CN102978591B - Inside-outside differential pressure chemical plating equipment for porous ceramic tube and film coating method for porous ceramic tube - Google Patents
Inside-outside differential pressure chemical plating equipment for porous ceramic tube and film coating method for porous ceramic tube Download PDFInfo
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- CN102978591B CN102978591B CN201210545057.0A CN201210545057A CN102978591B CN 102978591 B CN102978591 B CN 102978591B CN 201210545057 A CN201210545057 A CN 201210545057A CN 102978591 B CN102978591 B CN 102978591B
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Abstract
The invention discloses inside-outside differential pressure chemical plating equipment for a porous ceramic tube and a film coating method for the porous ceramic tube. The inside and outside differential pressure chemical plating equipment is provided with an intratubular plating solution circulation loop and an intertubular plating solution circulation loop which are used for realizing intratubular plating and intertubular plating, and is also provided with a novel water bath heating system, so that temperature control, water control and stirring for water bath are realized. When plating is carried out outside the porous ceramic tube, the intratubular circulation loop is closed, and the intertubular circulation loop is closed when the plating is carried out inside the porous ceramic tube, so that independent plating is realized. The inside-outside differential pressure chemical plating equipment disclosed by the invention combines heating in water bath with the intratubular and intertubular plating solution circulation loops and has application values in the fields of electroplating or chemical plating inside and outside pipe fittings.
Description
Technical field
The invention belongs to electroless plating technology field, is specifically inside and outside wall pressure reduction electroless plating specific equipment and method about porous ceramic pipe.
Background technology
In producing, petroleum and chemical industry has broad application prospects in the high temperature catalyzed reaction such as the separation of high temperature hydrogen-containing gas and the hydrogenation of hydrocarbons, dehydrogenation and coupling.The perforated tube (pottery, silica glass, stainless steel etc.) of take is carrier, take the inorganic substances compound membrane pipe that palladium or palldium alloy be teleblem, there is the advantages such as high temperature resistant, corrosion-resistant, permeability coefficient is large, separation factor is high, metal consumption is few and preparation cost is low, can be used for preparing high-purity hydrogen and significantly improve reaction conversion ratio.Palladium or palldium alloy can be plated on porous ceramics inside pipe wall or outer wall, and electroless plating, as a kind of plated film means, has application very widely.By retrieval, there are two with chemical plating method and device-dependent patent documentation, wherein, name is called " a kind of method and apparatus of chemical plating outside bath ", publication number is the chemical plating method that the patent documentation of CN 1102862 relates to a kind of tubular workpiece inwall, but have the following disadvantages: the one, lack plating solution stirring system, affect quality of coating; The 2nd, can only plate single workpiece at every turn, productive rate is lower; The 3rd, plating solution can only flow through in managing, and can only plate the inwall of pipe fitting, rete limited location.Another name is called " Water bath heating chemical plating plant ", application number is that 03211289 patent documentation relates to a kind of heating in water bath equipment, but this equipment has the following disadvantages: the one, lack water bath monitoring water level and automatic watering system, and can not realize real automatization; The 2nd, the larger weight of volume is heavier, mobile inconvenience; The 3rd, lack plating solution stirring system, affect quality of coating.Above two patent documentations all have its weak point, and first is only to have highlighted plating fluid circulating system and film coating method, and does not introduce the heating system outside plating solution, and this film coating method is only applicable to manage interior plating; Second is only to have introduced heating in water bath system, and does not introduce the recycle system and the film coating method of plating solution itself.These two patent documentations are separated the heating system of electroless plating and plating fluid circulating system, do not realize both combinations, can not realize electroless plating automatization, large-scale development.
Summary of the invention
For this reason, for the problems referred to above, the present invention seeks to adapt to the demand of electroless plating automatization, mass-producing and inside and outside wall plated film, propose a kind of equipment and film coating method thereof that can be applied to the inside and outside wall pressure reduction electroless plating of porous ceramic pipe.
For achieving the above object, the present invention takes following technical scheme: the inside and outside wall pressure reduction chemical plating method of porous ceramic pipe, it is characterized in that: it is provided with two groups of circulation loops plating solution circulation loop in the pipe that first group of circulation loop is comprised of plating solution vacuum flask, recycle pump, plated film pipe fitting and connecting tube; Second group of circulation loop forms vacuum loop in pipe by plated film pipe fitting, connecting tube, vacuum pump, forms the outer plating solution circulation loop of pipe by plating solution vacuum flask, recycle pump, bath trough and connecting tube simultaneously; In two groups of circulation loops, plated film pipe fitting and bath trough are all placed in the water-bath environment of temperature controllable.When giving plated film pipe fitting inner wall plated film, start first group of circulation loop, close second group of circulation loop, plating solution in plating solution vacuum flask is in recycle pump is squeezed into plated film pipe fitting, plating solution constantly flows at pipe internal recycle, pipe is outer is water-bath environment, and pipe inner tube forms positive pressure differential outward, plating in completing after a period of time pipe; When giving plated film pipe fitting outer wall plated film, close first group of circulation loop, start second group of circulation loop, plating solution in plating solution vacuum flask is in recycle pump is driven into bath trough, plated film pipe fitting is immersed in bath trough, in pipe, vacuumize, pipe inner tube forms Negative Pressure Difference outward, plating outside completing after a period of time pipe.
