CN108515470B - Preparation process of diamond composite grinding disc - Google Patents
Preparation process of diamond composite grinding disc Download PDFInfo
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- CN108515470B CN108515470B CN201810538590.1A CN201810538590A CN108515470B CN 108515470 B CN108515470 B CN 108515470B CN 201810538590 A CN201810538590 A CN 201810538590A CN 108515470 B CN108515470 B CN 108515470B
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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
Abstract
The invention discloses a preparation process of a diamond composite grinding disc, which comprises the following steps: (1) carrying out surface modification on the diamond grinding material; (2) preparing a diamond grinding disc by using unsaturated polyester resin bonded abrasive; (3) removing magnesium sulfate to obtain a porous unsaturated polyester resin diamond grinding disc; (4) and (3) soaking under a vacuum heating condition to prepare the diamond composite grinding disc. The grinding disc has mechanical grinding and chemical reaction removing effects on the monocrystalline silicon wafer in the grinding process, and the grinding efficiency is improved by more than one time compared with that of the existing mechanical grinding method.
Description
Technical Field
The invention relates to a preparation process of a diamond composite grinding disc, in particular to a preparation process of a special diamond composite grinding disc for plane grinding of monocrystalline silicon wafers, and belongs to the field of manufacturing of superhard material tools.
Background
With the development of science and technology, the requirement of the industry for the surface of a workpiece is higher and higher, and in many fields, in particular, ultra-precision processing of wafer materials is even required to reach the nanometer level. Silicon (Si) is currently the most important and most widely used semiconductor material, and single crystal silicon semiconductor substrates are widely used in large scale and very large scale integrated circuits. The surface quality of the silicon wafer is one of the most main factors influencing the electrical performance of the silicon wafer, wherein the flatness error of the silicon wafer directly influences the focusing of a photoetching system, the roughness influences the size and the precision of a scribed line, and the number and the depth of defects influence the integration level and the reliability of elements. At present, the plane finish machining of monocrystalline silicon mainly adopts mechanical grinding and polishing, sheet-shaped white corundum with the grain diameter of 7-14 microns is purchased by manufacturers as an abrasive, and then the abrasive, water (or an organic solvent) and a dispersing agent are prepared into an alumina grinding fluid. The double-end-face grinding equipment for monocrystalline silicon wafer adopts a special double-face vertical grinding machine, the upper end face and the lower end face of the grinding machine are respectively provided with a cast iron disc during grinding, the prepared alumina grinding liquid is dripped between the cast iron discs and the monocrystalline silicon wafer, and the grinding process is carried outThe medium cast iron disc and the monocrystalline silicon generate relative motion, and the white corundum abrasive positioned between the grinding disc and the monocrystalline silicon realizes free rolling grinding on the surface of the monocrystalline silicon to be processed. The process has the following problems: (1) the grinding medium in the existing grinding process is corundum, and the hardness and the sharpness are not ideal. The grinding efficiency is low, the grinding time of each silicon wafer exceeds 15min, and the stress-altered layer on the surface of the silicon wafer exceeds 1 micron, so that great side effect is generated on high-end application of the monocrystalline silicon material. (2) After the white corundum grinding fluid is used, the white corundum used as a grinding medium is broken and passivated, and cannot be recycled. Some manufacturers try to grind the surface of a monocrystalline silicon wafer by using a diamond grinding disc bonded with resin, but because diamond grinding materials are expensive, in order to prolong the service life of the diamond grinding disc as much as possible, a large amount of resin is added into the grinding disc at present, the diamond is firmly bonded to a grinding surface, and if the granularity D is selected90The surface smoothness of the single crystal silicon ground by the diamond resin grinding disc smaller than 7 microns can reach Ra0.08 microns, but the working efficiency is very low, and 5N/cm is always loaded on a silicon wafer to ensure the working efficiency2The working pressure of the grinding machine can reach the efficiency of the existing white corundum grinding process, but the high working pressure can enable the stress layer on the surface of the ground silicon wafer to be larger than 1 micron, and the quality of the silicon wafer is seriously influenced. If granularity D is selected90Grinding silicon wafer with diamond resin grinding disc larger than 7 microns, although only loading 1N/cm on the silicon wafer2The working pressure can reach the efficiency of the existing white corundum grinding process, the surface stress layer of the silicon wafer is less than 0.1 micron, but the surface smoothness of the silicon wafer exceeds Ra0.1 micron, and the technical requirement of a chip with the line width of less than 20 nanometers cannot be met.
