435A CN110983435A CN201911348078.1A CN201911348078A CN110983435A CN 110983435 A CN110983435 A CN 110983435A CN 201911348078 A CN201911348078 A CN 201911348078A CN 110983435 A CN110983435 A CN 110983435A
- Authority
- CN
- China
- Prior art keywords
- seed crystal
- growth layer
- combined body
- tool
- laser
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
-
- 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
- B28D5/0005—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by breaking, e.g. dicing
-
- 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
- C30B29/02—Elements
- C30B29/04—Diamond
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for separating a CVD single crystal diamond seed crystal from a growth layer, which comprises the steps of pretreating the seed crystal surface of a combination, cutting off polycrystal on the outer surface of the combination by adopting a unidirectional and bidirectional laser cutting method, polishing and cleaning the growth layer surface of the combination, separating the seed crystal from the growth layer by adopting a bidirectional laser cutting method, and finally polishing and cleaning the seed crystal and the growth layer respectively to obtain the separated seed crystal and the growth layer. The method provided by the invention adopts a bidirectional laser cutting method to separate the seed crystal and the growth layer, and can save 30-50% of time compared with the existing unidirectional repeated cutting method. In addition, the separation of the seed crystal and the growth layer can be realized by oppositely cutting twice by adopting a bidirectional laser cutting method, and the single crystal loss with the thickness of 0.1-0.3 mm can be reduced compared with the existing unidirectional repeated cutting method.
Description
Technical Field
The invention relates to the technical field of growth of single crystal diamond materials, in particular to a separation method of a CVD single crystal diamond seed crystal and a growth layer.
Background
The seed crystal is epitaxially grown by utilizing a Microwave Plasma Chemical Vapor Deposition (MPCVD) method, and the growth speed of the seed crystal is easily influenced by growth conditions (comprising seed crystal support design, seed crystal surface pretreatment, temperature and reaction gas); point defects, dislocation, surface defects, body defects, internal stress and other defects are easy to occur in the epitaxial growth process of the seed crystal; in addition, because the temperature of the edge of the seed crystal is high in the epitaxial growth process, polycrystal is generated at the edge, the polycrystal at the edge gradually invades into the single crystal along with the growth, and meanwhile, the polishing efficiency is influenced by the polycrystal, so that the technical requirement of the single crystal is not met. In order to improve the yield of the deposition and the quality of the growth layer, improve the processing efficiency and reduce the single crystal loss so as to facilitate the secondary growth of the seed crystal, the seed crystal is separated from the growth layer after the CVD single crystal diamond is epitaxially grown to a certain thickness in microwave plasma equipment, and the surface treatment of the seed crystal and the growth layer is particularly important.
The conventional method for separating the seed crystal from the growth layer is to adopt high-power laser to carry out unidirectional repeated cutting, and the method has the defects of long separation time, high cutting loss and easy tip breakage and cracking; the separation time is 0.5 to 2 hours according to the external dimension of the single crystal, the cutting gap is 0.2 to 0.5mm, and the cutting loss is large due to the width of the cutting gap.
Disclosure of Invention
The invention provides a separation method of a CVD single crystal diamond seed crystal and a growth layer, which is used for overcoming the defects of long separation time, large cutting loss, easy tip breakage and cracking and the like in the prior art, realizing double-sided cutting and joint of cutting and cutting joints after cutting and separation, ensuring short separation time and small cutting loss and avoiding tip breakage and cracking.
In order to achieve the above object, the present invention provides a method for separating a CVD single crystal diamond seed crystal and a growth layer, comprising:
s1: defining a structure comprising a polycrystal, a seed crystal and a growth layer as a combined body, and pretreating the seed crystal surface of the combined body;
s2: detachably connecting the seed crystal surface pretreated by S1 with one end surface of a tool post, vertically arranging the tool post in a laser equipment workbench tool and cutting off polycrystal around the combined body by adopting a unidirectional laser cutting method, and then transversely arranging the tool post in the laser equipment workbench tool and cutting off polycrystal on the growth layer surface of the combined body by adopting a bidirectional laser cutting method;
s3: taking out the tool post, unloading the combined body from the tool post, and polishing and cleaning the growth layer surface of the combined body;
s4: detachably connecting the seed crystal surface of the combined body passing through the S3 with one end surface of a tool post, transversely placing the tool post in a laser equipment workbench tool, and separating the seed crystal and the growth layer by adopting a bidirectional laser cutting method;
s5: and taking out the tool column and the cut growth layer, unloading the seed crystal from the tool column, and polishing and cleaning the seed crystal and the growth layer respectively to obtain the separated seed crystal and the growth layer.