In described two groups of circulation loops, plating solution vacuum flask, recycle pump and connecting tube in first group of loop, with plating solution vacuum flask, recycle pump and connecting tube in second group of circulation loop for sharing; During plating inner membrance, only need be by connecting tube and plated film pipe fitting internal communication; During plating adventitia, only connecting tube need be communicated with bath trough, plated film inside pipe fitting be communicated with vacuum pump simultaneously, form vacuum loop.
In the bottom of described plating solution vacuum flask and/or the bottom of bath trough one magnetic agitation mechanism is set, plating solution is stirred, this mechanism is included in the magnetic stir bar of placing in plating solution and the magnetic force placed outside equipment is wrapped and power supply.
Between described plated film pipe fitting and connecting tube, adopt rapid abutting joint head to be connected, while having a plated film pipe fitting in loop, adopt single passage rapid abutting joint head to connect, while having many plated film pipe fittings in loop, adopt hyperchannel rapid abutting joint head to connect; Described rapid abutting joint head adds set nut Sealing Method with the employing back taper sealing-ring that is connected between plated film pipe fitting.
When giving plated film pipe fitting inner wall plated film, the mode that pipe inner tube forms positive pressure differential is outward: increase the flowing pressure of plating solution in pipe; Or in plating solution, add certain density sucrose or rare earth ion, as Yttrium trinitrate, lanthanum nitrate etc., make to manage the inside and outside ionic concn pressure reduction that forms.
A kind of inside and outside wall pressure reduction chemical plating plant of realizing the porous ceramic pipe of aforesaid method, comprise heating in water bath system and plating fluid circulating system two portions, described heating in water bath system comprises water bath, temperature controller, and the temperature sensor arranging in water bath and heating tube, it is characterized in that: a boss concaving is arranged at the bottom of described water bath, on boss, be placed with bath trough, outside at described water bath is also provided with level sensor power supply and pilot circuit, water level sensor, automatically controlled water intaking valve is connected in pilot circuit, water level sensor is placed in water bath near top, water level sensor is with pointer, pointer is connected with the switch of water-level control circuit, on described bath trough, there are outer connect valve, external lower valve and water injection valve.Described plating fluid circulating system has two kinds of forms, and a kind of form is the interior plating solution circulation loop of pipe that comprises that plating solution vacuum flask, recycle pump, plated film pipe fitting and connecting tube form, and connecting tube is communicated with plated film pipe fitting; Described plated film pipe fitting is placed in bath trough, and two end supports is on cell wall; In described bath trough, fill water; Another kind of form is the interior vacuum loop of pipe that comprises that plated film pipe fitting, connecting tube, vacuum pump form, and the outer plating solution circulation loop of pipe of plating solution vacuum flask, recycle pump, bath trough and connecting tube composition; Described vacuum pump is communicated with plated film pipe fitting by connecting tube, and described plating solution vacuum flask, recycle pump are communicated with bath trough by connecting tube, and described plated film pipe fitting is placed in bath trough, and two end supports is on cell wall; In described bath trough, fill plating solution.
Bottom at described water bath is also provided with castor.
Outside at described water bath is also provided with magnetic agitation mechanism, and this mechanism comprises that magnetic agitation power supply, magnetic force are wrapped, magnetic stir bar, the wrapped outer bottom that is arranged on described plating solution vacuum flask outer bottom and described water bath of described magnetic force; Described magnetic stir bar is placed in described plating solution vacuum flask portion in portion and described water bath.
Between described connecting tube and plated film pipe fitting, adopt rapid abutting joint head to connect, when only having a plated film pipe fitting to be connected with connecting tube, adopt single passage rapid abutting joint head, when the many plated film pipe fittings while in parallel is connected with connecting tube, adopt hyperchannel rapid abutting joint head.
Described rapid abutting joint head comprises a tapered elastic rubber ring, a stainless steel sleeve and a set nut, the termination of plated film pipe fitting is first nested in tapered elastic rubber ring, both are together nested in stainless steel sleeve again, and stainless steel sleeve inside, with internal thread, screws with the outside screw of set nut; The other end of described stainless steel sleeve is connected with described connecting tube.
Another object of the present invention is to provide the inside and outside wall pressure reduction electroless plating film coating method of porous ceramic pipe.
