CN111347354A - Grinding wheel for thinning silicon carbide crystal, preparation method and application thereof - Google Patents
Grinding wheel for thinning silicon carbide crystal, preparation method and application thereof Download PDFInfo
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- CN111347354A CN111347354A CN202010289636.8A CN202010289636A CN111347354A CN 111347354 A CN111347354 A CN 111347354A CN 202010289636 A CN202010289636 A CN 202010289636A CN 111347354 A CN111347354 A CN 111347354A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
- B24D3/28—Resins or natural or synthetic macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/0009—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses
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Abstract
The invention provides a grinding wheel for thinning a silicon carbide crystal, a preparation method and application thereof, wherein the grinding wheel has a porous structure, and comprises the following raw materials in percentage by weight: 15-40% of diamond abrasive, 10-35% of phenolic resin powder, 3-15% of foaming agent, 5-20% of calcium fluoride, 3-15% of tungsten disulfide, 3-15% of cerium oxide, 5-20% of cryolite and 0.5-6% of zinc stearate. The resin combined grinding wheel prepared by the method has a porous structure and high porosity, can play a role in accommodating chips during grinding, and improves the sharpness of the grinding wheel. Meanwhile, the bonding agent bridge established by the porous structure is effectively broken during grinding, the self-sharpening performance of the grinding wheel is good, and the dressing frequency is reduced. The specific calcium fluoride and lubricant materials in the grinding wheel system can reduce the friction coefficient of the grinding wheel, thereby effectively reducing the grinding heat and improving the surface quality of the ground silicon carbide wafer.
Description
Technical Field
The invention relates to the field of superhard abrasive grinding tools, in particular to a grinding wheel for thinning a silicon carbide crystal, a preparation method and application thereof.
Background
Silicon carbide crystals are of great interest as the most promising third generation semiconductor materials due to their wider forbidden band width, higher breakdown electric field, higher thermal conductivity, greater electronic saturation and higher radiation resistance. However, the Mohs hardness of the silicon carbide crystal reaches 9.5, the hardness is second to that of diamond, the strength is high, and the processing difficulty is extremely high. Compared with the common workpiece, in the processing process of the silicon carbide semiconductor, due to the fact that the material with high hardness is difficult to remove, the heat generated is high due to the fact that large grinding force is generated; and the powdery abrasive dust easily blocks the grinding wheel, and the grinding wheel loses the removing capability. Currently, there is no effective method for silicon carbide crystal processing in the industry. The silicon carbide crystal is thinned by adopting a method of grinding by using a liquid free abrasive, but the processing allowance of the silicon carbide crystal material is larger, and when the liquid grinding processing is adopted, the period is long, the efficiency is low, the precision of a ground workpiece is low, the reject ratio of the workpiece is high, and the liquid abrasive causes larger environmental pollution.
Disclosure of Invention
The invention provides a grinding wheel for thinning a silicon carbide crystal, a preparation method and application thereof. Meanwhile, the bonding agent bridge established by the porous structure is effectively broken during grinding, the self-sharpening performance of the grinding wheel is good, and the dressing frequency is reduced. The specific calcium fluoride and lubricant materials in the grinding wheel system can reduce the friction coefficient of the grinding wheel, thereby effectively reducing the grinding heat and improving the surface quality of the ground silicon carbide wafer.
The technical scheme for realizing the invention is as follows:
the grinding wheel for thinning the silicon carbide crystal is of a porous structure, and comprises the following raw materials in percentage by weight: 15-40% of diamond abrasive, 10-35% of phenolic resin powder, 3-15% of foaming agent, 5-20% of calcium fluoride, 3-15% of tungsten disulfide, 3-15% of cerium oxide, 5-20% of cryolite and 0.5-6% of zinc stearate.
The diamond abrasive particle size is 1500# -4000#, the porous structure of the grinding wheel is a continuous porous structure, and the porosity is distributed in the range of 10-80%.
