CN102146573A - Method for preparing nano composite material by supercritical fluid electroforming - Google Patents
Method for preparing nano composite material by supercritical fluid electroforming Download PDFInfo
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- CN102146573A CN102146573A CN 201110060620 CN201110060620A CN102146573A CN 102146573 A CN102146573 A CN 102146573A CN 201110060620 CN201110060620 CN 201110060620 CN 201110060620 A CN201110060620 A CN 201110060620A CN 102146573 A CN102146573 A CN 102146573A
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 31
- 238000005323 electroforming Methods 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000012530 fluid Substances 0.000 title claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012266 salt solution Substances 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 239000002105 nanoparticle Substances 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 7
- 239000002113 nanodiamond Substances 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 150000002815 nickel Chemical class 0.000 claims description 6
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- -1 ether compound Chemical class 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000000306 recurrent effect Effects 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 150000001879 copper Chemical class 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 238000013268 sustained release Methods 0.000 claims description 2
- 239000012730 sustained-release form Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract 4
- 239000010410 layer Substances 0.000 description 17
- 230000000694 effects Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000746 Structural steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for preparing nano composite material by supercritical fluid electroforming, which comprises the following steps of: (1) adding metal salt solution, nano granules and composite additive into a reactor of an electroforming device, stirring uniformly, introducing carbon dioxide gas, and stirring at the temperature of between 35 and 50 DEG C under the pressure of 8 to 20MPa to generate supercritical fluid electroforming solution containing the nano granules; (2) setting pulse interval at 1 to 5 microseconds, setting the pulse width at 10 to 30 microseconds, setting the current density at 1 to 3A/dm<2>, switching on a direct-current power supply, and making the metal ions and the nano granules in the metal salt solution deposited on a cathode template together to obtain a nano composite electroforming layer; and (3) after the deposition is completed, obtaining the nano composite material by corresponding treatment. The method can electroform the nano composite material electroforming layer with uniform nano granule dispersion, flat surface, compact tissue, fine crystal grain and excellent performance.
Description
Technical field
The invention belongs to the electro-chemical machining field, be specifically related to the method that a kind of supercutical fluid electrotyping forming prepares nano composite material.
Background technology
The principle of composite electroformed technology is that the particle that will have property joins in the electroforming solution as pottery, diamond etc., utilize conductive grand master pattern (perhaps metal parts) to make negative electrode, the metal sheet that is used for electroforming is made anode, under electric field action, make metal ion constantly with particle capture, become metal in cathodic reduction, common deposited is on cathode surface.During this time, anode metal becomes ion continuously and is dissolved in the electroforming solution and replenishes, and makes GOLD FROM PLATING SOLUTION belong to ionic concentration and remains unchanged.When the composite electroforming deposit of negative electrode grand master pattern meets the requirements of thickness gradually, make itself and grand master pattern separate i.e. acquisition the electroforming part with excellent composite property opposite with the grand master pattern profile.If what negative electrode adopted is metal parts, can with the electroformed layer firm attachment on piece surface, form nano composite material protective layer (coating).Because the nano particle of unique properties is compounded in the middle of the metallic matrix, and the nano composite material of formation is having excellent properties aspect mechanical property and the physicals, thereby in fields such as machinery, chemical industry and automobiles the important application prospect is arranged.
But in composite electroformed process, especially in that evenly being compounded in, nano particle also has a lot of problems in the metal matrix material.Wherein the most outstanding is agglomeration traits and the relatively poor problem of macro-uniformity that nano particle is taken place in the electroforming process.Adopt modes such as stirring, ultrasonic vibration to handle the agglomeration of nano particle at present mostly, but because of grand master pattern (metal parts) different, electric field during electroforming, flow field uniformity are wayward etc., still can cause nanoparticle agglomerates and skewness in the nano combined electroformed layer.The employing dispersion agent that also has solves agglomeration traits, but because of the effective content that has dispersion agent be difficult to control and its influence the factors such as difficult grasp of the performance impact rule of cast layer, still can not solve nanoparticle agglomerates and problem pockety well.The reunion of nano particle and skewness will cause the cast layer mechanical property difference of different sites huge, have a strong impact on its use properties.
