CN103173842B - The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment - Google Patents

The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment Download PDF

Info

Publication number
CN103173842B
CN103173842B CN201310057756.5A CN201310057756A CN103173842B CN 103173842 B CN103173842 B CN 103173842B CN 201310057756 A CN201310057756 A CN 201310057756A CN 103173842 B CN103173842 B CN 103173842B
Authority
CN
China
Prior art keywords
high pressure
reactor
pressure
electroplate liquid
electroplating technology
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201310057756.5A
Other languages
Chinese (zh)
Other versions
CN103173842A (en
Inventor
鄢浩
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Jingshiyuan Energy And Environmental Protection Research Institute Co ltd
Original Assignee
University of Shanghai for Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Shanghai for Science and Technology filed Critical University of Shanghai for Science and Technology
Priority to CN201310057756.5A priority Critical patent/CN103173842B/en
Publication of CN103173842A publication Critical patent/CN103173842A/en
Application granted granted Critical
Publication of CN103173842B publication Critical patent/CN103173842B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

Carry out the device of electroplating technology and electroplate liquid development experiments under the invention discloses a kind of hyperbaric environment, comprise trapezoidal reactor, anode, negative electrode, external source, high pressure electrochemistry reactor, CO 2delivery system, pressure control system, temperature controlling system and stirring system, and have and be applicable to electrode under condition of high voltage and the insulation and sealing structure be connected between reaction vessel, the defect of reaction under high pressure condition cannot be met at solution normal pressure hull cell testing device, and overcome the not competent condition of high voltage of the insulating material particularly overcritical or subcritical CO such as the conventional synthetic glass of normal pressure hull cell testing device or rigid polyvinyl chloride 2in easily to expand the problem of deterioration and electrode sealed insulation, can obtain the electroplating effect at wider current density range plating solution easily at short notice, be high pressure CO 2electroplating technology research under existing, plating solution formula exploitation and electroplating technology control to offer help.

