CN106521403A - Rotating salt bath equipment for tantalum surface treatment and treatment method - Google Patents
Rotating salt bath equipment for tantalum surface treatment and treatment method Download PDFInfo
- Publication number
- CN106521403A CN106521403A CN201611260609.8A CN201611260609A CN106521403A CN 106521403 A CN106521403 A CN 106521403A CN 201611260609 A CN201611260609 A CN 201611260609A CN 106521403 A CN106521403 A CN 106521403A
- Authority
- CN
- China
- Prior art keywords
- salt bath
- tantalum
- linking arm
- bin
- bar
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention belongs to the field of tantalum wire surface treatment, and relates to rotating salt bath equipment for surface oxidation treatment in the process of tantalum wire production and a tantalum wire surface treatment method using the equipment. The rotating salt bath equipment comprises a rotary rack, a moving motor connected with the rotating rack, and a control cabinet. The rotary rack comprises a rotating motor, a connecting frame connected with the rotating motor, and a rack body connected with the connecting frame. Tantalum strips are subjected to surface treatment using the rotary salt bath equipment, the surface oxide layer thicknesses of the tantalum strips can be controlled, the tantalum strip surfaces can be oxidized uniformly, the oxygen content of oxide layers is controlled, and surface smoothness of the finished tantalum wire surface is improved.
Description
Technical field
The invention belongs to tantalum wire field of surface treatment, is related to one kind in tantalum wire production process, uses during surface oxidation treatment
Rotation salt bath equipment, and the surface treatment method that tantalum material is carried out using the equipment.
Background technology
Capacitor is widely used in the fields such as communication, computer, automobile, household electrical appliances, Aero-Space now, makees sun with tantalum powder
The tantalum electrolytic capacitor of anode tap making is made in pole, tantalum wire, and with small volume, capacitance is big, chip type degree is high, reliability
The characteristics of excellent combination properties such as good, long service life, thus can be in many other capacitors such as capacitor such as ceramics, aluminium film
Normal work under incompetent harsh conditions.
As the tantalum wire of tantalum capacitor anodes lead, it is desirable to which chemical purity is high, surface smoothness is good, accurate size, machine
Tool performance, chemical property meet the strict demand of capacitor.For example, the specific requirement to tantalum wire surface smoothness is：60
Above basis of microscopic observation surface is without defects such as obvious groove, burr, hole points again；The specific requirement of chemical property is leakproof
Stream, leakage current are less, and performance is better.
It is as follows that the producing of tantalum wire starts technique from bar：
Raw bar material → type rolls → and surface film process → intermediate annealing → drawing → cleaning → after-combustion → quality inspection → be packaged into
Storehouse.
Surface membrane treatment process is mainly for the protection of tantalum wire surface, it is ensured that tantalum wire surface smoothness in drawing process.Table
Facial mask handling process is mainly surface-treated and is aoxidized benefit film surface treatment and constitutes by salt bath.
Salt bath furnace refers to melting saline solution as heating medium, workpiece is immersed the industrial furnace heated in saline solution, chlorine is generally used
Change the salts such as sodium, potassium chloride, barium chloride, sodium hydride, potassium cyanide, sodium nitrate, potassium nitrate as heating medium.Salt bath furnace can be used for
The heat treatment heating such as quenching, annealing, tempering, cyaniding, timeliness to carbon steel, steel alloy, tool steel, mould steel and aluminium alloy etc.,
Can also be used for slight oxidization heating during steel precision forging.Tantalum belongs to refractory metal, and 2996 DEG C of fusing point is not occurred with oxygen in normal temperature anti-
Should；In 280 DEG C to 300 DEG C very slight surface oxidations；350 DEG C of slight oxidation surfaces are by xanthochromia is red, purpling, become blue；390℃
To 440 DEG C of blackening, 480 DEG C or so change lead, 500 DEG C engender oxide white.The surface treatment of tantalum bar salt bath furnace is logical
The salts such as the sodium chloride of well-beaten molten condition, potassium chloride, barium chloride, sodium nitrate, potassium nitrate are crossed as heating medium pair
Do oxidation processes in tantalum bar surface.Tantalum bar makees the lead of tantalum capacitor after being used for drawing tantalum wire, it is desirable to which chemical composition purity is high, tantalum wire
Middle oxygen content≤100ppm.The time that tantalum bar is immersed in salt bath furnace strictly must control, to ensure after salt bath furnace process
Tantalum bar oxygen content in controlled range.
