CN109841793A - A kind of positive pole plate of lithium-sulfur cell and preparation method thereof - Google Patents
A kind of positive pole plate of lithium-sulfur cell and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of positive pole plate of lithium-sulfur cell and preparation method thereof, it is intended to reduce the shuttle effect in lithium-sulfur cell charge and discharge process, while improve energy density and charge-discharge performance under positive pole plate of lithium-sulfur cell high load.The positive pole plate of lithium-sulfur cell includes positive active material, the first conductive agent, first binder, additive and composite substrate, used C/WS2- TCF/S structure has flexibility and porosity, has good self-supporting ability and electric conductivity, can remove the use of metal collector to have more volume to change space, to make guarantee to the superperformance under high load.
Description
Technical field
The present invention relates to battery technology field, in particular to a kind of positive pole plate of lithium-sulfur cell and preparation method thereof.
Background technique
In today that science and technology continues to develop, portable electronic device has incorporated the every aspect of people's life, production, because
The importance of this its power supply is also self-evident.Lithium ion battery as the power supply type for being widely used in portable electronic device,
Have many advantages, such as that high capacity, cycle performance are preferable.It is enriched as the functionality of electronic equipment is more next, nowadays the appearance of battery
Amount, energy density and cycle performance are also difficult to meet growing requirement gradually.
Lithium-sulfur cell is a kind of lithium battery of the lithium metal as cathode using element sulphur as anode.Sulfenyl material because
To be much higher than cobalt acid lithium used in current mainstream battery manufacturer etc. with very high theoretical lithium storage content (1675mAh/g)
Lithium ion battery, while there are the advantages such as environmental-friendly, cost is relatively low, therefore sulfenyl material becomes the heat of lithium ion battery instantly
Door research direction.
Although lithium-sulfur cell has many advantages, such as, sulfenyl material can bring huge volume during embedding lithium takes off lithium
Variation, seriously affects the cycle performance of battery.There are many researchers at present overcomes this defect with different means, including with more
Kind of carbon main body material dipping sulphur, using porous hollow carbon, sulphur-carbon nanotube, graphene, metal oxide framework and hydrophilic viscous
Mixture etc..Although these methods based on carbon help to limit sulphur and reduce polysulfide shuttle effect, above method is set
Meter is complicated, and its cycle life and sulphur load limit the energy density of battery.Polysulfide Li2SxIt is a kind of lithium-sulfur cell
Generated reactant in middle sulphur anode charge and discharge cycles can cause shuttle effects battery performance.
Therefore, how overcome sulfenyl material embedding lithium take off lithium during bring enormousness change, optimize it and follow
Ring performance, while the adverse effect of above method being avoided to become research emphasis.
Summary of the invention
The invention proposes a kind of positive pole plate of lithium-sulfur cell, it is intended to reduce the shuttle effect in lithium-sulfur cell charge and discharge process
It answers, while improving energy density and charge-discharge performance under positive pole plate of lithium-sulfur cell high load, the anode pole piece packet
Include positive active material, the first conductive agent, first binder and composite substrate, wherein the composite substrate is netted bandage warp
Immersion conducting solution is crossed to obtain.
By adopting the above technical scheme, the conducting solution contains the second conductive agent, additive and the second binder.
Using above-mentioned each technical solution, the positive active material and first conductive agent and the first binder
Mass ratio be 7~8:1~1.5:1~1.5；Also, second conductive agent and the additive and second binder
Mass ratio be 3~4.5:3~4.5:1~4.
Using above-mentioned each technical solution, first conductive agent and second conductive agent are respectively conductive black, or
Person is respectively one or more of Super P, KS-6, carbon nanotube, carbon nano-fiber.Conductive black (Super P) can be assigned
The ability of product conduction or antistatic is given, feature is small partial size, large specific surface area and coarse, clean surface.Conductive agent is main
Effect is to enhance the electronic conductance ability of anode pole piece.
Using above-mentioned each technical solution, the additive is WS2And LiNO3One or more of.Wherein, WS2It can
Effectively inhibit the shuttle effect in battery charge and discharge process, the deposition of polysulfide is reduced, to improve the cycle performance of battery.
