CN109824356A - A kind of barium phthalate base high performance piezoelectric ceramic material and preparation method thereof - Google Patents
A kind of barium phthalate base high performance piezoelectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of barium phthalate base high performance piezoelectric ceramic material and preparation method thereof, chemical structural formula BaTiO3‑xCuSO4‑yLi2CO3X=0.005~0.13, y=0.005~0.02, the piezoceramic material sintering temperature is 1250~1300 DEG C, piezoelectric constant is 240~300pC/N, and mechanical quality factor is 130~150, and electromechanical coupling factor is 0.25~0.3, crystallite dimension is 0.5~1 μm, and bulk density is 5.6~5.95g/cm3.Barium phthalate base high performance piezoelectric ceramic material piezoelectric property provided by the invention is high, and sintering temperature is lower, and is prepared with common material, cheap, has broad application prospects.
Description
Technical field
The invention belongs to lead-free piezoceramic material technical fields, and in particular to a kind of barium phthalate base high performance piezoelectric ceramics
Material and preparation method thereof.
Background technique
With science and technology fast development, present electronics industry to the miniaturization of electronic component, functionalization, it is low at
Originally, the requirement of high stability is higher, and in order to meet environmental requirements, the research of leadless piezoelectric ceramics is then particularly important.
In the research of the leadless piezoelectric ceramics in modern age, have a few class piezoelectric properties are relatively stable, electromechanical coupling factor hand over it is big
Lead-free piezoelectric material be of concern, such as: perovskite structure, bismuth laminated and tungsten bronze structure leadless piezoelectric ceramics.
And Ca-Ti ore type lead-free systems become recent researches since its piezoelectric property is preferable and Curie temperature lower (~120 DEG C)
Important object.Ca-Ti ore type lead-free ceramics system mainly includes that barium titanate series leadless piezoelectric ceramics, base metal niobate system are unleaded
Piezoelectric ceramics, bismuth-sodium titanate series lead-free piezoelectric ceramic.Barium titanate series leadless piezoelectric ceramics is to study earliest and most study
Piezoceramic material, it is the Typical Representative of perovskite structural material, its piezoelectricity can be improved by the means of doping vario-property
Performance and temperature stability.But current BaTiO3The piezoelectric property of base ceramic material is still not ideal enough.
The present invention provides a kind of new BaTiO with high tension performance, high volume density3Base ceramic material, and
Its sintering temperature is substantially reduced, and can substantially reduce production cost.Meanwhile low in raw material price involved in this kind of material system,
Technique requirement is lower, is suitable for producing in enormous quantities, have broad application prospects.
Summary of the invention
It is a kind of with height the technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide
Piezoelectric property and the barium phthalate base high performance piezoelectric ceramic material of lower sintering temperature and preparation method thereof.
In order to solve the above technical problems, present invention provide the technical scheme that
A kind of barium phthalate base high performance piezoelectric ceramic material, chemical structural formula BaTiO are provided3-xCuSO4-
yLi2CO3, x=0.005~0.13, y=0.005~0.02, which is 1250~1300 DEG C, pressure
Electric constant is 240~300pC/N, and mechanical quality factor is 130~150, and electromechanical coupling factor is 0.25~0.3, crystallite dimension
It is 0.5~1 μm, bulk density is 5.6~5.95g/cm3。
The present invention also provides above-mentioned barium phthalate base high performance piezoelectric ceramic material (BaTiO3-xCuSO4-yLi2CO3, x=
0.005~0.13, y=0.005~0.02) preparation method, the specific steps are as follows:
1) raw material is weighed in materials chemistry formula ratio, it is spare；
2) prepare barium titanate suspension: barium titanate mixed with dehydrated alcohol, acetic acid aqueous solution, gained mixed liquor 30~
30~60min is stirred at 60 DEG C, subsequent ultrasonic disperse obtains barium titanate suspension；
3) it prepares copper sulphate-Lithium carbonate solution: copper sulphate, lithium carbonate is added to the mixed solvent of ethyl alcohol and deionized water
In, preparation obtains copper sulphate-Lithium carbonate solution；
4) copper sulphate obtained by step 3)-Lithium carbonate solution is added in barium titanate suspension obtained by step 2), gained is mixed
Liquid 30~60min of stirring in water bath at 30~60 DEG C is closed, subsequent ultrasonic disperse is uniform, adjusts pH value to 6~8, then with ammonium hydroxide
2~4h of stirring in water bath at normal temperature is then aged 12~for 24 hours and is dried to obtain the BaTiO by surface modification3Powder；
5) by the BaTiO obtained by step 4) Jing Guo surface modification3Bonding is added after cooling in powder pre-burning in air atmosphere
Agent is granulated, is sieved, positive pressure forming, then carries out dumping processing, is then sintered sample after molding to get the high property of barium phthalate base is arrived
It can piezoceramic material (BaTiO3-xCuSO4-yLi2CO3, x=0.005~0.13, y=0.005~0.02).