Pure material will be according to the difference of temperature and pressure, present change of state such as liquid, gas, solid, if raising temperature and pressure, come the variation of observation state, can find so, if reach specific temperature, pressure, the phenomenon that liquid and gas interface disappear can appear, this point is called as stagnation point, near stagnation point, all fluidic rerum naturas such as fluidic density, viscosity, solubleness, thermal capacity, specific inductivity can occur phenomenon jumpy takes place.For example: when the temperature and the pressure of water is elevated to (t=374.15 ℃ of stagnation point, when p=22.115MPa) above, just be in a kind of gaseous state that both had been different from, also be different from liquid and solid-state new fluid attitude--above-critical state, the water of this state promptly is referred to as supercritical water.The critical temperature of carbonic acid gas is 31.1 ℃, and emergent pressure is 7.39Mpa.Chinese patent literature CN101092716A(application number 200710021504.1) trickle electroforming process of a kind of supercutical fluid and device thereof are disclosed, the document mainly is the electrotyping forming micro-structure part, and be single metal plating layer, be provided with from the additive, electrical parameter and the anode and cathode that adopt, it is unsuitable for containing the composite electroformed moulding of nano particle.
Summary of the invention
The objective of the invention is in the electroforming process, easily reunite at nano particle, problems such as the electroformed layer homogeneity is wayward, provide a kind of nanoparticulate dispersed evenly, surfacing, dense structure, crystal grain supercutical fluid electrotyping forming tiny, excellent performance prepare the method for nano composite material.
The technical scheme that realizes the object of the invention is: a kind of supercutical fluid electrotyping forming prepares the method for nano composite material, have following steps: 1. in the reactor of electrotyping forming device, add metal salt solution, nano particle and composite additive, feed carbon dioxide after stirring, under 32 ℃～50 ℃ temperature and the pressure of 8MPa～20MPa, stir and generate the supercutical fluid electroforming solution that contains nano particle; Described electrotyping forming device also has negative electrode, anode, heater coil and mechanical stirrer; Described negative electrode comprises negative electrode template and cathode body, and described anode comprises anode template and anode body; 2. recurrent interval is set is 1 microsecond～5 microseconds, and pulse width is 10 microseconds～30 microseconds, and current density is 1A/dm
2～3A/dm
2, connect direct supply, the metal ion in the metal salt solution is deposited on the negative electrode template with nano particle, obtain nano combined electroformed layer; 3. after deposition finishes, obtain nano composite material by respective handling.
The metal salt solution of above-mentioned steps described in 1. is nickel salt solution or copper salt solution; Described nano particle is Nano diamond particle or nano-ceramic particle; Described composite additive is made up of dodecyl compounds and ether compound.The concentration of described metal salt solution is 200g/L～500g/L, and the concentration of described nano particle is 5g/L～15g/L, and the concentration of described composite additive is 0.3g/L～3.0g/L.
Above-mentioned steps 1. in preparation also can add boric acid during electroforming solution as the galvanic deposit sustained release dosage, the concentration of boric acid is 30g/L～60g/L.
The anode template of above-mentioned steps described in 1. is net-shaped metal plate; Negative electrode template and the equal horizontal positioned of anode template, and the anode template is positioned at the top of negative electrode template.
Described electrotyping forming device also has the adjustment plate; Step also is included in 2. in the electroforming process with described adjustment plate and adjusts distance between negative electrode template and the anode template in the scope of 1cm～5cm.
The described mechanical stirrer of above-mentioned steps in 1. has two, and alr mode is that level is to intermittently stirring.
Described negative electrode template is grand master pattern or metal parts.
Described negative electrode template is a grand master pattern; The respective handling of step described in 3. is: utilize thermal expansivity different of nano combined electroformed layer and grand master pattern, by heating or cooling, nano combined electroformed layer is separated from grand master pattern, obtain the nano combined electroformed layer opposite with the grand master pattern profile; Perhaps add acid/alkali grand master pattern is corroded, keep nano combined electroformed layer.
Described negative electrode template is a metal parts; The respective handling of step described in 3. is: by pickling, make nano combined electroformed layer firmly be deposited on the metal parts surface, obtain nano-composite plate.
