CN105002485A - Formula of composite phosphate film solution which adapts to hot stamping of ultra-high-strength steel sheet material blank - Google Patents
Formula of composite phosphate film solution which adapts to hot stamping of ultra-high-strength steel sheet material blank Download PDFInfo
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- CN105002485A CN105002485A CN201510517726.7A CN201510517726A CN105002485A CN 105002485 A CN105002485 A CN 105002485A CN 201510517726 A CN201510517726 A CN 201510517726A CN 105002485 A CN105002485 A CN 105002485A
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- China
- Prior art keywords
- ultra
- phosphate
- phosphoric acid
- sheet material
- lithium
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 17
- 239000010452 phosphate Substances 0.000 title claims abstract description 17
- 229910000797 Ultra-high-strength steel Inorganic materials 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title claims abstract description 11
- 239000002131 composite material Substances 0.000 title claims abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 46
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 34
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 22
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 22
- 150000001875 compounds Chemical class 0.000 claims description 16
- AYMOKVDHVKHGNU-UHFFFAOYSA-L calcium lithium sulfate Chemical compound [Ca+2].S(=O)(=O)([O-])[O-].[Li+] AYMOKVDHVKHGNU-UHFFFAOYSA-L 0.000 claims description 14
- 229910000831 Steel Inorganic materials 0.000 claims description 11
- 239000010959 steel Substances 0.000 claims description 11
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 4
- 229940116007 ferrous phosphate Drugs 0.000 claims description 3
- 229910000155 iron(II) phosphate Inorganic materials 0.000 claims description 3
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229910010710 LiFePO Inorganic materials 0.000 claims description 2
- 230000006978 adaptation Effects 0.000 claims 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 19
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 238000004381 surface treatment Methods 0.000 abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006356 dehydrogenation reaction Methods 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- -1 lithium iron phosphate-calcium sulphate Chemical compound 0.000 abstract description 3
- 238000007127 saponification reaction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000005461 lubrication Methods 0.000 abstract description 2
- 235000011007 phosphoric acid Nutrition 0.000 abstract 4
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 abstract 3
- 229910052493 LiFePO4 Inorganic materials 0.000 abstract 2
- 229910052925 anhydrite Inorganic materials 0.000 abstract 2
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 abstract 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 abstract 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 abstract 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 abstract 1
- 235000019838 diammonium phosphate Nutrition 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 235000019837 monoammonium phosphate Nutrition 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000005554 pickling Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000005480 shot peening Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 238000000641 cold extrusion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
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- Chemical Treatment Of Metals (AREA)
Abstract
The invention relates to the field of phosphate solution formulas. The phosphate solution is quite suitable for the parkerizing process performed on the ultra-high-strength steel sheet material blank before hot stamping; a composite phosphate solution is used for performing surface treatment on the ultra-high-strength steel sheet material blank, so as to obtain a high-temperature resistant composite lithium iron phosphate-calcium sulphate film which is used for improving the service life of molds. A composite lithium iron phosphate-calcium sulphate surface treatment liquid which adapts to hot stamping of the ultra-high-strength steel sheet material blank is prepared according to the chemical composition ratio provided by the invention, and the preparation method is as follows: firstly, synthesizing lithium iron phosphate using iron oxide Fe2O3, lithium hydroxide LiOH.H2O, lithium hydroxide LiOH.H2O, ammonium dihydrogen phosphate (NH4)2HPO4 and a carbon source C; then, mixing calcium sulfate CaSO4 ultra-fine powder, lithium iron phosphate LiFePO4 ultra-fine powder, phosphoric acid H3PO4 and distilled water H2O according to a mass ratio of calcium sulfate CaSO4 ultra-fine powder, lithium iron phosphate LiFePO4 ultra-fine powder, phosphoric acid H3PO4 to distilled water H2O being (40-60):(10-30):(5-10):(808-912) to prepare a phosphating solution; placing the to-be-treated ultra-high-strength steel sheet material blank into the phosphating solution at 55-60 DEG C, so that the blank can be coated with a dark gray phosphating film; finally, carrying out heating dehydrogenation process on the blank, so as to reduce the harm caused by hydrogen embrittlement; carrying out the saponification process to further improve the lubrication between the hot stamped sheet material and the mold.