WS2, tungsten disulfide (Tungsten disulfide), molecular weight 247.97 is the fine crystalline or powder of fascia cinerea metallic luster
End belongs to hexagonal crystal system, there is semiconductive and diamagnetism, and natural minerals are tungstenite；Layer structure, legibility is from having and graphite
Similar lubricating property, is commonly used for lubricant, is such as used for aerosol.
Using above-mentioned each technical solution, the first binder and the second binder be respectively PVDF (hexafluoropropene),
(Kynoar-hexafluoropropene, appearance are translucent or white powder or particle to PVDF-HFP, and the arrangement of molecule interchain is close, again
There is stronger hydrogen bond, oxygen index (OI) 46% is non-ignitable, crystallinity 65%~78%, 1.77~1.80g/cm of density3, fusing point 172
DEG C, 112~145 DEG C of heat distortion temperature, long-term use temperature be -40~150 DEG C), PTFE (polytetrafluoroethylene (PTFE)), PVA (polyethylene
Alcohol), one or more of PP (polypropylene) and PE (polyethylene).Binder can not only provide cohesive force for anode pole piece,
Thickening power can also be provided for solution.
Using above-mentioned each technical solution, the composite substrate is to impregnate the netted bandage that conducting solution obtains by two panels
(also referred to as distortion measuring fiber, twisted cloth fiber, TCF) is by the two-layer compound substrate of lamination compacting.
Using above-mentioned each technical solution, the positive active material is sublimed sulfur or sulfur-containing compound.Positive electrode active material
Matter main function is to provide capacity for anode pole piece.
Positive pole plate of lithium-sulfur cell of the present invention is that 3D distorts measuring fiber TCF structure, intermediate composite sulfuration tungsten, tungsten sulfide
The shuttle effect in battery charge and discharge process can effectively be inhibited, reduce the deposition of polysulfide, to improve the circulation of battery
Performance.Sulfur granules and carbon particle are deposited on distortion measuring fiber TCF surface and inside, and wherein sulfur granules can significantly improve the anode
The capacity of active material, and the distortion measuring fiber TCF structure for having wrapped up carbon particle can not only increase material as conductive network
Electronic conductance performance, moreover it is possible to provide buffering for the expansion of sulfur granules, further increase the cycle performance of the positive active material.
The invention also provides the preparation methods of above-mentioned positive pole plate of lithium-sulfur cell comprising following steps:
(1) the second conductive agent, additive and the first solvent are uniformly mixed and form solution I, wherein second conductive agent
Mass ratio with the additive is 3~4.5:3~4.5, and the mass percent that first solvent accounts for the solution I is
80%-95%；
(2) the second binder and the second solvent are uniformly mixed and form solution II, and mixed with the solution I in step (1)
Solution III is obtained after uniformly, wherein the mass ratio of second conductive agent and the additive and second binder is 3
~4.5:3~4.5:1~4, the mass percent that second solvent accounts for the solution II is 80%-95%；
(3) the netted bandage is immersed in solution III and is taken out after a period of time, obtain the composite substrate after dry；
(4) positive active material, the first conductive agent, first binder and third solvent are uniformly mixed and form solution IV,
Wherein, the positive active material and first conductive agent and the mass ratio of the first binder are 7~8:1~1.5:1
~1.5, the mass percent that the third solvent accounts for the solution IV is 80%-90%；
(5) solution IV is dispersed in the composite substrate, obtains the positive pole plate of lithium-sulfur cell after dry.
By adopting the above technical scheme, in step (3), the netted bandage with ethyl alcohol and is gone before immersing solution III
Ionized water cleaning, and dried 2~3 hours in 80 DEG C of normal pressures；The time that the netted bandage immerses in solution III is 2~3 small
When；The drying is that 80 DEG C of normal pressures are dried 12~14 hours.
Using above-mentioned each technical solution, in step (3), the netted bandage is immersed into a period of time in solution III
After taking out afterwards, it is compacted with slitter cut-parts, and by the tablet press machine of 2 netted layer of the bandage poststacks about 1MPa pressure；And
The composite substrate is obtained after 60 DEG C of vacuum dryings are 12~14 hours dry.
