CN105063589A - Preparation method for phosphating ferrous lithium high-temperature-resistant phosphating film material for metal - Google Patents
Preparation method for phosphating ferrous lithium high-temperature-resistant phosphating film material for metal Download PDFInfo
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- CN105063589A CN105063589A CN201510525203.7A CN201510525203A CN105063589A CN 105063589 A CN105063589 A CN 105063589A CN 201510525203 A CN201510525203 A CN 201510525203A CN 105063589 A CN105063589 A CN 105063589A
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Abstract
The invention relates to a preparation method for a phosphating ferrous lithium high-temperature-resistant phosphating film material for metal and belongs to the technical field of metal surface treatment. The preparation method includes the following steps that firstly, a metal matrix is selected, the surface of the metal is cleaned, chemical components are given according to the method, and the mass ratio of the chemical components is (159.68):(65.88):(115.03):(254.11):(12); the components are placed in a crucible, fully and evenly stirred through a glass bar and then placed in a box-type resistance furnace, the temperature is slowly increased from the room temperature of 20 DEG C, heat preservation is conducted for 30 min when the temperature of the resistance furnace is increased to 500-800 DEG C, and solid lithium iron phosphate is obtained; a phosphating solution is prepared from the obtained powder lithium iron phosphate and phosphoric acid according to the mass ratio of 1:2, a blank to be treated is placed in the phosphating solution, and a dark grey phosphating film can be obtained by the blank; a heating dehydrogenation process is finally conducted on the blank, so that the hazard of hydrogen embrittlement is reduced; and a saponification process is conducted, so that lubrication between the squeezed blank and a die is further enhanced.
Description
Technical field
The invention belongs to the phosphatize phosphate coat preparation field of Industrial Metal, particularly relate to a kind of for hot extrusion metal blank and half-finished resistant to elevated temperatures lubrication phosphatize phosphate coat thereof.Need to carry out surface treatment by phosphate solution to metal blank, obtain the resistant to elevated temperatures LiFePO 4 film of one deck energy at metal blank, improve hot extrude height die life and metal blank surface quality.
Background technology
Phosphorization technology carries out surface treatment with Phosphating Solution medicament to metal, in the process of even, fine and closely woven, the corrosion resistant phosphatize phosphate coat of its Surface Creation one deck, principle belongs to chemical conversion film process, so sometimes also phosphatization is referred to as chemical conversion film process.Bonderizing is industrially applied widely, main is used as antirust, lubrication and Coating Pretreatment.At present, very large by the Phosphating Solution amount of asking.The twentieth century initial stage is due to the invention of tool steel and metal surface phosphating technology, achieve the application that metallic surface is processed of ferrous metal widely, wherein to metallic surface carry out phosphatization for extrude industry need extruding, first the extruding of ferrous metal is applied to military project, most typical product is cartridge case, 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.
For the Phosphating Solution being adapted to ferrous metal extruding, require by Phosphating Solution phosphatization, form phosphate film at workpiece surface, this rete is quite soft, heat-resisting, in vesicular, to lubricant, there is very strong adsorption, 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.For the Phosphating Solution being adapted to ferrous metal extruding, 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.But due to the phosphate coating prepared by traditional Phosphating Solution be usually applicable to cold extrusion when working temperature higher than phosphate coating when 200 ° degrees Celsius usually start decompose.For metal fever extruding, general temperature is higher than metal recrystallization temperature, and at 1000 ° of degrees centigrade as the hot extrusion of steel, at this moment phosphate coating is destroyed, and can not obtain satisfied lubrication, greatly reduce the life-span of mould in extrusion process.
Therefore, based on above-mentioned purpose, one provided by the invention forms resistant to elevated temperatures lubrication phosphatize phosphate coat on metal blank and work in-process thereof, and this phosphatize phosphate coat can in the above stable components of metal recrystallization temperature.Need to carry out surface treatment by ferric solid-acid thing solution to ferrous metal blank, obtain the resistant to elevated temperatures nanometer phosphatization lubricant film of one deck energy, in extrusion process, this phosphatize phosphate coat attachment workpiece ability is strong, greatly can improve die life, have very important industrial application value.
Related to the present invention also has as Publication about Document.
[1] Li Xia, Ma Xicheng, scholar Lee is equal. electroless plating Au research [J] of carbon nanotube. and Materials Science and Engineering journal .2004,22 (1): 48-51
[2] Wang Quanfa, Li Yan. metal-conditioning treatment progress [J]. Yunnan industry .1994, (1): 13-17.