The positively effect that the present invention has: (1) method of the present invention can electroforming go out nanoparticulate dispersed evenly, the nano composite material electroformed layer of tiny, the excellent performance of surfacing, dense structure, crystal grain.(2) selection of additive is the factor of supercutical fluid electrotyping forming most critical, the present invention is directed to the characteristics of the electroforming solution that contains nano particle, selected dodecyl compounds and ether compound to form composite additive, and the concentration of composite additive is controlled at 0.3g/L～3.0g/L, and the concentration of nano particle is controlled at 5g/L～15g/L, make nano particle and metal ion well electroforming on the negative electrode template, realize the supercutical fluid electrotyping forming of nano composite material.(3) the present invention is by adopting cancellated anode template and anode template and negative electrode template horizontal positioned and negative electrode template being positioned at negative electrode template top, adopt level to the alr mode at intermittence simultaneously, make nano particle that sedimentation trend is arranged in electroforming solution like this, thereby improve homogeneity and consistence in the nano combined electroforming process.(4) the present invention can form the nano-composite plate of excellent performance on the metal parts surface.(5) the present invention can be according to using needs, and by the control to nano particle add-on and electrical parameter, the crystal grain of preparing different nano-particle content, different thickness is tiny, composition even, the nano combined electroformed layer of excellent performance.
Description of drawings
Fig. 1 is the schematic representation of apparatus that method of the present invention adopts.
Fig. 2 is that A among Fig. 1 is to partial schematic diagram, in order to expression mechanical stirrer and reactor location relation.
Mark in the above-mentioned accompanying drawing is as follows:
Electrotyping forming device 1, reactor 11, reactor linings 11-1, reactor body 11-2, inlet mouth 12, negative electrode 13, negative electrode template 13-1, cathode body 13-2, anode 14, anode template 14-1, anode body 14-2, adjustment plate 15, heater coil 16, mechanical stirrer 17, leakage fluid dram 18, carbon dioxide steel cylinder 2, high-pressure pump 3, direct supply 4, negative pole 41, anodal 42.
Embodiment
(embodiment 1)
See Fig. 1, the device that the method for present embodiment adopts comprises electrotyping forming device 1, carbon dioxide steel cylinder 2, high-pressure pump 3 and direct supply 4.
With the Nano diamond matrix material is example, and the preparation method has following steps:
1. in the reactor 11 of electrotyping forming device 1, add nickel salt solution, boric acid, Nano diamond particle and composite additive, stirred 30 minutes, make its thorough mixing even.Wherein nickel salt solution is the mixing solutions of single nickel salt and nickelous chloride, and additive is sodium lauryl sulphate and ether.The concentration of each material is: single nickel salt 370g/L, nickelous chloride 74g/L, boric acid 44g/L, Nano diamond particle 12 g/L, sodium lauryl sulphate 0.5g/L, ether 0.8 g/L.
Start high-pressure pump 3, carbon dioxide in the carbon dioxide steel cylinder 2 is passed into the reactor 11 from inlet mouth 12, control pressure is 8MPa, make exchange current pass through heater coil 16 simultaneously, and make reactor body 11-2 under the effect of electromagnetic induction, be heated, by the control of the size of the strength of current of exchange current is controlled at 50 ℃ with temperature, under above-mentioned pressure and temperature, stirs and form and contain Nano diamond particulate supercutical fluid electroforming solution.
The negative pole 41 of direct supply 4 is electrically connected with the cathode body 13-2 of electrotyping forming device 1, and cathode body 13-2 is electrically connected with negative electrode template 13-1; The positive pole 42 of direct supply 4 is electrically connected with the anode body 14-2 of electrotyping forming device 1, adjusting plate 15 electrical connections is fixed on the anode body 14-2, anode template 14-1 is electrically connected to be fixed on by its mounting rod and adjusts on the plate 15, and be positioned at a corresponding open holes place that adjusts plate 15, thereby make anode template 14-1 be electrically connected with anode body 14-2 by adjusting plate 15.The recurrent interval that direct supply 4 is set is 3 microseconds, and pulse width is 20 microseconds, and current density is 2A/dm
2With negative electrode template 13-1 and anode template 14-1 horizontal positioned, and anode template 14-1 is positioned at the top of negative electrode template 13-1, adjust the position of the open holes on the plate 15 simultaneously by selection, and make that the distance between negative electrode template 13-1 and the anode template 14-1 is 3cm.
Connect direct supply 4, make nickel ion and Nano diamond particle deposit to negative electrode template 13-1 quickly and efficiently, the crystal grain that obtains required nano-particle content and thickness is tiny, composition even, the nano combined electroformed layer of excellent performance.In the whole process, mechanical stirrer 17 adopts radially and intermittently stirs.
