CN115011049A - Preparation method of PTFE composite nanofiber material - Google Patents
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
The invention discloses a preparation method of a PTFE composite nanofiber material, which specifically comprises the following steps: step S1, taking polytetrafluoroethylene micro powder, fluorinated graphene, glass fiber, inorganic nano filler and sodium alginate according to a proportion, sequentially adding water, adding an emulsifier and an initiator, and polymerizing to form water emulsion; step S2, adding hydroxypropyl methyl cellulose ether into the aqueous emulsion, continuously stirring for 2-4 hours, cooling to room temperature, performing solid-liquid separation, collecting solids and drying; step S3, uniformly mixing the dried solids, and pressing to obtain a molding material; and S4, sintering the molding material in a sintering box to obtain the PTFE composite nanofiber material, wherein the modified carbon nanotube powder is modified by the nano silver powder, so that the performance of the PTFE composite nanofiber material can be greatly enhanced.
Description
Technical Field
The invention relates to the technical field of PTFE (polytetrafluoroethylene) materials, in particular to a preparation method of a PTFE composite nanofiber material.
Background
Polytetrafluoroethylene, commonly known as "plastic king", is a high molecular compound polymerized from tetrafluoroethylene, has excellent chemical stability, corrosion resistance, sealing property, high lubrication non-adhesiveness, electrical insulation property and good anti-aging endurance, can be used as engineering plastic to be made into polytetrafluoroethylene tubes, rods, belts, plates, films and the like, is generally applied to corrosion-resistant pipelines, containers, pumps, valves, radar, high-frequency communication equipment, radio equipment and the like with higher performance requirements, and the filling of fibers can effectively improve the strength and rigidity of the plastic and strengthen the plastic to be a rigid structural material.
In the prior art, because the auxiliary agent is added to improve the performance during molding and processing, a finished product is easy to contain a large number of micropores, the rigidity of the material is reduced, and transverse fracture is easy to cause in the stretching process.
Disclosure of Invention
The invention aims to provide a preparation method of a PTFE composite nanofiber material; the following technical problems are solved:
in the prior art, because the auxiliary agent is added to improve the performance during molding and processing, a finished product is easy to contain a large number of micropores, the rigidity of the material is reduced, and transverse fracture is easy to cause in the stretching process.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a PTFE composite nanofiber material specifically comprises the following steps:
step S1, taking polytetrafluoroethylene micro powder, fluorinated graphene, glass fiber, inorganic nano filler and sodium alginate according to a proportion, sequentially adding water, adding an emulsifier and an initiator, and polymerizing to form water emulsion;
step S2, adding hydroxypropyl methyl cellulose ether into the aqueous emulsion, continuously stirring for 2-4 hours, cooling to room temperature, performing solid-liquid separation, collecting solids and drying;
step S3, uniformly mixing the dried solid, and pressing to obtain a molding material;
and step S4, sintering the molding material in a sintering box to obtain the PTFE composite nanofiber material.
Preferably, the PTFE composite nano material comprises the following raw materials in parts by weight:
55-70 parts of polytetrafluoroethylene micro powder, 15-25 parts of fluorinated graphene, 2-6 parts of glass fiber, 1-4 parts of inorganic nano filler, 4-10 parts of sodium alginate, 0.5-2 parts of hydroxypropyl methyl cellulose ether, 80-120 parts of water, 10-20 parts of emulsifier and 4-9 parts of initiator.
Preferably, the particle size of the polytetrafluoroethylene micro powder is 25-35 um.
Preferably, the particle size of the fluorinated graphene is 30-50 nm.
Preferably, the inorganic nano filler is prepared by mixing modified carbon nano tubes and nano silicon dioxide in a mass ratio of 1: 2.
Preferably, the preparation method of the modified carbon nanotube is as follows:
a. mixing the carbon nano tube and the nano silver powder according to the weight ratio of 3: 1;
b. ultrasonically dispersing in 35-45% glycol solution for 40-60 min to obtain 35-45% solid content;
c. spray-drying for 15-30 minutes at the rotation speed of 4500-5500 rpm;
d. heat treatment is carried out for 2 to 5 hours at the temperature of 500-550 ℃, then grinding treatment is carried out, and the modified carbon nano tube can be obtained after 80-mesh sieve treatment.