Using above-mentioned each technical solution, first solvent, the second solvent, third solvent are respectively DMAC (N, N- bis-
Methylacetamide), DMF (dimethylformamide), one or more of NMP (N-Methyl pyrrolidone) and acetone.
Using above-mentioned each technical solution, the mixing temperature in step (1)~(5) is 20~40 DEG C.
The preparation method simple process of positive pole plate of lithium-sulfur cell provided by the invention, it is easy to implement, be conducive to improve life
It produces efficiency and saves production cost, and better than battery prepared by traditional positive pole plate of lithium-sulfur cell technique in comprehensive performance.
Compared with prior art, the beneficial effects of the present invention are:
First, it is added to WS2Additive reduces the shuttle effect of polysulfide in charge and discharge process, is guaranteeing battery
The cycle performance that battery is improved while high-energy density meets requirement of the 3C electronic product for lithium battery high capacity；
Second, used distortion measuring fiber TCF structure can play support battery simultaneously and accommodate positive active material
Effect, match with sulphur anode, hollow structure allow sulphur anode in charge and discharge process biggish volume expansion without destruction
Its structure, to improve the cyclical stability of battery.
Third, unique C/WS2Aluminum collector used in-TCF/S composite construction abandoning tradition battery, it is porous
Measuring fiber structure can carry enough conductive agents and guarantee its electric conductivity, while the characteristic that can be distorted keeps the mechanical performance of anode big
Width improves, and also further increases anode to the adaptability of volume expansion in charge and discharge process.
4th, it, can will be positive within the shorter time by using above-described method for mixing and preparation process
Solution mixes, and reduces production cost using cheap distortion measuring fiber TCF, greatly improves production efficiency, be prepared into
To positive pole plate of lithium-sulfur cell there is relatively high battery performance simultaneously.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
The structure shown according to these attached drawings obtains other attached drawings.
Fig. 1 is Al/S, Al-C/WS2- TCF/S and C/WS2The performance figure of-TCF/S anode under different loads；
Fig. 2 is C/WS2The performance figure of-TCF/S anode under different loads；
Fig. 3-a is discharge curve of the Al/S anode at 0.05C；
Fig. 3-b is the Raman spectrogram of Al/S anode；
Fig. 3-c is C/WS2Discharge curve of-TCF/S the anode at 0.05C；
Fig. 3-d is C/WS2The Raman spectrogram of-TCF/S anode.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
Embodiment 1
In the present embodiment, the preparation method of the positive pole plate of lithium-sulfur cell the following steps are included:
(1) by the second conductive agent Super P and additive WS2Stirring 2 hours in DMAC (DMAC N,N' dimethyl acetamide)
Form solution I, wherein Super P and WS2Mass ratio be 4.5:4.5, DMAC account for solution I mass fraction be 80%；
(2) will form solution II after the second binder PVDF-HFP and DMAC stirring solvent 2 hours, and by solution II with it is molten
It is spare that liquid I is mixed to form solution III, wherein Super P and WS2Mass ratio with PVDF-HFP is 4.5:4.5:1, and DMAC is accounted for
The mass percent of the solution II is 80%；
(3) netted bandage ethyl alcohol and deionized water are cleaned and is immersed after 80 DEG C of normal pressures dry drying in 2~3 hours and walked
Suddenly in (2) acquired solution III (i.e. conducting solution), then ultrasound 2 hours dries 12 hours under 80 DEG C of normal pressures, obtains C/
WS2- TCF composite substrate；By C/WS2- TCF composite substrate is cut into several round pole pieces with the slitter of aperture 14mm x 14mm,
Two pieces of pole pieces are stacked, is placed in tablet press machine and is combined together under the pressure of about 1MPa, weigh the bilayer obtained through tabletting
Composite substrate；
(4) by positive active material sublimed sulfur, the first conductive agent Super P, first binder PVDF-HFP and solvent
DMAC is stirred 12 hours formation solution IVs (i.e. positive solution), wherein the quality of sublimed sulfur and Super P and PVDF-HFP
Mass percent than accounting for the solution IV for 8:1:1, DMAC is 80%；
(5) it takes 5mL drop in two-layer compound substrate with liquid-transfering gun the solution IV in step (4), is dried in vacuo in 60 DEG C
12 hours, obtain C/WS2- TCF/S anode composite pole piece, i.e., positive pole plate of lithium-sulfur cell of the present invention.