Description
Technical field
The present invention relates to a kind of phosphate solution formulation art, the phosphating process that this solution carries out before being particularly adapted to the hot stamping of ultrahigh-strength steel plate blank, needing to carry out surface treatment by compound phosphoric acid salts solution to ultrahigh-strength steel plate blank, obtaining the resistant to elevated temperatures compound phosphoric acid ferrous lithium-calcium sulfate salt film of one deck energy for improving die life.
Background technology
At present, the application processed metallic surface by Phosphating Solution widely, the twentieth century initial stage is due to the invention of tool steel and metal surface phosphating technology, achieve the extruding of ferrous metal, first the extruding of ferrous metal is applied to military project, most typical product is cartridge case, and the nineteen fifties extruding of ferrous metal starts to be applied to civilian, manufactures field be at present widely used at automobile component.The technique forming phosphate film at workpiece surface obtains good application as the gordian technique of the extruding realizing ferrous metal.Wherein phosphatization being carried out for extruding being in great demand of industry to metallic surface, along with the development of hot stamping technology, phosphatization being carried out to ferrous metal plate blank, then carry out hot press-formedly can improving die life and workpiece surface quality.
For the Phosphating Solution being adapted to ferrous metal hot stamping, require by Phosphating Solution phosphatization, form phosphate film at workpiece surface, film thickness is generally 10-15 μm, and frictional coefficient is about 0.05.The phosphate film formed, is made up of tiny plate crystal tissue.Require that this rete is quite soft, heat-resisting, in vesicular, have very strong adsorption to lubricant, and have certain plasticity, can with workpiece viscous deformation.Therefore, the effect of phosphate coating is the isolation bed course between mould and workpiece, decreases surface friction, improves die life.But due to the phosphate coating prepared by traditional Phosphating Solution be usually applicable to cold extrusion when working temperature higher than phosphate coating during 200 ° of C usually start decompose.In recent years, the hot press-formed technology occurred, the quenching heat treatment to plate can be realized while being shaped, improving the forming property of material, greatly extend the range of application of high strength ultrahigh-strength steel at auto parts, for superstrength hot stamping, general temperature is slightly lower than superstrength recrystallization temperature, and at 900 ° of more than C as the hot stamping of steel, at this moment phosphate coating is destroyed, satisfied lubrication can not be obtained in punching course, greatly reduce the life-span of mould.
Therefore, based on above-mentioned purpose, a kind of ultrahigh-strength steel provided by the invention carries out hot stamping, need to carry out surface treatment by compound phosphoric acid ferrous lithium-calcium sulfate salt solution to ultrahigh-strength steel plate blank, obtain the resistant to elevated temperatures compound phosphoric acid ferrous lithium-calcium sulfate salt film of one deck energy, compound phosphoric acid ferrous lithium-calcium sulfate salt the film adopting the method to be formed can be high temperature resistant, in plate blank process, compound phosphoric acid ferrous lithium-calcium sulfate salt film attachment workpiece ability is strong, greatly can improve die life, there is very important industrial application value.
Summary of the invention
The object of patent of the present invention is: the technical deficiency of decomposing for hot stamping phosphate coating, there is provided that surface recombination LiFePO 4-calcium sulfate salt film adhesive ability is strong, high temperature resistant not to be decomposed, low production cost, non-pollution discharge, a kind of surface treatment method being adapted to superstrength steel hot can produced in conventional hot stamping condition undertissue, more traditional phosphoric acid zinc salt film can the feature of high temperature resistant, good stability.