In prior art, tantalum bar salt bath furnace handling process adopts external heating type salt bath furnace, is that the tantalum bar that will be tied is put into not
Rust steel material frame, is immersed in salt bath furnace, after appropriate reaction, can be in tantalum bar surface travel layer oxide film, in tantalum
Tantalum bar surface is formed in bar drawing process and protected.However, the tantalum bar that this equipment and process matching were processed, surface forms oxygen
Change layer in uneven thickness, local surfaces can form scratch and burr because of unprotected layer in tantalum bar drawing process, it is impossible to have
Effect ensures tantalum wire surface smoothness, and after drawing, in finished product tantalum wire, oxygen content is higher than 100PPM, it is difficult to meet current tantalum capacitor institute
Required with tantalum wire chemical purity.Additionally, salt bath furnace fire door temperature is high, condition of work is severe, and the fused salt liquid of molten condition meets water
Then there is splash phenomena, meet oil, charcoal and other organic matters and vigorous combustion and blast can occur.
The content of the invention
Present invention aim at a kind of rotation salt bath equipment is provided, for the salt bath surface oxidation treatment of tantalum bar, the rotation
Salt bath equipment can make tantalum bar when salt bath is processed, uniform to aoxidize, and form the homogeneous oxide layer of thickness, it is ensured that tantalum wire after drawing
Fineness and low oxygen content.
The present invention also aims to provide a kind of rotation salt bath equipment containing rotation bin.
The present invention also aims to provide a kind of method of tantalum bar surface treatment.
The above-mentioned purpose of the present invention is realized by following technological means：
A kind of rotation salt bath equipment：Described rotation salt bath equipment contains salt bath reacting furnace, and is located at salt bath reacting furnace
Interior salt bath reactor, described salt bath reactor can be equipped with the fused salt of melting, it is characterised in that also including rotation bin, institute
Stating rotation bin includes：
Electric rotating machine；
Bin；
Link；Described link is used to connect electric rotating machine and bin.Further, one end of described link
It is connected with electric rotating machine, the other end is connected with bin.
Described link contains the linking arm that connecting rod is connected with connecting rod, one end and the electric rotating machine phase of connecting rod
Even.As preferred embodiment, it is connected by shaft coupling between one end of connecting rod and electric rotating machine.The other end of connecting rod
It is connected with linking arm.
Described linking arm includes the first linking arm and the second linking arm.The first described linking arm and the second linking arm
One end is connected with the other end of connecting rod jointly.
The other end of the first described linking arm and the second linking arm is with the two ends of bin at least while detachably to connect
Connect.The straight line that first linking arm and the second linking arm are located with connecting rod is axisymmetricly.
Used as preferred embodiment, the first described linking arm and the second linking arm middle setting have fix bar, make two
Individual linking arm and fix bar form triangular structure, strengthen the stability of link.
Described bin is used to hang tantalum bar.As preferred embodiment, insulated column on bin, is provided with, for isolating
Fixed tantalum bar, tantalum bar is stably fixed on bin, uniform to aoxidize so as to whole rotation bin when rotated.As more excellent
The embodiment of choosing, is provided with multiple insulated columns on bin, the spacing of each insulated column is identical.
In invention, the other end of the first described linking arm and the second linking arm is connected with bin two ends respectively, wherein,
At least one linking arm is detachably connected with bin.By taking linking arm and bin apart, can be by the tantalum bar of disk rolling
Bin is hung up, and tantalum bar is fixed by the insulated column of bin, then connect bin and linking arm, you can rotation liquid oxidizing.Salt
Bath and cleaning take linking arm and bin apart after terminating, and remove tantalum bar.
In one embodiment of the invention, the described other end of the first linking arm and detachably connecting for one end of bin
Connect, the other end of the second linking arm is fixedly connected with the other end of bin.
In another embodiment of the invention, the other end of the first described linking arm and the second linking arm with bin
Two ends are detachably connected.
Further, being detachably connected for linking arm and bin is by clamping or is hinged or other detachably connect
Connect mode.
