CN101840791A - Processing method of aluminum foil in manufacturing process of solid aluminum electrolytic capacitor - Google Patents
Processing method of aluminum foil in manufacturing process of solid aluminum electrolytic capacitor Download PDFInfo
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- CN101840791A CN101840791A CN201010187775A CN201010187775A CN101840791A CN 101840791 A CN101840791 A CN 101840791A CN 201010187775 A CN201010187775 A CN 201010187775A CN 201010187775 A CN201010187775 A CN 201010187775A CN 101840791 A CN101840791 A CN 101840791A
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- 239000003990 capacitor Substances 0.000 title claims abstract description 49
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 39
- 239000007787 solid Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 238000003672 processing method Methods 0.000 title claims abstract description 21
- 239000011888 foil Substances 0.000 title abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005520 cutting process Methods 0.000 claims abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 6
- 239000010452 phosphate Substances 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 4
- 239000005030 aluminium foil Substances 0.000 claims description 64
- 238000000034 method Methods 0.000 claims description 31
- 230000015572 biosynthetic process Effects 0.000 claims description 12
- 239000007784 solid electrolyte Substances 0.000 claims description 11
- 230000000295 complement effect Effects 0.000 abstract 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 27
- 239000000243 solution Substances 0.000 description 20
- 230000008901 benefit Effects 0.000 description 19
- 239000007864 aqueous solution Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000004411 aluminium Substances 0.000 description 8
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 7
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 7
- 235000019837 monoammonium phosphate Nutrition 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 description 4
- 239000001741 Ammonium adipate Substances 0.000 description 4
- 235000019293 ammonium adipate Nutrition 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229920000128 polypyrrole Polymers 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a processing method of an aluminum foil in a manufacturing process of a solid aluminum electrolytic capacitor. The aluminum foil is subjected to complementary forming after being cut, an oxide-film dielectric layer is formed on a cutting place, and then a solid electrolytic layer is prepared. The processing method comprises at least one of the following step 1 and step 2: in step 1, solution prepared from at least one of citric acid or citrate is adopted to perform complementary forming and the concentration of solution is 0.1-10%; in step 2, solution prepared from at least one of phosphoric acid or phosphate is adopted to perform complementary forming and the concentration of solution is 0.01-5%. In the step 1 or the step 2, the pH value of solution is 4-7, the temperature is 40-85 DEG C, 0.7-1.1 time energized voltage is applied and the time for applying a constant voltage is 5-60min. The processing method of an aluminum foil in a manufacturing process of a solid aluminum electrolytic capacitor can effectively improve a drain current of a capacitor, increase production controllability and lower energy consumption.
Description
[technical field]
The present invention relates to the concrete operation in the solid aluminum electrolytic capacitor production process, particularly the processing method of aluminium foil in the solid aluminum electrolytic capacitor manufacture process.
[background technology]
Capacitor belongs to electronics and information industry basic device product, be that a kind of use is the widest, the consumption maximum, and the electronic component of not replacing, its output accounts for 40% of electronic component, along with the development of electronics and information industry, electronics and IT products output, kind constantly increase, and the demand of supporting with it capacitor also constantly increases.The performance of capacitor, kind and quality directly determine or affect the development of electronics and IT products.Adapt to surface mounting technology, chip type, miniaturization in order to solve the traditional liquid electrolytic capacitor, must solve electrolytical solidification.Plurality of advantages such as solid electrolytic capacitor has that volume is littler, performance is better, wide temperature, long-life, anti-high frequency, high reliability and high environmental protection adapt to the development trend and the surface mounting technology requirement of complete electronic set miniaturization, high frequencyization, high speed, highly reliable, high environmental protection.