According to the above scheme, step 2) the barium titanate partial size is 100~200nm.
According to the above scheme, the step 2) barium titanate and dehydrated alcohol, acetic acid aqueous solution mass volume ratio be 15g:50~
100mL:3~5mL, the acetic acid aqueous solution concentration are 15~20mol/L.
According to the above scheme, step 3) copper sulphate purity >=99%, lithium carbonate purity >=99%.
According to the above scheme, the volume ratio of the in the mixed solvent ethyl alcohol and deionized water of the step 3) ethyl alcohol and deionized water
For 1~2:1.
According to the above scheme, concentration of copper sulfate is 0.0005~0.1g/mL in the step 3) copper sulphate-Lithium carbonate solution,
Lithium carbonate concentration is 0.0005~0.1g/mL.
According to the above scheme, step 4) drying temperature be 100~150 DEG C, drying time be 18~for 24 hours.
According to the above scheme, step 5) calcined temperature is 500~700 DEG C, and burn-in time is 2~4h.
According to the above scheme, the step 5) binder is the PVA solution that mass concentration is 5%.
According to the above scheme, step 5) the positive pressure forming condition are as follows: push 30~60s in the positive pressure of 200~300Mpa.
According to the above scheme, step 5) the dumping treatment process condition are as follows: under air atmosphere, started to warm up from room temperature, with 2
DEG C/heating rate of min is warming up to 600~650 DEG C and keeps the temperature 2~4 hours.
According to the above scheme, the step 5) sintering process conditions are as follows: under air atmosphere, started to warm up from room temperature, with 3~5
DEG C/heating rate of min is warming up to 900~1000 DEG C, then 1250~1300 are warming up to the heating rate of 2~3 DEG C/min
DEG C heat preservation 2~4 hours.
Due to BaTiO3The sintering characteristic of ceramics, when the use of it being primary raw material, sintering temperature will be typically higher than 1300
DEG C, and copper sulphate-lithium carbonate can not only help ceramics to generate in the subsequent sintering process as a kind of low melting point sintering aid
Liquid phase reduces BT base ceramic sintering temperature, and the migration and crystal grain for improving crystal boundary rearrange rate, improves the contact between crystal grain
Area improves the consistency of ceramics to reduce the defect of stomata；Copper sulphate-lithium carbonate of barium titanate body surfaces modification simultaneously
It will form the second phase and enter principal crystalline phase and play a part of to improve electrical property, therefore the piezoelectricity of barium titanate ceramics can be increased substantially
Energy.
The beneficial effects of the present invention are: 1, provided by the invention barium phthalate base high performance piezoelectric ceramic material have high pressure
Electrical property and lower sintering temperature (the piezoceramic material sintering temperature is 1250~1300 DEG C, piezoelectric constant is 240~
300pC/N, mechanical quality factor are 130~150, and electromechanical coupling factor is 0.25~0.3, and crystallite dimension is 0.5~1 μm, body
Product density is 5.6~5.95g/cm3), and be prepared with common material, it is cheap, it has broad application prospects.2,
The present invention requires lower, at low cost, preparation method simple process to raw material, it is easy to accomplish, it is reproducible, there is preferable warp
Ji benefit.