Description

The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment
Technical field
The present invention relates to a kind of high pressure electrochemistry experiment conversion unit, particularly a kind of plant and instrument electroplating research and electroplating technology control, with supercritical CO 2or subcritical CO 2carry out Hull cell test in the homogeneous phase that/conductive soln is formed and heterogeneous system, under being applied to hyperbaric environment, carry out the development experiments of electroplating technology and electroplate liquid.
Background technology
Electroplating technology utilizes electrochemical principle at the process for treating surface of substrate deposit metal or alloy coating, is that metal membrane material prepares one of most important means, is widely applied in national economy every profession and trade.The fast development of current modern industry and technology, has higher requirement to the environmental protection of electroplating technology and the functional of coating.Find after deliberation, in conductive soln, introduce overcritical or subcritical CO 2inherently can improve the quality of metal plating as electrochemical reaction medium, effectively solve the pollution problem of conventional plating process.Disclose at present with supercritical CO 2or subcritical CO 2electric plating method is carried out, a kind of supercritical CO disclosed in patent WO02/016673A1 in the homogeneous phase that/conductive soln is formed and heterogeneous system 2electric plating method is carried out with electrolyte solution; CO disclosed in patent CN1918326A 2with the electro-plating method under aqueous metal salt concurrent conditions; Supercutical fluid disclosed in patent CN101092716B maintains electroforming process and device.Compared with existing electroplating technology, the coating surface free of pinholes that above-mentioned disclosed technology obtains, the crystal grain of formation is little, and hardness is high, corrosion-resistant, and can reduce the usage quantity of electroplate liquid, has good DEVELOPMENT PROSPECT.CO 2new process for electroplating under concurrent conditions, the new very worth research and development of electroplate liquid formulation, but there is no at present and be applicable to CO 2the device of the electroplating technology under concurrent conditions and the development experiments of electroplate liquid.
Under normal pressure, the alternative method of the development experiments of electroplating technology and electroplate liquid has multiple, such as: one utilizes miniature workpiece to do lab scale in small-sized coating bath, but fluid volume is large, and Anode-cathode Distance is near, truly can not reflect that large geometrical factor of producing is on the impact of dispersive ability etc., can only as novel process, new formula waits the subordinate phase test of research and development to use; One is test in beaker.Small beaker test is few with liquid, but can only reflect the situation under a certain certain current density; One is also had to be Hull cell test.Hull cell test just can obtain coating situation under wider current density range by the plating solution single test seldom measured, and is the research of modern electro-plating method, auxiliary agent exploitation and the simplest and the most direct indispensable instrument such as improvement and the control of plating solution process maintenance.But CO 2under 304.3K, 7.185MPa condition, just need can reach supercritical state, common normal pressure hull cell testing device cannot meet this kind of reaction under high pressure condition.
Summary of the invention
In order to solve prior art problem, the object of the invention is to the deficiency overcoming prior art existence, a kind of device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment is provided, solve the defect that normal pressure hull cell testing device cannot meet reaction under high pressure condition, and overcome the not competent condition of high voltage of the insulating material particularly overcritical or subcritical CO such as the conventional synthetic glass of normal pressure hull cell testing device or rigid polyvinyl chloride 2in easily to expand the problem of deterioration and electrode sealed insulation, can obtain the electroplating effect at wider current density range plating solution easily at short notice, be high pressure CO 2electroplating technology research under existing, plating solution formula exploitation and electroplating technology control to offer help.
Create object for reaching foregoing invention, the present invention adopts following technical proposals:
A kind of device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment, comprise trapezoidal reactor, anode, negative electrode and external source, electroplate liquid is held in trapezoidal reactor, the uneven opposite side of trapezoidal reactor places anode respectively and negative electrode forms two electrode systems, anode is by the positive terminal of anode electrode wire access external source, negative electrode, by the negative pole end of cathode electrode wire access external source, also comprises high pressure electrochemistry reactor, CO 2delivery system, pressure control system, temperature controlling system and stirring system, it is inner that trapezoidal reactor is arranged at high pressure electrochemistry reactor, is specially:
High pressure electrochemistry reactor is made up of the kettle cover of combining closely and autoclave body, the junction of kettle cover and autoclave body is placed sealing-ring and is sealed, kettle cover and autoclave body are connected and fixed by holding bolt, and anode electrode wire and cathode electrode wire pass kettle cover respectively by insulation and sealing structure; CO 2delivery system comprises CO 2gas bomb, high-pressure pump, CO 2high-pressure conduit and CO 2exhaust guide, CO 2high-pressure conduit and CO 2exhaust guide are each passed through kettle cover and insert high pressure electrochemistry reactor inside, from CO 2the CO that gas bomb exports 2gas enters in high-pressure pump pump chamber, is compressed to required pressure, then passes through CO through high-pressure pump 2high-pressure conduit, is transported in high pressure electrochemistry reactor, the CO of high pressure electrochemistry reactor inside 2gas is also by CO 2exhaust guide are discharged, and high-pressure pump preferably adopts manual scale pump; Pressure control system comprises steel cylinder tensimeter, high pressure aspirated pressure table, steel cylinder leaving air control valve, high pressure supply gas control valve and CO 2gas exhausting valve, the direct real-time testing CO of steel cylinder tensimeter 2pressure in gas bomb, high pressure aspirated pressure table is arranged at CO 2on high-pressure conduit, to CO 2the supply gas pressure of delivery system detects in real time, and steel cylinder leaving air control valve is arranged on CO 2near the air outlet of gas bomb, as CO 2gas bomb go out air cock, high pressure control valve of supplying gas is arranged at CO 2on high-pressure conduit, the CO in high pressure electrochemistry reactor 2when pressure reaches test requirements document, high pressure can be closed and supply gas control valve to keep the air pressure in high pressure electrochemistry reactor constant, CO 2gas exhausting valve is arranged at CO 2on exhaust guide, as the air discharge cook of high pressure electrochemistry reactor; Temperature controlling system comprises temperature sensor and thermostatic bath, the temperature-sensing probe of temperature sensor inserts high pressure electrochemistry reactor inside through kettle cover, thermostatic bath comprises temperature control device, the temperature in high pressure electrochemistry reactor is detected by temperature sensor, and by signal wire, temperature signal is inputed to temperature control device, temperature in high pressure electrochemistry reactor is regulated, makes the temperature in high pressure electrochemistry reactor reach set(ting)value needed for experiment; Stirring system is electromagnetic stirring system, comprise magnetic stirring apparatus and magnetic stir bar, it is outside that magnetic stirring apparatus is arranged at high pressure electrochemistry reactor, near trapezoidal reactor bottom in high pressure electrochemistry reactor, arrange the magnetic stir bar stirring electroplate liquid, the speed of rotation of magnetic stir bar is by magnetic stirring apparatus regulating and controlling.
As technical solution of the present invention, the pre-opened hole that above-mentioned anode electrode wire and cathode electrode wire are each passed through on teflon sleeve and kettle cover is combined closely, and namely teflon sleeve forms insulation and sealing structure.
As the technical scheme that the present invention improves, by utilizing tetrafluoroethylene standing bolt, trapezoidal reactor is made to be fixedly connected with installation with high pressure electrochemistry reactor.
Above-mentioned trapezoidal reactor is preferably prepared by polytetrafluoroethylmaterial material.
The wire appearance preferably at least entering the wire section of high pressure electrochemistry reactor at above-mentioned anode electrode wire and above-mentioned cathode electrode wire wraps up one deck teflon insulation layer.
Connect preferably by conductive resin between above-mentioned anode and anode electrode wire, also connect preferably by conductive resin between negative electrode and cathode electrode wire, smear epoxy resins insulation glue in conductive resin outside and wire exposed part.
Preferably utilize stainless steel to seal packing washer and stainless steel clamping nut to coordinate, the temperature probe of temperature sensor is fixed, and form insulation and sealing structure temperature sensor is through the pre-opened hole on the section of kettle cover and kettle cover.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. testing apparatus of the present invention can carry out electroplating technology and electroplate liquid development experiments under hyperbaric environment, and device structure is simple, and process maintenance controls simple and direct, and fluid volume is few, and application is convenient;
2. the present invention adopts polytetrafluoroethylmaterial material, solves the not competent condition of high voltage of the insulating material particularly overcritical or subcritical CO such as the conventional synthetic glass of normal pressure hull cell testing device or rigid polyvinyl chloride 2in easily to expand deterioration and electrode insulation sealing problem, the electroplating effect at wider current density range plating solution under hyperbaric environment can be obtained easily at short notice, to high pressure CO 2electroplating technology exploitation under existing, plating solution formula exploitation and electroplating device development research have important value.
Accompanying drawing explanation
Fig. 1 is the structure drawing of device that the embodiment of the present invention one carries out electroplating technology and electroplate liquid development experiments under hyperbaric environment.
Fig. 2 is electrode system, air delivering pipeline and temperature-sensing probe distribution schematic diagram on the kettle cover of the embodiment of the present invention one and kettle cover.
Fig. 3 is the structural representation of the trapezoidal reactor of the embodiment of the present invention two.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment one:
See Fig. 1 and Fig. 2, in the present embodiment, a kind of device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment, comprise trapezoidal reactor 1, anode 2, negative electrode 15 and external source 9, electroplate liquid is held in trapezoidal reactor 1, the uneven opposite side of trapezoidal reactor 1 places anode 2 respectively and negative electrode 15 forms two electrode systems, anode 2 accesses the positive terminal of external source 9 by anode electrode wire 19, negative electrode 15 accesses the negative pole end of external source 9 by cathode electrode wire 10, also comprises high pressure electrochemistry reactor, CO 2delivery system, pressure control system, temperature controlling system and stirring system, it is inner that trapezoidal reactor 1 is arranged at high pressure electrochemistry reactor, and external source 9 selects direct supply or the pulse power as required, is specially:
High pressure electrochemistry reactor is made up of the kettle cover 13 of combining closely and autoclave body 16, the junction of kettle cover 13 and autoclave body 16 is placed sealing-ring and is sealed, kettle cover 13 and autoclave body 16 are connected and fixed by holding bolt 21, and anode electrode wire 19 and cathode electrode wire 10 pass kettle cover 13 respectively by insulation and sealing structure; CO 2delivery system comprises CO 2gas bomb 3, high-pressure pump 5, CO 2high-pressure conduit 7 and CO 2exhaust guide 11, CO 2high-pressure conduit 7 and CO 2exhaust guide 11 are each passed through kettle cover 13 and insert high pressure electrochemistry reactor inside, from CO 2the CO that gas bomb 3 exports 2gas enters in high-pressure pump 5 pump chamber, is compressed to required pressure, then passes through CO through high-pressure pump 5 2high-pressure conduit 7, is transported in high pressure electrochemistry reactor, the CO of high pressure electrochemistry reactor inside 2gas is also by CO 2exhaust guide 11 are discharged; Pressure control system comprises steel cylinder tensimeter 4, high pressure aspirated pressure table 6, steel cylinder leaving air control valve V-1, high pressure supply gas control valve V-2 and CO 2gas exhausting valve V-3, steel cylinder tensimeter 4 is real-time testing CO directly 2pressure in gas bomb 3, high pressure aspirated pressure table 6 is arranged at CO 2on high-pressure conduit 7, to CO 2the supply gas pressure of delivery system detects in real time, and steel cylinder leaving air control valve V-1 is arranged on CO 2near the air outlet of gas bomb 3, as CO 2gas bomb 3 go out air cock, the high pressure control valve V-2 that supplies gas is arranged at CO 2on high-pressure conduit 7, the CO in high pressure electrochemistry reactor 2when pressure reaches test requirements document, high pressure can be closed and supply gas control valve V-2 to keep the air pressure in high pressure electrochemistry reactor constant, CO 2gas exhausting valve V-3 is arranged at CO 2on exhaust guide 11, as the air discharge cook of high pressure electrochemistry reactor; Temperature controlling system comprises temperature sensor 8 and thermostatic bath 12, the temperature-sensing probe of temperature sensor 8 inserts high pressure electrochemistry reactor inside through kettle cover 13, thermostatic bath 12 comprises temperature control device, the temperature in high pressure electrochemistry reactor is detected by temperature sensor 8, and by signal wire, temperature signal is inputed to temperature control device, temperature in high pressure electrochemistry reactor is regulated, makes the temperature in high pressure electrochemistry reactor reach set(ting)value needed for experiment; Stirring system is electromagnetic stirring system, comprise magnetic stirring apparatus 17 and magnetic stir bar 18, it is outside that magnetic stirring apparatus 17 is arranged at high pressure electrochemistry reactor, in high pressure electrochemistry reactor bottom trapezoidal reactor 1, arrange the magnetic stir bar 18 stirring electroplate liquid, the speed of rotation of magnetic stir bar 18 is by magnetic stirring apparatus 17 regulating and controlling.High pressure electrochemistry reactor is placed on magnetic stirring apparatus 17, and be placed on together with magnetic stirring apparatus 17 in thermostatic bath 12, magnetic stir bar 18 is placed in trapezoidal reactor 1 inside, by regulating the magnetic stirring apparatus 17 under reactor, the stirring velocity of magnetic stir bar 18 can be changed, still electrolyte inside is mixed, under the effect of external source 9, realizes electroplating technology and electroplate liquid exploitation under hyperbaric environment.
In the present embodiment, in fig. 1 and 2, CO 2gas in gas bomb 3 is entered in high-pressure pump 5 pump chamber after being discharged by valve V-1, then is compressed to required pressure through high-pressure pump 5, passes through CO 2high-pressure conduit 7, enter in high pressure electrochemistry reactor, still internal pressure is regulated by high-pressure pump 5, by being arranged on CO 2high pressure aspirated pressure table 6 on high-pressure conduit 7 shows, and closes CO when still internal pressure reaches requirement 2high pressure on high-pressure conduit 7 supplies gas control valve V-2 to keep the constant of still internal pressure.Temperature in still is conducted by the temperature sensor 8 be located on kettle cover 13, then sets adjustment by the temperature control device that temperature signal to be inputed to thermostatic bath 12 by wire, reaches the requirement accurately controlling temperature in the kettle.In the present embodiment, after electrolytic solution adds the trapezoidal reactor 1 of high pressure electrochemistry reactor, reach design temperature by thermostatic bath 12 temperature controlling system, import CO 2the pressure condition of change system, the top pressure that high pressure electrochemistry reactor can bear and temperature are respectively 20MPa and 373.15K.
