CN102637532B - Nanocable-containing DSC (dye-sensitized solar cell) photo-anode and preparation method thereof - Google Patents

Nanocable-containing DSC (dye-sensitized solar cell) photo-anode and preparation method thereof Download PDF

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CN102637532B
CN102637532B CN201210118099.6A CN201210118099A CN102637532B CN 102637532 B CN102637532 B CN 102637532B CN 201210118099 A CN201210118099 A CN 201210118099A CN 102637532 B CN102637532 B CN 102637532B
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nano
cable
dye
sensitized solar
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CN102637532A (en
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李燕
曾京辉
王晔峰
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Shaanxi Normal University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/542—Dye sensitized solar cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention belongs to the technical field of solar cells, and particularly relates to a nanocable-containing DSC (dye-sensitized solar cell) photo-anode (in which metals are introduced into a TiO2 nanorod array) and a preparation method thereof. The nanocable-containing DSC photo-anode comprises fluorine-doped tin oxide glass and a TiO2 nanoparticle layer adhered to the surface of the fluorine-doped tin oxide glass, and the TiO2 nanoparticle layer contains an Ag/TiO2 nano cable. The photo-anode disclosed by the invention is high in electron transmission rate, and can not reduce the dye adsorption capacity while more effectively transferring electrons to an external circuit, thereby greatly improving the photoelectric conversion efficiency; and the preparation method disclosed by the invention is simple in operation, low in cost and less in by-products.

Description

Dye-sensitized solar cells light anode that contains nano-cable and preparation method thereof
Technical field
The invention belongs to technical field of solar cells, be specifically related to one metal is introduced to TiO 2dye-sensitized solar cells light anode of nanometer stick array and preparation method thereof.
Background technology
Dye-sensitized solar cells is as a kind of novel low-carbon environment-friendly device, obtained more and more researchers' attention in the field of tapping a new source of energy, light anode is the core component of whole battery, be responsible for the important function of catching photon, generation electronics, injecting electronics, transmission electronic, directly affected the quality of battery performance.
Concentrate at present one of light anode part very distinct issues be exactly lower electric transmission speed.What traditional light anode used is to receive brilliant membrana granulosa, although the brilliant membrana granulosa of receiving has very large specific area can increase the adsorbance of dyestuff, but crystal boundary number is numerous in membrana granulosa, between particle and particle, very easily form unformed layer in high-temperature calcination process, and the residing chemical environment difference of each particle, makes it not provide effectively directly passage for the transmission of electronics.On this basis, also forming array films by people by titanium dioxide nano thread, nanometer rods, nanotube etc. improves conventional particles film, although utilize array films to provide direct path for the transmission of electronics, but because the specific area of array films is little, this just causes the dye load amount of array films few, the photogenerated charge total amount producing under illumination is so just few, and therefore the speed of transmission electronic is just greatly limited.
Summary of the invention
In order to solve the existing deficiency of light anode of dye-sensitized solar cells of the prior art, the invention provides the dye-sensitized solar cells light anode that a kind of electric transmission speed is higher, Dye Adsorption amount is many.
Meanwhile, another technical problem that the present invention solves has been to provide a kind of preparation method of the dye-sensitized solar cells light anode that contains nano-cable that can effectively accelerate electric transmission speed.
Solving the problems of the technologies described above adopted technical scheme is: the nano-TiO that it comprises fluorine doped tin oxide glass and is attached to fluorine doped tin oxide glass surface 2stratum granulosum, nano-TiO 2in stratum granulosum, include Ag/TiO 2nano-cable.
Above-mentioned Ag/TiO 2the diameter of nano-cable is 150～200nm, and length is 3～8 μ m.
Above-mentioned Ag/TiO 2nano-cable accounts for nano-TiO 2the mass percent of stratum granulosum is 0.5%～20%.
Above-mentioned Ag/TiO 2nano-cable accounts for nano-TiO 2the mass percent of stratum granulosum is 1～5%.
