CN103484016A - Method for processing surface of magnesium product by using D3 organosilicone liquid - Google Patents
Method for processing surface of magnesium product by using D3 organosilicone liquid Download PDFInfo
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- CN103484016A CN103484016A CN201310438838.4A CN201310438838A CN103484016A CN 103484016 A CN103484016 A CN 103484016A CN 201310438838 A CN201310438838 A CN 201310438838A CN 103484016 A CN103484016 A CN 103484016A
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Abstract
The invention discloses a method for processing the surface of a magnesium product by using a D3 organosilicone liquid. The method comprises the following steps: (1) hydrolyzing the following components in parts by weight under an alkali condition: 4-6 parts of D3, 10-30 parts of ethanol and 2-5 parts of ammonium acetate; (2) adding rare earth metal salt into the organosilicon liquid; (3) placing the magnesium product into a rare earth-organosilicon solution for dipping for 2-6 min; (4) baking the magnesium product subjected to the dipping by the organosilicon liquid for 35-60 min at the temperature of 90-115 DEG C. According to the method, the surface of the magnesium product is dipped by the solution prepared by adding the rare earth metal salt into the linear oligomer organosilicon liquid which contains a silicon-terminated hydroxyl and is obtained by the hydrolysis reaction of the D3, and is cured at high temperature for film forming so as to form an organic-inorganic composite film with a netlike molecular structure on the surface of the magnesium product, and the organic-inorganic composite film is relatively compact, and can improve the corrosion resistance of the magnesium product.
Description
Technical field
The present invention relates to metal products surface-treated technical field, relate in particular to a kind of method that the D3 of employing organosilicon liquid is processed the magnesium product surface.
Background technology
Magnesium is a kind of argenteous basic metal, and it is again structural metal the lightest and that the most easily process.Magnesium alloy has specific tenacity and specific rigidity is high, the advantage such as damping, anti-acoustic capability are good.The tensile strength of magnesium alloy and aluminium alloy approach, but specific tenacity is higher than aluminium alloy and some high-strength steel.So available magnesium alloy replaces aluminium alloy and steel, alleviate the weight of hardware.The Young's modulus of magnesium alloy is low, and damping property is good, can bear larger shock load, is suitable for manufacturing the component that bear strenuous vibration.The plasticity ratio aluminium of magnesium metal is low, under normal temperature viscous deformation little, can only, carrying out press working more than 235 ℃, should not carry out cold presswork.But the cutting ability of magnesium alloy is very good, dimensional stability is high, can carry out various mechanical cutting, also can carry out the welding of hydrogen arc weldering and other techniques.The fusing point of magnesium lower (648.8 ℃), forgeability are good, and its good low-temperature performance is applicable to manufacture the component of working under low temperature.The heat dispersion of magnesium alloy is not only high than plastics, but also is better than aluminium alloy.Magnesium alloy has very high shield electromagnetic interference performance, is applicable to do the shell of electronic equipment.In addition, it also has superconductivity and hydrogen storage property.The reclaiming of magnesium alloy is good, cheap, meets environmental requirement, can be widely used on the industrial goods such as military project, automobile, aircraft, mobile phone, computer, dynamo-electric five metals.
Though magnesium possesses above-mentioned series of advantages, the electropotential of magnesium very low (being-2.37V), even also can form oxide film in atmospheric environment, and the PBR value of this oxide film is less than 1 (being 0.99), constant temperature oxidation kinetics curve is linear.Therefore, the natural oxide film of magnesium is loose porous easily to come off, and can not play the protection matrix and avoid corroding; Also have the second-phase of alloy inside or the galvanic corrosion that impurity causes, easily origination point corrosion, cause the solidity to corrosion of magnesium and alloy thereof very poor, and application is restricted.Prior art has chemical conversion film, plating, electroless plating to the surface treatment method of magnesium goods.These methods are often fine and close not at the protective membrane formed, and have textural defect, cause the erosion resistance of surface treated magnesium goods than not being greatly improved without surface treatment magnesium goods.
Summary of the invention
In view of this, the invention provides a kind of method that the D3 of employing organosilicon liquid is processed the magnesium product surface, the method can form fine and close organic and inorganic composite membrane at the magnesium product surface, thereby improves the erosion resistance of magnesium goods.
A kind of method that adopts D3 organosilicon liquid to process the magnesium product surface comprises the following steps:
(1) according to mass fraction, 4～6 parts of hexamethyl cyclotrisiloxanes, 10～30 parts of ethanol and 2～5 parts of ammonium acetates are added in water and form mixed solution, the pH value of regulating this mixed solution is 8～11, under 50～65 ℃, disperses 1.5～3h to make organosilicon liquid;
(2) add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 5～15g/L Ce (NO
3)
3, 2～6g/L H
2o
2, 1～4g/L fluorochemical rare earth-organic silicon solution.