The foaming agent is 4, 4' -oxybis-benzenesulfonyl hydrazide, and is treated by the following steps: dissolving the foaming agent in an ethylene glycol solvent, then placing the mixture into a vacuum drying oven at 80 ℃ for 2h, crushing the mixture for 2h by a crusher, cooling the mixture by liquid nitrogen, carrying out ball milling and refining treatment for 4h, and finally sieving the mixture by 400# and 500# standard sieves to obtain the treated foaming agent with the particle size distribution of 40-50 microns.
The preparation method of the grinding wheel for thinning the silicon carbide crystal comprises the following steps:
(1) putting the processed foaming agent, zinc stearate and phenolic resin powder into a planetary mixer for ball mixing for 1h, and then sieving to obtain an adhesive;
(2) putting a diamond grinding material into a mortar, adding a silane coupling agent as a wetting agent and a coupling agent, grinding for 20min, pouring the ground diamond into the adhesive in the step (1), mixing and sieving;
(3) mixing and sieving calcium fluoride, tungsten disulfide, cryolite and cerium oxide, then adding the mixture into the diamond mixture sieved in the step (2), and sieving to obtain a molding material;
(4) and (3) putting the molding material and the matrix in the step (3) into an assembled special die, putting the die and the matrix into a hot press for prepressing, heating for pressing and molding after prepressing, removing pressure by the hot press, taking out the die, cooling the die to room temperature, removing the die, taking out a pressed grinding wheel block, putting the grinding wheel into an oven at 170 ℃ for heat preservation for 12 hours, cooling and performing finish machining to obtain the resin binder grinding wheel for silicon carbide crystal thinning.
Passing through a 200-mesh standard sieve for 3 times in the step (1) to obtain the adhesive; sieving for 5 times by using a 200-mesh sieve in the step (2); and (3) sieving the calcium fluoride, the molybdenum disulfide, the white corundum and the zinc oxide for 4 times by using a 300-mesh standard sieve, then adding the mixture into the diamond mixture sieved in the step (2), and sieving the mixture by using a 200-mesh sieve for 5 times to obtain a molding material.
And (4) pre-pressing at the temperature of 120-.
In the step (4), the substrate is an aluminum substrate, and 32 water holes are uniformly distributed on the substrate.
The invention has the beneficial effects that: the resin porous structure grinding wheel provided by the invention is used as a consolidation grinding tool, can realize the back thinning of the silicon carbide semiconductor by adopting an end face grinding method, has good chip-containing property, high temperature resistance and self-sharpening property, and can solve the grinding processing problem of the silicon carbide crystal. The grinding wheel greatly improves the processing efficiency of the silicon carbide crystal, ensures the size, thickness and surface quality of the wafer, and avoids environmental pollution caused by free grinding materials.
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 drawings without creative efforts.
FIG. 1 is a cross-sectional view of a grinding wheel layer prepared in example 1.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood 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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A resin bond grinding wheel for thinning silicon carbide crystals and a preparation method thereof are disclosed, the resin bond grinding wheel comprises the following components by weight percent: 25% of diamond abrasive, 35% of phenolic resin powder, 10% of azo foaming agent, 6% of calcium fluoride, 3% of tungsten disulfide, 10% of cerium oxide, 10% of cryolite and 1% of zinc stearate.
The processing method of the 4, 4' -oxybis-benzenesulfonyl hydrazide foaming agent comprises the following steps: dissolving the foaming agent in an ethylene glycol solvent, then putting the mixture into a vacuum drying oven at 80 ℃ for 2h, crushing the mixture for 2h by a crusher, cooling the mixture by liquid nitrogen, carrying out ball milling and refining treatment on the mixture for 4h by a planetary ball mill, and finally sieving the mixture by 400# and 500# standard sieves to obtain the treated foaming agent with the particle size distribution of 40-50 microns.