In the solid aluminum electrolytic capacitor manufacture process, at first aluminium foil is cut into (surface comprises oxide-film) size of needs, at this moment the oral thermometer face of cutting of aluminium foil does not have the capping oxidation film, usually need the aluminium foil of cutting is mended formation, with the oxide-film that regrows in incision, prepare solid electrolyte layer afterwards again, thereby reduce the aluminium foil leakage current.Because it is of crucial importance for the leakage current performance of aluminium electrolytic capacitor that the benefit of aluminium foil forms, that is to say that the benefit of aluminium foil forms the character that effect directly influences oxide film dielectric, finally influence the leakage current and the reliability of aluminium electrolytic capacitor.
The day for announcing is that on 08 03rd, 2005 China Patent No. is the patent of invention of CN200510041690.6, its name is called " manufacture method of solid sheet type electrolytic capacitor ", one of open solid aluminum electrolytic capacitor manufacturing step in this patent documentation: the aluminium foil cathode portion is immersed in the mixed aqueous solution of ammonium dihydrogen phosphate of the ammonium adipate that contains 0.1-1.0M and 0.01-0.1M, the control temperature is at 60-90 ℃ and add the voltage of 6-35V, the constant 15-45 of sustaining voltage minute, take out the back cleaning, drying, prepare solid electrolyte layer afterwards again.This processing method adopts the mixed aqueous solution of ammonium adipate and ammonium dihydrogen phosphate that aluminium foil is once changed into processing, and the capacitor finished product leakage current performance that obtains is still waiting further improvement, and simultaneously, the solution temperature of needs is higher, 90 ℃ of the highest temperature even needs.
The day for announcing is that on 06 04th, 2008 China Patent No. is the patent of invention of CN200610154775.X, its name is called " a kind of manufacture method of anode foil for aluminum electrolytic capacitor ", the manufacture method of aluminium electrolytic capacitor with aluminium foil also disclosed in this patent documentation, be that aluminium foil is corroded, change into then, thereby make the aluminium foil that capacitor needs, concrete method comprises immersion, three steps of high-temperature process and anodic oxidation, the anodic oxidation step is promptly to obtain aluminium electroloysis container anode foils finished product after concentration is to carry out anodized in the weak acid of 0.1-5% and the 0.1-5% ammonium salt solution through the anode foil for aluminum electrolytic capacitor semi-finished product after the high-temperature process, discloses citric acid in the weak acid described in the document.Above-mentioned patent documentation refers to it mainly is the aluminum foil preparation of aluminium foil producer, wherein in fact the anode oxidation process of disclosed aluminium foil is exactly the aluminium foil chemical synthesis technology, but this method mainly is the processing at high blocking, and high blocking generally is applied to the liquid aluminium capacitor, and the low-voltage aluminium foil normally of the aluminium foil in the solid aluminum electrolytic capacitor.
[summary of the invention]
The technical problem to be solved in the present invention, be to provide the processing method of aluminium foil in a kind of solid aluminum electrolytic capacitor manufacture process, by implementing this method, can improve the leakage current of capacitor, improve the production controllability, cut down the consumption of energy, can solve that the condenser leakage current performance that exists in the prior art remains further to be improved, the solution temperature problem of higher of needs.
The present invention is by solving the problems of the technologies described above by the following technical solutions: the processing method of aluminium foil in the solid aluminum electrolytic capacitor manufacture process, described aluminium foil is mended formation to aluminium foil after cutting, to form the oxide film dielectric layer at otch, prepare solid electrolyte layer afterwards again, wherein, described processing method comprises at least one in following steps 1 and the step 2: step 1: adopt at least a made solution that comprises in citric acid or the citrate that aluminium foil is mended formation, the concentration of described solution is 0.1-10%; Step 2: adopt at least a made solution that comprises in phosphoric acid or the phosphate that aluminium foil is mended formation, the concentration of described solution is 0.01-5%.
Further, in described step 1 or the step 2, the pH value of solution is 4-7, and temperature is 40-85 ℃.
Further, in described step 1 or the step 2, aluminium foil is applied the 0.7-1.1 voltage of doubly energizing, constant voltage time is 5-60min.
More preferably, in the described step 1, the concentration of solution is 0.5-2%.