Preferably, the emulsifier is ammonium perfluorooctanoate and the initiator is persulfate.
Preferably, in step S2, the collected solid is placed in a drying oven for drying and heat treatment at 120-130 ℃ for 1-2 hours.
Preferably, in step S3, the pressing process includes forward pressing and inverted pressing;
the pressure of the positive pressing is 10-20Mpa, and the pressing time is 4-10 minutes;
the pressure of the inverted pressing is 15-25Mpa, and the pressing time is 5-13 minutes.
Preferably, in step S4, the sintering process includes: the temperature is raised from room temperature to 230-240 ℃ at the temperature raising rate of 2-4 ℃/min, the temperature is maintained for 30-50 minutes, then the temperature is raised from 230-240 ℃ to 330-340 ℃ at the temperature raising rate of 1-2 ℃/min, the temperature is maintained for 15-25 minutes, the temperature is raised from 330-340 ℃ to 370-380 ℃ at the temperature raising rate of 1-2 ℃/min, the temperature is maintained for 50-100 minutes, then the temperature is lowered from 370-380 ℃ to 220-230 ℃ at the temperature lowering rate of 2-3 ℃, and finally the temperature is cooled to room temperature along with a sintering box.
The invention has the beneficial effects that:
(1) the glass fiber can improve the mechanical property of the polytetrafluoroethylene wear-resistant composite nanofiber material and play a role in modifying polytetrafluoroethylene so as to stabilize the friction coefficient of the polytetrafluoroethylene wear-resistant composite nanofiber material; the fluorinated graphene and the polytetrafluoroethylene have good compatibility, and can play a role in enhancing and toughening at the same time; the inorganic nano filler, the polytetrafluoroethylene micro powder, the fluorinated graphene, the glass fiber, the inorganic nano filler and the sodium alginate have a synergistic composite effect, so that the strength and toughness of the material can be improved, and the wear resistance of the material can be obviously improved; adding water, emulsifier and initiator to polymerize, so as to improve the interface bonding force between the raw materials and the polytetrafluoroethylene; further improving the strength and toughness of the polytetrafluoroethylene wear-resistant composite material;
(2) the modified carbon nanotube powder is modified by the nano silver powder, so that the wear resistance of the polytetrafluoroethylene composite nanofiber material can be greatly enhanced, and meanwhile, the mixture is placed into an ethylene glycol solution for ultrasonic dispersion, so that the probability of generating micropores in the process is reduced, the quality of a finished product is improved, and the production period is shortened.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
A preparation method of a PTFE composite nanofiber material specifically comprises the following steps:
s1, taking 55 parts of polytetrafluoroethylene micro powder, 15 parts of graphene fluoride, 2 parts of glass fiber, 1 part of inorganic nano filler and 4 parts of sodium alginate according to the proportion, sequentially adding 80 parts of water, 10 parts of ammonium perfluoro caprylate and 4 parts of persulfate, and polymerizing to form water emulsion;
wherein the particle size of the polytetrafluoroethylene micro powder is 25um, and the particle size of the fluorinated graphene is 30 nm;
the inorganic nano filler is prepared by mixing a modified carbon nano tube and nano silicon dioxide in a mass ratio of 1: 2;
the preparation method of the modified carbon nano tube comprises the following steps:
a. mixing the carbon nano tube and the nano silver powder according to the weight ratio of 3: 1;
b. ultrasonically dispersing the mixture in 35% glycol solution for 40 minutes, wherein the solid content is 35%;
c. spray-drying at 4500 rpm for 15 minutes;
d. heat-treating for 2 hours at 500 ℃, then grinding, and sieving with a 80-mesh sieve to obtain the modified carbon nanotube;
step S2, adding 0.5 part of hydroxypropyl methyl cellulose ether into the water emulsion, continuing stirring for 2 hours, cooling to room temperature, performing solid-liquid separation, collecting solids, and drying and heat-treating the collected solids in a drying oven at 120 ℃ for 1 hour;
step S3, uniformly mixing the dried solids, and pressing to obtain a molding material;
the pressing process comprises positive pressing and inverted pressing;
the pressure of the positive pressing is 10Mpa, and the pressing time is 4 minutes;
the pressure of the inverted pressing is 15Mpa, and the pressing time is 5 minutes;
step S4, placing the molding material into a sintering box for sintering, wherein the sintering process comprises the following steps: heating from room temperature to 230 ℃ at the heating rate of 2 ℃/min, preserving heat for 30 minutes, then heating from 230 ℃ to 330 ℃ at the heating rate of 1 ℃/min, preserving heat for 15 minutes, continuing heating from 330 ℃ to 370 ℃ at the heating rate of 1 ℃/min, preserving heat for 50 minutes, then cooling from 370 ℃ to 220 ℃ at the cooling rate of 2 ℃, and finally cooling to room temperature along with a sintering box to obtain the PTFE composite nanofiber material.