Disclosure of Invention
The invention aims to prepare a special diamond resin grinding disc for grinding silicon wafers, the processing efficiency of the special diamond resin grinding disc is higher than that of the existing white corundum grinding process, the surface smoothness Ra value of the processed silicon wafers is less than 0.08 micrometer, and the thickness of a stress layer is less than 0.1 micrometer. The precision processing level of the current monocrystalline silicon piece can be improved, and the progress of the chip preparation technology is promoted.
The technical scheme of the invention is to provide a preparation process of a diamond composite grinding disc, which comprises the following steps:
(1) surface modification of diamond abrasive:
weighing diamond grinding materials with the granularity of 3-6 microns, adding a surface modifier, mixing, and drying the mixed materials to obtain surface-modified diamond grinding materials;
the addition amount of the surface modifier accounts for 5-8% of the mass of the diamond abrasive; the surface modifier is obtained by weighing tetraethoxysilane and absolute ethyl alcohol according to the mass ratio of 8-12:90, pouring into a container, and stirring for more than 1 hour;
(2) preparation of the unsaturated polyester resin diamond grinding disc:
respectively weighing surface-modified diamond abrasive, unsaturated polyester resin, magnesium sulfate and cyclohexanone peroxide according to the mass ratio of (27-32) to (34-40) to (27-37) to 2; pouring the mixed slurry of the components into a forming mold, curing, and demolding to obtain the unsaturated polyester resin diamond grinding disc;
(3) preparation of porous unsaturated polyester resin diamond grinding disc:
soaking an unsaturated polyester resin diamond grinding disc in water to dissolve magnesium sulfate in the grinding disc, and drying the diamond grinding disc after the magnesium sulfate is dissolved out to obtain a porous unsaturated polyester resin diamond grinding disc;
(4) impregnation of porous unsaturated polyester resin diamond grinding disc:
placing a porous unsaturated polyester resin diamond grinding disc in an impregnation container, calculating the mass of an impregnant required for completely filling pores according to the porosity of the porous unsaturated polyester resin diamond grinding disc, placing the impregnant with the mass larger than the calculated mass on the porous unsaturated polyester resin diamond grinding disc, sealing the impregnation container, vacuumizing, heating the closed container to melt the impregnant when the pressure in the impregnation container is lower than 10Pa, preserving the heat for 10-15 minutes after melting, recovering the normal pressure, and cooling to obtain a diamond composite grinding disc;
the preparation method of the impregnant comprises the following steps: mixing calcium fluoride powder and ammonium bicarbonate powder according to the mass ratio of 1:1, and adding oleic acid, wherein the addition amount of the oleic acid is 5-6% of the total mass of the calcium fluoride powder and the ammonium bicarbonate powder; then mixing the mixed materials to obtain calcium fluoride and ammonium bicarbonate mixed powder coated with oleic acid on the surface; melting 15-45 parts of polyethylene glycol, adding 55-85 parts of mixed powder of calcium fluoride and ammonium bicarbonate with oleic acid coated on the surface, stirring, and cooling to obtain the impregnant.
Preferably, in step (4), the molecular weight of the polyethylene glycol is 8000-12000.
Preferably, a ball milling jar is used for mixing, polyurethane balls are used as ball milling balls, and the ball milling balls and the ball milling materials are preferably equal in quality.
Preferably, in step (2), the unsaturated polyester resin is 307 unsaturated polyester resin. 307 represents a resin type, which is a commonly used commercial resin product, and the 307 resin is produced by Zhangzhou Yabang chemical Co.
Preferably, in the step (2), the curing conditions are as follows: firstly, curing for 6-8 hours at 40-50 ℃; and standing for 40-50 hours after demolding to completely cure the resin.
Preferably, in step (4), the calcium fluoride powder has a diameter D90Below 5 microns; diameter D of ammonium bicarbonate powder90Below 7 microns.
Preferably, in the step (1), the ball milling condition is 40-100 r/min, and the ball milling time is 1-3 hours; in the step (4), the ball milling condition is 40-100 r/min, and the ball milling time is 20-30 hours.