(3) the magnesium goods are inserted in described rare earth-organic silicon solution and flooded 2～6min;
(4) will toast 35～60min under 90～115 ℃ through the impregnated magnesium goods of organosilicon liquid.
Wherein, in described step (1), the mass fraction of water is 60～90 parts.
Wherein, described step is added to hexamethyl cyclotrisiloxane, ethanol and ammonium acetate in water and is specially in (1): at first ethanol and ammonium acetate are dissolved in the water, then hexamethyl cyclotrisiloxane is slowly dripped in the water that is dissolved with ethanol and ammonium acetate, the time of described dropping is 30～60min.
Wherein, in described step (1), the dispersion of mixed solution adopts the mechanical stirring that rotating speed is 150～400rpm.
Wherein, in described step (3), the number of times of dipping is 1～5 time.
Wherein, according to by first to after order, described step (3) also comprises before successively to magnesium goods mechanical grinding, chemical alkali liquor oil removing and distilled water flushing.
Wherein, described chemical alkali liquor oil removing is specially: the magnesium goods are inserted in the chemical alkali lye that temperature is 70～80 ℃ and flooded 20～40min.
Wherein, described chemical alkali lye comprises 40～60g/L NaOH, 50～70g/L Na
3pO
4, 20～30g/L Na
2cO
3, 5～10g/L Na
2siO
3.
Wherein, described mechanical grinding is specially: first with 200 order sand paper, slightly polish, more carefully polish with 600 order sand paper.
In above technical scheme, hexamethyl cyclotrisiloxane in step (1), be called again D3, and it is a kind of silane coupling agent, and it take ethanol as catalyzer generation hydrolysis reaction under alkaline condition.The D3 ring opening hydrolysis generates the silanol that respectively there is a silicon hydroxyl at two ends, and the functionality of this silanol is 2, thereby the oligopolymer generated that occurs to shrink is linear.The process of this hydrolysis reaction is divided into following three phases: (1) ring opening hydrolysis becomes silanol; (2) shrink between silanol and react the oligopolymer that generates the end silicon hydroxyl that linear product is the master; (3) hydroxyl of the silicon hydroxyl of oligopolymer and oxidation on metal surface thing or hydrate forms hydrogen bond.In aforesaid three phases, sol particles nucleation and sol particles growth.The ammonium acetate added in step (1) can improve the degree of carrying out of hydrolysis reaction.The feed way of each reactive component adopts the organosilane monomer dripping method, and hexamethyl cyclotrisiloxane slowly drips in water, can make like this organosilane monomer in " hunger " state, thereby improves the transformation efficiency of organosilane monomer.
In step (2) with Ce (NO
3)
3as rare earth metal salt, than CeCl
3, the former strengthens the better effects if of the erosion resistance of magnesium goods.With H
2o
2as oxidation promotor, can be lowered into film temperature, improve rate of film build.Using fluorochemical as stablizer.
In step (4), will be in order to make organosilicon liquid at magnesium goods film-forming through the impregnated magnesium goods baking of organosilicon liquid.In the process of this film-forming, the crosslinked tridimensional network that forms occurs in the silicon hydroxyl of the oligopolymer of aforementioned linearity.The silicon hydroxyl of oligopolymer and the hydroxyl of substrate surface generate the covalent linkage that more bond energy is larger than hydrogen bond simultaneously.The composite membrane that the film formed after solidifying is the organic and inorganic phase, near magnesium surface in this composite membrane is to have siloxane bond and atoms metal bonding to form inorganic phase, this inorganic phase is the organic phase consisted of the netted macromolecular chain that contains the silica segment away from magnesium surface, organo-silicon coupling agent is the avtive spot as reaction by siloxanes, play " bridge " effect between inorganic phase and organic phase, the organic and inorganic composite membrane is introduced inorganic particle in organic network, improved network structure, strengthened the mechanical property of film, improved thermostability, pore structure and the distribution of improvement and modified membrane, adjustment apertures rate and the hydrophilic hydrophobic balance of adjustment, membrane permeability and separation selectivity have been improved.
The present invention soaked surface to be obtained the organosilicon liquid that contains the linear oligomer of holding the silicon hydroxyl by hydrolysis reaction by D3, then add rare earth metal salt in this organosilicon liquid, film-forming at high temperature, take at magnesium product surface formation molecular structure is netted organic and inorganic composite membrane, this organic and inorganic composite membrane is comparatively fine and close, improves the erosion resistance of magnesium goods.