Compared with the prior art, the invention has the beneficial effects that:
1. the method for separating the CVD single crystal diamond seed crystal and the growth layer comprises the steps of detachably connecting the seed crystal surface of the combination body passing through the S3 with one end surface of a tool post, transversely placing the tool post in a laser equipment workbench tool, and separating the seed crystal and the growth layer by adopting a bidirectional laser cutting method. The method comprises the steps of arranging two opposite cutting positions on an interface of a seed crystal and a growth layer, cutting one cutting position by a laser cutting method, rotating a combination by utilizing the rotating function of a tool column to enable the other cutting position on the combination to rotate to be overlapped with a laser cutting surface, cutting the other cutting position by the laser cutting method, and separating the seed crystal from the growth layer by two opposite cutting. Compared with the existing one-way repeated cutting method, the method can save 30-50% of time, can reduce the single crystal loss with the thickness of 0.1-0.3 mm, and improves the product yield of laser separation.
2. According to the method for separating the CVD single crystal diamond seed crystal and the growth layer, the tool column is connected with the combined body, so that the position of the combined body in the tool of the laser equipment workbench is accurately controlled, the complete butt joint of the cutting seams on the cutting object (namely the combined body) is realized, the polishing time is shortened, the single crystal loss is reduced, and the risk of waste products is avoided.
3. Because the temperature of the edge of the seed crystal is high in the epitaxial growth process, the edge of the seed crystal can generate polycrystal, so that the method for separating the CVD single crystal diamond seed crystal from the growth layer provided by the invention firstly adopts a laser cutting method to cut off the polycrystal on the outer surface of the combined body before separating the seed crystal from the growth layer, thereby improving the quality and the polishing efficiency of the growth layer.
4. The method for separating the CVD monocrystal diamond seed crystal from the growth layer provided by the invention has the advantages that the tool columns are sequentially vertically and transversely arranged in the tool of the laser equipment workbench, and polycrystals on the outer surface of the combined body are cut off by adopting a unidirectional laser cutting method and a bidirectional laser cutting method respectively. Vertically placing the tool column in a laser equipment workbench tool, and cutting off polycrystal around the combined body at one time by adopting a unidirectional laser cutting method; and transversely arranging the tool column in a tool of a workbench of laser equipment, and cutting off the polycrystal on the surface of the growth layer of the combined body by adopting a bidirectional laser cutting method. The invention combines the unidirectional laser cutting method and the bidirectional laser cutting method, thereby improving the cutting efficiency and cutting precision of the polycrystal.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a flow chart of a method of separating a CVD single crystal diamond seed and a growth layer provided by the present invention;
FIG. 2 is a structural view of a combined body according to an embodiment of the present invention;
FIG. 3 is a schematic view of a tool post + combination being vertically disposed according to an embodiment of the present invention;
fig. 4 is a schematic diagram of a tooling column + combination body placed transversely in an embodiment of the invention.
The reference numbers illustrate: 1: a tooling column; 2: a combination body; 21: seed crystal; 22: growing a layer; 3: and (4) polycrystallization.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The invention provides a method for separating a CVD single crystal diamond seed crystal from a growth layer, as shown in figure 1, comprising the following steps:
s1: defining a structure comprising a polycrystal, a seed crystal and a growth layer as a combined body, and pretreating the seed crystal surface of the combined body;
preferably, the pretreatment is to polish the seed crystal surface of the combined body so that the surface flatness of the seed crystal surface is less than 20nm, so as to facilitate connection with a tool column and simultaneously facilitate subsequent accurate control of the position and size of laser cutting.
The combination body can be in the shape of a cylinder, a cuboid, a cube and the like.
