CN112852362A - Method for inhibiting cracking damage of processing edge of hard and brittle material through adhesive solidification toughening - Google Patents
Method for inhibiting cracking damage of processing edge of hard and brittle material through adhesive solidification toughening Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
Abstract
The invention discloses a method for inhibiting the fracture damage of the processing edge of a hard and brittle material by adhesive curing toughening, which comprises the following steps: obtaining a toughening type adhesive; coating the edge of a hard and brittle material workpiece to be processed by using the toughening type adhesive; processing the hard and brittle material workpiece; and after the processing is finished, removing the toughening type adhesive on the hard and brittle material workpiece. According to the method, the toughening type adhesive is coated on the edge of the hard and brittle materials such as crystalline silicon, optical glass, engineering ceramic and the like, and an adhesive layer encapsulation structure with certain shear strength, peeling strength and flexibility is formed on the edge of the workpiece after curing, so that the impact strength of the edge of the hard and brittle material is enhanced, the phenomenon of edge cracking and damage of the workpiece of the hard and brittle material is reduced or eliminated, and the processing quality and the processing efficiency of silicon wafer semiconductors, ceramic structural members, optical glass elements and the like are improved.
Description
Technical Field
The invention belongs to the technical field of material processing, and particularly relates to a method for inhibiting fracture and damage of a processing edge of a hard and brittle material through adhesive solidification and toughening.
Background
Hard and brittle materials such as crystalline silicon chips, engineering ceramics, optical glass and the like are widely applied to the fields of solar cells, infrared and ray detectors, biomedical sensors, composite armor materials, rocket tail nozzle throat liners, engine parts and the like due to excellent mechanical or photoelectromagnetic and other physical properties. Generally, more than 60% of materials on the hard and brittle material components need to be removed by grinding with a diamond grinding wheel. However, the edge of the hard and brittle material is easy to generate random large-scale fracture damage in the grinding process, the yield and the use performance of electronic, optical, structural and other hard and brittle material device products are seriously reduced, and the hard and brittle material becomes a technical bottleneck that the processing quality of the hard and brittle material is difficult to control.
Currently, the control measures related to edge cracking damage proposed by scholars at home and abroad can be roughly classified into a processing parameter control method, an energy auxiliary method, a prestress control method and the like. The machining parameter control method is to realize machining parameter optimization through regression statistical analysis of a plurality of grinding machining tests, reduce the grinding depth or increase the grinding wheel speed on the basis of ensuring the machining efficiency and the surface quality, so that the material is machined in a ductile region, and brittle damage is avoided. However, the processing parameter control method is greatly influenced by equipment, manpower, etc., and it is difficult to form a general paradigm that can be popularized and applied. The energy-assisted method is to use a heat source such as laser, plasma arc and the like to perform heating-assisted cutting processing to inhibit the edge fracture damage of hard and brittle materials such as engineering ceramics and the like, but the precise control of heating is difficult to realize in the processing process, and the heat damage of workpieces can be caused. The prestress control method is to apply a certain compressive stress in advance through a mechanical mode of a specific clamp to achieve the toughening effect of the edge surface of the material, so that the edge fracture of the material processing is reduced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for inhibiting the fracture damage of the processing edge of a hard and brittle material by gluing, curing and toughening. The technical problem to be solved by the invention is realized by the following technical scheme:
the invention provides a method for inhibiting the fracture and damage of the processing edge of a hard and brittle material by adhesive curing and toughening, which comprises the following steps:
obtaining a toughening type adhesive;
coating the edge of a hard and brittle material workpiece to be processed by using the toughening type adhesive;
processing the hard and brittle material workpiece;
and after the processing is finished, removing the toughening type adhesive on the hard and brittle material workpiece.
In one embodiment of the present invention, a toughened adhesive is obtained comprising:
the toughening adhesive is prepared by uniformly mixing an adhesive and a toughening agent at normal temperature, wherein the adhesive is a liquid organic adhesive, the toughening agent is an organic active toughening agent, and the toughening agent accounts for 10-20% of the adhesive.