In an one exemplary embodiment of the present invention, the other end of first linking arm and/or the second linking arm arranges U
Shape connector, U-shaped connector are used to be removably secured bin.Further, two are provided with U-shaped connector relatively
Lock-joint, the first lock-joint and the second lock-joint.The end of bin, is provided with the 3rd lock-joint.First lock-joint, the second lock-joint and the 3rd pin
Mouth can be inserted into the pin of an activity on same straight line in lock-joint, bin and connection are kept away arm connection.During installation, will material
The end of frame is put into the U-shaped connector of linking arm, makes the 3rd lock-joint and the alignment of first, second lock-joint, inserts pin.U-shaped connection
A rotatable clamp is additionally provided with part, when rotate to block pin when, pin can be fixed, so as to linking arm and material
Frame.
Used as preferred embodiment, the rotation bin of the present invention also contains shaft coupling, for connecting electric rotating machine and company
Frame is connect, common rotation is allowed to.
Described rotation salt bath equipment is also containing the mobile motor being connected with the electric rotating machine of mobile bin, described movement
Motor is used to control moving up and down for rotation bin.
Described rotation salt bath equipment also contains switch board, and described switch board is used for the motion for controlling mobile motor, rotation
The rotation of rotating motor and the temperature adjustment of salt bath furnace.
Used as preferred embodiment, the rotation salt bath equipment of the present invention is also containing protection connection hanging scaffold, described protection
Connection hanging scaffold is used to fixing and carrying electric rotating machine, and being connected for electric rotating machine and mobile motor.
When operating the rotation salt bath equipment, switch board is adjusted, the temperature of molten salt in the reactor of salt bath furnace is adjusted to
It is 500-530 DEG C, standby.Then the clamp of rotation bin is taken out, extracts pin, tantalum bar is uniformly coiled in by insulated column
On bin, pin and clamp are installed, start mobile motor, the rotation bin with tantalum bar is hung in into salt bath by mobile motor
Reactor, is completely immersed in fused salt to tantalum bar, adjusts switch board, and startup is fixed on the electric rotating machine on protection connection hanging scaffold, presses
The speed of 50-100m/min is rotated, in fused salt inside holding 120-300sec.
Present invention also offers a kind of method of tantalum bar surface treatment, which comprises the steps of：
S1. tantalum bar is coiled into rolling；
S2. tantalum bar ultrasonic surface is cleaned；
S3. drying pretreatment is done to tantalum bar surface；
S4. tantalum bar is put in the salt bath furnace of molten condition and does surface of revolution oxidation processes；
S5. the tantalum bar for processing to salt bath does removing surface.
In step S1, the coil diameter of tantalum bar is Φ 200mm～Φ 300mm；Tantalum bar coiling curvature can not be too big, otherwise tantalum
Bar will occur significantly to bend on wire spool, it is impossible to meet use requirement.
In step S3, during drying and processing, the temperature of baking oven is 120-150 DEG C, and air quantity is 30-50m3/min；
In step S4, the temperature of salt bath is 500-530 DEG C, and time of salt bath is 120-300sec, the tantalum bar linear speed of rotation
Spend for 50-100m/min；
In step S5, it is to be rinsed using high-temperature high pressure water the step of removing surface, then boiling water immersion；Further, hydraulic pressure
For 0.5-1.0MPa, water temperature is 90 DEG C -100 DEG C, and washing time is to come out of the stove in 1-3min；Boiling water soak time is 15-30min.
In an embodiment of the present invention, the tantalum bar that rotated salt bath is processed, oxygen content preferably exist in below 200ppm
Below 160ppm is more preferably in below 140ppm, more preferably in below 120ppm.Oxygen content after the surface treatment of Standard tantalum bar
Typically in below 300ppm.In prior art, oxygen content oxygen typically after more than 200ppm, drawing after the surface treatment of tantalum bar salt bath
Content is typically in more than 100ppm.In an embodiment of the present invention, the tantalum bar that rotated salt bath is processed, after drawing, oxygen content exists
Below 100ppm.