The preparation method of the resin bond grinding wheel for thinning the silicon carbide crystal comprises the following steps:
(1) and (3) putting the treated foaming agent, zinc stearate and phenolic resin powder into a planetary mixer for ball mixing for 1h, and then sieving for 3 times by using a 200-mesh standard sieve. Putting the diamond abrasive into a mortar, adding a wetting agent and a coupling agent, grinding for 20min, then pouring the ground diamond into the sieved adhesive, and sieving for 5 times by using a 200-mesh sieve. Sieving calcium fluoride, tungsten disulfide, cryolite and cerium oxide for 4 times with a 300-mesh standard sieve. Then pouring the auxiliary materials into the dried diamond and the adhesive material, and sieving the mixture for 5 times by a 200-mesh sieve to obtain a molding material which is uniformly mixed.
(2) And putting the uniformly mixed molding material and the matrix into an assembled special die, putting the die on a 140 ℃ hot press for prepressing for 5min, wherein the prepressing pressure is 400KN, then heating the press to 170 ℃ at the speed of 5 ℃/min, deflating for 10 times in the process, increasing the pressure to 1600KN at the speed of 200KN/min, preserving the heat on the hot press for 2h, releasing the pressure by the press, and taking out the die. And cooling the mold to room temperature, unloading the mold, and taking out the pressed grinding wheel block. And (4) placing the grinding wheel in an oven at 170 ℃ for heat preservation for 12 h. Taking out and cooling.
(3) And (3) carrying out finish machining on the cooled semi-finished product by special turning, grinding and the like to obtain the resin bond grinding wheel for thinning the silicon carbide crystal, disclosed by the invention, after the required precision is reached.
The grinding wheel of example 1 was subjected to a silicon carbide wafer thinning test. Experimental items: grinding 4 inches of wafers on an Okamoto VG502 thinning machine, wherein the grinding allowance is 100 mu m, the rotating speed of a grinding wheel is 2600rpm, and the feeding speed is 0.2 mu m/s, the 450 wafers are not trimmed, and the surface TTV value is within 2 mu m.
As shown in figure 1, the cross section of the prepared grinding wheel layer is uniformly distributed with a continuous hole structure of about 80 microns, so that the grinding wheel layer has a good chip-containing effect on grinding and improves the grinding sharpness of the grinding wheel.
Example 2
The resin bonding agent sand for thinning the silicon carbide crystal comprises the following components in percentage by weight: 40% of diamond abrasive, 18% of phenolic resin powder, 5% of azo foaming agent, 5% of calcium fluoride, 8% of tungsten disulfide, 15% of cerium oxide, 5% of cryolite and 4% of zinc stearate.
The processing method of the 4, 4' -oxybis-benzenesulfonyl hydrazide foaming agent comprises the following steps: dissolving the foaming agent in an ethylene glycol solvent, then placing the mixture into a vacuum drying oven with the temperature of 80 ℃ for 2h, crushing the mixture for 2h by a crusher, cooling the mixture by liquid nitrogen, carrying out ball milling and refining treatment on the mixture for 4h by a planetary ball mill, and finally sieving the mixture by 400# and 500# standard sieves to obtain the treated foaming agent with the particle size distribution of 40-50 microns.
A preparation method of a resin bond grinding wheel for thinning a silicon carbide crystal comprises the following steps:
(1) and (3) putting the treated foaming agent, zinc stearate and phenolic resin powder into a planetary mixer for ball mixing for 1h, and then sieving for 3 times by using a 200-mesh standard sieve. Putting the diamond abrasive into a mortar, adding a wetting agent and a coupling agent, grinding for 20min, then pouring the ground diamond into the sieved adhesive, and sieving for 5 times by using a 200-mesh sieve. Sieving calcium fluoride, tungsten disulfide, cryolite and cerium oxide for 4 times with a 300-mesh standard sieve. Then pouring the auxiliary materials into the dried diamond and the adhesive material, and sieving the mixture for 5 times by a 200-mesh sieve to obtain a molding material which is uniformly mixed.