In above steps, temperature when being stirred is controlled at 20 DEG C.
Embodiment 2
In the present embodiment, the preparation method of the positive pole plate of lithium-sulfur cell the following steps are included:
(1) by the second conductive agent KS-6 and additive WS2It is formed within stirring 2 hours in DMAC (DMAC N,N' dimethyl acetamide)
Solution I, wherein KS-6 and WS2Mass ratio be 3.5:3.5, DMAC account for solution I mass fraction be 90%；
(2) solution II will be formed after the second binder PVDF and DMAC stirring solvent 2 hours, and by solution II and solution I
It is spare to be mixed to form solution III (i.e. conducting solution), wherein KS-6 and WS2Mass ratio with PVDF is 3.5:3.5:3, DMAC
The mass percent for accounting for the solution II is 90%；
(3) netted bandage ethyl alcohol and deionized water are cleaned and is immersed after 80 DEG C of normal pressures dry drying in 2~3 hours and walked
Suddenly in (2) acquired solution III, then ultrasound 2 hours dries 12 hours under 80 DEG C of normal pressures, obtains C/WS2- TCF composite base
Bottom；By C/WS2- TCF composite substrate is cut into several round pole pieces with the slitter of aperture 14mm x 14mm, and two pieces of pole pieces are folded
Together, it is placed in tablet press machine and is combined together under the pressure of about 1MPa, weigh the two-layer compound substrate obtained through tabletting；
(4) by positive active material sublimed sulfur, the first conductive agent Super P, first binder PVDF-HFP and solvent
DMAC is stirred 12 hours formation solution IVs (i.e. positive solution), wherein the quality of sublimed sulfur and Super P and PVDF-HFP
Mass percent than accounting for the solution IV for 7:1.5:1.5, DMAC is 83%；
(5) it takes 5mL drop in two-layer compound substrate with liquid-transfering gun the solution IV in step (4), is dried in vacuo in 60 DEG C
12 hours, obtain C/WS2- TCF/S anode composite pole piece, i.e., positive pole plate of lithium-sulfur cell of the present invention.
In above steps, temperature when being stirred is controlled at 30 DEG C.
Embodiment 3
In the present embodiment, the preparation method of the positive pole plate of lithium-sulfur cell the following steps are included:
(1) by the second conductive agent Super P and additive WS2Stirring 2 hours in DMAC (DMAC N,N' dimethyl acetamide)
Form solution I, wherein Super P and WS2Mass ratio be 3:3, DMAC account for solution I mass fraction be 95%；
(2) will form solution II after the second binder PVDF-HFP and DMAC stirring solvent 2 hours, and by solution II with it is molten
It is spare that liquid I is mixed to form solution III (i.e. conducting solution), wherein Super P and WS2Mass ratio with PVDF-HFP is 3:3:
4, the DMAC mass percents for accounting for the solution II are 95%；
(3) netted bandage ethyl alcohol and deionized water are cleaned and is immersed after 80 DEG C of normal pressures dry drying in 2~3 hours and walked
Suddenly in (2) acquired solution III, then ultrasound 2 hours dries 12 hours under 80 DEG C of normal pressures, obtains C/WS2- TCF composite base
Bottom；By C/WS2- TCF composite substrate is cut into several round pole pieces with the slitter of aperture 14mm x 14mm, and two pieces of pole pieces are folded
Together, it is placed in tablet press machine and is combined together under the pressure of about 1MPa, weigh the two-layer compound substrate obtained through tabletting；
(4) positive active material sublimed sulfur, the first conductive agent carbon nanotube, first binder PTFE and solvent DMAC are stirred
Mix 12 hours formation solution IVs (i.e. positive solution) of mixing, wherein the mass ratio of sublimed sulfur and carbon nanotube and PTFE are 7.5:
The mass percent that 1.3:1.2, DMAC account for the solution IV is 90%；
(5) it takes 5mL drop in two-layer compound substrate with liquid-transfering gun the solution IV in step (4), is dried in vacuo in 60 DEG C
12 hours, obtain C/WS2- TCF/S anode composite pole piece, i.e., positive pole plate of lithium-sulfur cell of the present invention.