More preferably, in the described step 2, the concentration of solution is 0.05-1%.
Further, in described step 1 or the step 2, the temperature of solution is 40-60 ℃.
The processing method of aluminium foil has following beneficial effect in the solid aluminum electrolytic capacitor manufacture process involved in the present invention:
1, the leakage current and the examination back leakage current performance of capacitor have been improved;
2, also can realize at a lower temperature, the rate of volatilization of water in the solution that slowed down, the controllability of raising production process also cuts down the consumption of energy simultaneously.
[description of drawings]
The present invention is further illustrated in conjunction with specific embodiments with reference to the accompanying drawings.
Fig. 1 is a solid aluminum electrolytic single-layer capacitor element structure chart.
Fig. 2 is the concrete structure figure of aluminium foil.
[embodiment]
See also shown in Figure 1, solid aluminum electrolytic capacitor, the oxide film dielectric 2 that comprises anode bodies 1, forms at the anode bodies outer surface, the solid electrolyte layer 3 that forms at oxide film dielectric 2 outer surfaces, the carbon containing cathode layer 41, carbon containing cathode layer 41 outer surfaces that form at solid electrolyte layer 3 outer surfaces form contains silver body cathode layer 42.Described anode bodies 1 is an aluminium, and oxide film dielectric 2 is an aluminium oxide, and described dielectric substrate 3 is electric conductive polymer or oxide, and described conducting polymer can also be polypyrrole, polythiophene, and polyaniline or derivatives thereof, oxide are manganese dioxide.
Again as shown in Figure 2, the raw material aluminium foil 6 of making anode bodies 1 and oxide film dielectric 2 is divided into aluminium lamination 61 and alumina layer 62, and alumina layer 62 is distributed in the surface of described aluminium lamination 61.
Shown in Fig. 1 and 2, the processing method of aluminium foil in the solid aluminum electrolytic capacitor manufacture process involved in the present invention, aluminium foil is mended formation to aluminium foil after cutting, and forms the oxide film dielectric layer at otch, prepares solid electrolyte layer again.Described processing method comprises at least one in following steps 1 and the step 2, and order is not limit.Can be independent implementation step 1, also can be independent implementation step 2, can also be that implementation step 1 carry out step 2 afterwards, maybe can be carry out step 1 again after the implementation step 2.
Wherein, described benefit forming process comprises in step 1 or the step 2 at least 1, and in the step 1, adopting concentration is that at least a made solution that comprises in citric acid or the citrate of 0.1-10% is mended formation to aluminium foil; In the step 2, adopting concentration is that at least a made solution that comprises in phosphoric acid or the phosphate of 0.01-5% is mended formation to aluminium foil; Further, in described step 1 or the step 2, the pH value of solution is 4-7, and temperature is 40-85 ℃, and applies the 0.7-1.1 voltage of doubly energizing, and constant voltage time is 5-60min.More preferably, solution concentration is 0.5-2% in the described step 1; More preferably, solution concentration is 0.05-1% in the described step 2.More preferably, in described step 1 or the step 2, solution temperature is 40-60 ℃.More preferably, increase heat treatment between described two steps, temperature is generally 200-500 ℃, and the time is 10-30min.
Embodiment 1
Specification is after the aluminium foil of 13Vf is cut, benefit forming process in carry out step 1 earlier, then cleaning, drying, then at 300 ℃ of heat treatment 30min, the benefit forming process in carry out step 2 then, prepare the solid electrolyte layer polypyrrole layer again, form the first cathode layer carbon-coating at the solid electrolyte layer outer surface, form the second cathode layer silver layer at the first cathode layer outer surface then, make the monolithic capacitor element, with capacitor element assembling and encapsulation, make solid aluminum electrolytic capacitor again.Benefit in the step 1 form be that the back aluminium foil immerses that temperature is that 70 ℃, concentration are 10% with cutting, the pH value is in 6.0 the aqueous citric acid solution, to apply the 13V constant voltage, constant voltage 10min; Benefit in the step 2 form be with the aluminium foil after the heat treatment immerse that temperature is that 85 ℃, concentration are 0.01%, the pH value is in 6.0 the ammonium dihydrogen phosphate aqueous solution, applies the 13V constant voltage, constant voltage 60min.