The technical scheme of patent of the present invention is: the present invention is a kind of compound phosphoric acid ferrous lithium-calcium sulfate salt surface treatment method being adapted to superstrength steel hot, as follows:
The present invention be adapted to the compound phosphoric acid ferrous lithium-calcium sulfate salt solution of superstrength steel hot, first by ferric oxide Fe
2o
3, lithium hydroxide LiOHH
2o, lithium hydroxide LiOHH
2o, primary ammonium phosphate (NH
4)
2hPO
4, carbon source C synthesizing lithium ferrous phosphate, its quality proportioning is: (159.68): (65.88): (115.03): (254.11): (12), reacts as follows:
LiOHH
2o=(heats 50-150 DEG C) LiOH+H
2o
(NH
4)
2hPO
4=(heating 50-210 DEG C) 2 (NH)
3+ H
3pO
4
LiOH+H
3pO
4=(heating 50-210 DEG C) LiH
2pO
4+ H
2o
2LiH
2pO
4+ Fe
2o
3+ C=(heating 480-900 DEG C) 2LiFePO
4+ 2H
2o+CO
Comprise calcium sulfate CaSO
4ultrafine powder, LiFePO 4 ultrafine powder LiFePO
4, phosphoric acid H
3pO
4with distilled water H
2o, its quality proportioning is: (40-60): (10-30): (5-10): (808-912).
Compound phosphoric acid ferrous lithium-calcium sulfate salt that the present invention produces is LiFePO
4and CaSO
4one deck salt film, superstrength steel hot can be adapted to.
Compound phosphoric acid ferrous lithium for the hot stamping of ultrahigh-strength steel plate blank of the present invention-calcium sulfate salt surface-treated method:
The first step: the plate blank after blanking is carried out Spheroidizing Annealing process, Heating temperature should be incubated 3-4 hour lower than this material re-crystallizes temperature 50 ° of below C;
Second step: plate blank is carried out shot peening 15Min by shotblasting machine, removes the burr that plate blank surface is tiny, strengthening surface quality;
3rd step: carry out pickling, adopts the sulphuric acid soln of 2% to carry out pickling;
4th step: the compound phosphoric acid ferrous lithium-calcium sulfate salt solution pending plate blank being put into 55 ° of-60 ° of C processes 5-10Min;
5th step: carry out heating dehydrogenation process, reduces the harm of hydrogen embrittlement.
6th step: carry out saponification process, strengthens further between plate blank blank and mould and lubricates.
Compared with prior art, tool of the present invention has the following advantages:
(1) superstrength steel hot is applicable to: the phosphate coating composition of acquisition is compound phosphoric acid ferrous lithium-calcium sulfate salt, generally just decomposes at 1200 ° of more than C, can high temperature resistantly not decompose, meet the requirement of superstrength steel hot.
(2) with low cost: the starting material of employing are basic chemical industry product, cheap, meet large-scale industrial application service requirements.
(3) easy and simple to handle: the present invention is not carrying out under large change condition, traditional phosphating soap metallization processes equipment can be used, reliably easy and simple to handle.
(4) phosphating time is short, effective: after blank adopts calcium salt overlay film, and rete is soft, heat-resisting, in vesicular, have very strong adsorption to lubricant, and has certain plasticity, and phosphating time is short, effective.
Embodiment
Provide most preferred embodiment of the present invention below:
Plate blank after blanking is carried out Spheroidizing Annealing process, and Heating temperature should be incubated 3-4 hour lower than this material re-crystallizes temperature 50 ° of below C; By shotblasting machine, plate blank is carried out shot peening 15Min, remove the burr that plate blank surface is tiny, strengthening surface quality; Carry out pickling, adopt the sulphuric acid soln of 2% to carry out pickling; Provide chemical composition ratio according to invention, configure a kind of compound phosphoric acid ferrous lithium-calcium sulfate salt surface treatment liquid being adapted to superstrength steel hot: first by ferric oxide Fe
2o
3, lithium hydroxide LiOHH
2o, lithium hydroxide LiOHH
2o, primary ammonium phosphate (NH
4)
2hPO
4, carbon source C synthesizing lithium ferrous phosphate, secondly will comprise calcium sulfate CaSO
4ultrafine powder, LiFePO 4 ultrafine powder LiFePO
4, phosphoric acid H
3pO
4, and distilled water H
2o, its quality proportioning is: (40-60): (10-30): (5-10): (808-912).In the present embodiment, its quality proportioning can select following any one: 40:10:5:808; 60:30:10:912; 45:15:8:830; 50:20:9:880.Compound phosphoric acid ferrous lithium-calcium sulfate salt solution that pending hot stamping plate blank puts into 55 ° of-60 ° of C is processed 5-10Min; Carry out heating dehydrogenation process, reduce the harm of hydrogen embrittlement.Carry out saponification process, strengthen further between plate blank blank and mould and lubricate.