Embodiment
Below the present invention is described in further detail in conjunction with the embodiments respectively.
In accordance with the following methods the magnesium goods of aftermentioned embodiment and Comparative Examples carried out to pre-treatment:
The magnesium goods are polished, at first slightly polished with 200 order sand paper, carefully polished with 600 order sand paper subsequently, polish to the magnesium product surface and expose metalluster.The magnesium goods of polishing are inserted in the chemical alkali lye that temperature is 70～80 ℃ and flooded 20～40min with oil removing, and the composition of this chemistry alkali lye is: 40～60g/L NaOH, 50～70g/L Na
3pO
4, 20～30g/L Na
2cO
3, 5～10g/L Na
2siO
3.The magnesium goods of oil removing are dried up with distilled water flushing and with nitrogen, with standby.
Embodiment 1
In mass parts, by 10 parts of ethanol, 2 parts of ammonium acetates be added in the four-hole boiling flask that fills 60 parts of deionized waters fully to stir it is dissolved, the pH value of regulating this solution is 8.Then four-hole boiling flask is inserted in the digital display type thermostat water bath, and on four mouths on four-hole boiling flask, mechanical stirring device, thermometer, constant pressure funnel and prolong are installed respectively, thermometer will insert below the liquid level of flask.By 4 parts of D3 constant pressure funnel of packing into, open mechanical stirring device, the control rotating speed is 150rpm.After the reading of thermometer is 50 ℃, open the valve of constant pressure funnel, the liquid uniform speed slow in it is dripped, controlling the time dripped is 30min.After the liquid in constant pressure funnel dropwises, constant temperature 3h, make organosilicon liquid.
Add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 5g/L Ce (NO
3)
3, 2g/L H
2o
2, the 1g/L fluorochemical rare earth-organic silicon solution.Pretreated magnesium goods are inserted in the rare earth-organic silicon solution of aforementioned preparation and flood 2min, the operation of repeated impregnations 5 times.To insert in baking oven and make its film-forming under 90 ℃ through the impregnated magnesium goods of organosilicon liquid, be 60min set time.
Embodiment 2
In mass parts, by 30 parts of ethanol, 5 parts of ammonium acetates be added in the four-hole boiling flask that fills 90 parts of deionized waters fully to stir it is dissolved, the pH value of regulating this solution is 9.Then four-hole boiling flask is inserted in the digital display type thermostat water bath, and on four mouths on four-hole boiling flask, mechanical stirring device, thermometer, constant pressure funnel and prolong are installed respectively, thermometer will insert below the liquid level of flask.By 6 parts of D3 constant pressure funnel of packing into, open mechanical stirring device, the control rotating speed is 400rpm.After the reading of thermometer is 65 ℃, open the valve of constant pressure funnel, the liquid uniform speed slow in it is dripped, controlling the time dripped is 60min.After the liquid in constant pressure funnel dropwises, constant temperature 2.5h, make organosilicon liquid.
Add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 15g/L Ce (NO
3)
3, 6g/L H
2o
2, the 4g/L fluorochemical rare earth-organic silicon solution.Pretreated magnesium goods are inserted in the rare earth-organic silicon solution of aforementioned preparation and flood 6min, the operation of repeated impregnations 1 time.To insert in baking oven and make its film-forming under 115 ℃ through the impregnated magnesium goods of organosilicon liquid, be 35min set time.
Embodiment 3.
In mass parts, by 20 parts of ethanol, 3.5 parts of ammonium acetates be added in the four-hole boiling flask that fills 75 parts of deionized waters fully to stir it is dissolved, the pH value of regulating this solution is 9.5.Then four-hole boiling flask is inserted in the digital display type thermostat water bath, and on four mouths on four-hole boiling flask, mechanical stirring device, thermometer, constant pressure funnel and prolong are installed respectively, thermometer will insert below the liquid level of flask.By 5 parts of D3 constant pressure funnel of packing into, open mechanical stirring device, the control rotating speed is 350rpm.After the reading of thermometer is 60 ℃, open the valve of constant pressure funnel, the liquid uniform speed slow in it is dripped, controlling the time dripped is 45min.After the liquid in constant pressure funnel dropwises, constant temperature 165min, make organosilicon liquid.
Add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 10g/L Ce (NO
3)
3, 4g/L H
2o
2, the 2.5g/L fluorochemical rare earth-organic silicon solution.Pretreated magnesium goods are inserted in the rare earth-organic silicon solution of aforementioned preparation and flood 4min, the operation of repeated impregnations 3 times.To insert in baking oven and make its film-forming under 105 ℃ through the impregnated magnesium goods of organosilicon liquid, be 47min set time.