When carrying out the inside pipe wall plated film of porous ceramic pipe, the method application of aforementioned equipment adopts following steps:
1) first by the temperature regulating device of heating in water bath system, level sensing device, and each parts connection of induction stirring mechanism puts in place;
2) plating solution vacuum flask, recycle pump, plated film pipe fitting are connected into plating solution circulation loop in pipe by connecting tube, and plated film pipe fitting is placed in bath trough, now bath trough outer connects valve, external lower valve cuts out, and water injection valve is opened, and makes the water in described water bath flow to bath trough;
3) press design temperature to water-bath heating system heating, start temperature controller and level sensing device is monitored simultaneously;
4) bath temperature reaches after preset value, starts recycle pump, makes the interior plating solution of plating solution vacuum flask in recycle pump is driven into plated film pipe fitting, plating solution constantly flows at pipe internal recycle, pipe is outer is water-bath environment, and pipe is interior, the outer positive pressure differential that forms of pipe, plating in completing after a period of time pipe;
When carrying out the pipe outer wall plated film of porous ceramic pipe, the method application of aforementioned equipment adopts following steps:
(1) first by the temperature regulating device of heating in water bath system, level sensing device, and each parts connection of induction stirring mechanism puts in place;
(2) plated film pipe fitting, vacuum pump are connected into vacuum loop in pipe by connecting tube, plating solution vacuum flask, recycle pump, bath trough are connected into the outer plating solution circulation loop of pipe by connecting tube simultaneously, and described plated film pipe fitting is placed in to described bath trough, now described bath trough outer connects valve, external lower valve is communicated with connecting tube, and water injection valve cuts out;
(3) press design temperature to water-bath heating system heating, start temperature controller and level sensing device is monitored simultaneously;
(4) bath temperature reaches after preset value, starts recycle pump, makes plating solution in plating solution vacuum flask in recycle pump is driven into bath trough, starts vacuum pump plated film inside pipe fitting is vacuumized, and pipe is interior, the outer Negative Pressure Difference that forms of pipe, plating outside completing after a period of time pipe.
In the inside and outside wall pressure reduction electroless plating film coating method of described porous ceramic pipe, when carrying out the inside pipe wall plated film of porous ceramic pipe, increase the flowing pressure of plating solution in plated film pipe fitting, form the inside and outside positive pressure differential plated film of pipe.
When carrying out the inside pipe wall plated film of porous ceramic pipe, in plating solution, add certain density sucrose or rare earth ion, increase the inside and outside ionic concn of pipe poor, form the inside and outside positive pressure differential plated film of pipe.
In the inside and outside wall pressure reduction electroless plating film coating method of described porous ceramic pipe, no matter when carrying out the inside pipe wall plated film of porous ceramic pipe or managing outer wall plated film, in plated film, start induction stirring mechanism and carry out plating solution stirring.
The present invention is owing to taking above technical scheme, and it has the following advantages the present invention:
1, the present invention has designed automatization water-bath heating system and two cover plating fluid circulating systems, automatization water-bath heating system is on the basis of the existing water-bath technology of succession, having increased automatic water level control and temperature controls, in the bottom of water bath, also increased castor and magnetic agitation mechanism, water bath has been realized that water temperature is controlled, water level is controlled, can have been stirred; Two cover plating fluid circulating systems are a set of is internal circulation system, and a set of is external circulating system, and application internal circulation system has been realized the method for inside pipe wall pressure reduction plating, and application external circulating system has been realized the method for pipe outer wall pressure reduction plating, and this is to belong to Promethean.New system has larger competitive power in plating or the electroless plating field of the inside and outside wall of pipe fitting.
2, the bath trough in water bath of the present invention can meet respectively the demand of the inside and outside wall film of plating pipe fitting, form pressure reduction plated film, optimize quality of coating: external valve and lower external valve on one be set respectively coating bath is upper and lower, upside also has a water injection valve, when plating pipe fitting inner wall, upper and lower external valve cuts out, and water injection valve is opened, and water bath communicates with bath trough; In pipe fitting, connect plating fluid circulating system, make plating solution realize constant temperature, positive pressure differential plated film.Stirring system under bath trough has guaranteed the homogeneity of plating solution; When plating pipe fitting outer wall, upper and lower external valve connects plating fluid circulating system, circulation plating solution in bath trough, water injection valve cuts out, inside pipe fitting connects pumped vacuum systems, realizes Negative Pressure Difference plated film, improves the density of rete and the bonding strength that improves rete and pipe fitting matrix.
3, plating fluid circulating system of the present invention selects hyperchannel rapid abutting joint head to realize the quick connection of multi-pipeline, can meet multitube part, the requirement of different size plating simultaneously, and the use of back taper sealing-ring screw thread sealing-in method in pipeline connects also guaranteed the stopping property of system.
4, water bath bottom is provided with four wheels, has realized the convenient mobile of equipment.
5, when plating pipe outer wall film, pipe fitting is vacuumized and mobilization dynamic support, negative pressure is effective.