Above-mentioned Ag/TiO 2one end of nano-cable connects with fluorine doped tin oxide glass.
Above-mentioned Ag/TiO 2nano-cable is at nano-TiO 2in stratum granulosum, being nano-array distributes.
The preparation method of the above-mentioned dye-sensitized solar cells light anode that contains nano-cable, comprises following steps:
1) synthetic Ag/TiO 2nano-cable
After being mixed, silver nitrate, ethylene glycol adds metatitanic acid fourth fat, the mass ratio of silver nitrate, ethylene glycol and metatitanic acid fourth fat is 0.5～1: 79: 2～4, after fully stirring under lucifuge condition, transfer in the high-temperature high-pressure reaction kettle that polytetrafluoroethylene is liner, 245 DEG C are incubated 14 hours, be cooled to room temperature, by the product obtaining, through distilled water washing, ethanol washs, at the baking oven inner drying of 80 DEG C, obtain Ag/TiO 2nano-cable;
2) the dye-sensitized solar cells light anode that preparation contains nano-cable
Take Ag/TiO 2nano-cable and ground TiO 2powder mixes, and adds distilled water, Ag/TiO 2nano-cable and TiO 2the mass ratio of powder is 0.5～20: 100, Ag/TiO 2nano-cable and TiO 2the solid content of powder is 0.4%, through magnetic agitation, ultrasonic dispersion, concentrated, forms Ag/TiO 2nano-cable and TiO 2the solid content of powder is 13% slurry, the film that is 8～12 μ m by slurry blade coating at fluorine doped tin oxide formation thickness on glass with blade, after film is naturally dried in air, be placed in intensification Muffle furnace and be incubated 30～50 minutes at 450～500 DEG C, be down to room temperature with stove, must contain the dye-sensitized solar cells light anode of nano-cable.
Above-mentioned steps 2) in, in the slurry forming, add polyethylene glycol, polyethylene glycol and TiO 2the mass ratio of powder is 3～4: 10.
Above-mentioned steps 1) middle Ag/TiO 2nano-cable and TiO 2the mass ratio of powder is 1～5: 100.
It is raw material that the present invention utilizes ethylene glycol, silver nitrate and metatitanic acid fourth fat, adopts hydro thermal method at TiO 2the TiO of stratum granulosum 2in array, introduce galactic nucleus, synthetic coaxial galactic nucleus titanium dioxide shell nano cable structure, and utilize TiO 2nano particle is by synthetic Ag/TiO 2nano-cable props up in photo-anode film, forms an electron propagation ducts fast, when can more effectively electronics being delivered to external circuit, do not reduce the adsorbance of dyestuff, greatly improved photoelectric conversion efficiency, preparation method of the present invention is simple to operate, with low cost, accessory substance is few.
Brief description of the drawings
Fig. 1 is the structural representation of the dye-sensitized solar cells light anode that contains nano-cable of embodiment 1.
Fig. 2 is that smooth anode of the present invention becomes the I-V curve chart with a series of battery with smooth anode assembling of the prior art.
Fig. 3 becomes the absorption curve figure of the dyestuff adsorbing with a series of battery to light for smooth anode of the present invention with smooth anode assembling of the prior art.
Fig. 4 is that smooth anode of the present invention becomes the electrochemical impedance test curve figure with a series of battery with smooth anode assembling of the prior art.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the invention is not restricted to these embodiment.
Embodiment 1
Referring to Fig. 1, the dye-sensitized solar cells light anode that contains nano-cable of the present embodiment is by fluorine tin oxide glass 3, nano-TiO 2stratum granulosum 2 forms, nano-TiO 2stratum granulosum 2 is attached on fluorine tin oxide glass 3, at nano-TiO 2in stratum granulosum 2, be embedded with mass percent and be 1% Ag/TiO 2nano-cable 1, Ag/TiO 2the diameter of nano-cable 1 is 175nm, and length is 5 μ m, Ag/TiO 2nano-cable 1 is at nano-TiO 2stratum granulosum 2 is nano-array distribution with the side that fluorine doped tin oxide glass 3 closes on, and Ag/TiO 2one end of nano-cable 1 connects with fluorine doped tin oxide glass 3.