The bonded body 2 in this embodiment is, as shown in fig. 2, a rectangular parallelepiped including a seed crystal 21, a growth layer 22, and a polycrystal 3 grown around the bonded body 2 and on the growth layer side of the bonded body 2.
The seed crystal surface of the combination body 2 is the surface of the seed crystal 21 far from the growth layer 22;
the growth layer surface of the bonded body 2 is the surface of the growth layer 22 far from the seed crystal 21.
S2: detachably connecting the seed crystal surface pretreated by S1 with one end surface of a tool post, vertically arranging the tool post in a laser equipment workbench tool and cutting off polycrystal around the combined body by adopting a unidirectional laser cutting method, and then transversely arranging the tool post in the laser equipment workbench tool and cutting off polycrystal on the growth layer surface of the combined body by adopting a bidirectional laser cutting method;
the tool post is a separately designed device, belongs to a cutting tool, is a shaft part, and has the requirements on the perpendicularity and the concentricity of the end surface during processing; the area of the end surface is smaller than that of the seed crystal surface so as to avoid damaging the tool column by cutting the tool end surface in the laser cutting process.
Preferably, the S2 is specifically:
s21: detachably connecting the seed crystal surface pretreated by S1 with one end surface of the tool column to enable the perpendicularity of the tool column and the seed crystal surface to be less than 0.01mm, and aiming at reducing the butting error after rotating 180 degrees in the subsequent operation, so that the separation surface is closer to a plane to reduce the polishing difficulty;
preferably, the detachable connection is an adhesive connection. Such as 502 glue.
In the embodiment, as shown in fig. 3, the seed crystal face pretreated by S1 is connected with one end face of the cylindrical tool post 1 by gluing, in the embodiment, one end face of the cylindrical tool post 1 is glued with the center position of the seed crystal face, compressed air is always opened during cutting, and the central position is chosen for gluing, so that the problem that the combination and the tool post are not firmly bonded and separated due to uneven impact force of the compressed air can be avoided; in addition, the center position is selected for adhesive connection, so that the problem that the tool column cannot be reused due to the fact that the tool column is cut by laser can be avoided.
S22: vertically placing a tool post connected with a combined body in a laser equipment workbench tool so that laser can vertically strike the growth layer surface of the combined body, using a laser equipment imaging system, taking the size of a seed crystal face of the combined body as a cutting size, taking the thickness of the combined body as a laser cutting depth, and cutting off polycrystal on the periphery of the combined body by using a laser cutting method;
preferably, the laser power of the laser cutting method is 5-15W, the cutting speed is 10-30 mm/min, and the specific power is determined according to the thickness of the combined body. And 5-15W of low power is adopted to ensure that the polycrystalline silicon is not cracked and cracked in the polycrystalline silicon cutting process. Such as: the thickness is 2mm, the laser power is 8W, and the cutting speed is 25 mm/min; the thickness is 4mm, the laser power is 12w, and the cutting speed is 15 mm/min.
In this embodiment, as shown in fig. 3, the tool post connected with the combined body is vertically placed in the tool of the laser device workbench, that is, the polycrystal 3 around the combined body is subjected to laser ablation in a transverse clamping manner. Wherein the cutting size is the size of the crystal face of the combined body (namely, the length and width of the surface of the seed crystal 21 far away from the growth layer 22), and the laser cutting depth is the thickness of the combined body (namely, the thickness of the seed crystal 21 plus the thickness of the growth layer 22).
All polycrystals 3 around the combined body can be cut at one time by adopting a laser cutting method, and the cutting precision is obviously improved by the position limiting effect of the tool column.