(2) And putting the uniformly mixed molding material and the matrix into an assembled special die, putting the die on a 140 ℃ hot press for prepressing for 5min, wherein the prepressing pressure is 400KN, then heating the press to 170 ℃ at the speed of 5 ℃/min, deflating for 10 times in the process, increasing the pressure to 1600KN at the speed of 200KN/min, preserving the heat on the hot press for 2h, releasing the pressure by the press, and taking out the die. And cooling the mold to room temperature, unloading the mold, and taking out the pressed grinding wheel block. And (4) placing the grinding wheel in an oven at 170 ℃ for heat preservation for 12h, taking out and cooling.
(3) And (3) carrying out finish machining on the cooled semi-finished product by special turning, grinding and the like to obtain the resin bond grinding wheel for thinning the silicon carbide crystal, disclosed by the invention, after the required precision is reached.
The grinding wheel of example 2 was subjected to a silicon carbide wafer thinning test. Experimental items: grinding 4-inch wafers on an Okamoto VG502 thinning machine, wherein the grinding allowance is 80 mu m, the rotating speed of a grinding wheel is 2800rpm, and the feeding speed is 0.15 mu m/s, 300 grinding pieces are not trimmed, and the surface TTV value is within 2 mu m.
Example 3
A resin bond grinding wheel for thinning silicon carbide crystals comprises the following components in percentage by weight: 19% of diamond abrasive, 15% of phenolic resin powder, 5% of azo foaming agent, 15% of calcium fluoride, 10% of tungsten disulfide, 10% of cerium oxide, 20% of cryolite and 6% of zinc stearate.
The processing method of the 4, 4' -oxybis-benzenesulfonyl hydrazide foaming agent comprises the following steps: dissolving the foaming agent in an ethylene glycol solvent, then placing the mixture into a vacuum drying oven with the temperature of 80 ℃ for 2h, crushing the mixture for 2h by a crusher, cooling the mixture by liquid nitrogen, carrying out ball milling and refining treatment on the mixture for 4h by a planetary ball mill, and finally sieving the mixture by 400# and 500# standard sieves to obtain the treated foaming agent with the particle size distribution of 40-50 microns.
A preparation method of a resin bond grinding wheel for thinning a silicon carbide crystal comprises the following steps:
(1) and (3) putting the treated foaming agent, zinc stearate and phenolic resin powder into a planetary mixer for ball mixing for 1h, and then sieving for 3 times by using a 200-mesh standard sieve. Putting the diamond abrasive into a mortar, adding a wetting agent and a coupling agent, grinding for 20min, then pouring the ground diamond into the sieved adhesive, and sieving for 5 times by using a 200-mesh sieve. Sieving calcium fluoride, tungsten disulfide, cryolite and cerium oxide for 4 times with a 300-mesh standard sieve. Then pouring the auxiliary materials into the dried diamond and the adhesive material, and sieving the mixture for 5 times by a 200-mesh sieve to obtain a molding material which is uniformly mixed.
(2) And putting the uniformly mixed molding material and the matrix into an assembled special die, placing the die on a 120 ℃ hot press for prepressing for 15min, wherein the prepressing pressure is 400KN, then heating the press to 150 ℃ at the speed of 5 ℃/min, deflating for 5 times in the process, increasing the pressure to 1400KN at the speed of 200KN/min, preserving the heat on the hot press for 3h, releasing the pressure by the press, and taking out the die. And cooling the mold to room temperature, unloading the mold, and taking out the pressed grinding wheel block. And (4) placing the grinding wheel in an oven at 170 ℃ for heat preservation for 12 h. Taking out and cooling.
(3) And (3) carrying out finish machining on the cooled semi-finished product by special turning, grinding and the like to obtain the resin bond grinding wheel for thinning the silicon carbide crystal, disclosed by the invention, after the required precision is reached.
The grinding wheel of example 3 was subjected to a silicon carbide wafer thinning test. Experimental items: grinding 4-inch wafers on an Okamoto VG502 thinning machine, wherein the grinding allowance is 60 mu m, the rotating speed of a grinding wheel is 2800rpm, and the feeding speed is 0.1 mu m/s, 560 grinding pieces are not trimmed, and the surface TTV value is within 2 mu m.