In one embodiment of the invention, the adhesive is an epoxy resin, a phenolic resin or an acrylate.
In one embodiment of the invention, the toughening agent is one or more of polyurethane, polyamide, liquid nitrile or liquid polysulfide.
In one embodiment of the present invention, the coating the edge of the workpiece made of hard and brittle material to be processed with the toughening type adhesive includes:
coating the toughening adhesive on the surface of a region to be processed of the hard and brittle material workpiece;
and curing the toughening adhesive to form a colloid film layer on the surface of the hard and brittle material workpiece.
In one embodiment of the present invention, the curing process includes reaction curing, normal temperature curing, heat curing, or radiation curing.
In one embodiment of the present invention, removing the toughening type adhesive on the hard and brittle material workpiece includes:
dissolving the toughening adhesive on the hard and brittle material workpiece by using a debonding reagent;
and carrying out ultrasonic cleaning on the surface of the hard and brittle material workpiece.
In one embodiment of the present invention, the dispergation agent is an organic solvent of alcohols, esters or ketones.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the method for inhibiting the fracture damage of the processing edge of the hard and brittle material by adhesive curing and toughening, the toughening adhesive is coated on the edge of the hard and brittle material such as crystalline silicon, optical glass, engineering ceramic and the like, and an adhesive layer encapsulation structure with certain shear strength, peeling strength and flexibility is formed at the edge of a workpiece after curing, so that the impact strength of the edge of the hard and brittle material is enhanced, the fracture damage phenomenon of the edge of the workpiece of the hard and brittle material is reduced or eliminated, the processing quality and the processing efficiency of a silicon wafer semiconductor, a ceramic structural member, an optical glass element and the like are improved, and the method has very important engineering practical value.
2. The method of the invention has the advantages of simple operation, low economic cost and convenient popularization and utilization in practical production.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a flow chart of a method for suppressing edge chipping damage in processing of a hard and brittle material by adhesive curing and toughening according to an embodiment of the present invention;
FIG. 2 is a diagram illustrating the processing effect of a single crystal silicon wafer workpiece with a toughening type adhesive curing layer coated on the edge;
FIG. 3 is a diagram illustrating the processing effect of a single-crystal silicon wafer workpiece without a toughening type adhesive curing layer coated on the edge;
FIG. 4 is a diagram illustrating the processing effect of the silicon nitride engineering ceramic workpiece without the toughening type adhesive curing layer coated on the edge;
FIG. 5 is a diagram illustrating the processing effect of the silicon nitride engineering ceramic workpiece with a toughening type adhesive curing layer coated on the edge.
Detailed Description
In order to further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description is provided with reference to the accompanying drawings and the detailed description for a method for suppressing edge chipping and damage of a hard and brittle material by adhesive curing and toughening according to the present invention.
The foregoing and other technical matters, features and effects of the present invention will be apparent from the following detailed description of the embodiments, which is to be read in connection with the accompanying drawings. The technical means and effects of the present invention adopted to achieve the predetermined purpose can be more deeply and specifically understood through the description of the specific embodiments, however, the attached drawings are provided for reference and description only and are not used for limiting the technical scheme of the present invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or device that comprises a list of elements does not include only those elements but may include other elements not expressly listed. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of additional like elements in the article or device comprising the element.
Example one
Referring to fig. 1, fig. 1 is a flowchart of a method for suppressing edge chipping damage of a hard and brittle material by adhesive curing and toughening according to an embodiment of the present invention. The method comprises the following steps:
s1: obtaining a toughening type adhesive;
the toughening adhesive suitable for the adhesion occasions with high peel strength and high impact strength can be selected, or the toughening adhesive with high toughness can be formed by mixing the toughening agent with the adhesive according to a certain proportion.
In this embodiment, the process of configuring the toughening adhesive with the toughening agent and the adhesive includes:
the toughening adhesive is prepared by uniformly mixing an adhesive and a toughening agent at normal temperature, wherein the adhesive is a liquid organic adhesive, the toughening agent is an organic active toughening agent, and the toughening agent accounts for 10-20% of the adhesive.