The beneficial effect that the present invention is obtained：
1 present invention is first in tantalum wire field of surface treatment, there is provided a kind of rotation salt bath equipment, the equipment can be in tantalum bar
During the film process of salt bath surface, by the rotation to tantalum bar, tantalum bar uniformly oxidation filming is made, and is easily controlled tantalum bar film forming
Thickness.The tantalum bar that rotated salt bath is processed, oxygen content can be even reached in below 200ppm, even up to below 160ppm, more
Below 120ppm.The tantalum bar that rotated salt bath is processed, in follow-up tantalum bar drawing process, can effectively heighten the wire drawing die longevity
Life, after tantalum bar is drawn into tantalum wire, surface smoothness is high, and oxygen content disclosure satisfy that the chemistry of tantalum capacitor in below 100ppm
Purity requirement.Before this, in the salt bath process field of tantalum bar, never someone expected, also non-someone salt bath by the way of rotation
Tantalum bar is processed, to improve the uniformity and chemical purity of tantalum bar oxidation filming, more nobody provides a kind of rotation salt bath equipment and uses
Process in the salt bath of tantalum bar.
The rotation salt bath device structure of 2 present invention is simple, easy to use.
The rotation salt bath equipment safety reliability of 3 present invention：Fix bar is provided between two support arms, the steady of triangle is formed
Fixed structure, electric rotating machine are fixed on protection connection hanging scaffold；By using rotation salt bath equipment, salt bath table can be completed by switch board
Face is processed, it is not necessary to which operator is close to salt bath furnace.Because fire door temperature is high, condition of work is severe, the fused salt liquid of molten condition
Meet water and splash phenomena then occurs.
4 reduce the temperature retention time in salt bath processing procedure, improve treatment effeciency.
The 5 tantalum bars processed using rotation salt bath, in drawing process, can effectively improve the wire drawing die life-span to wire drawing die,
Finished product φ 0.15mm tantalum wires, from originally often set can 2.4 myriametre of drawing bring up to can about 3.6 myriametre of a drawing.
Description of the drawings
Rotation salt bath equipment shown in Fig. 1 embodiment of the present invention 1
The rotation bin of salt bath equipment is rotated in Fig. 2 embodiment of the present invention 1
The schematic diagram being detachably connected shown in Fig. 3 embodiment of the present invention 1 and 2
Tantalum wire prepared by Fig. 4 embodiments 3 exterior view under an electron microscope
Tantalum wire prepared by Fig. 5 comparative examples 1 exterior view under an electron microscope
Tantalum wire prepared by Fig. 6 embodiments 4 exterior view under an electron microscope
Tantalum wire prepared by Fig. 7 comparative examples 2 exterior view under an electron microscope
Tantalum wire prepared by Fig. 8 embodiments 5 exterior view under an electron microscope
Tantalum wire prepared by Fig. 9 comparative examples 3 exterior view under an electron microscope
Schema explanation：
1 mobile motor, 2 electric rotating machine
3. protection connects 4. shaft coupling of hanging scaffold
5. 6. link of salt bath reactor
7. 8. salt bath furnace of bin
9 tantalum bar, 10. switch board
61 connecting rod, 62 first linking arm
63 second linking arm, 64 fix bar
651 first lock-joint of 65U types connector
652 second lock-joint, 653 clamp
The 3rd lock-joint of 71 insulated column 72
73 pins
Specific embodiment
Technical scheme is further illustrated below by way of specific embodiment, specific embodiment is not represented to this
The restriction of bright protection domain.Other people still fall within this according to some nonessential modifications and adjustment that theory of the present invention is made
Bright protection domain.
A kind of 1 rotation salt bath equipment of embodiment
Rotation salt bath equipment as shown in Figure 1, containing salt bath reacting furnace 8, and positioned at the salt bath reaction of salt bath reacting furnace 8
Kettle 5.Described salt bath reactor 5 can be equipped with the fused salt of melting.
Described rotation salt bath equipment is also containing rotation bin (as illustrated in fig. 1 and 2).Described rotation bin contains rotation
Motor 2, and bin 7.Between electric rotating machine 2 and bin 7, connected by link 6.
Link 6 contains connecting rod 61, the linking arm being connected with connecting rod.Linking arm contains the first linking arm 62 and second
Linking arm 63.One end of connecting rod 61 is connected by shaft coupling 4 with electric rotating machine 2, and the other end of connecting rod 61 is connected with first
Arm 62 is connected jointly with one end of the second linking arm 63.First linking arm 62 and the second linking arm 63 are straight with what connecting rod 61 was located
Line, axisymmetricly.Used as preferred embodiment, the first described linking arm 62 and 63 middle setting of the second linking arm have fixation
Bar 64, makes two linking arms and fix bar 64 form triangular structure, strengthens the stability of link 6.