Example 4
A resin bond grinding wheel for thinning silicon carbide crystals comprises the following components in percentage by weight: 30% of diamond abrasive, 10% of phenolic resin powder, 3% of azo foaming agent, 20% of calcium fluoride, 15% of tungsten disulfide, 3% of cerium oxide, 16% of cryolite and 3% of zinc stearate.
The processing method of the 4, 4' -oxybis-benzenesulfonyl hydrazide foaming agent comprises the following steps: dissolving the foaming agent in an ethylene glycol solvent, then placing the mixture into a vacuum drying oven with the temperature of 80 ℃ for 2h, crushing the mixture for 2h by a crusher, cooling the mixture by liquid nitrogen, carrying out ball milling and refining treatment on the mixture for 4h by a planetary ball mill, and finally sieving the mixture by 400# and 500# standard sieves to obtain the treated foaming agent with the particle size distribution of 40-50 microns.
A preparation method of a resin bond grinding wheel for thinning a silicon carbide crystal comprises the following steps:
(1) and (3) putting the treated foaming agent, zinc stearate and phenolic resin powder into a planetary mixer for ball mixing for 1h, and then sieving for 3 times by using a 200-mesh standard sieve. Putting the diamond abrasive into a mortar, adding a wetting agent and a coupling agent, grinding for 20min, then pouring the ground diamond into the sieved adhesive, and sieving for 5 times by using a 200-mesh sieve. Sieving calcium fluoride, tungsten disulfide, cryolite and cerium oxide for 4 times with a 300-mesh standard sieve. Then pouring the auxiliary materials into the dried diamond and the adhesive material, and sieving the mixture for 5 times by a 200-mesh sieve to obtain a molding material which is uniformly mixed.
(2) And putting the uniformly mixed molding material and the matrix into an assembled special die, placing the die on a 160 ℃ hot press for prepressing for 2min, wherein the prepressing pressure is 400KN, then heating the press to 200 ℃ at the speed of 5 ℃/min, deflating for 20 times in the process, increasing the pressure to 2000KN at the speed of 200KN/min, preserving the heat on the hot press for 5h, releasing the pressure by the press, and taking out the die. And cooling the mold to room temperature, unloading the mold, and taking out the pressed grinding wheel block. And (4) placing the grinding wheel in an oven at 170 ℃ for heat preservation for 12 h. Taking out and cooling.
(3) And (3) carrying out finish machining on the cooled semi-finished product by special turning, grinding and the like to obtain the resin bond grinding wheel for thinning the silicon carbide crystal, disclosed by the invention, after the required precision is reached.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The utility model provides a emery wheel is used in carborundum crystal attenuate which characterized in that: the grinding wheel has a porous structure, and the raw materials comprise the following components in percentage by weight: 15-40% of diamond abrasive, 10-35% of phenolic resin powder, 3-15% of foaming agent, 5-20% of calcium fluoride, 3-15% of tungsten disulfide, 3-15% of cerium oxide, 5-20% of cryolite and 0.5-6% of zinc stearate.
2. The grinding wheel for silicon carbide crystal thinning according to claim 1, wherein: the diamond abrasive particle size is 1500# -4000#, the porous structure of the grinding wheel is a continuous porous structure, and the porosity is distributed in the range of 10-80%.
3. The grinding wheel for silicon carbide crystal thinning according to claim 1, wherein the foaming agent is 4, 4' -oxybis-benzenesulfonylhydrazide, and the foaming agent is treated by: dissolving the foaming agent in an ethylene glycol solvent, then placing the mixture into a vacuum drying oven at 80 ℃ for 2h, crushing the mixture for 2h by a crusher, cooling the mixture by liquid nitrogen, carrying out ball milling and refining treatment for 4h, and finally sieving the mixture by 400# and 500# standard sieves to obtain the treated foaming agent with the particle size distribution of 40-50 microns.