Detailed description of the invention
Fig. 1 is the TEM photo of barium phthalate base high performance piezoelectric ceramic material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of barium phthalate base high performance piezoelectric ceramic material prepared by embodiment 2；
Fig. 3 is the XRD diagram of barium phthalate base high performance piezoelectric ceramic material prepared by embodiment 1；
Fig. 4 is that barium phthalate base high performance piezoelectric ceramic material piezoelectric constant prepared by embodiment 3 changes with sintering temperature
Characteristic curve.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing to the present invention make into
One step detailed description.
Barium titanate partial size used in the embodiment of the present invention is 200nm, copper sulphate purity >=99% used, lithium carbonate purity used
>=99%.
The manufacturing process that the present invention uses is similar to sol-gel method, is adjusted by control copper sulphate-lithium carbonate content
The piezoelectric property of whole barium titanate piezoelectric ceramics, is denoted as BaTiO3-xCuSO4-yLi2CO3, (x=0.005~0.13, y=0.005
~0.02).Firstly, improving charge, that is, activated b T particle of BT particle surface by the processing of acetic acid, by BaTiO3, ethyl alcohol and vinegar
Acid mixes in proportion, is placed in 30~60 DEG C of 30~60min of stirred in water bath, is then ultrasonically treated 30~60min and obtains barium titanate
Suspension.Then, another beaker will be added and prepared to obtain copper sulphate-carbon by copper sulphate-lithium carbonate of rational proportion, second alcohol and water
Sour lithium solution.Barium titanate suspension is mixed with copper sulphate-Lithium carbonate solution, 30~60min of stirring in water bath at 30~60 DEG C, with
30~60min ultrasonic treatment is carried out afterwards, later, ammonium hydroxide slowly drips regulation system pH value=6~8 by base buret,
2~4h is stirred in room-temperature water bath device, forms the BaTiO with metal ion surface modification3Suspension.The suspension that will be obtained
Ageing 12~for 24 hours at room temperature, then dry 18 in 100~150 DEG C of baking oven~for 24 hours.Based on the above operation, can obtain
By the BaTiO of surface modification3Powder, then 2~4 hours removal organic matters of pre-burning at 500~700 DEG C, are added 5% PVA
Solution is granulated as adhesive, is sieved in the sieve of 50~100 mesh, 200~300Mpa direct draught pressure maintaining 30~
60s carries out positive pressure forming, is warming up at 600~650 DEG C with the heating rate of 2 DEG C/min and keeps the temperature 2~4h progress dumping processing,
Porcelain is sintered at 1250~1300 DEG C, obtains the barium phthalate base high performance piezoelectric ceramic material by surface modification.
Embodiment 1
Prepare a kind of barium phthalate base high performance piezoelectric ceramic material, chemical structural formula BaTiO3-xCuSO4-
yLi2CO3, x=0.005, y=0.005, it is specific the preparation method is as follows:
1) barium titanate suspension is prepared: by 15g barium titanate and 50mL dehydrated alcohol, 3mL acetic acid aqueous solution (17.5mol/L)
Mixing, gained mixed liquor stir 40min at 40 DEG C, and subsequent ultrasonic disperse 30min obtains barium titanate suspension；
2) it prepares copper sulphate-Lithium carbonate solution: 10mL ethyl alcohol and 5mL is added in 0.051g copper sulphate, 0.023g lithium carbonate
The in the mixed solvent of deionized water, preparation obtain copper sulphate-Lithium carbonate solution；
3) copper sulphate obtained by step 2)-Lithium carbonate solution is added in barium titanate suspension obtained by step 1), it will be described mixed
Liquid stirring in water bath 30min at 40 DEG C, subsequent ultrasonic disperse 30min are closed, adjusts pH value to 6 with ammonium hydroxide, then water at normal temperature
Bath stirring 2h, is then aged 12h and dry 18h obtains the BaTiO of surface modification in 150 DEG C of baking oven3Powder；
4) by the BaTiO of surface modification obtained by step 3)3Powder in 500 DEG C of pre-burning 2h, adds after cooling in air atmosphere
Enter binder (PVA solution that mass concentration is 5%) to be granulated, is sieved with the sieve of 50 mesh, then pushes 30s in 200MPa positive pressure
It is 12mm that molding, which obtains diameter, with a thickness of the disk of 0.8mm, by disk in air atmosphere with the heating rate liter of 2 DEG C/min
2h is kept the temperature to 600 DEG C and carries out dumping processing, is then placed in sample after molding on the corundum plate of laying titanium dioxide zirconium powder,
It is started to warm up under air atmosphere from room temperature, 1000 DEG C is warming up to the heating rate of 5 DEG C/min, then with the heating of 2 DEG C/min
Rate is warming up to 1250 ± 10 DEG C and is sintered 2 hours, ceramic disks, that is, barium phthalate base high performance piezoelectric ceramic material of firing
(BaTiO3-xCuSO4-yLi2CO3, x=0.005, y=0.005).