Claims (1)
1. adapt to a composite phosphate coating solution formula for ultrahigh-strength steel plate hot stamping, it is characterized in that first by ferric oxide Fe
2o
3, lithium hydroxide LiOHH
2o, lithium hydroxide LiOHH
2o, primary ammonium phosphate (NH
4)
2hPO
4, carbon source C synthesizing lithium ferrous phosphate, then will comprise calcium sulfate CaSO
4ultrafine powder, LiFePO 4 ultrafine powder LiFePO
4, phosphoric acid H
3pO
4with distilled water H
2it is LiFePO that O synthesizes compound phosphoric acid ferrous lithium-calcium sulfate salt
4and CaSO
4one deck salt film:
A () LiFePO 4 is by ferric oxide Fe
2o
3, lithium hydroxide LiOHH
2o, lithium hydroxide LiOHH
2o, primary ammonium phosphate (NH
4)
2hPO
4, carbon source C synthesizes;
Compound phosphoric acid ferrous lithium-each the composition proportion of calcium phosphate salt solution of (b) superstrength degree steel hot: calcium sulfate CaSO
4ultrafine powder, LiFePO 4 ultrafine powder LiFePO
4, phosphoric acid H
3pO
4with distilled water H
2o, its quality proportioning is: 40-60): (10-30): (5-10): (808-912);
One deck salt film of what c the composite phosphate coating solution formula of () described adaptation superstrength degree steel plate material hot stamping was produced is a kind of compound phosphoric acid ferrous lithium-calcium sulfate salt, the high temperature of this composition ability 1200 ° of C, can be adapted to the hot stamping of superstrength degree steel plate material.
Priority Applications (1)
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---|---|---|---|
CN201510517726.7A CN105002485B (en) | 2015-08-22 | 2015-08-22 | A kind of composite phosphate coating solution formula for adapting to unimach plate drop stamping |
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---|---|---|---|
CN201510517726.7A CN105002485B (en) | 2015-08-22 | 2015-08-22 | A kind of composite phosphate coating solution formula for adapting to unimach plate drop stamping |
Publications (2)
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CN105002485A true CN105002485A (en) | 2015-10-28 |
CN105002485B CN105002485B (en) | 2018-03-06 |
Family
ID=54375335
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CN201510517726.7A Expired - Fee Related CN105002485B (en) | 2015-08-22 | 2015-08-22 | A kind of composite phosphate coating solution formula for adapting to unimach plate drop stamping |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101956191A (en) * | 2010-11-08 | 2011-01-26 | 大连三达奥克化学股份有限公司 | Car cast aluminum alloy cylinder body and manganese black phosphating agent for piston and preparation method thereof |
CN103643230A (en) * | 2013-12-07 | 2014-03-19 | 山东建筑大学 | Surface treatment method for composite sulfuric acid-phosphomycin calcium applicable to warm extrusion |
CN104250742A (en) * | 2013-06-28 | 2014-12-31 | 无锡洛社科技创业有限公司 | Phosphatization liquid for steel pipe cold rolling processing pretreatment |
-
2015
- 2015-08-22 CN CN201510517726.7A patent/CN105002485B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101956191A (en) * | 2010-11-08 | 2011-01-26 | 大连三达奥克化学股份有限公司 | Car cast aluminum alloy cylinder body and manganese black phosphating agent for piston and preparation method thereof |
CN104250742A (en) * | 2013-06-28 | 2014-12-31 | 无锡洛社科技创业有限公司 | Phosphatization liquid for steel pipe cold rolling processing pretreatment |
CN103643230A (en) * | 2013-12-07 | 2014-03-19 | 山东建筑大学 | Surface treatment method for composite sulfuric acid-phosphomycin calcium applicable to warm extrusion |
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