The preparation method of the above-mentioned dye-sensitized solar cells light anode that contains nano-cable is made up of following steps:
Step 1: synthetic Ag/TiO 2nano-cable
Weigh the silver nitrate of 0.127g, measuring concentration is the 12ml ethylene glycol of 1.115g/ml, stir by magnetic stirring apparatus lucifuge, measuring concentration is the butyl titanate solution 0.34ml of 0.997g/ml, the mass ratio of silver nitrate, ethylene glycol and butyl titanate is 0.75: 79: 2, in whipping process, be added drop-wise in the mixed liquor of silver nitrate and ethylene glycol, continue to stir 2 hours, the solution after having stirred is transparent micro-yellow state; Above-mentioned solution is transferred in the high-temperature high-pressure polytetrafluoroethylwelding liner of 45ml, 245 DEG C are incubated 14 hours, obtain after cooling khaki sediment; To in sediment, add distilled water to carry out centrifugation, rotating speed 4500r/min, remove after supernatant liquor adding distil water again, sample after disperseing is precipitated through centrifuge, cyclic washing 4 times, with ethanolic solution supersound washing 1 time, ensures that the organic substance such as acid and alcohols producing in ethylene glycol excessive in reactant and course of reaction is removed, finally the khaki sample of acquisition is placed in the baking oven of 80 DEG C dryly, obtains Ag/TiO 2nano-cable.
Step 2: preparation contains Ag/TiO 2the dye-sensitized solar cells light anode of nano-cable
Weigh the TiO of 1.5g 2powder, is put in agate mortar powder is ground, and adds the Ag/TiO of 0.015g 2nano-cable; TiO 2powder and Ag/TiO 2nano-cable mass ratio is 100: 1, measures 378.75ml distilled water, mixes and makes liquid be suspension; By the suspension preparing stir process after ultrasonic dispersion, use Rotary Evaporators concentration to volume for 11.65ml be good, i.e. Ag/TiO 2nano-cable and TiO 2the solid content of powder is 13% slurry, with khaki, and sealed storage; After taking out a small pieces fluorine doped tin oxide glass and drying, use 3M adhesive tape, standard 50 μ m thickness cross the square that an effective area is 1.0cm × 1.0cm size on fluorine doped tin oxide glass, use blade by the slurry blade coating of preparation in the above, forming thickness is the film of 10 μ m, naturally after drying, can observe slightly gloss of film, the film after drying is put in Muffle furnace and at 450 DEG C, calcined 50 minutes, be down to room temperature with stove, obtain containing Ag/TiO 2the dye-sensitized solar cells light anode of nano-cable.
Embodiment 2
Ag/TiO in the dye-sensitized solar cells light anode that contains nano-cable of the present embodiment 2nano-cable 1 accounts for nano-TiO 2the mass percent of stratum granulosum 2 is 5%, Ag/TiO 2the diameter of nano-cable 1 is 150nm, and length is 3 μ m.
The preparation method of the above-mentioned dye-sensitized solar cells light anode that contains nano-cable is made up of following steps:
In step 2, weigh the TiO of 1.5g 2powder, is put in agate mortar powder mortar, adds the Ag/TiO of 0.075g 2nano-cable; TiO 2powder and Ag/TiO 2nano-cable mass ratio is 100: 5, add distilled water, through magnetic agitation, ultrasonic dispersion, concentrated, with blade by slurry blade coating at fluorine doped tin oxide formation film on glass, after film is naturally dried in air, be placed in intensification Muffle furnace and be incubated 30 minutes at 500 DEG C, be down to room temperature with stove, in this step, other step is identical with embodiment 1.