The preferred adhesive comprises liquid organic adhesives such as epoxy resin, phenolic resin, acrylate and the like, and the preferred toughening agent comprises one or a mixture of more of organic active toughening agents such as polyurethane, polyamide, liquid butyronitrile, liquid polysulfide and the like.
S2: coating the edge of a hard and brittle material workpiece to be processed by using the toughening type adhesive;
specifically, this step can be implemented in two different ways: the first mode is as follows: coating the toughening adhesive on the edge of the surface of the region to be processed of the hard and brittle material workpiece, and curing the toughening adhesive to form a colloid film layer on the surface of the hard and brittle material workpiece; the second way is that for thin-layer sheet-shaped hard and brittle material workpieces such as silicon wafers and the like, the bottom surface can be directly immersed in the toughening type adhesive and adhered to the metal substrate, the edge of the hard and brittle material workpiece is covered by the toughening type adhesive in a submerged mode, and then the hard and brittle material workpiece is taken out for curing treatment. It should be noted that the coating thickness of the toughening adhesive is related to the parameters of the cutting process, and is preferably 0.1mm to 3 mm.
The curing treatment process can adopt modes of reaction curing, normal-temperature curing, heating curing or radiation curing and the like, wherein the reaction curing refers to a process of drying and film forming of the coated toughening type adhesive and the surface of a workpiece made of a hard and brittle material through a crosslinking reaction, and the radiation curing refers to a process of curing and film forming of the coated toughening type adhesive by means of energy irradiation such as ultraviolet rays.
The hard and brittle material can be crystalline silicon, optical glass, engineering ceramics and the like.
S3: processing the hard and brittle material workpiece;
specifically, a hard and brittle material workpiece coated with a toughening type adhesive film layer is clamped and fixed by a clamp, and then the workpiece is subjected to cutting processing, wherein the cutting processing can be grinding, turning, milling, drilling, scribing and the like.
S4: and after the processing is finished, removing the toughening type adhesive on the hard and brittle material workpiece.
Specifically, a debonding agent is used for dissolving a toughening adhesive on the hard and brittle material workpiece, and then the surface of the hard and brittle material workpiece is subjected to ultrasonic cleaning.
The dispergation reagent is preferably an organic solvent such as alcohols, esters or ketones.
Example two
This example further illustrates the method of the present invention by taking the single crystal diamond as an example for scribing a single crystal silicon wafer.
Step 101: the LOCTITE 330 extended toughening adhesive is directly selected.
The toughening adhesive is suitable for bonding the surfaces of various different base materials such as glass, ceramics, metal and the like, and can form an acrylate adhesive layer with high impact strength and high peel strength after being cured.
Step 102: immersing the monocrystalline silicon wafer workpiece to be processed with the N-type (111) crystal orientation and the size specification of 8mm multiplied by 1mm into the toughening type adhesive to be adhered on the steel block substrate, enabling the toughening type adhesive to submerge and wrap the peripheral edge of the surface of the monocrystalline silicon wafer workpiece with the size specification of 8mm multiplied by 8mm, and standing for half an hour at normal temperature to enable the toughening type adhesive to be solidified into a toughening film layer at the edge of the workpiece.
Step 103: scribing monocrystalline silicon wafer with monocrystalline diamond abrasive particles
Specifically, this example employs an antopan Paar MST2 type micro-scratch system in antopan, and selects a Berkovich type single crystal diamond abrasive grain to cut from one edge to the other edge on the surface of a single crystal silicon wafer at a scribing speed of 100mm/min and a normal load of 600 mN.
Step 104: after the surface of the monocrystalline silicon wafer is processed, an acrylate adhesive layer is formed by dissolving ethanol serving as a dispergation reagent, and then the surface of a workpiece is cleaned in water in an ultrasonic mode.
In order to analyze the effect of suppressing the edge cracking damage of the scribing process by curing the toughening type adhesive, a scribing process comparison test group in which the edge of the scribing process surface of the monocrystalline silicon wafer is not encapsulated with the toughening type adhesive is also prepared in this embodiment, and the damage morphology features of the surface scratches are observed by using an optical microscope.