Example 2
A preparation method of a PTFE composite nanofiber material specifically comprises the following steps:
s1, taking 62 parts of polytetrafluoroethylene micro powder, 20 parts of fluorinated graphene, 4 parts of glass fiber, 2 parts of inorganic nano filler and 7 parts of sodium alginate according to the proportion, sequentially adding 100 parts of water, 15 parts of ammonium perfluoro caprylate and 7 parts of persulfate, and polymerizing to form water emulsion;
wherein the particle size of the polytetrafluoroethylene micro powder is 30um, and the particle size of the fluorinated graphene is 40 nm;
the inorganic nano filler is a modified carbon nano tube and nano silicon dioxide according to the weight ratio of 1: 2;
the preparation method of the modified carbon nano tube comprises the following steps:
a. mixing the carbon nano tube and the nano silver powder according to the weight ratio of 3: 1;
b. ultrasonically dispersing in 40% glycol solution for 50 min to obtain 40% solid content;
c. spray-drying at 5000 rpm for 22 min;
d. heat-treating for 4 hours at the temperature of 525 ℃, then grinding, and sieving with a 80-mesh sieve to obtain the modified carbon nanotube;
step S2, adding 1.5 parts of hydroxypropyl methyl cellulose ether into the water emulsion, continuing stirring for 3 hours, cooling to room temperature, performing solid-liquid separation, collecting solids, and drying and heat-treating the collected solids in a drying oven at 125 ℃ for 1.5 hours;
step S3, uniformly mixing the dried solids, and pressing to obtain a molding material;
the pressing process comprises positive pressing and inverted pressing;
the pressure of the positive pressing is 15Mpa, and the pressing time is 6 minutes;
the pressure of the inverted pressing is 20Mpa, and the pressing time is 8 minutes;
step S4, placing the molding material into a sintering box for sintering, wherein the sintering process comprises the following steps: heating from room temperature to 235 ℃ at the heating rate of 3 ℃/min, preserving heat for 40 minutes, then heating from 235 ℃ to 335 ℃ at the heating rate of 1 ℃/min, preserving heat for 20 minutes, then continuously heating from 335 ℃ to 375 ℃ at the heating rate of 14 ℃/min, preserving heat for 80 minutes, then cooling from 375 ℃ to 225 ℃ at the cooling rate of 3 ℃, and finally cooling to room temperature along with a sintering box to obtain the PTFE composite nanofiber material.