Other step is identical with embodiment 1.
Embodiment 3
Ag/TiO in the dye-sensitized solar cells light anode that contains nano-cable of the present embodiment 2nano-cable 1 accounts for nano-TiO 2the mass percent of stratum granulosum 2 is 0.5%, Ag/TiO 2the diameter of nano-cable 1 is 200nm, and length is 8 μ m.
The preparation method of the above-mentioned dye-sensitized solar cells light anode that contains nano-cable is made up of following steps:
In step 2, weigh the TiO of 1.5g 2powder, is put in agate mortar powder mortar, adds the Ag/TiO of 0.0075g 2nano-cable; TiO 2powder and Ag/TiO 2nano-cable mass ratio is 100: 0.5, and in this step, other step is identical with embodiment 1.
Other step is identical with embodiment 1.
Embodiment 4
Ag/TiO in the dye-sensitized solar cells light anode that contains nano-cable of the present embodiment 2nano-cable 1 accounts for nano-TiO 2the mass percent of stratum granulosum 2 is 20%, Ag/TiO 2the diameter of nano-cable 1 is 200nm, and length is 6 μ m.
The preparation method of the above-mentioned dye-sensitized solar cells light anode that contains nano-cable is made up of following steps:
In step 2) in weigh the TiO of 1.5g 2powder, is put in agate mortar powder mortar, adds the Ag/TiO of 0.3g 2nano-cable; TiO 2powder and Ag/TiO 2nano-cable mass ratio is 100: 20, and in this step, other step is identical with embodiment 1.
Other step is identical with embodiment 1.
Embodiment 5
In the step 1 of above-described embodiment 1～4, weigh the silver nitrate of 0.17g, measuring concentration is the 12ml ethylene glycol of 1.115g/ml again, after stirring, adding concentration is the butyl titanate solution 0.34ml of 0.997g/ml, the mass ratio of silver nitrate, ethylene glycol and butyl titanate is 1: 79: 2, and in this step, other step is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 6
In the step 1 of above-described embodiment 1～4, weigh the silver nitrate of 0.085g, measuring concentration is the 12ml ethylene glycol of 1.115g/ml again, after stirring, adding concentration is the butyl titanate solution 0.68ml of 0.997g/ml, the mass ratio of silver nitrate, ethylene glycol and butyl titanate is 0.5: 79: 4, and in this step, other step is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 7
In the step 2 of above-described embodiment 1～6, at Ag/TiO 2nano-cable and TiO 2in the suspension of powder, add polyethylene glycol, polyethylene glycol and TiO 2the mass ratio of powder is 3: 10, and after it dissolves, stirred suspension is concentrated into Ag/TiO 2nano-cable and TiO 2the solid content of powder is 13% slurry, and in this step, other step is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 8
In the step 2 of above-described embodiment 1～6, at Ag/TiO 2nano-cable and TiO 2in the suspension of powder, add polyethylene glycol, polyethylene glycol and TiO 2the mass ratio of powder is 4: 10, and after it dissolves, stirred suspension is concentrated into Ag/TiO 2nano-cable and TiO 2the solid content of powder is 13% slurry, and in this step, other step is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 9
In the step 2 of above-described embodiment 1～6, at Ag/TiO 2nano-cable and TiO 2in the suspension of powder, add polyethylene glycol, polyethylene glycol and TiO 2the mass ratio of powder is 3.5: 10, and after it dissolves, stirred suspension is concentrated into Ag/TiO 2nano-cable and TiO 2the solid content of powder is 13% slurry, and in this step, other step is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 10
In the step 2 of above-described embodiment 1～9, the film that is 8 μ m by slurry blade coating at fluorine doped tin oxide formation thickness on glass with blade, in this step, other step is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 11
In the step 2 of above-described embodiment 1～9, the film that is 12 μ m by slurry blade coating at fluorine doped tin oxide formation thickness on glass with blade, in this step, other step is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