In trapezoidal reactor 1, inject electrolytic solution and place magnetic stir bar 18, select suitable anode and cathode, and after the anode 2 handled well and negative electrode 15 anode electrode wire 19 and cathode electrode wire 10 are connected, by electrode cable through insulation and sealing structure, utilize stainless steel to seal packing washer, electrode cable is fixed and is sealed by stainless steel clamping nut.Cover kettle cover 13, screw the holding bolt 21 on kettle cover 13, after sealing fixed temperature sensor 8, autoclave body 16 is inserted in heat insulation and heating equipment thermostatic bath 12.Connect high pressure electrochemistry reactor and CO 2high-pressure conduit 7 and CO 2exhaust guide 11.First open each stopping valve, namely opens steel cylinder leaving air control valve V-1, high pressure supplies gas control valve V-2 and CO 2gas exhausting valve V-3, passes into low pressure CO 2gas removes other gas in pipeline and high pressure electrochemistry reactor, uses wire to connect the temperature regulating device of temperature sensor 8 and thermostat container 12, and is heated to design temperature.Close CO 2gas exhausting valve V-3, rotary manual scale pump imports CO 2still internal pressure is reached after setting requires, close steel cylinder leaving air control valve V-1 and high pressure and to supply gas control valve V-2, make high pressure electrochemistry reactor keep high-temperature high-pressure state.The magnetic stirring apparatus 17 opening strong magnetic makes the magnetic stir bar 18 of High Temperature High Pressure rotate to setting speed.High pressure aspirated pressure table 6 shows the pressure in still, temperature sensor 8 shows the temperature in still, and magnetic stirring apparatus 17 shows the speed of rotation of magnetic stir bar 18.Open external source 9, under the control of external source 9, at cathode base substrates metal under different electrolytes formula and different electrical parameters condition.After reaction terminates, cathode base is taken out, contrasts with Hull slot standard model, realize the experimental development to electroplating technology under hyperbaric environment and electroplate liquid.
In the present embodiment, see Fig. 1, anode electrode wire 19 and cathode electrode wire 10 are each passed through teflon sleeve 14 and combine closely with the pre-opened hole on kettle cover 13, and namely teflon sleeve 14 forms insulation and sealing structure.Stainless steel sealing packing washer and stainless steel clamping nut is utilized to be fixed by each electrode cable and seal, teflon insulation sleeve pipe ensures that each electrode cable and kettle 16 insulate, and is formed and is more applicable for electrode under condition of high voltage and the insulation and sealing structure be connected between reaction vessel.
In the present embodiment, see Fig. 1, trapezoidal reactor 1 is prepared by polytetrafluoroethylmaterial material, and size and the internal volume of trapezoidal reactor 1 are identical with normal pressure Hull Cell.Trapezoidal reactor 1 adopts polytetrafluoroethylmaterial material, solves under the not competent condition of high voltage of insulating material such as the conventional synthetic glass of normal pressure hull cell testing device or rigid polyvinyl chloride particularly at overcritical or subcritical CO 2in easily to expand deterioration and electrode insulation sealing problem, the electroplating effect at wider current density range plating solution under hyperbaric environment can be obtained easily at short notice, to high pressure CO 2electroplating technology exploitation under existing, plating solution formula exploitation and electroplating device development research are significant.
embodiment two:
The present embodiment is substantially identical with embodiment one, and special feature is:
In the present embodiment, see Fig. 3, by utilizing tetrafluoroethylene standing bolt 20, trapezoidal reactor 1 is made to be fixedly connected with installation with high pressure electrochemistry reactor.Standing bolt adopts polytetrafluoroethylmaterial material, solves under the not competent condition of high voltage of insulating material such as the conventional synthetic glass of normal pressure hull cell testing device or rigid polyvinyl chloride particularly at overcritical or subcritical CO 2in easily to expand deterioration and electrode insulation sealing problem, the electroplating effect at wider current density range plating solution under hyperbaric environment can be obtained easily at short notice, to high pressure CO 2electroplating technology exploitation under existing, plating solution formula exploitation and electroplating device development research are significant.
embodiment three:
The present embodiment and previous embodiment are substantially identical, and special feature is:
In the present embodiment, the wire appearance at least entering the wire section of high pressure electrochemistry reactor at anode electrode wire 19 and cathode electrode wire 10 wraps up one deck teflon insulation layer, can adapt to supercritical CO 2or subcritical CO 2carry out Hull cell test in the homogeneous phase that/conductive soln is formed and heterogeneous system, adopt teflon insulation coating to reach the object of electrode cable insulation.
embodiment four:
The present embodiment and previous embodiment are substantially identical, and special feature is:
In the present embodiment, connected by conductive resin between anode 2 and anode electrode wire 19, also connected by conductive resin between negative electrode 15 and cathode electrode wire 10, epoxy resins insulation glue is smeared in conductive resin outside and wire exposed part, improve insulating property, improve device work-ing life.
embodiment five:
The present embodiment and previous embodiment are substantially identical, and special feature is:
In the present embodiment, stainless steel is utilized to seal packing washer and the cooperation of stainless steel clamping nut, the temperature probe of temperature sensor 8 is fixed, and form insulation and sealing structure temperature sensor 8 is through the pre-opened hole on the section of kettle cover 13 and kettle cover 13, reach the object that better insulate.
By reference to the accompanying drawings the embodiment of the present invention is illustrated above; but the invention is not restricted to above-described embodiment; multiple change can also be made according to the object of innovation and creation of the present invention; change, the modification made under all spirit according to technical solution of the present invention and principle, substitute, combination, to simplify; all should be the substitute mode of equivalence; as long as goal of the invention according to the invention; only otherwise deviate from know-why and the inventive concept that the present invention carries out the device of electroplating technology and electroplate liquid development experiments under hyperbaric environment, all protection scope of the present invention is belonged to.