Ceramic disks obtained by the present embodiment are subjected to XRD test by surface polishing, it is normal to measure its breakdown strength, dielectric
Number, bulk density, piezoelectric constant, mechanical quality factor and electromechanical coupling factor, the data obtained are shown in Table 1.
Table 1
It is as shown in Figure 1 the TEM photo of barium phthalate base high performance piezoelectric ceramic material prepared by the present embodiment, can sees
Particle surface has one layer of apparent " layer " shape substance out, illustrates it with microcosmic " core-shell structure copolymer " structure.Fig. 3 is the present embodiment institute
The XRD diagram of the barium phthalate base high performance piezoelectric ceramic material of preparation, sample barium phthalate base known to analysis show typical calcium titanium
Mine structure, and have apparent peak splitting (002)/(200) at 45 °, show typical tetragonality.
Embodiment 2
Prepare a kind of barium phthalate base high performance piezoelectric ceramic material, chemical structural formula BaTiO3-xCuSO4-
yLi2CO3, x=0.005, y=0.005, it is specific the preparation method is as follows:
1) barium titanate suspension is prepared: by 15g barium titanate and 100mL dehydrated alcohol, 5mL acetic acid aqueous solution (17.5mol/
L it) mixes, gained mixed liquor stirs 60min at 60 DEG C, and subsequent ultrasonic disperse 60min obtains barium titanate suspension；
2) it prepares copper sulphate-Lithium carbonate solution: 20mL ethyl alcohol and 10mL is added in 0.051g copper sulphate, 0.023g lithium carbonate
The in the mixed solvent of deionized water, preparation obtain copper sulphate-Lithium carbonate solution；
3) copper sulphate obtained by step 2)-Lithium carbonate solution is added in barium titanate suspension obtained by step 1), it will be described mixed
Liquid stirring in water bath 60min at 60 DEG C, subsequent ultrasonic disperse 60min are closed, adjusts pH value to 8 with ammonium hydroxide, then water at normal temperature
Bath stirring 4h, is then aged for 24 hours and dries the BaTiO for obtaining surface modification for 24 hours in 120 DEG C of baking oven3Powder；
4) by the BaTiO of surface modification obtained by step 3)3Powder in 600 DEG C of pre-burning 2h, adds after cooling in air atmosphere
Enter binder (PVA solution that mass concentration is 5%) to be granulated, be sieved with the sieve of 100 mesh, the pressure maintaining under 300MPa pressure
It is 12mm that 60s positive pressure forming, which obtains diameter, with a thickness of the disk of 0.8mm, by disk in air atmosphere with the heating of 2 DEG C/min
Rate, which rises at 650 DEG C, keeps the temperature 4h progress dumping processing, then sample after molding is placed in the corundum of laying titanium dioxide zirconium powder
It on plate, is started to warm up in air atmosphere from room temperature, 900 DEG C is warming up to the heating rate of 3 DEG C/min, then with 2 DEG C/min
Heating rate be warming up to 1300 ± 10 DEG C be sintered 2 hours, ceramic disks, that is, barium phthalate base high performance piezoelectric ceramics material of firing
Expect (BaTiO3-xCuSO4-yLi2CO3, x=0.005, y=0.005).
Ceramic disks obtained by the present embodiment are tested by surface polishing, measure its breakdown strength, dielectric constant, body
Product density, piezoelectric constant, mechanical quality factor and electromechanical coupling factor, the data obtained are shown in Table 2.