Embodiment 2
With different among the embodiment 1 be, only adopt the benefit forming process in the step 1, specifically be that the back aluminium foil immerses that temperature is that 40 ℃, concentration are 0.1% with cutting, the pH value is in 6.0 the aqueous citric acid solution, to apply the 13V constant voltage, constant voltage 30min.The benefit of no heat treatment and step 2 forms, and other are with embodiment 1.
Embodiment 3
With different among the embodiment 1 be, only adopt the benefit forming process in the step 1, specifically be with aluminium foil immerse that temperature is that 60 ℃, concentration are 5%, the pH value is 6.0 ammonium dihydrogen phosphate aqueous solution, applies the 13V constant voltage, constant voltage 30min.The benefit of no heat treatment and step 2 forms, and other are with embodiment 1.
Embodiment 4
Adopt earlier the benefit of step 2 to form aluminium foil is handled, specifically be that aluminium foil immerses that temperature is that 60 ℃, concentration are 0.05%, the pH value is 6.0 phosphate aqueous solution, applies 13V constant voltage constant voltage 15min; Then at 300 ℃ of heat treatment 30min; Adopt the benefit forming process of step 1 that aluminium foil is handled then, specifically be that the back aluminium foil immerses that temperature is that 50 ℃, concentration are 0.5% with cutting, the pH value is in 6.0 the ammonium citrate aqueous solution, to apply the 13V constant voltage, constant voltage 5min.Other are with embodiment 1.
Embodiment 5
Adopt earlier the benefit of step 1 to form aluminium foil is handled, specifically be that the back aluminium foil immerses that temperature is that 50 ℃, concentration are 2% with cutting, the pH value is in 6.0 the ammonium citrate aqueous solution, to apply the 13V constant voltage, constant voltage 5min; Then at 300 ℃ of heat treatment 30min; And then adopt the benefit forming process of step 2 that aluminium foil is handled, specifically be with the aluminium foil after the heat treatment immerse that temperature is that 60 ℃, concentration are 1%, the pH value is 6.0 phosphate aqueous solution, applies the 13V constant voltage, constant voltage 10min.Other are with embodiment 1.
Adopt earlier the benefit of step 1 to form aluminium foil is handled, specifically be that the back aluminium foil immerses that temperature is that 50 ℃, concentration are 1.5% with cutting, the pH value is in 6.0 the ammonium citrate aqueous solution, to apply the 13V constant voltage, constant voltage 15min; Then at 300 ℃ of heat treatment 30min; And then adopt the benefit forming process of step 2 that aluminium foil is handled, specifically be with the aluminium foil after the heat treatment immerse that temperature is that 60 ℃, concentration are 0.5%, the pH value is 6.0 ammonium dihydrogen phosphate aqueous solution, applies the 13V constant voltage, constant voltage 10min.Other are with embodiment 1.
Comparative Examples 1
Specification is after the aluminium foil of 13Vf is cut paper tinsel, carry out earlier mending the first time and form, then cleaning, drying then at 300 ℃ of heat treatment 30min, carries out mending the second time formation then, prepare the solid electrolyte layer polypyrrole layer again, form the first cathode layer carbon-coating at the solid electrolyte layer outer surface, form the second cathode layer silver layer at the first cathode layer outer surface then, make the monolithic capacitor element, with capacitor element assembling and encapsulation, make solid aluminum electrolytic capacitor again.Mend for the first time to form and mend for the second time and form that all to adopt 80 ℃, pH value be 6.0 5% ammonium adipate and the mixed aqueous solution of 0.5% ammonium dihydrogen phosphate, apply the 13V constant voltage, constant voltage 30min.