The other end of the first linking arm 62 and the second linking arm 63 is detachably connected with the two ends of bin 7 respectively.More specifically
Ground, as shown in Figure 3 (by taking one side as an example), the other end of the first linking arm 62 arranges U-shaped connector 65 to the mode being detachably connected,
For fixing bin 7；The first lock-joint 651 and the second lock-joint 652 are provided with the U-shaped arm of U-shaped connector 65, the end of bin sets
The 3rd lock-joint 72 is equipped with, first and third, two lock-joints can run through pin 73, bin 7 is connected with the first linking arm 62；Described is U-shaped
Connector 65 also has rotatable clamp 653, for clasping pin 73, fixed bin 7 and the first linking arm 62.
Bin 7 is used to hang tantalum bar 9.On bin 7, multiple insulated columns 71 are uniformly provided with, so as to entirely rotate bin
During rotation, tantalum bar 9 can be stably fixed on bin 7, uniform to aoxidize.
Also containing the mobile motor 1 being connected with electric rotating machine 2, mobile motor 1 is used to drive described rotation salt bath equipment
Rotate moving up and down for bin.
The rotation salt bath equipment also rotates salt bath equipment and contains switch board 10, and switch board 10 is used to control mobile motor 1
Motion, the rotation of electric rotating machine 2 and the temperature adjustment of salt bath furnace 8.
Also containing protection connection hanging scaffold 3, described protection connection hanging scaffold 3 is used for fixed and carries rotation rotation salt bath equipment
Motor 2, and being connected for electric rotating machine 2 and mobile motor 1.
When operating the rotation salt bath equipment, switch board 10 is adjusted, the temperature of molten salt in the reactor 5 of salt bath furnace is adjusted to
It is 500-530 DEG C, standby.Then the clamp 653 of rotation bin is taken out, extracts pin 73, tantalum bar 9 is uniform by insulated column 71
Be coiled on bin 7, install pin 73 and clamp 653, start mobile motor 1, the rotation bin with tantalum bar 9 is passed through
Mobile motor 1 hangs in salt bath reactor 5, is completely immersed in fused salt to tantalum bar 9, adjusts switch board 10, and startup is fixed on protection and connects
The electric rotating machine 2 on hanging scaffold is connect, is rotated by the speed of 50-100m/min, in fused salt inside holding 120-300sec.
A kind of 2 rotation salt bath equipment of embodiment
Repeat embodiment 1, have following difference with embodiment 1：
The other end of the first linking arm 62 and one end of bin 7 are detachably connected that (mode being detachably connected is shown in embodiment 1
With shown in Fig. 3), the other end of the second linking arm 63 is fixedly connected with the other end of bin 7.
A kind of method of 3 tantalum bar of embodiment surface treatment
The length of side of roll forming is L=7.05mm regular hexahedron tantalum bars, and disk is immersed in and is equipped with into the volume of diameter 300mm
In the ultrasonic water tank of degreaser, behind water temperature >=60 DEG C, 120min is rinsed；Regular hexahedron tantalum bar after rinsing is immersed in equipped with clear
In the ultrasonic water tank of water, 60min is cleaned in water temperature >=60 DEG C.Hexahedron tantalum bar after cleaning carries out surface using circulation baking oven
Pretreatment, is first put into the regular hexahedron tantalum bar after cleaning in baking oven, starts circulation baking oven, is passed through through filtered air, rises
Temperature is incubated 30min, tantalum bar surface is carried out except water process to 135 DEG C.
Temperature of molten salt in the reactor 5 of salt bath furnace is adjusted to 520 DEG C by adjustment switch board 10, standby.Then will rotation
The clamp 653 of bin takes out, and extracts pin 73, and regular hexahedron tantalum bar 9 is uniformly coiled on bin 7 by insulated column 71,
Pin 73 and clamp 653 are installed, starts mobile motor 1, the rotation bin with tantalum bar 9 is hung in into salt by mobile motor 1
Bath reactor 5, is completely immersed in fused salt to regular hexahedron tantalum bar 9, adjusts switch board 10, and startup is fixed on protection connection hanging scaffold 3
On electric rotating machine 2, by 80m/min speed rotate, in composite fused salt inside holding 210sec.