4. A method for preparing a grinding wheel for silicon carbide crystal thinning according to any one of claims 1 to 3, characterized by comprising the steps of:
(1) putting the processed foaming agent, zinc stearate and phenolic resin powder into a planetary mixer for ball mixing for 1h, and then sieving to obtain an adhesive;
(2) putting a diamond grinding material into a mortar, adding a silane coupling agent, grinding for 20min, pouring the ground diamond into the adhesive in the step (1), mixing and sieving;
(3) mixing and sieving calcium fluoride, tungsten disulfide, cryolite and cerium oxide, then adding the mixture into the diamond mixture sieved in the step (2), and sieving to obtain a molding material;
(4) and (3) putting the molding material and the matrix in the step (3) into an assembled special die, putting the die and the matrix into a hot press for prepressing, heating for pressing and molding after prepressing, removing pressure by the hot press, taking out the die, cooling the die to room temperature, removing the die, taking out a pressed grinding wheel block, putting the grinding wheel into an oven at 170 ℃ for heat preservation for 12 hours, cooling and performing finish machining to obtain the resin binder grinding wheel for silicon carbide crystal thinning.
5. The method for preparing a grinding wheel for silicon carbide crystal thinning according to claim 4, wherein: passing through a 200-mesh standard sieve for 3 times in the step (1) to obtain the adhesive; sieving for 5 times by using a 200-mesh sieve in the step (2); and (3) sieving the calcium fluoride, the molybdenum disulfide, the white corundum and the zinc oxide for 4 times by using a 300-mesh standard sieve, then adding the mixture into the diamond mixture sieved in the step (2), and sieving the mixture by using a 200-mesh sieve for 5 times to obtain a molding material.
6. The method for preparing a grinding wheel for silicon carbide crystal thinning according to claim 4, wherein: and (4) pre-pressing at the temperature of 120-.
7. The method for preparing a grinding wheel for silicon carbide crystal thinning according to claim 4, wherein: in the step (4), the substrate is an aluminum substrate, and 32 water holes are uniformly distributed on the substrate.
8. Use of the grinding wheel of any one of claims 1 to 3 for thinning a silicon carbide crystal.
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| CN113787465A (en) * | 2021-09-29 | 2021-12-14 | 河南工业大学 | Preparation method and application of grinding wheel for thinning back of silicon wafer |
| CN114571377A (en) * | 2021-11-15 | 2022-06-03 | 宜兴市泽润高分子新材料有限公司 | PAI resin-based grinding wheel and preparation method thereof |
| CN115446742A (en) * | 2022-09-14 | 2022-12-09 | 无锡市锡山区半导体先进制造创新中心 | Composite abrasive grinding wheel and preparation method and application thereof |
| CN115519483A (en) * | 2022-09-21 | 2022-12-27 | 青岛新韩金刚石工业有限公司 | Multi-groove grinding wheel for chamfering LCD (liquid crystal display) ultrathin screen glass and preparation method thereof |
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| CN113787465A (en) * | 2021-09-29 | 2021-12-14 | 河南工业大学 | Preparation method and application of grinding wheel for thinning back of silicon wafer |
| CN114571377A (en) * | 2021-11-15 | 2022-06-03 | 宜兴市泽润高分子新材料有限公司 | PAI resin-based grinding wheel and preparation method thereof |
| CN114571377B (en) * | 2021-11-15 | 2023-07-28 | 宜兴市泽润高分子新材料有限公司 | PAI resin-based grinding wheel and preparation method thereof |
| CN115446742A (en) * | 2022-09-14 | 2022-12-09 | 无锡市锡山区半导体先进制造创新中心 | Composite abrasive grinding wheel and preparation method and application thereof |
| CN115519483A (en) * | 2022-09-21 | 2022-12-27 | 青岛新韩金刚石工业有限公司 | Multi-groove grinding wheel for chamfering LCD (liquid crystal display) ultrathin screen glass and preparation method thereof |
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