Example 3
A preparation method of a PTFE composite nanofiber material specifically comprises the following steps:
step S1, taking 60 parts of polytetrafluoroethylene micro powder, 20 parts of graphene fluoride, 5 parts of glass fiber, 2 parts of inorganic nano filler and 8 parts of sodium alginate according to the proportion, sequentially adding 110 parts of water, 16 parts of ammonium perfluoro octoate and 8 parts of persulfate, and polymerizing to form water emulsion;
wherein the particle size of the polytetrafluoroethylene micro powder is 30um, and the particle size of the fluorinated graphene is 40 nm;
the inorganic nano filler is prepared by mixing a modified carbon nano tube and nano silicon dioxide in a mass ratio of 1: 2;
the preparation method of the modified carbon nano tube comprises the following steps:
a. mixing the carbon nano tube and the nano silver powder according to the weight ratio of 3: 1;
b. ultrasonically dispersing the mixture in 42% glycol solution for 55 minutes, wherein the solid content is 42%;
c. spray-drying at 5200 rpm for 26 min;
d. heat-treating for 4 hours at 530 ℃, then grinding, and sieving with a 80-mesh sieve to obtain the modified carbon nanotube;
step S2, adding 1.5 parts of hydroxypropyl methyl cellulose ether into the water emulsion, continuing stirring for 3 hours, cooling to room temperature, performing solid-liquid separation, collecting solids, and drying and heat-treating the collected solids in a drying oven at 125 ℃ for 2 hours;
step S3, uniformly mixing the dried solids, and pressing to obtain a molding material;
the pressing process comprises positive pressing and inverted pressing;
the pressure of the positive pressing is 18Mpa, and the pressing time is 8 minutes;
the pressure of the inverted pressing is 22Mpa, and the pressing time is 12 minutes;
step S4, placing the molding material into a sintering box for sintering, wherein the sintering process comprises the following steps: heating from room temperature to 235 ℃ at the heating rate of 2 ℃/min, preserving heat for 45 minutes, then heating from 4 ℃ to 340 ℃ at the heating rate of 2 ℃/min, preserving heat for 22 minutes, then continuing heating from 3 ℃ to 372 ℃ at the heating rate of 1 ℃/min, preserving heat for 90 minutes, then cooling from 376 ℃ to 226 ℃ at the cooling rate of 2 ℃, and finally cooling to room temperature along with a sintering box to obtain the PTFE composite nanofiber material.
Example 4
A preparation method of a PTFE composite nanofiber material specifically comprises the following steps:
step S1, taking 70 parts of polytetrafluoroethylene micro powder, 25 parts of graphene fluoride, 6 parts of glass fiber, 4 parts of inorganic nano filler and 10 parts of sodium alginate according to the proportion, sequentially adding 120 parts of water, 20 parts of ammonium perfluoro caprylate and 9 parts of persulfate, and polymerizing to form water emulsion;
wherein the particle size of the polytetrafluoroethylene micro powder is 35um, and the particle size of the fluorinated graphene is 50 nm;
the inorganic nano filler is prepared by mixing a modified carbon nano tube and nano silicon dioxide in a mass ratio of 1: 2;
the preparation method of the modified carbon nano tube comprises the following steps:
a. mixing the carbon nano tube and the nano silver powder according to the weight ratio of 3: 1;
b. ultrasonically dispersing in a glycol solution with the mass concentration of 45% for 60 minutes, wherein the solid content is 45%;
c. spray-drying at 5500 rpm for 30 min;
d. heat treating for 5 hours at 550 ℃, then grinding, and sieving with a 80-mesh sieve to obtain the modified carbon nano tube;
step S2, adding 2 parts of hydroxypropyl methyl cellulose ether into the water emulsion, continuing stirring for 4 hours, cooling to room temperature, performing solid-liquid separation, collecting solids, and placing the collected solids in a drying oven for drying and heat treatment at 130 ℃ for 2 hours;
step S3, uniformly mixing the dried solids, and pressing to obtain a molding material;
the pressing process comprises forward pressing and inverted pressing;
the pressure of the positive pressing is 20Mpa, and the pressing time is 10 minutes;
the pressure of the inverted pressing is 25Mpa, and the pressing time is 13 minutes;
step S4, placing the molding material into a sintering box for sintering, wherein the sintering process comprises the following steps: heating from room temperature to 240 ℃ at the heating rate of 4 ℃/min, preserving heat for 50 minutes, then heating from 240 ℃ to 340 ℃ at the heating rate of 2 ℃/min, preserving heat for 25 minutes, continuing heating from 340 ℃ to 380 ℃ at the heating rate of 2 ℃/min, preserving heat for 100 minutes, then cooling from 380 ℃ to 230 ℃ at the cooling rate of 3 ℃, and finally cooling to room temperature along with a sintering box to obtain the PTFE composite nanofiber material.