Preferably, the amount of the infiltrant added is 1.1 to 1.3 times the mass required for calculation.
Preferably, in the step (2), the weighed unsaturated polyester resin is poured into a container, and the weighed surface-modified diamond abrasive is added at the stirring speed of 1500-; after stirring for 1-2 hours, adding weighed magnesium sulfate, stirring for 2-3 hours at the stirring speed of 1500-.
Preferably, in step (1), the drying conditions are as follows: drying at 110-130 deg.C for 2-3 hours.
The invention is further explained below:
1. diamond surface modification
The diamond powder used in industry has very stable chemical property and small surface tension, and is difficult to wet with resin and realize chemical bonding when preparing a resin grinding wheel, which causes that the unsaturated polyester resin used as a bonding agent in the grinding disc is difficult to firmly bond the diamond used as an abrasive, and causes that the diamond falls off too early in the grinding process, thereby influencing the service life of the grinding disc. In the invention, under the condition of ball milling, the diamond micro powder is mixed with diluted ethyl orthosilicate, the ethyl orthosilicate is oily and has good wettability on the surface of the diamond, and a uniform film layer can be formed on the surface of the diamond (figure 1). And then the diamond is dried at 120 ℃, and the diamond and the tetraethoxysilane can form C-O-Si bonds at the temperature, so that the bonding property of the tetraethoxysilane to the diamond substrate is improved.
2. Preparation of porous unsaturated polyester resin diamond grinding disc
The diamond with the surface modified by the tetraethoxysilane is mixed with the unsaturated polyester resin, and ester bond functional groups of the tetraethoxysilane can be well compatible with the unsaturated polyester resin, so that the uniform dispersion of the diamond micropowder in the unsaturated polyester resin is realized, and the improvement of the tissue uniformity of the prepared diamond millstone is facilitated. After the unsaturated polyester resin is cured, ether bonds can be formed between the unsaturated polyester resin and tetraethoxysilane on the surface of the diamond, the tetraethoxysilane on the surface of the diamond plays a role of a coupling agent, one end of the tetraethoxysilane and the diamond grinding material form a C-O-Si bond, and the other end of the tetraethoxysilane and the cured unsaturated polyester resin form ether bonds, so that the bonding force of the unsaturated polyester resin to the diamond grinding material can be greatly improved. A certain amount of magnesium sulfate is added into the cast diamond grinding disc material, and during the curing process of the diamond resin grinding disc, the magnesium sulfate does not generate any chemical reaction with the unsaturated polyester resin, so that the bonding force of the unsaturated polyester resin to the diamond grinding disc material is influenced. After the millstone is solidified, the magnesium sulfate is distributed in the diamond millstone in the form of dispersed solid particles, the solubility of the magnesium sulfate in water reaches 25 g/100 g at room temperature, the magnesium sulfate is easily dissolved in the water, and the magnesium sulfate is quickly dissolved in the water when the millstone is immersed in the water with the temperature of 60 ℃, so that a large amount of air holes are generated in the resin millstone. The porosity of the soaked porous diamond grinding disc can be accurately controlled by adjusting the addition amount of magnesium sulfate in the resin diamond grinding disc. Meanwhile, pure water for soaking the diamond grinding wheel can be changed into magnesium sulfate solution, magnesium sulfate crystals can be obtained newly after drying, and the magnesium sulfate crystals are added into the diamond grinding wheel again for use.
3. Preparation of diamond millstone impregnant
CaF2And NH4HCO3The micro powder is inorganic powder, and a layer of adsorbed water is formed on the surface of the micro powder and is difficult to disperse in the molten polyethylene glycol. Oleic acid is liquid at room temperature, has small surface tension of 33.8dyne/cm and strong molecular polarity, and can easily coat CaF with water adsorbed on the surface under the condition of ball milling and mixing2And NH4HCO3Micropowder of CaF2And NH4HCO3The micro powder realizes the surface organic modification. At 75-85 deg.C, polyethylene glycol with molecular weight of 10000 can be changed from solid into liquid with larger viscosity, and the surface is coated with CaF of oleic acid2And NH4HCO3The mixed powder is easily wetted by the molten polyethylene glycol, uniformly dispersed polyethylene glycol mixed slurry is obtained under the condition of high-speed stirring, and when the polyethylene glycol with the molecular weight of 10000 is cooled to room temperature, the uniformly dispersed mixed slurry becomes a uniformly dispersed solid impregnant.