S23: taking out the tool post, transversely placing the tool post connected with the combined body in a tool of a workbench of laser equipment so that the direction of the maximum overall dimension of the combined body is parallel to the Y axis of the workbench of the laser equipment, taking the pretreated seed crystal surface as a reference surface, and adjusting the fixed angle of the tool post in the tool of the workbench of the laser equipment so that the reference surface is completely superposed with the Y axis motion track surface of the workbench of the laser equipment; taking one half of the maximum overall dimension of the combination as laser cutting depth, taking the thickness dimension of the combination as an X-axis feeding value of a laser equipment workbench, and cutting off the polycrystal on the growth layer surface of the combination by adopting a laser cutting method;
the fixture column is fixed on the laser equipment workbench fixture by pressing the fixture column through a pressing block. During pressing, the tool column can slightly swing on an XY plane, and the axis of the tool column is parallel to the X-axis movement direction, namely the axis of the tool column is converted into a reference plane and the Y-axis movement track which are completely overlapped, so that the consistency of the thickness of seed crystals and growth layers separated by double-sided cutting can be ensured. Wherein, the Y-axis motion track is the laser cutting surface.
S24: rotating the tool post by 180 degrees, taking the preprocessed seed crystal surface as a reference surface, and adjusting the fixed angle of the tool post to enable the reference surface to be superposed with a Y-axis motion track surface of the laser equipment workbench; and taking one half of the maximum overall dimension of the combined body as the laser cutting depth, taking the thickness dimension of the combined body as the X-axis feeding value of a laser equipment workbench, and cutting off the polycrystal on the growth layer surface of the combined body by adopting a laser cutting method to complete the cutting off of the polycrystal on the outer surface of the combined body.
Preferably, in the steps S23 and S24, the laser power of the laser cutting method is 5-15W, the cutting speed is 10-30 mm/min, and the specific cutting parameters are determined according to the maximum external dimension of the combined body 2. And 5-15W of low power is adopted to ensure that the seed crystal and the growth layer are not cracked and cracked in the separation process. Such as: when the maximum external dimension is 9, the laser power is 13w, and the cutting speed is 15 mm/min; when the maximum external dimension is 6, the power is 8w, and the cutting speed is 20 mm/min.
And if the combined body is a cuboid, the size of the combined body comprises length, width and height, and the largest of the length, the width and the height is the maximum external size of the combined body.
In this embodiment, the maximum outer dimension of the combined body is the length a thereof, and the direction of the maximum outer dimension of the combined body is the direction of the length a thereof.
In this embodiment, as shown in fig. 4, a cylindrical tool post 1 is transversely placed in a tool of a laser device workbench so that the length a direction of a combined body is parallel to the Y axis of the laser device workbench, a preprocessed seed crystal surface is used as a reference surface, and the reference surface is completely overlapped with the Y axis motion trajectory surface of the laser device workbench by adjusting the fixed angle of the tool post 1; taking one half of the length a of the combined body as laser cutting depth, taking an X-axis feeding value of a laser equipment workbench as the thickness dimension of the combined body, and cutting off polycrystal on the growth layer surface of the combined body by adopting a laser cutting method; after the processing is finished, rotating the tool post by 180 degrees, taking the pretreated seed crystal surface as a reference surface, and adjusting the fixed angle of the tool post to ensure that the reference surface is completely superposed with the Y-axis motion track surface of the laser equipment workbench; and taking one half of the length a of the combined body as the laser cutting depth, taking the X-axis feeding value of a laser equipment workbench as the thickness dimension of the combined body, and cutting off the polycrystal on the growth layer surface of the combined body by adopting a laser cutting method to complete the cutting off of the polycrystal on the outer surface of the combined body. The above operation requires that the single crystal on the growth layer be cut as little as possible to reduce the single crystal loss on the premise of complete removal of the polycrystal 3.
S3: taking out the tool post, unloading the combined body from the tool post, and polishing and cleaning the growth layer surface of the combined body;
preferably, the S3 is specifically:
and taking out the tool column, heating the bonding part of the tool column and the seed crystal face of the combined body by adopting a local heating method to separate the combined body from the tool column, polishing the growth layer of the combined body to ensure that the surface flatness of the growth layer is less than 20nm, and cleaning the combined body by using an ultrasonic cleaning machine.
In this embodiment, the local heating method is alcohol burner heating.
S4: detachably connecting the seed crystal surface of the combined body passing through the S3 with one end surface of a tool post, transversely placing the tool post in a laser equipment workbench tool, and separating the seed crystal and the growth layer by adopting a bidirectional laser cutting method;
the tool post is a copper shaft part, the end face of the tool post is connected with the surface of the combined seed crystal or the growth layer in an adhesive mode, laser used for cutting is always vertically punched out from the Z-axis direction, and only the laser equipment workbench can move. When the tool post is transversely clamped, the tool post can be used for cutting polycrystal on a growth layer surface or separating seed crystals and the growth layer; when the tool post is vertically clamped, the tool post can be used for cutting polycrystal around the combined body.