3. the negative electrode template 13-1 of present embodiment is a grand master pattern, after electroforming finishes, mode by heating is separated nano combined electroformed layer from grand master pattern (negative electrode template 13-1), obtain promptly that nano particle is evenly distributed, dense structure, crystal grain are tiny, surfacing, nano composite material electroformed layer excellent performance, opposite with the grand master pattern profile, by leakage fluid dram 18 the supercutical fluid electroforming solution is imported in the gas-liquid separator at last, isolating carbon dioxide and electroforming solution are recovered to recycle in the retrieving arrangement respectively.
Claims (10)
1. a supercutical fluid electrotyping forming prepares the method for nano composite material, it is characterized in that having following steps:
1. in the reactor (11) of electrotyping forming device (1), add metal salt solution, nano particle and composite additive, feed carbon dioxide after stirring, under 32 ℃～50 ℃ temperature and the pressure of 8MPa～20MPa, stir and generate the supercutical fluid electroforming solution that contains nano particle; Described electrotyping forming device (1) also has negative electrode (13), anode (14), heater coil (16) and mechanical stirrer (17); Described negative electrode (13) comprises negative electrode template (13-1) and cathode body (14-2), and described anode (14) comprises anode template (14-1) and anode body (14-2);
2. recurrent interval is set is 1 microsecond～5 microseconds, and pulse width is 10 microseconds～30 microseconds, and current density is 1A/dm
2～3A/dm
2, connect direct supply (4), the metal ion in the metal salt solution is deposited on the negative electrode template (13-1) with nano particle, obtain nano combined electroformed layer;
3. after deposition finishes, obtain nano composite material by respective handling.
2. supercutical fluid electrotyping forming according to claim 1 prepares the method for nano composite material, it is characterized in that: the metal salt solution of step described in 1. is nickel salt solution or copper salt solution; Described nano particle is Nano diamond particle or nano-ceramic particle; Described composite additive is made up of dodecyl compounds and ether compound.
3. supercutical fluid electrotyping forming according to claim 1 and 2 prepares the method for nano composite material, it is characterized in that: the concentration of described metal salt solution is 200g/L～500g/L, the concentration of described nano particle is 5g/L～15g/L, and the concentration of described composite additive is 0.3g/L～3.0g/L.
4. supercutical fluid electrotyping forming according to claim 1 prepares the method for nano composite material, it is characterized in that: step 1. in preparation also can add boric acid during electroforming solution as the galvanic deposit sustained release dosage, the concentration of boric acid is 30g/L～60g/L.
5. supercutical fluid electrotyping forming according to claim 1 prepares the method for nano composite material, it is characterized in that: the anode template (14-1) of step described in 1. is net-shaped metal plate; Negative electrode template (13-1) and the equal horizontal positioned of anode template (14-1), and anode template (14-1) is positioned at the top of negative electrode template (13-1).
6. supercutical fluid electrotyping forming according to claim 1 prepares the method for nano composite material, it is characterized in that: described electrotyping forming device (1) also has adjustment plate (15); Step also is included in 2. in the electroforming process with described adjustment plate (15) and adjusts distance between negative electrode template (13-1) and the anode template (14-1) in the scope of 1cm～5cm.
7. supercutical fluid electrotyping forming according to claim 1 prepares the method for nano composite material, it is characterized in that: the described mechanical stirrer (17) of step in 1. has two, and alr mode is that level is to intermittently stirring.
8. supercutical fluid electrotyping forming according to claim 1 prepares the method for nano composite material, it is characterized in that: described negative electrode template (13-1) is grand master pattern or metal parts.
9. supercutical fluid electrotyping forming according to claim 8 prepares the method for nano composite material, it is characterized in that: described negative electrode template (13-1) is a grand master pattern; The respective handling of step described in 3. is: utilize thermal expansivity different of nano combined electroformed layer and grand master pattern, by heating or cooling, nano combined electroformed layer is separated from grand master pattern, obtain the nano combined electroformed layer opposite with the grand master pattern profile; Perhaps add acid/alkali grand master pattern is corroded, keep nano combined electroformed layer.
10. supercutical fluid electrotyping forming according to claim 8 prepares the method for nano composite material, it is characterized in that: described negative electrode template (13-1) is a metal parts; The respective handling of step described in 3. is: by pickling, make nano combined electroformed layer firmly be deposited on the metal parts surface, obtain nano-composite plate.
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