4. Preparation of diamond composite grinding disc
When the diamond composite grinding disc prepared by the process is used for carrying out plane grinding on monocrystalline silicon, on one hand, under the action of grinding pressure, the tip grinding edge of W5 diamond micropowder in the grinding disc can scratch the surface of the monocrystalline silicon, so that the monocrystalline silicon material is mechanically ground. On the other hand, CaF is filled in the pores of the diamond grinding disc2、NH4HCO3And polyethylene glycol mixture, NH4HCO3Can be dissolved in water-based cooling liquid to generate NH with certain concentration on the working surface of the grinding disc4 +NH of the catalyst4 +CaF that can be adsorbed in the pores of the grinding disc2The following reactions take place on the surface of the particles:
CaF2+NH4 +＝[HF2]-+NH3↑+Ca2+
wherein [ HF ]2]-H-F hydrogen bond is present in the catalyst, so that the catalyst is easily decomposed into HF and F-Reaction of produced [ HF ]2]-Ions can be mixed with SiO on the surface of the monocrystalline silicon piece2The oxide layer undergoes the following chemical reaction:
2[HF2]-+SiO2+2H+＝SiF4↑+2H2O
therefore, when the composite diamond grinding disc grinds the monocrystalline silicon material, CaF filled in the pores of the diamond grinding disc2And NH4HCO3Will react to produce [ HF ]2]-Ion etching of SiO on the surface of silicon wafer2And an oxide layer, and removing materials from the silicon wafer by using a chemical reaction method. The polyethylene glycol filled in the pores of the diamond grinding disc can seal the air holes, prevent grinding fluid from infiltrating into the grinding wheel, and realize only the CaF on the grinding working surface2And NH4HCO3Production of [ HF ] under the action of water2]-Ions. Compared with the prior art, when the diamond grinding disc prepared by the invention is used for grinding monocrystalline silicon wafers, the diamond grinding disc has the following beneficial effects:
the grinding disc has mechanical grinding and chemical reaction removing effects on the monocrystalline silicon wafer in the grinding process, and the grinding efficiency is improved by more than one time compared with that of the existing mechanical grinding method. The composite diamond grinding disc made of W5 diamond is loaded with 1N/cm2At an operating pressure of 3 minutes per wafer for a 6 inch wafer, and 8 minutes for a corundum milling process. The stress layer on the surface of the silicon wafer processed by the composite grinding disc is less than 0.1 micron (figure 4), but the surface finish value of the silicon wafer is lower than Ra0.08 micron (figure 5), which is superior to that of the silicon wafer processed by the corundum grinding method.
Drawings
Fig. 1 shows a diamond abrasive coated with tetraethoxysilane.
Figure 2 shows a porous unsaturated polyester resin binder diamond grinding disc.
Figure 3 shows the composite diamond disk microtopography.
FIG. 4 shows the surface stress layer morphology of the silicon wafer after the composite diamond grinding disc is processed.
FIG. 5 shows surface topography and roughness measurements of a silicon wafer after composite diamond disk processing.
Detailed Description
The present invention will be further described with reference to the following examples.
Examples
The embodiment provides a preparation process of a diamond composite grinding disc for plane grinding of a monocrystalline silicon piece, which comprises the following specific steps:
(1) after industrial-grade ethyl orthosilicate and absolute ethyl alcohol are weighed according to the ratio of 10:90, the mixture is poured into a container, stirred for 1 hour at the stirring speed of 1000 revolutions per minute, and then the mixture is filled into a closed container, so that the diamond abrasive surface modifier is obtained.
(2) Weighing a certain amount of diamond grinding materials with the granularity of W5, putting the diamond grinding materials into a ball milling jar with the diameter of 400mm, adding 6% by mass of the diamond surface modifier obtained in the step (1), weighing polyurethane balls with the diameter of 3 cm and the same weight as the diamond, putting the polyurethane balls into the ball milling jar, sealing the mouth of the ball milling jar, and carrying out ball milling for 2 hours at the rotating speed of 60 r/min. And (4) pouring out the diamond grinding material subjected to ball milling, then placing the diamond grinding material into a tray, and drying for 3 hours in a 120-degree oven to obtain the surface modified diamond grinding material.