The X axis and the Y axis of the workbench of the laser device are used for controlling the workbench to move along the X axis and the Y axis; the transverse clamping of the tool post needs to be aligned in the clamping direction so as to ensure the precision and accuracy of double-sided cutting (alignment principle, the reference surface and the Y-axis motion track surface of the workbench are completely overlapped after the tool post is fixed).
Preferably, the S4 is specifically:
s41: detachably connecting the seed crystal surface of the combined body with one end surface of the tool column to enable the perpendicularity of the tool column and the seed crystal surface to be less than 0.01 mm;
s42: transversely arranging a tool post connected with a combined body in a tool of a workbench of laser equipment so that the direction of the maximum overall dimension of the combined body is parallel to the Y axis of the workbench of the laser equipment, taking the seed crystal surface of the combined body as a reference surface, and adjusting the fixed angle of the tool post so that the reference surface is superposed with the Y axis motion track surface of the workbench of the laser equipment; taking one half of the maximum overall dimension of the combination as laser cutting depth, taking the X-axis feeding value of a laser equipment workbench as the thickness dimension of the seed crystal, and separating the seed crystal and the growth layer of the combination by adopting a laser cutting method;
s43: rotating the tool post by 180 degrees, taking the seed crystal surface of the combined body as a reference surface, and adjusting the fixed angle of the tool post to enable the reference surface to be superposed with the Y-axis motion track surface of the laser equipment workbench; and taking one half of the maximum overall dimension of the combination as the laser cutting depth, taking the X-axis feeding value of a laser equipment workbench as the thickness dimension of the seed crystal, and separating the seed crystal and the growth layer of the combination by adopting a laser cutting method.
The operation of S4 is similar to that of S23-S24. In this embodiment, the maximum outer dimension of the combination is the length a of the combination, as shown in fig. 4, a tool post connected with the combination is transversely placed in a tool of a laser device workbench so that the length a direction of the combination is parallel to the Y axis of the laser device workbench, the seed crystal surface of the combination is used as a reference surface, and the reference surface is overlapped with the Y axis motion trajectory surface of the laser device workbench by adjusting the fixed angle of the tool post; taking one half of the length a of the combined body as laser cutting depth, taking an X-axis feeding value of a laser equipment workbench as the thickness size of the seed crystal, and separating the seed crystal and the growth layer of the combined body by adopting a laser cutting method; after the machining is finished, rotating the tool post by 180 degrees, taking the seed crystal surface of the combined body as a reference surface, and adjusting the fixed angle of the tool post to enable the reference surface to be superposed with the Y-axis motion track surface of the laser equipment workbench; and taking one half of the length a of the combined body as the laser cutting depth, taking the X-axis feeding value of a laser equipment workbench as the thickness dimension of the seed crystal, and separating the seed crystal and the growth layer of the combined body by adopting a laser cutting method. In the embodiment, the separation of the seed crystal and the growth layer can be realized by two times of laser cutting, and the cutting precision is high.
Preferably, in the steps S42 and S43, the laser power of the laser cutting method is 5-15W, the cutting speed is 10-30 mm/min, the kerf width is 0.1-0.25 mm, and the specific parameters are determined according to the maximum outer dimension of the combined body. For example, 9 x 9 CVD single crystal diamond blank seed crystal and growth layer were separated, with a kerf width actually measured 0.312mm for single face separation and 0.162mm for double face separation; the kerf width was reduced by 0.15 mm.
S5: and taking out the tool column and the cut growth layer, unloading the seed crystal from the tool column, and polishing and cleaning the seed crystal and the growth layer respectively to obtain the separated seed crystal and the growth layer.