Table 2
It is illustrated in figure 2 the SEM figure of barium phthalate base high performance piezoelectric ceramic material prepared by the present embodiment, it can be seen that
The sample crystallite dimension is more uniform, and size is between 0.5~1 μm.
Embodiment 3
Prepare a kind of barium phthalate base high performance piezoelectric ceramic material, chemical structural formula BaTiO3-xCuSO4-
yLi2CO3, x=0.13, y=0.02, it is specific the preparation method is as follows:
1) barium titanate suspension is prepared: by 15g barium titanate and 50mL dehydrated alcohol, 5mL acetic acid aqueous solution (17.5mol/L)
Mixing, gained mixed liquor stir 60min at 30 DEG C, and subsequent ultrasonic disperse 60min obtains barium titanate suspension；
2) it prepares copper sulphate-Lithium carbonate solution: 10mL ethyl alcohol and 10mL is added in 1.323g copper sulphate, 0.095g lithium carbonate
The in the mixed solvent of deionized water, preparation obtain copper sulphate-Lithium carbonate solution；
3) copper sulphate obtained by step 2)-Lithium carbonate solution is added in barium titanate suspension obtained by step 1), it will be described mixed
Liquid stirring in water bath 60min at 30 DEG C, subsequent ultrasonic disperse 30min are closed, adjusts pH value to 6 with ammonium hydroxide, then water at normal temperature
Bath stirring 2h, is then aged for 24 hours and dries the BaTiO for obtaining surface modification for 24 hours in 100 DEG C of baking oven3Powder；
4) by the BaTiO of surface modification obtained by step 3)3Powder in 600 DEG C of pre-burning 2h, adds after cooling in air atmosphere
Enter binder (PVA solution that mass concentration is 5%) to be granulated, be sieved with the sieve of 100 mesh, the pressure maintaining under 200MPa pressure
It is 12mm that 30s positive pressure forming, which obtains diameter, with a thickness of the disk of 0.8mm, by disk in air atmosphere with the heating of 2 DEG C/min
Rate, which rises at 600 DEG C, keeps the temperature 2h progress dumping processing, then sample after molding is placed in the corundum of laying titanium dioxide zirconium powder
It on plate, is started to warm up in air atmosphere from room temperature, 1000 DEG C is warming up to the heating rate of 5 DEG C/min, then with 2 DEG C/min
Heating rate be warming up to 1300 ± 10 DEG C be sintered 2 hours, ceramic disks, that is, barium phthalate base high performance piezoelectric ceramics material of firing
Expect (BaTiO3-xCuSO4-yLi2CO3, x=0.13, y=0.02).
Ceramic disks obtained by the present embodiment are tested by surface polishing, measure its breakdown strength, dielectric constant, body
Product density, piezoelectric constant, mechanical quality factor and electromechanical coupling factor, the data obtained are shown in Table 3.
Table 3
Barium phthalate base high performance piezoelectric ceramic material piezoelectric constant prepared by the present embodiment is illustrated in figure 4 with sintering temperature
Spend the characteristic curve of variation, it can be seen that the piezoelectric constant of the sample is much higher than the piezoelectric constant of pure BT material.
Comparative example 1
The test that potsherd made from barium titanate ceramics of the partial size for 200nm is carried out to piezoelectric property, implements with the present invention
The sample that example 1-3 processed is obtained carries out performance comparison, it is specific the preparation method is as follows:
Taking 15g partial size is the barium titanate of 200nm, and binder (PVA solution that mass concentration is 5%) is added thereto and makes
Grain, be sieved with the sieve of 100 mesh, pressure maintaining 30s positive pressure forming obtains diameter under 200MPa pressure is 12mm, with a thickness of
Disk is risen at 600 DEG C with the heating rate of 2 DEG C/min in air atmosphere and is kept the temperature at 2h progress dumping by the disk of 0.8mm
Sample after molding, is then placed on the corundum plate of laying titanium dioxide zirconium powder, starts to warm up in air atmosphere from room temperature by reason,
1000 DEG C are warming up to the heating rate of 5 DEG C/min, 1360 ± 10 DEG C of sintering 2 are then warming up to the heating rate of 2 DEG C/min
Hour, sample obtained by ceramic disks, that is, comparative example of firing.