Accompanying drawing explanation
Plating solution circulation loop schematic diagram when Fig. 1 is the interior plated film of pipe of the present invention;
Vacuum loop schematic diagram when Fig. 2 a is the outer plated film of pipe of the present invention;
Plating solution circulation loop schematic diagram when Fig. 2 b is the outer plated film of pipe of the present invention;
Fig. 3 is the structural representation of filming equipment of the present invention;
Fig. 4 is the STRUCTURE DECOMPOSITION figure of the rapid abutting joint head at C place in Fig. 1.
Fig. 5 a is that the present invention does not add the film surface shape appearance figure after positive pressure differential (with no pressure) inside pipe wall plated film;
Fig. 5 b is that the present invention adds the film surface shape appearance figure after positive pressure differential inside pipe wall plated film;
Fig. 6 a is that the present invention does not add the film surface shape appearance figure after Negative Pressure Difference (with no pressure) pipe outer wall plated film;
Fig. 6 b is that the present invention adds the film surface shape appearance figure after Negative Pressure Difference pipe outer wall plated film;
In figure, 1-plating solution vacuum flask, 2-recycle pump, 3-plated film pipe fitting, 4-connecting tube, 5-vacuum pump, 6-bath trough, 7-water bath, 8-magnetic stir bar, 9-magnetic force is wrapped, 10-rapid abutting joint head, 11-temperature controller, 12-temperature sensor, 13-heating tube, 14-stainless steel casing, 15-plastic, thermal-insulation layer, 16-urethane liner, 17-boss, 18-magnetic agitation power supply, 19-level sensor power supply, 20-water level sensor, 21-automatically controlled water intaking valve, 22-castor, 23-stainless steel casing, 24-ammonia ester liner, 25-connect valve outward, 26-external lower valve 26, 27-water injection valve, 28-tapered elastic rubber ring, 29-stainless steel sleeve, 30-set nut.
Embodiment
Below in conjunction with accompanying drawing, illustrate embodiments of the present invention.
The present invention is the method and apparatus for the poor electroless plating of inside and outside wall pressure of porous ceramics pipe fitting, it has two groups of circulation loops, first group of circulation loop as shown in Figure 1, by plating solution vacuum flask 1, recycle pump 2, plated film pipe fitting 3 and connecting tube 4, form plating solution circulation loop in a pipe, for inside pipe wall plated film.Second group of circulation loop is as shown in Fig. 2 a～2b, by plated film pipe fitting 3, connecting tube 4, vacuum pump 5, form vacuum loop in a pipe, by plating solution vacuum flask 1, recycle pump 2, bath trough 6 and connecting tube 4, form the outer plating solution circulation loop of a pipe simultaneously, plated film pipe fitting 3 is placed in bath trough 6, realizes pipe outer wall plated film.Two groups of loops are all placed in the water bath 7 of temperature controllable, guarantee film coating environment temperature.
When giving inside pipe wall plated film, start first group of loop, close second group of loop.Plating solution in plating solution vacuum flask 1 is in recycle pump 2 is squeezed into plated film pipe fitting 3, and plating solution constantly flows at pipe internal recycle, completes electroless plating through after a period of time.During plated film, plated film pipe fitting 3 is placed in to water bath 7, keeps bath temperature, suitably increase the flowing pressure of plating solution in pipe, make overpressure be greater than the water-bath pressure outside pipe, form the inside and outside positive pressure differential plated film of pipe; Or in plating solution, add certain density sucrose or rare earth ion (as Yttrium trinitrate, lanthanum nitrate etc.), to increase positive pressure differential inside and outside the inside and outside ionic concn pressure initiation pipe of pipe.
When giving pipe outer wall plated film, close first group of loop, start second group of loop.Plating solution in plating solution vacuum flask 1 is in recycle pump 2 is driven into bath trough 6, and plated film pipe fitting 3 is immersed in bath trough 6, owing to being stopped up by vacuum loop in pipe fitting, so plating solution can only flow through from pipe outer wall, realizes the outer plated film of pipe.Suitably add the outer plating solution circulating pressure of bassoon, in the pipe in addition consisting of plated film pipe fitting 3, connecting tube 4, vacuum pump 5, vacuum loop is manufactured negative pressure, has just formed pipe outer wall Negative Pressure Difference plated film.
In two groups of above-mentioned loops, can have partial common, as the plating solution vacuum flask 1 in first group of loop, recycle pump 2 and connecting tube 4, can with second group of loop in plating solution vacuum flask 1, recycle pump 2 and connecting tube 4 share.Plating is during inner membrance, only connecting tube 4 need be communicated with plated film pipe fitting 3 by rapid abutting joint 10; During plating adventitia, only connecting tube 4 need be communicated with bath trough 6; While plating adventitia, plated film pipe fitting 3 is communicated with to formation vacuum loop with connecting tube 4, vacuum pump 5 by rapid abutting joint 10 simultaneously.