Claims (9)

1. one kind is carried out the device of electroplating technology and electroplate liquid development experiments under hyperbaric environment, comprise trapezoidal reactor (1), anode (2), negative electrode (15) and external source (9), electroplate liquid is held in described trapezoidal reactor (1), the uneven opposite side of described trapezoidal reactor (1) places described anode (2) respectively and described negative electrode (15) forms two electrode systems, described anode (2) accesses the positive terminal of described external source (9) by anode electrode wire (19), described negative electrode (15) accesses the negative pole end of described external source (9) by cathode electrode wire (10), it is characterized in that, also comprise high pressure electrochemistry reactor, CO 2delivery system, pressure control system, temperature controlling system and stirring system, it is inner that trapezoidal reactor (1) is arranged at described high pressure electrochemistry reactor, is specially:
Described high pressure electrochemistry reactor is made up of the kettle cover of combining closely (13) and autoclave body (16), the junction of described kettle cover (13) and described autoclave body (16) is placed sealing-ring and is sealed, described kettle cover (13) and described autoclave body (16) are connected and fixed by holding bolt (21), and described anode electrode wire (19) and described cathode electrode wire (10) pass described kettle cover (13) respectively by insulation and sealing structure;
Described CO 2delivery system comprises CO 2gas bomb (3), high-pressure pump (5), CO 2high-pressure conduit (7) and CO 2exhaust guide (11), described CO 2high-pressure conduit (7) and described CO 2exhaust guide (11) are each passed through described kettle cover (13) and insert high pressure electrochemistry reactor inside, from described CO 2the CO that gas bomb (3) exports 2gas enters in described high-pressure pump (5) pump chamber, is compressed to required pressure through high-pressure pump (5), then by described CO 2high-pressure conduit (7), is transported in described high pressure electrochemistry reactor, the CO of described high pressure electrochemistry reactor inside 2gas is also by described CO 2exhaust guide (11) are discharged;
Described pressure control system comprises steel cylinder tensimeter (4), high pressure aspirated pressure table (6), steel cylinder leaving air control valve (V-1), high pressure supply gas control valve (V-2) and CO 2gas exhausting valve (V-3), described steel cylinder tensimeter (4) is CO described in real-time testing directly 2pressure in gas bomb (3), described high pressure aspirated pressure table (6) is arranged at described CO 2on high-pressure conduit (7), to described CO 2the supply gas pressure of delivery system detects in real time, and described steel cylinder leaving air control valve (V-1) is arranged on described CO 2near the air outlet of gas bomb (3), as described CO 2gas bomb (3) go out air cock, described high pressure control valve (V-2) of supplying gas is arranged at described CO 2on high-pressure conduit (7), the CO in described high pressure electrochemistry reactor 2when pressure reaches test requirements document, described high pressure can be closed and supply gas control valve (V-2) to keep the air pressure in described high pressure electrochemistry reactor constant, described CO 2gas exhausting valve (V-3) is arranged at described CO 2on exhaust guide (11), as the air discharge cook of described high pressure electrochemistry reactor;
Described temperature controlling system comprises temperature sensor (8) and thermostatic bath (12), the temperature-sensing probe of described temperature sensor (8) inserts described high pressure electrochemistry reactor inside through described kettle cover (13), described thermostatic bath (12) comprises temperature control device, the temperature in described high pressure electrochemistry reactor is detected by described temperature sensor (8), and by signal wire, temperature signal is inputed to described temperature control device, temperature in described high pressure electrochemistry reactor is regulated, makes the temperature in described high pressure electrochemistry reactor reach set(ting)value needed for experiment;
Described stirring system is electromagnetic stirring system, comprise magnetic stirring apparatus (17) and magnetic stir bar (18), it is outside that described magnetic stirring apparatus (17) is arranged at described high pressure electrochemistry reactor, near trapezoidal reactor (1) bottom in described high pressure electrochemistry reactor, arrange the described magnetic stir bar (18) stirring electroplate liquid, the speed of rotation of described magnetic stir bar (18) is by described magnetic stirring apparatus (17) regulating and controlling.
2. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 1, it is characterized in that: described anode electrode wire (19) and described cathode electrode wire (10) are each passed through teflon sleeve (14) and combine closely with the pre-opened hole on described kettle cover (13), and described teflon sleeve (14) namely forms insulation and sealing structure.
3. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 1 and 2, it is characterized in that: by utilizing tetrafluoroethylene standing bolt (20), making described trapezoidal reactor (1) be fixedly connected with installation with described high pressure electrochemistry reactor.
4. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 1 and 2, is characterized in that: described trapezoidal reactor (1) is prepared by polytetrafluoroethylmaterial material.
5. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 3, is characterized in that: described trapezoidal reactor (1) is prepared by polytetrafluoroethylmaterial material.
6. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 1 and 2, is characterized in that: the wire appearance at least entering the wire section of described high pressure electrochemistry reactor described anode electrode wire (19) and described cathode electrode wire (10) wraps up one deck teflon insulation layer.
7. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 3, is characterized in that: the wire appearance at least entering the wire section of described high pressure electrochemistry reactor described anode electrode wire (19) and described cathode electrode wire (10) wraps up one deck teflon insulation layer.
8. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 3, it is characterized in that: connected by conductive resin between described anode (2) and described anode electrode wire (19), also connected by conductive resin between described negative electrode (15) and described cathode electrode wire (10), smear epoxy resins insulation glue in conductive resin outside and wire exposed part.
9. the device carrying out electroplating technology and electroplate liquid development experiments under hyperbaric environment according to claim 3, it is characterized in that: utilize stainless steel to seal packing washer and the cooperation of stainless steel clamping nut, the temperature probe of described temperature sensor (8) is fixed, and form insulation and sealing structure described temperature sensor (8) is through the pre-opened hole on the section of described kettle cover (13) and described kettle cover (13).
CN201310057756.5A 2013-02-25 2013-02-25 The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment Expired - Fee Related CN103173842B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310057756.5A CN103173842B (en) 2013-02-25 2013-02-25 The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310057756.5A CN103173842B (en) 2013-02-25 2013-02-25 The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment

Publications (2)

Publication Number Publication Date
CN103173842A CN103173842A (en) 2013-06-26
CN103173842B true CN103173842B (en) 2016-03-30

Family

ID=48634015

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310057756.5A Expired - Fee Related CN103173842B (en) 2013-02-25 2013-02-25 The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment

Country Status (1)

Country Link
CN (1) CN103173842B (en)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104157595B (en) * 2014-07-10 2016-11-02 中南大学 Microelectronics Packaging pin interconnection method and apparatus based on electrochemical growth
CN106048693B (en) * 2014-08-20 2018-06-08 江苏理工学院 A kind of overcritical composite plating processing drill method based on mobile anode
CN104313657A (en) * 2014-11-10 2015-01-28 临安振有电子有限公司 Electro-deposition device of through hole of HDI printed circuit board
CN105987940A (en) * 2015-02-13 2016-10-05 亚申科技研发中心(上海)有限公司 High-pressure electrochemical reaction tank and under pressure system
CN104611755B (en) * 2015-03-10 2017-03-08 莱芜职业技术学院 A kind of novel high-pressure bright nickel plating electroplanting device and its nickel plating process
CN106283170B (en) * 2016-08-29 2018-05-29 中航动力股份有限公司 A kind of low-pressure turbine disk blueness anodic attack auxiliary device
CN106596389B (en) * 2017-02-16 2023-08-11 天津大学 Reaction kettle for electrochemical test in strong corrosion medium and application method thereof
CN107190286B (en) * 2017-05-09 2019-01-25 贵州振华群英电器有限公司(国营第八九一厂) A kind of experimental rig and its test method of through-hole covering power
CN108130587A (en) * 2018-02-05 2018-06-08 西南石油大学 A kind of supercritical CO2Under the conditions of visualization electroplanting device and method
TWI694175B (en) * 2018-12-25 2020-05-21 台灣可林生化科技有限公司 Automatic electrolysis device
CN109745944A (en) * 2019-03-04 2019-05-14 中国民用航空飞行学院 It is a kind of can magnetic agitation and filling with inert gas protection hydrothermal synthesis reaction kettle
CN113529115B (en) * 2020-04-16 2022-09-16 中国科学院大连化学物理研究所 Double-cell high-voltage electrochemical reaction device
CN113061966A (en) * 2021-03-26 2021-07-02 江苏理工学院 Supercritical electrodeposition device for preparing composite material and use method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06248487A (en) * 1993-02-26 1994-09-06 Imura Japan Kk Method for forming electrodeposited thin film
JPH1199199A (en) * 1997-09-29 1999-04-13 Shigeo Maruno Manufacture of calcium phosphate film
CN1763258A (en) * 2005-09-29 2006-04-26 陕西科技大学 Method and apparatus for preparing coating or film by microwave hydrothermal electrodeposition
CN1766175A (en) * 2005-09-29 2006-05-03 陕西科技大学 Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology
JP2006214751A (en) * 2005-02-01 2006-08-17 Nec Tokin Corp Evaluation device for electroplating liquid, and evaluation method of electroplating liquid
CN101092716A (en) * 2007-04-27 2007-12-26 江苏技术师范学院 Superfine electroform technique of supercutical fluid, and equipment
CN101818358A (en) * 2009-12-28 2010-09-01 上海大学 Supercritical CO2 high-temperature high-pressure synthetic high molecular conducting film device