In above steps, temperature when being stirred is controlled at 40 DEG C.
Examples 1 to 3 proves, each component mass percent carries out conjunction slurry respectively with aforementioned proportion, the slurry prepared
With optimal stability and uniformity, the positive pole plate of lithium-sulfur cell further prepared has optimal caking property, leads
Electrical property and energy density, the lithium-sulfur cell finally prepared have optimal capacity and cycle performance.
Embodiment 4
The present embodiment is the performance test of common positive pole plate of lithium-sulfur cell and positive pole plate of lithium-sulfur cell of the present invention
Experiment.
Al/S is common lithium-sulfur cell, just extremely sulphur anode, is usually applied to cut-parts on aluminium foil, when assembled battery can sulphur just
It extremely installs Al collector additional afterwards and plays afflux, supporting role；Al-C/WS2- TCF/S is to be had using prepared by the method for the invention
3D distorts the composite sulfur anode of measuring fiber TCF structure, and installs the lithium-sulfur cell that Al matter collector is assembled additional；C/WS2-TCF/S
To only use the lithium-sulfur cell that the composite sulfur anode of the method for the invention preparation is assembled.Three groups of batteries are tested in 2mgcm-2,3.5mg·cm-2And 5mgcm-2Performance under different loads, test result are as depicted in figs. 1 and 2.
Fig. 1 shows Al/S, Al-C/WS under 1C multiplying power2- TCF/S and C/WS2The discharge capacity and coulomb of-TCF/S anode
Than Fig. 2 shows C/WS under 1C multiplying power2The performance of-TCF/S anode under different loads.C indicates battery charging and discharging ability
Current strength when multiplying power, 1C indicate to discharge completely for battery one hour.As shown in Figure 1, C/WS2- TCF/S composite sulfur anode is opposite
(4.5mgcm under higher load-2) show than Al/S, Al-C/WS2- TCF/S organizes (2mgcm under a low load-2) higher
Discharge capacity and more stable cycle performance.As shown in Figure 2, sulphur load is 2mgcm-2、3.5mg·cm-2And 5mgcm-2
Have C/WS of the present invention2The sulphur anode of-TCF/S structure recycles 400 circles under the multiplying power of 1C can respectively reach 751mA
h·g-1、444mA·h·g-1And 340mAhg-1Discharge capacity, capacity can retain 73%, 58% and 54% respectively.
Embodiment 5
In order to study the shuttle effect of polysulfide, using in-situ Raman spectrum analysis polysulfide in discharge cycles mistake
The formation of long-chain and short chain in journey, as shown in Fig. 3-a, Fig. 3-b, Fig. 3-c and Fig. 3-d.The Raman of long-chain and short-chain polysulphides
Spectrum peak is highlighted in specific peak position.Fig. 3-a is discharge process of the Al/S anode under different voltages, and Fig. 3-b is Al/S
Anode Raman shift image corresponding to discharge process under different voltages.Fig. 3-c is C/WS2- TCF/S anode is in different voltages
Under discharge process, Fig. 3-d be C/WS2- TCF/S anode Raman shift image corresponding to discharge process under different voltages.
When first region of discharge process starts, there are three feature peak intensity (155cm in 2.38V-1、219cm-1And 478cm-1), this is because long-chain polysulphides Li2S8 15Generation.When discharge process enters Two Areas, S8 2-Ion peak intensity drop
Low, more peaks start to occur, and the range of peak position is from 398cm-1To 420cm–1, correspond to middle chain polysulfide (Li2S6With
Li2S4), peak value 440cm-1-480cm–1Correspond to short-chain polysulphides.Al/S anode Raman peaks are shown in entire discharge process
Serious shuttle effect out.However, C/WS2Raman signal peak strength is smaller during-TCF/S positive discharge, such as Fig. 3-c and
Shown in Fig. 3-d.In entire discharge process, C/WS2- TCF/S anode inhibits the generation of polysulfide type, maintains lithium sulphur
The higher specific capacity of battery.