For strengthening homogeneity and the velocity of flow of plating solution, the bottom of the plating solution vacuum flask 1 of being everlasting and/or the bottom of bath trough 6 arrange a magnetic agitation mechanism, and this mechanism is included in and in plating solution, places magnetic stir bar 8 and the magnetic force wrapped 9 of placement equipment outside.
Above-mentioned plating solution vacuum flask 1 effect is to provide constant temperature plating solution, therefore also can be with selecting other storing units.
Each group can arrange many plated film pipe fittings 3 in loop, by hyperchannel rapid abutting joint 10, is connected with connecting tube 4, as shown in Figure 1, realizes the requirement of a loop multi-work piece while plating.
For taking into account the poor electroless plating of inside and outside wall pressure, in same equipment, can both realize, and make plating solution system and heat-insulation system be applied to electroless plating simultaneously, the present invention arranges the inside and outside wall pressure reduction chemical plating plant that a specific equipment is porous ceramic pipe, comprises heating in water bath system and plating fluid circulating system two portions.
As shown in Figure 3, heating in water bath system of the present invention is used for reference the part-structure of existing heating in water bath equipment, comprises water bath 7, temperature controller 11, temperature sensor 12, heating tube 13.Water bath 7 consists of 16 3 layers of stainless steel casing 14, plastic, thermal-insulation layer 15 and urethane liners.Temperature controller 11 is arranged on water bath outside, is connected with temperature sensor 12, heating tube 13 simultaneously, and temperature sensor 12 is placed on close top in water bath, and heating tube 13 is placed in water bath near bottom.
The local improvement that the present invention does water bath 7 is, a boss concaving 17 is produced in the bottom of water bath 7, places bath trough 6 on boss 17, places magnetic stir bar 8 in bath trough 6, at the outer bottom of boss 17, is equipped with magnetic force wrapped 9.
In addition, in the outside of water bath 7, be also provided with magnetic agitation power supply 18 and level sensor power supply 19.Magnetic agitation power supply 18 is connected with magnetic force wrapped 9; Level sensor power supply 19 and pilot circuit, water level sensor 20, automatically controlled water intaking valve 21 are connected in pilot circuit, and water level sensor 20 is placed on close upper position in water bath, and automatically controlled water intaking valve 21 is placed in water bath near bottom.Upper and lower the floating of liquid buoyancy promotion water level sensor 20 pointers in application water bath, pointer is connected with pilot circuit, the opening and closing of the upper and lower unsteady detonator circuit switch of pointer, the opening and closing of circuit are indicated the opening and closing of automatically controlled water intaking valve 21, complete water level controlled.Outer bottom at water bath 7 is provided with castor 22.
On boss 17 in water bath 7, place bath trough 6, bath trough 6 is by stainless steel casing 23 and urethane liner 24 is two-layer forms; On bath trough 6, there are outer connect valve 25, external lower valve 26 and water injection valve 27.
As shown in Figure 1, 2, plating fluid circulating system of the present invention has two kinds of forms, and a kind of is the interior plating solution circulation loop of pipe that comprises that plating solution vacuum flask 1, recycle pump 2, plated film pipe fitting 3 and connecting tube 4 form.Plating solution vacuum flask 1 water supply valve device for cleaning pipeline is crossed connecting tube 4 and is connected with recycle pump 2, and the other end of recycle pump 2 is connected with one end of plated film pipe fitting 3 by connecting tube 4 again; 1 time water valve device for cleaning pipeline of plating solution vacuum flask is crossed connecting tube 4 and is connected with the other end of plated film pipe fitting 3.Junction at connecting tube 4 with plated film pipe fitting 3, adopt hyperchannel or single passage rapid abutting joint 10, when only having a plated film pipe fitting 3 to be connected with connecting tube 4, adopt single passage rapid abutting joint head, when many plated film pipe fittings 3 while in parallel is connected with connecting tube 4, adopt hyperchannel rapid abutting joint head.Plated film pipe fitting 3 is placed in bath trough 6, and two ends are supported in groove through cell wall by rapid abutting joint head; Bath trough 6 is placed in water bath 7.But for plating in pipe, now outer in bath trough connects valve 25, external lower valve 26 cuts out, and water injection valve 27 is opened, and what in bath trough 6, inject is water; Now also can say, the plated film pipe fitting 3 that connects loop is to be directly placed in water bath 7.In plating solution vacuum flask 1, be placed with magnetic stir bar 8, vacuum flask outer setting has magnetic force wrapped 9, is connected with magnetic force power supply.
Another kind of form is the interior vacuum loop of pipe that comprises that plated film pipe fitting 3, connecting tube 4, vacuum pump 5 form, and the outer plating solution circulation loop of pipe of plating solution vacuum flask 1, recycle pump 2, bath trough 6 and connecting tube 4 compositions.The other end that the discrepancy end of vacuum pump 5 respectively connects 4, two connecting tubes 4 of a connecting tube is connected respectively to the two ends of plated film pipe fitting 3, and there is rapid abutting joint 10 plated film pipe fitting 3 ports, and connecting tube 4 and rapid abutting joint 10 is connected.Rapid abutting joint 10 have single passage and hyperchannel minute, different forms is with internal recycle loop.