Comparative example 1
A preparation method of a PTFE composite nanofiber material specifically comprises the following steps:
step S1, taking 60 parts of polytetrafluoroethylene micro powder, 20 parts of graphene fluoride, 5 parts of glass fiber, 2 parts of inorganic nano filler and 8 parts of sodium alginate according to the proportion, sequentially adding 110 parts of water, 16 parts of ammonium perfluoro octoate and 8 parts of persulfate, and polymerizing to form water emulsion;
wherein the particle size of the polytetrafluoroethylene micro powder is 30um, and the particle size of the fluorinated graphene is 40 nm;
the inorganic nano filler is nano silicon dioxide;
step S2, adding 1.5 parts of hydroxypropyl methyl cellulose ether into the water emulsion, continuing stirring for 3 hours, cooling to room temperature, performing solid-liquid separation, collecting solids, and drying and heat-treating the collected solids in a drying oven at 125 ℃ for 2 hours;
step S3, uniformly mixing the dried solids, and pressing to obtain a molding material;
the pressing process comprises positive pressing and inverted pressing;
the pressure of the positive pressing is 18Mpa, and the pressing time is 8 minutes;
the pressure of the inverted pressing is 22Mpa, and the pressing time is 12 minutes;
step S4, placing the molding material into a sintering box for sintering, wherein the sintering process comprises the following steps: heating from room temperature to 235 ℃ at the heating rate of 2 ℃/min, preserving heat for 45 minutes, then heating from 4 ℃ to 340 ℃ at the heating rate of 2 ℃/min, preserving heat for 22 minutes, then continuing heating from 3 ℃ to 372 ℃ at the heating rate of 1 ℃/min, preserving heat for 90 minutes, then cooling from 376 ℃ to 226 ℃ at the cooling rate of 2 ℃, and finally cooling to room temperature along with a sintering box to obtain the PTFE composite nanofiber material.
Comparative example 2
A preparation method of a PTFE composite nanofiber material specifically comprises the following steps:
step S1, taking 60 parts of polytetrafluoroethylene micro powder, 20 parts of graphene fluoride, 5 parts of glass fiber, 2 parts of inorganic nano filler and 8 parts of sodium alginate according to the proportion, sequentially adding 110 parts of water, 16 parts of ammonium perfluoro octoate and 8 parts of persulfate, and polymerizing to form water emulsion;
wherein the particle size of the polytetrafluoroethylene micro powder is 30um, and the particle size of the fluorinated graphene is 40 nm;
the inorganic nano-filler is carbon nano-tube and nano-silica according to the weight proportion of 1: 2;
step S2, adding 1.5 parts of hydroxypropyl methyl cellulose ether into the water emulsion, continuing stirring for 3 hours, cooling to room temperature, performing solid-liquid separation, collecting solids, and drying and heat-treating the collected solids in a drying oven at 125 ℃ for 2 hours;
step S3, uniformly mixing the dried solids, and pressing to obtain a molding material;
the pressing process comprises positive pressing and inverted pressing;
the pressure of the positive pressing is 18Mpa, and the pressing time is 8 minutes;
the pressure of the inverted pressing is 22Mpa, and the pressing time is 12 minutes;
step S4, placing the molding material into a sintering box for sintering, wherein the sintering process comprises the following steps: heating from room temperature to 235 ℃ at the heating rate of 2 ℃/min, preserving heat for 45 minutes, then heating from 4 ℃ to 340 ℃ at the heating rate of 2 ℃/min, preserving heat for 22 minutes, then continuing heating from 3 ℃ to 372 ℃ at the heating rate of 1 ℃/min, preserving heat for 90 minutes, then cooling from 376 ℃ to 226 ℃ at the cooling rate of 2 ℃, and finally cooling to room temperature along with a sintering box to obtain the PTFE composite nanofiber material.
Test examples
The PTFE composite nanofiber materials prepared in examples 1-4 and comparative examples 1-2 were tested and the results are shown in the following table:
testing the tensile strength according to the GB/T1040.2-2006 standard;
testing the elongation at break according to the GB/T1040.2-2006 standard;
according to GB/T3960-2016 standard, volume wear rate;
in conclusion, the PTFE composite nanofiber materials prepared in examples 1 to 4 are remarkably improved in tensile strength, elongation at break and volumetric wear rate compared with those prepared in comparative examples 1 to 2.