Preferably, the S5 is specifically:
and taking out the tool column and the cut growth layer, heating the bonding part of the tool column and the crystal face of the combined seed by adopting a local heating method to separate the seed crystal from the tool column, respectively polishing the seed crystal and the growth layer to ensure that the surface flatness of the seed crystal and the growth layer is less than 20nm, and then cleaning the seed crystal and the growth layer by using an ultrasonic cleaning machine to obtain the separated seed crystal and the growth layer.
In this embodiment, the local heating method is alcohol burner heating.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method of separating a CVD single crystal diamond seed and a growth layer, comprising:
s1: defining a structure comprising a polycrystal, a seed crystal and a growth layer as a combined body, and pretreating the seed crystal surface of the combined body;
s2: detachably connecting the seed crystal surface pretreated by S1 with one end surface of a tool post, vertically arranging the tool post in a laser equipment workbench tool and cutting off polycrystal around the combined body by adopting a unidirectional laser cutting method, and then transversely arranging the tool post in the laser equipment workbench tool and cutting off polycrystal on the growth layer surface of the combined body by adopting a bidirectional laser cutting method;
s3: taking out the tool post, unloading the combined body from the tool post, and polishing and cleaning the growth layer surface of the combined body;
s4: detachably connecting the seed crystal surface of the combined body passing through the S3 with one end surface of a tool post, transversely placing the tool post in a laser equipment workbench tool, and separating the seed crystal and the growth layer by adopting a bidirectional laser cutting method;
s5: and taking out the tool column and the cut growth layer, unloading the seed crystal from the tool column, and polishing and cleaning the seed crystal and the growth layer respectively to obtain the separated seed crystal and the growth layer.
2. A CVD single crystal diamond seed and growth layer separation method as claimed in claim 1, wherein in S1, the pretreatment is polishing the seed surface of the combination to a surface flatness of the seed plane < 20 nm.
3. A method of separating a CVD single crystal diamond seed and growth layer as claimed in claim 1, wherein S2 is in particular:
s21: detachably connecting the seed crystal surface pretreated by S1 with one end surface of the tool column to enable the perpendicularity of the tool column and the seed crystal surface to be less than 0.01 mm;
s22: vertically placing a tool post connected with a combined body in a laser equipment workbench tool so that laser can vertically strike a growing layer of the combined body, using a laser equipment imaging system, taking the size of the growing layer of the combined body as a cutting size, taking the thickness of the combined body as a laser cutting depth, and cutting off polycrystal on the periphery of the combined body by using a laser cutting method;
s23: taking out the tool post, transversely placing the tool post connected with the combined body in a tool of a workbench of laser equipment so that the direction of the maximum overall dimension of the combined body is parallel to the Y axis of the workbench of the laser equipment, taking the pretreated seed crystal surface as a reference surface, and adjusting the fixed angle of the tool post in the tool of the workbench of the laser equipment so that the reference surface is completely superposed with the Y axis motion track surface of the workbench of the laser equipment; taking one half of the maximum overall dimension of the combination as laser cutting depth, taking the thickness dimension of the combination as an X-axis feeding value of a laser equipment workbench, and cutting off the polycrystal on the growth layer surface of the combination by adopting a laser cutting method;
s24: rotating the tool post by 180 degrees, taking the preprocessed seed crystal surface as a reference surface, and adjusting the fixed angle of the tool post to enable the reference surface to be superposed with a Y-axis motion track surface of the laser equipment workbench; and taking one half of the maximum overall dimension of the combined body as the laser cutting depth, taking the thickness dimension of the combined body as the X-axis feeding value of a laser equipment workbench, and cutting off the polycrystal on the growth layer surface of the combined body by adopting a laser cutting method to complete the cutting off of the polycrystal on the outer surface of the combined body.
4. A method of separating a CVD single crystal diamond seed and growth layer as claimed in claim 3, wherein in S21 the detachable connection is an adhesive connection.
5. A CVD single crystal diamond seed crystal and growth layer separation method according to claim 3, wherein in the step S22, the laser cutting method is performed at a laser power of 5 to 15W and a cutting speed of 10 to 30 mm/min.
6. A method of separating a CVD single crystal diamond seed crystal and a growth layer according to claim 3, wherein in the S23 and S24, the laser power of the laser cutting method is 5 to 15W, and the cutting speed is 10 to 30 mm/min.