[3] people are got more than. the research [J] of environment protection type corrosion resistant phosphating liquor of iron series. material protection .2004 (07): 20-22
[4] Xiao Xianju, Tang Xuehong. metal-conditioning treatment technology [J]. scientific and technological economic market .2007 (9): 36-41.
Summary of the invention
The object of patent of the present invention is: for the labile problem of hot extrusion phosphate coating, and invention is a kind of can be high temperature resistant, easily adheres to, the ferric solid-acid film of high lubricating effect.This phosphating liquor of iron series is the high temperature resistant phosphating liquor of iron series of a kind of environment-protecting asepsis, and bonderizing speed is fast, and sediment is few.
The technical scheme of patent of the present invention is: the present invention is a kind of blank surface prescription for the treatment of liquid being adapted to hot extrusion technique, as follows:
The present invention is the Iron hemiphosphide lithium mixture being adapted to metal fever extruding, and the present invention adopts the phosphatize phosphate coat material utilizing chemical preparation LiFePO 4, adopts 45 steel to be matrix, with Fe
2o
3, LiOHH
2o; (NH
4)
2hPO
4; Carbon source is raw material.Its quality proportioning is: (159.68): (65.88): (115.03): (254.11): (12), reacts as follows:
LiOH·H
2O=LiOH+H
2O(at50-150℃)
(NH
4)
2HPO
4=2(NH)
3+H
3PO
4(at150-210℃)
LiOH+H
3PO
4=LiH
2PO
4+H
2O(at150-210℃)
2LiH
2PO
4+Fe
2O
3+C=2LiFePO
4+2H
2O+CO(at480-900℃)
The fusing point of the LiFePO 4 that the present invention produces, up to 1520-1564 ° of C, can be adapted to ferrous metal Warm Extrusion.LiH
2pO
4fusing point is high, has hydrophobicity, and this tunic protects iron, improves its oxidation and corrosion ability.
Greatly can improve paint film adhesion and counter-bending distortion, the performance such as shock-resistant.
Surface-treated method for the hot extrusion of ferrous metal blank of the present invention:
The first step: the blank after blanking is carried out Spheroidizing Annealing process, Heating temperature should be incubated 3-4 hour lower than this material re-crystallizes temperature less than 50;
Second step: blank is carried out shot peening 15Min by shotblasting machine, removes the burr that 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: by dried LiOHH
2o, (NH
4)
2hPO
4put into together with load weighted ferric oxide and carbon, chamber type electric resistance furnace is put into after fully stirring evenly with glass stick, slowly heat up from room temperature 20 ° of C, 30min is incubated when resistance furnace is raised to 500-800 ° of C, take out after cooling and can obtain grey block, be LiFePO 4 solid, taken out by obtained block and put in mortar, fine grinding is until obtain the powder of fine sand shape.The pulverulent solids obtained is sieved uniformly powder by screen cloth for subsequent use.Phosphoric acid is poured into and uniform stirring acquisition Phosphating Solution in the uniform powder finally obtained.
4th step: pending blank is immersed completely this solution 15 minutes, phosphatization temperature is 30 ° of C, and blank can obtain a kind of phosphatize phosphate coat of Dark grey.
5th step: carry out heating dehydrogenation process, reduces the harm of hydrogen embrittlement.
6th step: carry out saponification process, strengthens further between extrusion billet and mould and lubricates.
Compared with prior art, tool of the present invention has the following advantages:
(1) ferrous metal hot extrusion is applicable to: the phosphate coating composition of acquisition is the ferrous mixture of compound phosphoric acid, generally just decomposes at 1500 ° of more than C, can high temperature resistantly not decompose, meet the requirement of ferrous metal Warm Extrusion.
(2) good erosion resistance.
(3) in process and application process, there is long-term stability
(4) phosphating time is short, effective: have very strong adsorption to lubricant, and has certain plasticity, and phosphating time is short, effective.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure after test button phosphatization.