Embodiment 4
In mass parts, by 15 parts of ethanol, 3 parts of ammonium acetates be added in the four-hole boiling flask that fills 70 parts of deionized waters fully to stir it is dissolved, the pH value of regulating this solution is 10.Then four-hole boiling flask is inserted in the digital display type thermostat water bath, and on four mouths on four-hole boiling flask, mechanical stirring device, thermometer, constant pressure funnel and prolong are installed respectively, thermometer will insert below the liquid level of flask.By 4.5 parts of D3 constant pressure funnel of packing into, open mechanical stirring device, the control rotating speed is 300rpm.After the reading of thermometer is 55 ℃, open the valve of constant pressure funnel, the liquid uniform speed slow in it is dripped, controlling the time dripped is 35min.After the liquid in constant pressure funnel dropwises, constant temperature 175min, make organosilicon liquid.
Add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 8g/L Ce (NO
3)
3, 3g/L H
2o
2, the 2g/L fluorochemical rare earth-organic silicon solution.Pretreated magnesium goods are inserted in the rare earth-organic silicon solution of aforementioned preparation and flood 3min, the operation of repeated impregnations 4 times.To insert in baking oven and make its film-forming under 100 ℃ through the impregnated magnesium goods of organosilicon liquid, be 40min set time.
Embodiment 5
In mass parts, by 25 parts of ethanol, 4 parts of ammonium acetates be added in the four-hole boiling flask that fills 85 parts of deionized waters fully to stir it is dissolved, the pH value of regulating this solution is 11.Then four-hole boiling flask is inserted in the digital display type thermostat water bath, and on four mouths on four-hole boiling flask, mechanical stirring device, thermometer, constant pressure funnel and prolong are installed respectively, thermometer will insert below the liquid level of flask.By 5 parts of D3 constant pressure funnel of packing into, open mechanical stirring device, the control rotating speed is 250rpm.After the reading of thermometer is 60 ℃, open the valve of constant pressure funnel, the liquid uniform speed slow in it is dripped, controlling the time dripped is 50min.After the liquid in constant pressure funnel dropwises, constant temperature 160min, make organosilicon liquid.
Add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 12g/L Ce (NO
3)
3, 4.5g/L H
2o
2, the 3.5g/L fluorochemical rare earth-organic silicon solution.Pretreated magnesium goods are inserted in the rare earth-organic silicon solution of aforementioned preparation and flood 5min, the operation of repeated impregnations 2 times.To insert in baking oven and make its film-forming under 110 ℃ through the impregnated magnesium goods of organosilicon liquid, be 52min set time.
Embodiment 6
In mass parts, by 20 parts of ethanol, 3.5 parts of ammonium acetates be added in the four-hole boiling flask that fills 90 parts of deionized waters fully to stir it is dissolved, the pH value of regulating this solution is 10.5.Then four-hole boiling flask is inserted in the digital display type thermostat water bath, and on four mouths on four-hole boiling flask, mechanical stirring device, thermometer, constant pressure funnel and prolong are installed respectively, thermometer will insert below the liquid level of flask.By 5 parts of D3 constant pressure funnel of packing into, open mechanical stirring device, the control rotating speed is 250rpm.After the reading of thermometer is 63 ℃, open the valve of constant pressure funnel, the liquid uniform speed slow in it is dripped, controlling the time dripped is 40min.After the liquid in constant pressure funnel dropwises, constant temperature 170min, make organosilicon liquid.
Add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 10g/L Ce (NO
3)
3, 3.5g/L H
2o
2, the 3g/L fluorochemical rare earth-organic silicon solution.Pretreated magnesium goods are inserted in the rare earth-organic silicon solution of aforementioned preparation and flood 5min, the operation of repeated impregnations 1 time.To insert in baking oven and make its film-forming under 105 ℃ through the impregnated magnesium goods of organosilicon liquid, be 50min set time.
Comparative Examples
Undressed magnesium goods.
A small amount of water is splashed into as method surface-treated brass work surface as described in embodiment and Comparative Examples, until water droplet, after the abundant drawout in surface, adopt the German dataphysics OCA20 of company type contact angle measurement to be tested water contact angle.
Adopt the corrosion potential test of Japanese BAS company 2323 type potentiostats to above embodiment and Comparative Examples.Be specially, adopt three electrodes, using saturated calomel electrode as reference electrode, using platinum electrode as supporting electrode, test is at room temperature carried out.Solution medium is selected the NaCI solution that massfraction is 3.5%, with the sweep velocity of 180mV/min, is measured, and before test, sample is soaked to 20min in this solution medium, so that etchant solution evenly, stably immerses in the sample measured surface.According to gathering and process the electric current that obtains and the Tafel polarization curve of potential variation.The software carried with equipment is analyzed just and can be obtained corrosion potential this polarization curve.