Referring to fig. 2 and fig. 3, fig. 2 is a diagram illustrating the processing effect of a single crystal silicon wafer workpiece without a toughening type adhesive curing layer coated on the edge; fig. 3 is a processing effect diagram of the edge of the monocrystalline silicon piece coated with the toughening type adhesive curing layer, wherein the magnification of the image is 50 times. Fig. 3 is obtained before dissolving the toughening adhesive with a debonding agent. As can be seen from fig. 2, when the edge of the single crystal silicon wafer workpiece is not coated with the toughened adhesive cured layer, the scratch outlet portion has significant notch-like peeling and edge chipping phenomena of cracks. As can be seen from fig. 3, when the edge of the monocrystalline silicon piece is coated with the toughening type adhesive curing layer, no notch-shaped brittle peeling phenomenon is found at the scratch outlet, because the adhesive curing film layer has a better toughening effect, the impact resistance and the peeling resistance of the edge of the silicon piece can be effectively improved.
EXAMPLE III
This example further illustrates the method of the present invention by taking the single crystal diamond grinding processing of silicon nitride engineering ceramics as an example.
Step 201: and mixing a polyurethane toughening agent with the modified LOCTITE E-120HP Hysol epoxy resin adhesive to form the toughening adhesive, wherein the polyurethane toughening agent accounts for 10% of the epoxy resin adhesive. The toughening adhesive is suitable for bonding the surfaces of various different base materials such as glass, ceramics, metal and the like.
Step 202: selecting a silicon nitride engineering ceramic material workpiece to be processed with the dimension specification of 20mm multiplied by 40mm, coating and wrapping the toughening adhesive on the peripheral edge of the surface of the silicon nitride engineering ceramic workpiece with the dimension specification of 40mm multiplied by 40mm, and standing for 6 hours at the temperature of about 40 ℃ so as to ensure that the toughening adhesive is completely cured into a high-toughness colloid film layer on the edge of the workpiece. And then, loading the processed workpiece into a machine tool clamp for clamping and fixing.
Step 203: the silicon nitride engineering ceramic workpiece is ground and processed by using a single diamond grinding wheel
Specifically, in the embodiment, an XD250AH horizontal-axis rectangular-table precision surface grinding machine is adopted, and a diamond grinding wheel with the diameter of 200 multiplied by 10 multiplied by 31.75mm is selected to grind and machine the surface of the silicon nitride engineering ceramic workpiece with the grinding speed of 3500r/min, the workpiece feeding speed of 9m/min and the grinding depth of 0.015mm on the surface of 40mm multiplied by 40 mm.
Step 204: after the surface of the silicon nitride engineering ceramic workpiece is processed, the toughening type adhesive is dissolved by using a debonding reagent, and then the surface of the workpiece is cleaned by ultrasonic cleaning in water.
The present embodiment preferably utilizes N-methyl pyrrolidone (NMP) as a debonding agent to dissolve the epoxy glue layer formed on the surface of the workpiece.
In order to analyze the effect of inhibiting the edge chipping damage of the grinding process by curing the toughening type adhesive, a grinding process comparison test group in which the toughening type adhesive is not encapsulated at the peripheral edge of the surface of the silicon nitride engineering ceramic workpiece is also prepared in this embodiment, and the damage morphology features of the surface scratches are observed by using an optical microscope.
Referring to fig. 4 and 5, fig. 4 is a diagram illustrating the processing effect of the silicon nitride engineering ceramic workpiece without the edge coated with the toughening type adhesive curing layer; fig. 5 is a processing effect diagram of the silicon nitride engineering ceramic workpiece with the edge coated with the toughening type adhesive curing layer, wherein the magnification of the image is 50 times. Fig. 5 is obtained after dissolving the toughening adhesive with a debonding agent. As can be seen from FIG. 4, when the edge of the surface of the silicon nitride engineering ceramic workpiece is not coated with the toughening type adhesive curing layer, the edge of the workpiece has a plurality of small-sized notch-shaped edge chipping phenomena. It can be seen from fig. 5 that when the edge of the surface of the silicon nitride engineering ceramic workpiece is coated with the toughening type adhesive curing layer, the edge chipping damage degree of the edge of the test piece is obviously reduced, because the adhesive curing film layer has a better toughening effect, the impact resistance and the peeling resistance of the edge of the silicon nitride test piece can be effectively improved.