In order to prove beneficial effect of the present invention, inventor is by the Ag/TiO that contains of the present invention 2the dye-sensitized solar cells that the dye-sensitized solar cells light anode assembling of nano-cable becomes is tested, specifically by the Ag/TiO that contains of the present invention 2the dye-sensitized solar cells light anode of nano-cable and the Ag/TiO that do not contain of the prior art 2the dye-sensitized solar cells light anode of nano-cable under the same conditions, is assembled into a series of battery and tests, specific as follows:
In experiment, use the ethanolic solution of N719 of 0.3mmol/ml as the sensitizer of light anode, in order to increase the adsorbance of dyestuff, avoid multilayer absorption simultaneously, by the photo-anode film making in baking oven 80 DEG C insulation 1 hour, be immersed in this ethanolic solution 12 hours by lucifuge, sheet glass is pulled out, rinsed well with ethanolic solution, be placed in fume hood dry under air stream.What in experiment, use is platinum electrode.Chloroplatinic acid and isopropyl alcohol are configured to solution by a certain percentage, utilize spray pyrolysis, spray to fluorine doped tin oxide glass FTO with holes upper, put into 380 DEG C of insulations of Muffle furnace 30 minutes, then lower the temperature with stove.Good sensitization light anode and platinum electrode are bonded together by heat-sealing film, are fixed into sandwich structure through hot press, heat-sealing film couples together two work electrodes, also plays the problem that prevents from being filled into electrolyte leakage wherein simultaneously.Finally use capillary that electrolyte is incorporated in packaged battery by the hole at the electrode back side.The packaged respond well nothing of battery request light anode sensitization comes off, and electrolyte filling effect is even, nothing is leaked.The content of electrolyte solution is that the concentration of LiI is 0.5mol/L, I 2concentration be that the concentration of 0.05mol/L, 4-tert .-butylpyridine is 0.3mol/L.
1, adopt PROVA 200 solar cell analyzers (AM1.5100mWcm under mock standard sunlight -2), measure the I-V curve of the above-mentioned dye-sensitized solar cells being assembled into, test result is shown in Fig. 2, and calculates its electricity conversion according to following formula:
FF＝P max/(I sc×V oc)＝(I max×V max)/(I sc×V oc)
η＝P max/P in＝(FF×I sc×V oc)/P in
In formula, Voc is open circuit voltage, and Isc is short circuit current, and Pmax is peak power output, Vmax is optimum operating voltage, and Imax is recommended current, and FF is fill factor, curve factor, Pin is the energy that incides solar cell surface, and η is electricity conversion, and result of calculation is in table 1.
The performance parameter comparison of two kinds of dye-sensitized solar cells light anode assembling batteries of table 1
Figure BDA0000155210360000071
From table 1, the dye-sensitized solar cells that smooth anode assembling of the present invention becomes with do not contain Ag/TiO 2the dye-sensitized solar cells light anode of nano-cable is compared, and its photoelectric conversion efficiency has improved 39.57%.
Light anode prepared by embodiment 1 with do not contain Ag/TiO 2the dye-sensitized solar cells light anode of nano-cable has carried out the test of Dye Adsorption amount.To use the titanium dioxide layer in the light anode that N719 dye sensitization is good to scrape off with blade, putting into total amount is the water of 0.1M and the sodium hydroxide solution of ethanol of 30ml, be wherein 1: 1 as the water of solvent and the volume ratio of ethanol, when room temperature, be immersed in wherein 8 hours.Work as TiO 2powder and Ag/TiO 2after the whole desorbs of dyestuff on nano-cable surface, get a certain amount of remaining solution and transfer to the test of having carried out UV, visible light absorption in cuvette, what in this experiment, use is the U-3900/3900H ultraviolet-uisible spectrophotometer of HIT, and sweep limits is 320～800nm.The result of test as shown in Figure 3.