(3) According to the mass ratio of 30: 40: 28: 2, respectively weighing the surface modified diamond abrasive material in the step (2), 307 unsaturated polyester resin, magnesium sulfate and cyclohexanone peroxide. Firstly, weighed 307 unsaturated polyester resin (produced by Zhangzhou Yabang chemical Co., Ltd.) is poured into a clean container, then weighed diamond grinding materials are added at the stirring speed of 2000 r/min, weighed magnesium sulfate is added after stirring for 2 hours, then stirring is carried out for 2 hours at the stirring speed of 2000 r/min, then cyclohexanone peroxide is added, stirring is carried out for 15 minutes at the stirring speed of 3000 r/min, and then mixed slurry is poured into a forming die of a grinding disc, the size of the die is processed according to the size of the diamond grinding disc, and the material is cast iron. And (3) placing the mould after the slurry pouring into a 40-degree oven for curing for 8 hours, then demolding to obtain a primarily cured unsaturated polyester resin bonding agent diamond grinding disc, and then placing the unsaturated polyester resin bonding agent diamond grinding disc for 48 hours at room temperature to obtain a fully cured diamond grinding disc.
(4) And (3) soaking the fully-cured diamond grinding disc obtained in the step (3) in pure water of 60 ℃, fishing out the grinding disc from the pure water after magnesium sulfate in the grinding disc is completely melted, repeatedly washing with clear water until the pH value of the washing liquid is neutral, and then putting the grinding disc into an oven of 60 ℃ to dry for 24 hours to obtain the porous unsaturated polyester resin binder diamond grinding disc (see fig. 2).
(5) Weighing the diameter D according to the mass ratio of 1:190CaF finer at 5 μm2And diameter D90Fine NH at 7 μm4HCO3Adding the powder into a ball milling jar with the diameter of 400mm, adding oleic acid with the mass of 6% of the mixed powder, weighing polyurethane balls with the diameter of 1 cm and the weight equal to that of the mixed powder, putting the polyurethane balls into the ball milling jar, sealing the opening of the ball milling jar, enabling the rotating speed of the ball milling jar to be 60 r/min, ball milling the polyurethane balls for 24 hours, pouring the mixed powder out, and filling the mixed powder into a sealed container for standby application to obtain CaF with the surface coated with the oleic acid2And NH4HCO3And mixing the powders.
(6) According to the mass ratio of 25: 75 respectively weighing the CaF coated with the oleic acid on the surface obtained in the step (5)2And NH4HCO3Mixing the powder with polyethylene glycol with molecular weight of 10000, heating to 75-85 deg.C in water bath in polyethylene glycol container, adding weighed CaF at stirring speed of 2000 r/min after polyethylene glycol is completely melted2And NH4HCO3And mixing the powder, stirring for 3 hours, pouring the polyethylene glycol mixed slurry into a metal tray, and cooling at room temperature to obtain the block porous saturated polyester resin binder diamond millstone impregnant.
(7) And (3) horizontally placing the porous unsaturated polyester resin bonding agent diamond grinding disc obtained in the step (4) into a closed impregnation container with a heating function, calculating the mass of an impregnant required for completely filling pores according to the porosity (the measured porosity is 50%) of the diamond grinding disc, weighing the impregnant obtained in the step (6) according to 1.2 times of the theoretically required impregnation amount, placing the impregnant at the upper end of the porous grinding disc, covering the closed container for vacuumizing, heating the closed container at a heating speed of 10 ℃ per minute when the pressure in the container is lower than 10Pa, keeping the temperature for 15 minutes after heating to 80 ℃, then placing air into the closed container, cooling the container, and taking out the diamond grinding disc filled with the impregnant in the pores (see figure 3).