Ceramic disks obtained by this comparative example are tested by surface polishing, measure its breakdown strength, dielectric constant, body
Product density, piezoelectric constant, mechanical quality factor and electromechanical coupling factor, the data obtained are shown in Table 4.
Table 4
Claims (10)
1. a kind of barium phthalate base high performance piezoelectric ceramic material, which is characterized in that its chemical structural formula is BaTiO3-xCuSO4-
yLi2CO3, x=0.005~0.13, y=0.005~0.02, which is 1250~1300 DEG C, pressure
Electric constant is 240~300pC/N, and mechanical quality factor is 130~150, and electromechanical coupling factor is 0.25~0.3, crystallite dimension
It is 0.5~1 μm, bulk density is 5.6~5.95g/cm3。
2. a kind of preparation method of barium phthalate base high performance piezoelectric ceramic material described in claim 1, which is characterized in that specific
Steps are as follows:
1) raw material is weighed in materials chemistry formula ratio, it is spare；
2) it prepares barium titanate suspension: barium titanate being mixed with dehydrated alcohol, acetic acid aqueous solution, gained mixed liquor is at 30~60 DEG C
30~60min of lower stirring, subsequent ultrasonic disperse obtain barium titanate suspension；
3) it prepares copper sulphate-Lithium carbonate solution: copper sulphate, lithium carbonate being added to the in the mixed solvent of ethyl alcohol and deionized water, matched
Copper sulphate-Lithium carbonate solution is made；
4) copper sulphate obtained by step 3)-Lithium carbonate solution is added in barium titanate suspension obtained by step 2), by gained mixed liquor
30~60min of stirring in water bath at 30~60 DEG C, subsequent ultrasonic disperse is uniform, adjusts pH value to 6~8, then normal with ammonium hydroxide
Lower 2~the 4h of stirring in water bath of temperature is then aged 12~for 24 hours and is dried to obtain the BaTiO by surface modification3Powder；
5) by the BaTiO obtained by step 4) Jing Guo surface modification3Powder pre-burning in air atmosphere is added binder after cooling and makes
Grain, sieving, positive pressure forming, then dumping processing is carried out, then sample after molding is sintered to get barium phthalate base high-performance pressure is arrived
Electroceramics material.
3. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
2) the barium titanate partial size is 100~200nm；Step 2) the barium titanate and dehydrated alcohol, acetic acid aqueous solution mass volume ratio
For 15g:50~100mL:3~5mL, the acetic acid aqueous solution concentration is 15~20mol/L.
4. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
3) copper sulphate purity >=99%, lithium carbonate purity >=99%.
5. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
3) volume ratio of the in the mixed solvent ethyl alcohol and deionized water of the ethyl alcohol and deionized water is 1~2:1；Step 3) the sulfuric acid
Concentration of copper sulfate is 0.0005~0.1g/mL in copper-Lithium carbonate solution, and lithium carbonate concentration is 0.0005~0.1g/mL.
6. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
4) drying temperature be 100~150 DEG C, drying time be 18~for 24 hours.
7. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
5) calcined temperature is 500~700 DEG C, and burn-in time is 2~4h；Step 5) the binder is that the PVA that mass concentration is 5% is molten
Liquid.
8. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
5) the positive pressure forming condition are as follows: push 30~60s in the positive pressure of 200~300Mpa.
9. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
5) the dumping treatment process condition are as follows: under air atmosphere, start to warm up from room temperature, be warming up to the heating rate of 2 DEG C/min
600~650 DEG C keep the temperature 2~4 hours.
10. the preparation method of barium phthalate base high performance piezoelectric ceramic material according to claim 1, which is characterized in that step
Rapid 5) the described sintering process conditions are as follows: under air atmosphere, start to warm up from room temperature, be warming up to the heating rate of 3~5 DEG C/min
900~1000 DEG C, 1250~1300 DEG C then are warming up to the heating rate of 2~3 DEG C/min and keeps the temperature 2~4 hours.
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Application publication date: 20190531 |