Although one embodiment of the present invention has been described in detail, the description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. A preparation method of a PTFE composite nanofiber material is characterized by comprising the following steps:
step S1, taking polytetrafluoroethylene micro powder, fluorinated graphene, glass fiber, inorganic nano filler and sodium alginate according to a proportion, sequentially adding water, adding an emulsifier and an initiator, and polymerizing to form water emulsion;
step S2, adding hydroxypropyl methyl cellulose ether into the aqueous emulsion, continuously stirring for 2-4 hours, cooling to room temperature, performing solid-liquid separation, collecting solids and drying;
step S3, uniformly mixing the dried solids, and pressing to obtain a molding material;
and step S4, sintering the molding material in a sintering box to obtain the PTFE composite nanofiber material.
2. The preparation method of the PTFE composite nano-fiber material according to claim 1, wherein the PTFE composite nano-fiber material comprises the following raw materials in parts by weight:
55-70 parts of polytetrafluoroethylene micro powder, 15-25 parts of fluorinated graphene, 2-6 parts of glass fiber, 1-4 parts of inorganic nano filler, 4-10 parts of sodium alginate, 0.5-2 parts of hydroxypropyl methyl cellulose ether, 80-120 parts of water, 10-20 parts of emulsifier and 4-9 parts of initiator.
3. The preparation method of the PTFE composite nanofiber material as set forth in claim 1, wherein the particle size of the polytetrafluoroethylene micro powder is 25-35 um.
4. The preparation method of the PTFE composite nanofiber material as set forth in claim 3, wherein the particle size of the fluorinated graphene is 30-50 nm.
5. The preparation method of the PTFE composite nanofiber material as set forth in claim 2, wherein the inorganic nano filler is prepared by mixing the modified carbon nanotube and the nano silica in a mass ratio of 1: 2.
6. The preparation method of the PTFE composite nanofiber material as set forth in claim 5, wherein the preparation method of the modified carbon nanotube is as follows:
a. mixing the carbon nano tube and the nano silver powder according to the weight ratio of 3: 1;
b. ultrasonically dispersing in 35-45% glycol solution for 40-60 min to obtain 35-45% solid content;
c. spray-drying for 15-30 minutes at the rotation speed of 4500-5500 rpm;
d. heat treatment is carried out for 2 to 5 hours at the temperature of 500-550 ℃, then grinding treatment is carried out, and the modified carbon nano tube can be obtained after 80-mesh sieve treatment.
7. The method for preparing PTFE composite nanofiber material as claimed in claim 5, wherein said emulsifier is ammonium perfluorooctanoate and said initiator is persulfate.
8. The method as claimed in claim 2, wherein the collected solid is dried and heat treated in a drying oven at 120-130 ℃ for 1-2 hours in step S2.
9. The method for preparing a PTFE composite nanofiber material according to claim 2, wherein in step S3, the pressing process includes a forward pressing and an inverted pressing;
the pressure of the positive pressing is 10-20Mpa, and the pressing time is 4-10 minutes;
the pressure of the inverted pressing is 15-25Mpa, and the pressing time is 5-13 minutes.
10. The method for preparing a PTFE composite nanofiber material according to any one of claims 1 to 9, wherein in step S4, the sintering process comprises: the temperature is raised from room temperature to 230-240 ℃ at the temperature raising rate of 2-4 ℃/min, the temperature is maintained for 30-50 minutes, then the temperature is raised from 230-240 ℃ to 330-340 ℃ at the temperature raising rate of 1-2 ℃/min, the temperature is maintained for 15-25 minutes, the temperature is raised from 330-340 ℃ to 370-380 ℃ at the temperature raising rate of 1-2 ℃/min, the temperature is maintained for 50-100 minutes, then the temperature is lowered from 370-380 ℃ to 220-230 ℃ at the temperature lowering rate of 2-3 ℃, and finally the temperature is cooled to room temperature along with a sintering box.
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