As seen from the above embodiment, the composite sulfur with 3D distortion measuring fiber TCF structure of the method for the invention preparation
Anode has good cyclical stability while capable of reaching higher discharge capacity, and cost is relatively low, preparation process letter
It is single, can be applied among various portable electronic equipments as the energy, such as mobile phone, laptop, video camera,
Unmanned plane etc..In addition, the development of new-energy automobile is extremely rapid, the present invention is also the power battery of electronic, mixed electrical automobile
Extensive manufacture provides possibility.
The above is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (10)
1. a kind of positive pole plate of lithium-sulfur cell characterized by comprising positive active material, the first conductive agent, first binder
And composite substrate, wherein the composite substrate is that netted bandage is obtained by impregnating conducting solution.
2. positive pole plate of lithium-sulfur cell according to claim 1, which is characterized in that the conducting solution contains the second conduction
Agent, additive and the second binder, also, the additive is WS2And LiNO3In any one or two kinds.
3. positive pole plate of lithium-sulfur cell according to claim 2, which is characterized in that the positive active material and described the
One conductive agent and the mass ratio of the first binder are 7~8:1~1.5:1~1.5；Also, second conductive agent and institute
The mass ratio for stating additive and second binder is 3~4.5:3~4.5:1~4.
4. positive pole plate of lithium-sulfur cell according to claim 2, which is characterized in that first conductive agent and described second
Conductive agent is respectively conductive black, or one of respectively Super P, KS-6, carbon nanotube, carbon nano-fiber or several
Kind；Also, the first binder and second binder are respectively in PVDF, PVDF-HFP, PTFE, PVA, PP and PE
It is one or more of.
5. positive pole plate of lithium-sulfur cell according to claim 1, which is characterized in that the composite substrate is to be impregnated by two panels
The netted bandage that conducting solution obtains passes through the two-layer compound substrate of lamination compacting.
6. positive pole plate of lithium-sulfur cell as described in claim 1, which is characterized in that the positive active material be sublimed sulfur or
Sulfur-containing compound.
7. a kind of preparation method of any one of claim 1-6 positive pole plate of lithium-sulfur cell, which is characterized in that the preparation
Method the following steps are included:
(1) the second conductive agent, additive and the first solvent are uniformly mixed and form solution I, wherein second conductive agent and institute
The mass ratio for stating additive is 3~4.5:3~4.5, and the mass percent that first solvent accounts for the solution I is 80%-
95%；
(2) the second binder and the second solvent are uniformly mixed and form solution II, and be uniformly mixed with the solution I in step (1)
After obtain solution III, wherein the mass ratio of second conductive agent and the additive and second binder is 3~
4.5:3~4.5:1~4, the mass percent that second solvent accounts for the solution II is 80%-95%；
(3) the netted bandage is immersed in solution III and is taken out after a period of time, obtain the composite substrate after dry；
(4) positive active material, the first conductive agent, first binder and third solvent are uniformly mixed and form solution IV, wherein
The positive active material and first conductive agent and the mass ratio of the first binder are 7~8:1~1.5:1~1.5,
The mass percent that the third solvent accounts for the solution IV is 80%-90%；
(5) solution IV is dispersed in the composite substrate, obtains the positive pole plate of lithium-sulfur cell after dry.
8. preparation method as claimed in claim 7, which is characterized in that in step (3), the netted bandage is immersing solution
It is cleaned before III with ethyl alcohol and deionized water, and is dried 2~3 hours in 80 DEG C of normal pressures；The netted bandage immerses solution III
In time be 2~3 hours；The drying is that 80 DEG C of normal pressures are dried 12~14 hours.
9. preparation method as claimed in claim 7, which is characterized in that in step (3), the netted bandage is immersed solution
After being taken out for a period of time in III, with slitter cut-parts, and by the tabletting of the 2 netted layer of the bandage poststack about 1MPa pressure
Machine compacting；And the composite substrate is obtained after 60 DEG C of vacuum dryings are 12~14 hours dry.
10. preparation method as claimed in claim 7, which is characterized in that first solvent, second solvent, described
Three solvents are respectively one or more of DMAC, DMF, NMP and acetone；Alternatively, the mixing temperature in step (1)~(5) is
20~40 DEG C.
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