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06248487A (en) * 1993-02-26 1994-09-06 Imura Japan Kk Method for forming electrodeposited thin film
JPH1199199A (en) * 1997-09-29 1999-04-13 Shigeo Maruno Manufacture of calcium phosphate film
JP2006214751A (en) * 2005-02-01 2006-08-17 Nec Tokin Corp Evaluation device for electroplating liquid, and evaluation method of electroplating liquid
CN1763258A (en) * 2005-09-29 2006-04-26 陕西科技大学 Method and apparatus for preparing coating or film by microwave hydrothermal electrodeposition
CN1766175A (en) * 2005-09-29 2006-05-03 陕西科技大学 Method and device for preparing coating or film using supersonic, water-heating and electrodeposition technology
CN101092716A (en) * 2007-04-27 2007-12-26 江苏技术师范学院 Superfine electroform technique of supercutical fluid, and equipment
CN101818358A (en) * 2009-12-28 2010-09-01 上海大学 Supercritical CO2 high-temperature high-pressure synthetic high molecular conducting film device

Also Published As

Publication number Publication date
CN103173842A (en) 2013-06-26

Similar Documents

Publication Publication Date Title
CN103173842B (en) The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment
CN206916248U (en) A kind of electro-deposition sample preparation instrument prepared suitable for αsource
CN203855675U (en) Electroplating device
CN206731075U (en) A kind of lanthanum chloride hydrate gas-liquid cycle control loop system
CN208829786U (en) A kind of electroplanting device
CN206470167U (en) A kind of device for simulating lower cathodic protection hydrogen permeability test different in flow rate
CN202041585U (en) On-line conductivity monitoring device for charged filed bath solution
CN205719905U (en) A kind of for electrochemical corrosion measurement device
CN110205646B (en) Small-size pilot scale experimental apparatus of electrolysis trough
CN107227482A (en) A kind of electro-deposition sample preparation instrument prepared suitable for αsource
CN103526264A (en) Experimental device for preparing cathode electrophoresis film
CN106706744B (en) A kind of electrochemical detection device and its processing method and purposes
CN210458379U (en) Small pilot test experimental device for electrolytic cell
CN205711363U (en) Carbon fiber constant part
CN208751994U (en) Autoclave reactor and electrochemical appliance for measuring pollutant hydrothermal oxidization system
CN108385156A (en) The flexibly coating or passivation layer preparation facilities and application method of control environmental parameter
CN203385692U (en) Electrochemical testing device for three-electrode system
CN203855676U (en) Portable electroplating machine
CN207623278U (en) A kind of electrolytic cell
CN111257214A (en) In-situ electrochemical cell device capable of measuring electrochemical corrosion performance under electromagnetic field
CN103048220B (en) Iodine hydroiodic acid container capable of displaying liquid concentration on line
CN206706403U (en) The online pH adjusting meanss of dyeing and finishing line
CN212433043U (en) Online instrument calibration equipment of thermal power plant's water sample
CN214612829U (en) Energy-saving mobile phone accessory electroplating device
CN211929160U (en) Enameled copper wire painting device

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20211119

Address after: 221116 comprehensive service building, zone B, Fenghuangshan community, Tongshan street, Tongshan District, Xuzhou City, Jiangsu Province

Patentee after: Jiangsu jingshiyuan energy and Environmental Protection Research Institute Co.,Ltd.

Address before: 200444 No. 99, upper road, Shanghai, Baoshan District

Patentee before: Shanghai University

CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160330