To sum up, in the method for suppressing the fracture damage of the processing edge of the hard and brittle material through adhesive curing and toughening according to the embodiment of the invention, the toughening type adhesive is coated on the edge of the hard and brittle material such as crystalline silicon, optical glass, engineering ceramic and the like, and an adhesive layer encapsulation structure with certain shear strength, peeling strength and flexibility is formed at the edge of the workpiece after curing, so that the impact strength of the edge of the hard and brittle material is enhanced, the fracture damage phenomenon of the edge of the hard and brittle material workpiece is reduced or eliminated, the processing quality and the processing efficiency of a silicon wafer semiconductor, a ceramic structural member, an optical glass element and the like are improved, and the method has very important engineering practical value. In addition, the method is very simple and easy to operate, low in economic cost and convenient to popularize and utilize in practical production.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (8)
1. A method for inhibiting the fracture damage of the processing edge of a hard and brittle material by adhesive curing toughening is characterized by comprising the following steps:
obtaining a toughening type adhesive;
coating the edge of a hard and brittle material workpiece to be processed by using the toughening type adhesive;
processing the hard and brittle material workpiece;
and after the processing is finished, removing the toughening type adhesive on the hard and brittle material workpiece.
2. The method for inhibiting edge chipping damage in hard and brittle material processing by adhesive curing toughening according to claim 1, characterized in that a toughening adhesive is obtained, comprising:
the toughening adhesive is prepared by uniformly mixing an adhesive and a toughening agent at normal temperature, wherein the adhesive is a liquid organic adhesive, the toughening agent is an organic active toughening agent, and the toughening agent accounts for 10-20% of the adhesive.
3. The method for inhibiting edge chipping damage in processing of hard and brittle materials according to claim 2, characterized in that the adhesive is epoxy resin, phenolic resin or acrylate.
4. The method for inhibiting edge chipping damage in processing of hard and brittle materials according to claim 2 wherein said toughening agent is one or more of polyurethane, polyamide, liquid nitrile or liquid polysulfide.
5. The method for suppressing the edge chipping damage of the hard and brittle material processed according to claim 1, wherein the step of coating the edge of the hard and brittle material workpiece to be processed with the toughening type adhesive comprises the following steps:
coating the toughening adhesive on the surface of a region to be processed of the hard and brittle material workpiece;
and curing the toughening adhesive to form a colloid film layer on the surface of the hard and brittle material workpiece.
6. The method for inhibiting edge chipping damage in hard and brittle materials according to claim 5, wherein the curing treatment comprises reaction curing, normal temperature curing, heat curing or radiation curing.
7. The method for inhibiting edge chipping damage in hard and brittle material processing according to claim 1, wherein removing the toughening adhesive on the hard and brittle material workpiece comprises:
dissolving the toughening adhesive on the hard and brittle material workpiece by using a debonding reagent;
and carrying out ultrasonic cleaning on the surface of the hard and brittle material workpiece.
8. The method for suppressing edge chipping damage in hard and brittle material processing according to claim 7, wherein the debonding agent is an organic solvent of alcohols, esters or ketones.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011638606.XA CN112852362A (en) | 2020-12-31 | 2020-12-31 | Method for inhibiting cracking damage of processing edge of hard and brittle material through adhesive solidification toughening |
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| CN114163262A (en) * | 2021-12-27 | 2022-03-11 | 中国人民解放军陆军装甲兵学院 | Material for enhancing surface toughness of hard and brittle material and preparation method thereof |
| CN114276165A (en) * | 2021-12-24 | 2022-04-05 | 中国人民解放军陆军装甲兵学院 | Method for reducing surface brittleness of hard and brittle material |
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Application publication date: 20210528 |