Magnesium goods through above embodiment and Comparative Examples processing are carried out to the corrosion weight loss test.Adopt complete immersion zero-G test method, sample is immersed respectively in the NaCl solution of the NaOH solution of 20wt% and 3.5wt%, the corrosion experiment time length is respectively 240h and 340h, and keep the corrosive medium temperature is 40 ℃ simultaneously, then the weightlessness after its corrosion is measured, tried to achieve erosion rate.Before and after corrosion, sample is all through deionized water rinsing, ethanol ultrasonic cleaning, vacuum-drying, four steps of weighing.Erosion rate is calculated according to following formula:
Erosion rate=(quality after quality before corrosion-corrosion)/(etching time * corrosion surface is long-pending).
The above test result of embodiment and Comparative Examples is as follows:
As can be seen from the above table, the corrosion weight loss rate of 10wt%NaOH, the 3.5wt%NaCl of the surface treated magnesium goods of embodiment obviously reduces than the not surface treated magnesium goods of Comparative Examples; The negativity of the corrosion potential of the surface treated magnesium goods of embodiment significantly diminishes than the not surface treated magnesium goods of Comparative Examples, and this all illustrates that the surface treatment of the embodiment of the present invention has strengthened the erosion resistance of magnesium goods largely.The contact angle of the surface treated magnesium goods of embodiment has obvious change large than Comparative Examples, and this explanation hydrophobicity of magnesium goods after surface treatment is greatly improved.
Should be noted that and understand, in the situation that do not break away from the spirit and scope of accompanying claim the present invention for required protection, can make to the present invention of foregoing detailed description various modifications and improvement.Therefore, the scope of claimed technical scheme is not subject to the restriction of given any specific exemplary teachings.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.The person of ordinary skill in the field should understand, any improvement in the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. a method that adopts D3 organosilicon liquid to process the magnesium product surface, is characterized in that, comprises the following steps:
(1) according to mass fraction, 4～6 parts of hexamethyl cyclotrisiloxanes, 10～30 parts of ethanol and 2～5 parts of ammonium acetates are added in water and form mixed solution, the pH value of regulating this mixed solution is 8～11, under 50～65 ℃, disperses 1.5～3h to make organosilicon liquid;
(2) add Ce (NO in described organosilicon liquid
3)
3, H
2o
2and fluorochemical, fully dissolve to form and contain 5～15g/L Ce (NO
3)
3, 2～6g/L H
2o
2, 1～4g/L fluorochemical rare earth-organic silicon solution;
(3) the magnesium goods are inserted in described rare earth-organic silicon solution and flooded 2～6min;
(4) will toast 35～60min under 90～115 ℃ through the impregnated magnesium goods of described rare earth-organic silicon solution.
2. method according to claim 1, is characterized in that, in described step (1), the mass fraction of water is 60～90 parts.
3. method according to claim 1, it is characterized in that, described step is added to hexamethyl cyclotrisiloxane, ethanol and ammonium acetate in water and is specially in (1): at first ethanol and ammonium acetate are dissolved in the water, then hexamethyl cyclotrisiloxane is slowly dripped in the water that is dissolved with ethanol and ammonium acetate, the time of described dropping is 30～60min.
4. method according to claim 3, is characterized in that, in described step (1), the dispersion of mixed solution adopts the mechanical stirring that rotating speed is 150～400rpm.
5. method according to claim 3, is characterized in that, in described step (3), the number of times of dipping is 1～5 time.
6. method according to claim 1, is characterized in that, described fluorochemical is NaF and/or KF.
7. method according to claim 1, is characterized in that, according to by first to after order, described step (3) also comprises before successively to magnesium goods mechanical grinding, chemical alkali liquor oil removing and distilled water flushing.
8. method according to claim 7, is characterized in that, described chemical alkali liquor oil removing is specially: the magnesium goods are inserted in the chemical alkali lye that temperature is 70～80 ℃ and flooded 20～40min.
9. method according to claim 7, is characterized in that, described chemical alkali lye comprises 40～60g/L NaOH, 50～70g/L Na
3pO
4, 20～30g/L Na
2cO
3, 5～10g/L Na
2siO
3.
10. method according to claim 7, is characterized in that, described mechanical grinding is specially: first with 200 order sand paper, slightly polish, more carefully polish with 600 order sand paper.
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Application publication date: 20140101 |