(8) According to the size and the dynamic balance requirement of the diamond grinding disc, machining an outer circle, an inner hole and a plane machine of the grinding disc on a lathe, and after the machining size is qualified, performing dynamic balance correction on the diamond grinding disc on a dynamic balancing instrument to obtain a final product.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (10)
1. A preparation process of a diamond composite grinding disc is characterized by comprising the following steps:
(1) surface modification of diamond abrasive:
weighing diamond grinding materials with the granularity of 3-6 microns, adding a surface modifier, mixing, and drying the mixed diamond grinding materials to obtain surface-modified diamond grinding materials;
the addition amount of the surface modifier accounts for 5-8% of the mass of the diamond abrasive; the surface modifier is obtained by weighing ethyl orthosilicate and absolute ethyl alcohol according to the mass ratio of 8-12:90, pouring into a container, mixing and stirring for more than 1 hour;
(2) preparation of the unsaturated polyester resin diamond grinding disc:
respectively weighing surface-modified diamond abrasive, unsaturated polyester resin, magnesium sulfate and cyclohexanone peroxide according to the mass ratio of (27-32) to (34-40) to (27-37) to 2; pouring the mixed slurry of the components into a forming mold, curing, and demolding to obtain the unsaturated polyester resin diamond grinding disc;
(3) preparation of porous unsaturated polyester resin diamond grinding disc:
soaking an unsaturated polyester resin diamond grinding disc in water to dissolve magnesium sulfate in the grinding disc, and drying the diamond grinding disc after the magnesium sulfate is dissolved out to obtain a porous unsaturated polyester resin diamond grinding disc;
(4) dipping of the diamond grinding disc:
placing a porous unsaturated polyester resin diamond grinding disc in an impregnation container, calculating the mass of an impregnant required for completely filling pores according to the porosity of the porous unsaturated polyester resin diamond grinding disc, placing the impregnant with the mass larger than the calculated mass on the porous unsaturated polyester resin diamond grinding disc, sealing the impregnation container, vacuumizing, heating the closed container to melt the impregnant when the pressure in the impregnation container is lower than 10Pa, preserving the heat for 10-15 minutes after melting, recovering the normal pressure, and cooling to obtain a diamond composite grinding disc;
the preparation method of the impregnant comprises the following steps: mixing calcium fluoride powder and ammonium bicarbonate powder according to the mass ratio of 1:1, and adding oleic acid, wherein the addition amount of the oleic acid is 5-6% of the total mass of the calcium fluoride powder and the ammonium bicarbonate powder; then mixing the materials to obtain mixed powder of calcium fluoride and ammonium bicarbonate with the surface coated with oleic acid; melting 15-45 parts of polyethylene glycol, adding 55-85 parts of mixed powder of calcium fluoride and ammonium bicarbonate with oleic acid coated on the surface, stirring, and cooling to obtain the impregnant.
2. The process according to claim 1, wherein in step (4), the molecular weight of the polyethylene glycol is 8000-12000.
3. The process according to claim 1, wherein in the step (2), the curing conditions are as follows: firstly, curing for 6-8 hours at 40-50 ℃; and standing for 40-50 hours after demolding to completely cure the resin.
4. The production process according to claim 1, wherein in the step (4), the calcium fluoride powder has a diameter D90Below 5 microns; diameter D of ammonium bicarbonate powder90Below 7 microns.
5. The process according to claim 1, wherein in the steps (1) and (4), the mixing is carried out using a ball mill jar, and polyurethane balls are used as the ball milling balls.
6. The process according to claim 5, wherein the polyurethane spheres have a diameter of 0.5 to 3 cm.
7. The process according to claim 5, wherein in the step (1), the ball milling is carried out under the conditions of 40-100 rpm for 1-3 hours; in the step (4), the ball milling condition is 40-100 r/min, and the ball milling time is 20-30 hours.
8. The production process according to claim 1, wherein the theoretical addition amount of the infiltrant is calculated based on the porosity, and the actual addition amount of the infiltrant is 1.1 to 1.3 times the theoretical addition amount by mass.
9. The preparation process according to claim 1, wherein in the step (2), the weighed unsaturated polyester resin is poured into a container, and the weighed surface-modified diamond abrasive is added at a stirring speed of 1500-; after stirring for 1-2 hours, adding weighed magnesium sulfate, stirring for 2-3 hours at the stirring speed of 1500-.
10. The process according to claim 1, wherein in the step (1), the drying conditions are as follows: drying at 110-130 deg.C for 2-3 hours.
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