7. A method of separating a CVD single crystal diamond seed and growth layer as claimed in claim 1, wherein S3 is in particular:
and taking out the tool column, heating the joint of the tool column and the seed crystal face of the combined body by adopting a local heating method to separate the combined body from the tool column, polishing the growth layer of the combined body to ensure that the surface flatness of the growth layer is less than 20nm, and cleaning the combined body by using an ultrasonic cleaning machine.
8. A method of separating a CVD single crystal diamond seed and growth layer as claimed in claim 1, wherein S4 is in particular:
s41: detachably connecting the seed crystal surface of the combined body with one end surface of the tool column to enable the perpendicularity of the tool column and the seed crystal surface to be less than 0.01 mm;
s42: transversely arranging a tool post connected with a combined body in a tool of a workbench of laser equipment so that the direction of the maximum overall dimension of the combined body is parallel to the Y axis of the workbench of the laser equipment, taking the seed crystal surface of the combined body as a reference surface, and adjusting the fixed angle of the tool post so that the reference surface is superposed with the Y axis motion track surface of the workbench of the laser equipment; taking one half of the maximum overall dimension of the combination as laser cutting depth, taking the X-axis feeding value of a laser equipment workbench as the thickness dimension of the seed crystal, and separating the seed crystal and the growth layer of the combination by adopting a laser cutting method;
s43: rotating the tool post by 180 degrees, taking the seed crystal surface of the combined body as a reference surface, and adjusting the fixed angle of the tool post to enable the reference surface to be superposed with the Y-axis motion track surface of the laser equipment workbench; and taking one half of the maximum overall dimension of the combination as the laser cutting depth, taking the X-axis feeding value of a laser equipment workbench as the thickness dimension of the seed crystal, and separating the seed crystal and the growth layer of the combination by adopting a laser cutting method.
9. A method of separating a CVD single crystal diamond seed crystal and a growth layer as claimed in claim 8, wherein in the S42 and S43, the laser power of the laser dicing method is 5 to 15W, the dicing speed is 10 to 30mm/min, and the slit width is 0.1 to 0.25 mm.
10. A method of separating a CVD single crystal diamond seed and growth layer as claimed in claim 1, wherein S5 is in particular:
and taking out the tool column and the cut growth layer, heating the bonding part of the tool column and the crystal face of the combined seed by adopting a local heating method to separate the seed crystal from the tool column, respectively polishing the seed crystal and the growth layer to ensure that the surface flatness of the seed crystal and the growth layer is less than 20nm, and then cleaning the seed crystal and the growth layer by using an ultrasonic cleaning machine to obtain the separated seed crystal and the growth layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911348078.1A CN110983435A (en) | 2019-12-24 | 2019-12-24 | Separation method of CVD single crystal diamond seed crystal and growth layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911348078.1A CN110983435A (en) | 2019-12-24 | 2019-12-24 | Separation method of CVD single crystal diamond seed crystal and growth layer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110983435A true CN110983435A (en) | 2020-04-10 |
Family
ID=70076283
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911348078.1A Pending CN110983435A (en) | 2019-12-24 | 2019-12-24 | Separation method of CVD single crystal diamond seed crystal and growth layer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110983435A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114318531A (en) * | 2022-01-06 | 2022-04-12 | 济南金刚石科技有限公司 | Stripping method applied to MPCVD large-size diamond polycrystal |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773929A (en) * | 2012-07-13 | 2012-11-14 | 乐山新天源太阳能科技有限公司 | Method and device for cutting seed crystal for pseudo-single crystal |