As shown in Figure 3, preparation method is identical, and the test condition that UV, visible light absorbs is also identical, but the amount of dye that on two class light anodes, desorb is got off is different.The amount of dye that wherein desorb is got off from the light anode that contains nano-cable is little, and its absorption intensity to light is than not containing Ag/TiO 2a little less than the dyestuff that the light anode desorb of nano-cable is got off is wanted the absorption of light.Can infer thus Ag/TiO 2the introducing of nano-cable has increased the electric transmission speed in light anode, and more electronics is directed to external circuit, has further formed and has contained Ag/TiO 2the short circuit current of the battery of nano-cable will be much larger than not containing Ag/TiO 2the short circuit current of nano-cable, has improved photoelectric conversion efficiency.
2, the battery two class light anodes being packaged into has carried out the test of AC impedance, and the instrument of use is the electrochemical workstation CHI660D of Shanghai Chen Hua Instrument Ltd., and not biasing, at 100mWcm -2analog light source irradiate under, battery is added to the disturbing signal of a 10mV, surface sweeping frequency range is that 20mHz-500KHz tests, test result is as Fig. 4, in Fig. 4, can find out, it is less that second half radius of a circle played on the battery left side that the light anode that contains nano-cable is packaged into, and this shows, contains Ag-TiO 2the sample charge transfer resistance of nano-cable is little, and in the process of charge recombination, electronics loses less, Ag/TiO 2the transmission of electronics has more effectively been accelerated in the introducing of nano-cable.

Claims (3)

1. contain a preparation method for the dye-sensitized solar cells light anode of nano-cable, this dye-sensitized solar cells light anode comprises fluorine doped tin oxide glass (3) and is attached to the nano-TiO on fluorine doped tin oxide glass (3) surface 2stratum granulosum (2), nano-TiO 2stratum granulosum includes Ag/TiO in (2) 2nano-cable (1), is characterized in that its preparation method is made up of following steps:
1) synthetic Ag/TiO 2nano-cable
After being mixed, silver nitrate, ethylene glycol adds metatitanic acid fourth fat, the mass ratio of silver nitrate, ethylene glycol and metatitanic acid fourth fat is 0.5～1:79:2～4, after fully stirring under lucifuge condition, transfer in the high-temperature high-pressure reaction kettle that polytetrafluoroethylene is liner, 245 DEG C are incubated 14 hours, be cooled to room temperature, by the product obtaining, through distilled water washing, ethanol washs, at the baking oven inner drying of 80 DEG C, obtain Ag/TiO 2nano-cable;
2) the dye-sensitized solar cells light anode that preparation contains nano-cable
Take Ag/TiO 2nano-cable and ground TiO 2powder mixes, and adds distilled water, Ag/TiO 2nano-cable and TiO 2the mass ratio of powder is 0.5～20:100, Ag/TiO 2nano-cable and TiO 2the solid content of powder is 0.4%, through magnetic agitation, ultrasonic dispersion, concentrated, forms Ag/TiO 2nano-cable and TiO 2the solid content of powder is 13% slurry, the film that is 8～12 μ m by slurry blade coating at fluorine doped tin oxide formation thickness on glass with blade, after film is naturally dried in air, be placed in intensification Muffle furnace and be incubated 30～50 minutes at 450～500 DEG C, be down to room temperature with stove, must contain the dye-sensitized solar cells light anode of nano-cable.
2. the preparation method of the dye-sensitized solar cells light anode that contains nano-cable according to claim 1, is characterized in that: described step 2) in, in the slurry forming, add polyethylene glycol, polyethylene glycol and TiO 2the mass ratio of powder is 3～4:10.
3. the preparation method of the dye-sensitized solar cells light anode that contains nano-cable according to claim 1 and 2, is characterized in that: Ag/TiO in described step 1) 2nano-cable and TiO 2the mass ratio of powder is 1～5:100.
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