The outer plating solution circulation loop of pipe that plating solution vacuum flask 1, recycle pump 2, bath trough 6 and connecting tube 4 form, plating solution vacuum flask 1 water supply valve device for cleaning pipeline is crossed connecting tube 4 and is connected with recycle pump 2, the other end of recycle pump 2 is connected with the outer valve 25 that connects of bath trough 6 by connecting tube 4 again, 1 time water valve device for cleaning pipeline of plating solution vacuum flask is crossed connecting tube 4 and is connected with the external lower valve 26 of bath trough 6, and now the water injection valve 27 of bath trough 6 cuts out.Plated film pipe fitting 3 is placed in bath trough 6, and two ends are supported in groove through cell wall by rapid abutting joint head.Bath trough 6 is placed in water bath 7 equally.Now, except bath trough 6 bottoms arrange magnetic agitation mechanism, can in plating solution vacuum flask 1 bottom, magnetic agitation mechanism be set, to strengthen mixing effect simultaneously.
Two kinds of forms of above-mentioned plating solution system, one is for plating inside pipe wall, one is that both can not enable simultaneously for plating pipe outer wall.
The above-mentioned single passage of mentioning or hyperchannel rapid abutting joint 10 is connected with plated film pipe fitting 3, is to adopt back taper sealing-ring to add locking screw Sealing Method.As shown in Figure 4, rapid abutting joint 10 comprises a tapered elastic rubber ring 28, a stainless steel sleeve 29 and a set nut 30.Tapered elastic rubber ring 28 is first inserted in the termination of plated film pipe fitting 3, both are nested into plated film pipe fitting 3 and tapered elastic rubber ring 28 in stainless steel sleeve 29 again, and stainless steel sleeve 29 inside are with internal thread, and set nut 30 is with outside screw, set nut 30 is screwed on, reached the effect of locking and sealing.The other end of stainless steel sleeve 29 is connected with connecting tube 4 again.
On the connecting tube of the above-mentioned connecting tube of mentioning 4 and plating solution vacuum flask 1 or pump, appropriate location all arranges valve, and this belongs to routine techniques, at this, does not do too much introduction.
The above-mentioned plating solution vacuum flask of mentioning 1 effect is to provide constant temperature plating solution, therefore also can be with selecting other storing units.
Below two case study on implementation.
Embodiment 1: inside pipe wall positive pressure differential plated film
(1) water-bath system connects.According to Fig. 3, water bath 7 each systems are ready to, the inside packs water into, and opening power temperature defaults to 40～60 ℃; According to the weight ratio of 1:100, in plating solution, add the rare earth ion (as Yttrium trinitrate, lanthanum nitrate etc.) of sucrose or 0.1～0.5g/l; Bath trough 6 is placed in water bath 7, connects valve 24 outward and external lower valve 25 cuts out, and water injection valve 26 is opened, and makes water in water bath 7 inject bath trough.
(2) plating fluid circulating system connects.By first group of loop requirement, with connecting tube 4, plating solution vacuum flask 1, recycle pump 2, plated film pipe fitting 3 are connected, open magnetic agitation power supply, give wrapped 9 energisings of magnetic force of plating solution vacuum flask 1 bottom, plated film pipe fitting 3 is placed in bath trough 6, and plating solution injects vacuum flask 1.
(3) when the interior temperature of water bath 7 is raised to design temperature, open each valve, ON cycle pump 2, inside pipe wall positive pressure differential electroless plating starts.Thicknesses of layers according to actual needs, continues plated film 2～6 hours, after plated film finishes, first closes water valve under vacuum flask, and the complete plating solution of question response is all pressed into vacuum flask by recycle pump, waste liquid recycling.
Due to what adopt, it is pressure reduction plated film, the plated film time significantly shortens, obtain the rete that 8 μ m are thick and can taper to 3 hours by original 8 hours, effect is enhanced about more than once, and the rete obtaining is more fine and close, rete and basal body interface bonding force rise to 45N(film surface shape appearance figure by original 25N and see Fig. 5 a, Fig. 5 b).In addition, that whole coating process can be realized is temperature automatically controlled, control water, plating solution automated cycle, and a people can operate multiple devices, and single device, owing to having adopted hyperchannel rapid abutting joint technology, can complete the plated film of multi units tube part simultaneously, accomplishes scale production.
Embodiment 2: pipe outer wall Negative Pressure Difference plated film
(1) water-bath system connects.According to Fig. 3, water bath 7 each systems are ready to, the inside packs water into, and opening power temperature defaults to 50～70 ℃, opens magnetic agitation power supply, gives wrapped 9 energisings of magnetic force of bath trough 6 bottoms.