Comparative Examples 2
Different with Comparative Examples 1 is, only adopts to mend for the first time to form, and specifically is that to immerse 80 ℃, pH value be the mixed aqueous solution of 6.0,5% ammonium adipate and 0.5% ammonium dihydrogen phosphate with cutting the back aluminium foil, applies the 13V constant voltage, constant voltage 30min.No heat treatment and benefit formation for the second time, other are with Comparative Examples 1.
Be prepared into 6.3V/150 μ F capacitor at last, and through 60 ℃, 90RH%, the examination of 500h Steadydamp-heat.Prepared 30 capacitor volume of the various embodiments described above and Comparative Examples, loss, ESR, leakage current value mean value and examination back leakage current average data are as shown in table 1.
Table 1 embodiment and Comparative Examples electrical property are relatively
| Project | Finished product capacity (μ F) | The finished product loss | Finished product ESR (m Ω) | Finished product leakage current (μ A) | Examination back leakage current (μ A) |
| Embodiment 1 | ??143 | ??0.019 | ??20 | ??9.3 | ??31.1 |
| Embodiment 2 | ??143 | ??0.018 | ??22 | ??9.1 | ??30.9 |
| Embodiment 3 | ??146 | ??0.019 | ??19 | ??8.4 | ??21.4 |
| Embodiment 4 | ??144 | ??0.020 | ??22 | ??7.3 | ??19.8 |
| Embodiment 5 | ??145 | ??0.018 | ??21 | ??6.8 | ??22.1 |
| |
??144 | ??0.019 | ??21 | ??6.6 | ??20.9 |
| Comparative Examples 1 | ??144 | ??0.020 | ??24 | ??27.2 | ??983 |
| Comparative Examples 2 | ??141 | ??0.019 | ??23 | ??31.9 | ??1512 |
The data of table 1 show, adopt the processing method of aluminium foil in the solid aluminum electrolytic capacitor manufacture process provided by the present invention, in embodiment 1-6, the leakage current value of prepared capacitor, the leakage current value of Steadydamp-heat examination back capacitor all is starkly lower than the leakage current value in the Comparative Examples, particularly embodiment 4,5, and 6.
Claims (6)
1. the processing method of aluminium foil in the solid aluminum electrolytic capacitor manufacture process, described aluminium foil is mended formation to aluminium foil after cutting, to form the oxide film dielectric layer at otch, prepare solid electrolyte layer afterwards again, it is characterized in that: described processing method comprises at least one in following steps 1 and the step 2:
Step 1: adopt at least a made solution that comprises in citric acid or the citrate that aluminium foil is mended formation, the concentration of described solution is 0.1-10%;
Step 2: adopt at least a made solution that comprises in phosphoric acid or the phosphate that aluminium foil is mended formation, the concentration of described solution is 0.01-5%.
2. according to the processing method of aluminium foil in the described solid aluminum electrolytic capacitor manufacture process of claim 1, it is characterized in that: in described step 1 or the step 2, the pH value of solution is 4-7, and temperature is 40-85 ℃.
3. according to the processing method of aluminium foil in the described solid aluminum electrolytic capacitor manufacture process of claim 1, it is characterized in that: in described step 1 or the step 2, aluminium foil is applied the 0.7-1.1 voltage of doubly energizing, constant voltage time is 5-60min.
4. according to the processing method of aluminium foil in the described solid aluminum electrolytic capacitor manufacture process of claim 1, it is characterized in that: in the described step 1, the concentration of solution is 0.5-2%.
5. according to the processing method of aluminium foil in the described solid aluminum electrolytic capacitor manufacture process of claim 1, it is characterized in that: in the described step 2, the concentration of solution is 0.05-1%.
6. according to the processing method of aluminium foil in the described solid aluminum electrolytic capacitor manufacture process of claim 2, it is characterized in that: in described step 1 or the step 2, the temperature of solution is 40-60 ℃.
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Application publication date: 20100922 |