Embodiment
Provide most preferred embodiment of the present invention below:
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 less than 50; By shotblasting machine, blank is carried out shot peening 15Min, remove the burr that 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, comprise Fe
2o
3, LiOHH
2o; (NH
4)
2hPO
4; Carbon source, its quality proportioning is: (159.68): (65.88): (115.03): (254.11): (12).By dried LiOHH
2o, (NH
4)
2hPO
4put into together with load weighted ferric oxide and carbon, put into chamber type electric resistance furnace after fully stirring evenly with glass stick, slowly heat up from room temperature 20 ° of C, when resistance furnace is raised to 500-800 ° of C, be incubated 30min, take out after cooling and can obtain grey block, be LiFePO 4 solid.Configure a kind of surface treatment liquid being adapted to the extruding of ferrous metal height: taken out by obtained LiFePO 4 block and put in mortar, fine grinding is until obtain the powder of fine sand shape.Be the phosphating solution of 1:2 by ferrous phosphate lithium powder and phosphoric acid by its quality proportioning, pending blank is put into this phosphating solution, and blank can obtain a kind of phosphatize phosphate coat of Dark grey.Finally heating dehydrogenation process is carried out to blank, reduce the harm of hydrogen embrittlement.Carry out saponification process, strengthen further between extrusion billet and mould and lubricate.
Claims (3)
1. a preparation method for the high temperature resistant phosphatize phosphate coat material of metal Iron hemiphosphide lithium, is characterized in that the phosphatize phosphate coat material utilizing chemical preparation LiFePO 4, adopts 45 steel to be matrix, with Fe
2o
3, LiOHH
2o; (NH
4)
2hPO
4; Carbon source is raw material, proportioning is carried out by quality, LiFePO 4 is generated by reaction, phosphoric acid is poured into and uniform stirring acquisition Phosphating Solution in acquisition LiFePO 4 uniform powder, blank, again through shot-peening, pickling, above-mentioned solution phosphatization, dehydrogenation and saponification, namely obtains the metal fever extrusion billet with compound phosphoric acid ferrous lithium mixture surface film;
A () preparation is applicable to each composition proportion of LiFePO 4 of metal fever compressive surface phosphatize phosphate coat: comprise Fe
2o
3, LiOHH
2o; (NH
4)
2hPO
4; Carbon source, its quality proportioning is: (159.68): (65.88): (115.03): (254.11): (12), final acquisition LiFePO 4 block;
B LiFePO 4 block is made uniform powder by () for subsequent use, be the phosphating solution of 1:2 by ferrous phosphate lithium powder and phosphoric acid by its quality proportioning, pending blank is put into this phosphating solution, blank can obtain a kind of phosphatize phosphate coat of Dark grey, heating dehydrogenation process is carried out to blank, reduce the harm of hydrogen embrittlement, carry out saponification process, strengthen further between extrusion billet and mould and lubricate;
The c ferrous phosphate lithium salts being attached to matrix surface that () the present invention generates is one deck salt film, the high temperature of this composition ability 1500 ° of C, can be adapted to metal fever extruding.
2. the preparation method of the high temperature resistant phosphatize phosphate coat material of a kind of metal Iron hemiphosphide lithium according to claim 1, it is characterized in that with low cost, technological operation is easy: the starting material of employing are basic chemical industry product, cheap, meet large-scale industrial application service requirements, do not carrying out under large technique change condition simultaneously, traditional phosphating soap metallization processes equipment can be used, reliably easy and simple to handle.
3. the preparation method of the high temperature resistant phosphatize phosphate coat material of a kind of metal Iron hemiphosphide lithium according to claim 1, it is characterized in that: after blank adopts LiFePO 4 overlay film, rete is soft, high temperature resistant, in vesicular, to lubricant, there is very strong adsorption, and having certain plasticity, phosphating time is short, effective.
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| CN201510525203.7A CN105063589B (en) | 2015-08-25 | 2015-08-25 | A kind of preparation method of metal Iron hemiphosphide lithium high temperature resistant phosphatization membrane material |
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Citations (2)
| 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 |
| CN102011110A (en) * | 2009-09-08 | 2011-04-13 | 日本帕卡濑精株式会社 | Iron group metal material after black surface treatment and manufacturing method thereof |
-
2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011110A (en) * | 2009-09-08 | 2011-04-13 | 日本帕卡濑精株式会社 | Iron group metal material after black surface treatment and manufacturing method thereof |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 肖先举等: "金属磷化技术", 《贵州化工》 * |
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Effective date of registration: 20180613 Address after: 523000 No. 146 fo fo two street, rhinoceros Po village, Dalang Town, Dongguan, Guangdong Patentee after: Dongguan Ying Xing metal surface treatment material Co., Ltd. Address before: 250101 College of materials, Shandong Jianzhu University, 1000, Feng Ming Road, Lingang Development Zone, Ji'nan, Shandong Patentee before: Shandong Construction University |
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