(2) plating fluid circulating system connects.By second group of loop requirement, with connecting tube 4, the outer valve 24 that connects of plating solution vacuum flask 1, recycle pump 2 and bath trough 6 is connected with external lower valve 25, the water injection valve 26 of bath trough 6 cuts out, and makes by vacuum flask 1, to flow into bath trough 6 containing the plating solution of palladium ion or silver ions or cupric ion.Bath trough 6 is placed in water bath 7, and plated film pipe fitting 3 is placed in bath trough 6.
(3) vacuum-lines connects.The two ends of plated film pipe fitting 3 are connected with vacuum pump 5 by connecting tube 4, form vacuum loop, in pipe fitting, vacuumize.
(4) when the interior temperature of water bath 7 is raised to design temperature, open each valve, ON cycle pump 2, vacuum pump 5, pipe outer wall Negative Pressure Difference plated film starts.Thicknesses of layers according to actual needs, continues plated film 2～6 hours, after plated film finishes, first closes water valve under vacuum flask, and the complete plating solution of question response is all pressed into vacuum flask by recycle pump, waste liquid recycling.
Due to what adopt, it is pressure reduction plated film, the plated film time significantly shortens, obtain the rete that 8 μ m are thick and can taper to 4 hours by original 8 hours, effect doubles, and the rete obtaining is more fine and close, rete and basal body interface bonding force rise to 40N(film surface shape appearance figure by original 25N and see Fig. 6 a, Fig. 6 b).In addition, that whole coating process can be realized is temperature automatically controlled, control water, plating solution automated cycle, and a people can operate multiple devices, and single device, owing to having adopted hyperchannel rapid abutting joint technology, can complete the plated film of multi units tube part simultaneously, accomplishes scale production.
Claims (10)
1. the inside and outside wall pressure reduction chemical plating plant of a porous ceramic pipe, comprise heating in water bath system and plating fluid circulating system two portions, described heating in water bath system comprises water bath, temperature controller, and the temperature sensor being connected with temperature controller and the heating tube that in water bath, arrange, described plating solution system comprises a bath trough, it is characterized in that:
The bottom of described water bath is manufactured with to a boss to groove indent, on boss, places described bath trough, at boss outer bottom, be provided with magnetic agitation mechanism;
On described bath trough, be provided with outer connect valve, external lower valve and water injection valve;
Described heating in water bath system also includes level sensing device;
Described plating fluid circulating system has two kinds of forms, a kind of is to comprise plating solution vacuum flask, recycle pump, plated film pipe fitting is interior, plating solution circulation loop in the pipe composing in series by connecting tube, wherein said plated film pipe fitting is porous ceramic pipe, be placed in described bath trough, in described bath trough, be connected with the water in heating in water bath system, in plating solution vacuum flask, plating solution is in recycle pump is driven into plated film pipe fitting, increasing the flowing pressure of plating solution in pipe makes overpressure be greater than the water-bath pressure outside pipe, form the inside and outside positive pressure differential plated film of pipe, or, in plating solution, add sucrose or rare earth ion to increase in pipe, outer ionic concn is poor, form in pipe, outer positive pressure differential plated film, another kind is to comprise vacuum pump, plated film pipe fitting, vacuum loop in the pipe composing in series by connecting tube, and comprise plating solution vacuum flask, recycle pump, bath trough, the outer plating solution circulation loop of pipe composing in series by connecting tube, wherein said plated film pipe fitting is porous ceramic pipe, be placed in described bath trough, in described bath trough, fill plating solution, in plating solution vacuum flask, plating solution is in recycle pump is driven into bath trough, vacuum pump vacuumizes plated film inside pipe fitting, formation Negative Pressure Difference plated film in pipe, outside pipe.
2. the inside and outside wall pressure reduction chemical plating plant of porous ceramic pipe according to claim 1, it is characterized in that: between described connecting tube and plated film pipe fitting, adopt rapid abutting joint head to connect, when only having a plated film pipe fitting to be connected with connecting tube, adopt single passage rapid abutting joint head, when having the many plated film pipe fittings while in parallel to be connected with connecting tube, adopt hyperchannel rapid abutting joint head.
3. the inside and outside wall pressure reduction chemical plating plant of porous ceramic pipe according to claim 2, it is characterized in that: described rapid abutting joint head comprises a tapered elastic rubber ring, a stainless steel sleeve and a set nut, the termination of described plated film pipe fitting is nested in tapered elastic rubber ring, both are together nested in stainless steel sleeve again, stainless steel sleeve inside is with internal thread, screw with the outside screw of set nut, the other end of described stainless steel sleeve is connected with described connecting tube.
4. the inside and outside wall pressure reduction chemical plating plant of porous ceramic pipe according to claim 1, it is characterized in that: described level sensing device is included in level sensor power supply and the pilot circuit of described water bath outer setting, at inner water level sensor and the automatically controlled water intaking valve arranging of water bath, described water level sensor and automatically controlled water intaking valve are connected in pilot circuit, the pointer of water level sensor is connected with the switch of pilot circuit, the unlatching of automatically controlled water intaking valve described in described on-off control.