| WO2016073233A1 (en) * | 2014-11-06 | 2016-05-12 | Ii-Vi Incorporated | Highly twinned, oriented polycrystalline diamond film and method of manufacture thereof |
| CN206912504U (en) * | 2017-06-14 | 2018-01-23 | 广州华之尊光电科技有限公司 | A kind of multi-faceted placement material extension laser equipment |
| CN108103570A (en) * | 2017-12-11 | 2018-06-01 | 湖北碳六科技有限公司 | A kind of method and system for splicing growth single-crystal diamond |
| CN108251892A (en) * | 2018-02-26 | 2018-07-06 | 湖北碳六科技有限公司 | Laser enhancing plasma CVD prepares single-crystal diamond devices and methods therefor |
| CN110230091A (en) * | 2019-06-26 | 2019-09-13 | 北京科技大学 | It is a kind of vertically to splice preparation large scale cvd diamond and cutting method |
-
2019
- 2019-12-24 CN CN201911348078.1A patent/CN110983435A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773929A (en) * | 2012-07-13 | 2012-11-14 | 乐山新天源太阳能科技有限公司 | Method and device for cutting seed crystal for pseudo-single crystal |
| WO2016073233A1 (en) * | 2014-11-06 | 2016-05-12 | Ii-Vi Incorporated | Highly twinned, oriented polycrystalline diamond film and method of manufacture thereof |
| CN206912504U (en) * | 2017-06-14 | 2018-01-23 | 广州华之尊光电科技有限公司 | A kind of multi-faceted placement material extension laser equipment |
| CN108103570A (en) * | 2017-12-11 | 2018-06-01 | 湖北碳六科技有限公司 | A kind of method and system for splicing growth single-crystal diamond |
| CN108251892A (en) * | 2018-02-26 | 2018-07-06 | 湖北碳六科技有限公司 | Laser enhancing plasma CVD prepares single-crystal diamond devices and methods therefor |
| CN110230091A (en) * | 2019-06-26 | 2019-09-13 | 北京科技大学 | It is a kind of vertically to splice preparation large scale cvd diamond and cutting method |
Non-Patent Citations (1)
| Title |
|---|
| 宋修曦: "单晶金刚石同质外延生长的应力研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114318531A (en) * | 2022-01-06 | 2022-04-12 | 济南金刚石科技有限公司 | Stripping method applied to MPCVD large-size diamond polycrystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4750519B2 (en) | Cutting method and cutting apparatus | |
| CN103132071B (en) | A kind of laser repairing supersonic vibration coupling device | |
| CN106513986A (en) | Laser and ultrasound combined type drilling system and machining method thereof | |
| CN110983435A (en) | Separation method of CVD single crystal diamond seed crystal and growth layer | |
| CN110039672A (en) | A kind of processing technology of hexagon silicon single crystal rod | |
| CN103501975A (en) | Method for fixing a single-crystal workpiece to be treated on a processing device | |
| CN102152420A (en) | Low-loss oriented cutting method of large-size sapphire crystal blanks | |
| CN101130265A (en) | Technique for cutting horizontal gallium arsenide single-crystal wafer with inside diameter slicer | |
| CN110653668A (en) | Three-dimensional variable-parameter rotary ultrasonic grinding device for hard and brittle materials for automobiles | |
| CN202639371U (en) | Polycrystalline cubic boron nitride (PCBN) cutter for machining cylinder body | |
| CN102120344A (en) | Single-crystal material cutting method based on fluctuation characteristic of cutting force and fine tuning tool rest | |
| CN201979618U (en) | Bonding clamp for single crystal rod | |
| CN103086597A (en) | Method for improving laser cutting quality of pendulous reed of accelerometer | |
| CN209873179U (en) | Device for eliminating CBN cutter stress | |
| JP2006339431A (en) | Method of processing nitride semiconductor substrate | |
| JP2002075923A (en) | Machining method of silicon single-crystal ingot | |
| CN219443900U (en) | Fixing device for laser cutting/polishing diamond seed crystal | |
| CN211680197U (en) | Single crystal milling cutter | |
| CN111778561B (en) | Sapphire substrate, processing method and preparation method of light-emitting diode | |
| CN107433694B (en) | Workpiece fixing mechanism, wire saw trimming device and workpiece trimming method | |
| AU2020101554A4 (en) | A composite vibration drilling method suitable for CFRP / titanium (aluminum) alloy laminate materials | |
| CN206578311U (en) | A kind of processed finished products blind flange external diameter frock clamp | |
| CN205393582U (en) | Split type ultrasonic knife utensil | |
| CN111136801A (en) | Numerical control machining process method for light weight structure of optical glass | |
| CN109129664A (en) | Ultrasonic cutting device for flat-panel monitor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200410 |