5. the inside and outside wall pressure reduction chemical plating plant of porous ceramic pipe according to claim 1, it is characterized in that: described magnetic agitation mechanism, comprise that to be arranged on the magnetic force of described water bath boss outer bottom wrapped, and be placed on the magnetic stir bar in described bath trough; Also comprise that to be arranged on the magnetic force of described plating solution vacuum flask outer bottom wrapped, and be placed on the magnetic stir bar in described plating solution vacuum flask.
6. the inside and outside wall pressure reduction chemical plating plant of porous ceramic pipe according to claim 1, is characterized in that: the bottom at described water bath is provided with castor.
7. an inside and outside wall pressure reduction electroless plating film coating method for the porous ceramic pipe that the equipment of application as described in one of claim 1～6 is implemented, is characterized in that:
When carrying out the inside pipe wall plated film of porous ceramic pipe, adopt following steps:
1) first by the temperature regulating device of heating in water bath system, level sensing device, and each parts connection of induction stirring mechanism puts in place;
2) plating solution vacuum flask, recycle pump, plated film pipe fitting are connected into plating solution circulation loop in pipe by connecting tube, and plated film pipe fitting is placed in bath trough, now bath trough outer connects valve, external lower valve cuts out, and water injection valve is opened, and makes the water in described water bath flow to bath trough;
3) press design temperature to water-bath heating system heating, start temperature controller and level sensing device is monitored simultaneously;
4) bath temperature reaches after preset value, starts recycle pump, makes the interior plating solution of plating solution vacuum flask in recycle pump is driven into plated film pipe fitting, plating solution constantly flows at pipe internal recycle, pipe is outer is water-bath environment, and pipe is interior, the outer positive pressure differential that forms of pipe, plating in completing after a period of time pipe;
When carrying out the pipe outer wall plated film of porous ceramic pipe, adopt following steps:
(1) first by the temperature regulating device of heating in water bath system, level sensing device, and each parts connection of induction stirring mechanism puts in place;
(2) plated film pipe fitting, vacuum pump are connected into vacuum loop in pipe by connecting tube, plating solution vacuum flask, recycle pump, bath trough are connected into the outer plating solution circulation loop of pipe by connecting tube simultaneously, and described plated film pipe fitting is placed in to described bath trough, now described bath trough outer connects valve, external lower valve is communicated with connecting tube, and water injection valve cuts out;
(3) press design temperature to water-bath heating system heating, start temperature controller and level sensing device is monitored simultaneously;
(4) bath temperature reaches after preset value, starts recycle pump, makes plating solution in plating solution vacuum flask in recycle pump is driven into bath trough, starts vacuum pump plated film inside pipe fitting is vacuumized, and pipe is interior, the outer Negative Pressure Difference that forms of pipe, plating outside completing after a period of time pipe.
8. the inside and outside wall pressure reduction electroless plating film coating method of porous ceramic pipe according to claim 7: it is characterized in that: when carrying out the inside pipe wall plated film of porous ceramic pipe, increase the flowing pressure of plating solution in plated film pipe fitting, form the inside and outside positive pressure differential plated film of pipe.
9. the inside and outside wall pressure reduction electroless plating film coating method of porous ceramic pipe according to claim 7: it is characterized in that: when carrying out the inside pipe wall plated film of porous ceramic pipe, in plating solution, add certain density sucrose or rare earth ion, increase the inside and outside ionic concn of pipe poor, form the inside and outside positive pressure differential plated film of pipe.
10. the inside and outside wall pressure reduction electroless plating film coating method of porous ceramic pipe according to claim 7: it is characterized in that: no matter while carrying out the inside pipe wall plated film of porous ceramic pipe or pipe outer wall plated film, in plated film, start induction stirring mechanism and carry out plating solution stirring.
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| CN106435536B (en) * | 2016-11-18 | 2018-08-28 | 中国科学院金属研究所 | For slender rectangular tube inner surface chemical plating and the device and method of Ni-P |
| CN108251822A (en) * | 2017-12-25 | 2018-07-06 | 中国石油天然气股份有限公司 | Internal corrosion prevention construction device and method for oil and gas field pipeline based on chemical plating |
| CN108394856A (en) * | 2018-01-31 | 2018-08-14 | 华东师范大学 | The method that transparent material is internally integrated three-dimensional conductive metal micro-nanostructure |
| CN113564591B (en) * | 2021-08-03 | 2022-08-09 | 江苏鹏举半导体设备技术有限公司 | Porous gas flow distribution plate film coating system |
| CN118668196A (en) * | 2024-08-23 | 2024-09-20 | 中国科学院金属研究所 | In-situ online chemical plating method for copper alloy heat transfer tube of heat exchanger |
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