Regular hexahedron tantalum bar 9 is hung out salt bath reactor rapidly by 210sec after rotating heat-insulation soaking in salt bath reactor
5, specified location is moved to, 9 surface of regular hexahedron tantalum bar is rinsed using giant, hydraulic pressure 0.8MPa, 90 DEG C of water temperature,
Rinse 2 minutes.Flushed regular hexahedron tantalum bar 9 is soaked into into boiling in boiling clear water, is taken out after 20 minutes.
Through the above-mentioned regular hexahedron tantalum bar for processing, through the operation such as secondary rolling and filament rolling, the operation of rolling makes
Cooling is lubricated with rolling white oil, qualified tantalum capacitor anodes lead circle tantalum wire, tantalum wire diameter is rolled into
A kind of method of 4 tantalum bar of embodiment surface treatment
Repeat embodiment 3, have following difference：
Raw material be regular hexahedron tantalum bar, length of side L=6.05m.
The rotation of regular hexahedron tantalum bar is immersed in salt bath reactor, rotary speed 80m/min, and temperature of molten salt is 520 DEG C, is protected
Warm time 190sec.
Through the above-mentioned regular hexahedron tantalum bar for processing, through the operation such as secondary rolling and filament rolling, the operation of rolling makes
Cooling is lubricated with rolling white oil, qualified tantalum capacitor anodes lead circle tantalum wire, tantalum wire diameter is rolled into
A kind of surface treatment method of 5 tantalum bar of embodiment
Repeat embodiment 3, have following difference：
Raw material be regular hexahedron tantalum bar, length of side L=5.05mm.
Operation 6 is as follows：The rotation of regular hexahedron tantalum bar is immersed in salt bath reactor, rotary speed 80m/min, temperature of molten salt
For 520 DEG C, temperature retention time 170sec.
Through the above-mentioned regular hexahedron tantalum bar for processing, through the operation such as secondary rolling and filament rolling, the operation of rolling makes
Cooling is lubricated with rolling white oil, qualified tantalum capacitor anodes lead circle tantalum wire, tantalum wire diameter is rolled into
Comparative example 1：
Repeat embodiment 3, have following difference：
Do not start electric rotating machine during tantalum bar salt bath, in immersion salt bath furnace, holding time to 240sec.Due to not stirring
Mix pattern, tantalum bar be inactive state, deficiency of time in immersion in the case of tantalum bar surface, especially tantalum bar and bin contact
Contact between position, and tantalum bar and tantalum bar relatively closely where, have that selective oxidation is incomplete or oxidated layer thickness not enough,
Once there is local not aoxidize, the direct fracture of wire of meeting in follow-up drawing process, it is impossible to drawing, once there is continuous fracture of wire, whole
Silk can be scrapped, and only keep enough temperature retention times, just can guarantee that whole tantalum bar surface oxidation is complete.Therefore compared to embodiment
3 increased prolongation temperature retention time.
Comparative example 2：
Repeat embodiment 4, have following difference：
Electric rotating machine is not started during tantalum bar salt bath.
Comparative example 3：
Repeat embodiment 5, have following difference：
Tantalum bar salt bath does not start electric rotating machine.
The measure of 6 tantalum bar of embodiment and tantalum wire oxygen content
To embodiment 3-5, in comparative example 1-3, under three states, tantalum material oxygen content and surface smoothness are measured,
It is 1. tantalum bar salt bath before processings respectively
2. after tantalum bar salt bath is processed
3. the tantalum wire Jing after drawing
Determination of oxygen content method：According to National Standard of the People's Republic of China《GB3463-1995 tantalum wires》The method of regulation
Carry out.
Measurement result see the table below 1.
Table 1
Fineness sensing equipment：Measure under SEM electron microscope X200
The test result of fineness is shown in Figure of description 4-9.
Experimental result：As shown in Table 1, the tantalum bar surface oxygen content Jing after the rotation salt bath equipment of the present invention is processed is far below
Without the tantalum bar surface oxygen content of rotation processing.Tantalum wire Jing after drawing, rotation processing cross tantalum wire oxygen content less than 100ppm, energy
Enough meet tantalum wire chemical purity requirement used by current tantalum capacitor, and the then up to 200ppm of the tantalum wire oxygen content after comparative example drawing
More than.
Tantalum wire surface smoothness Jing after the rotation salt bath equipment of the present invention is processed is good, no obvious scratch and burr,
And comparative example then scratch is more and obvious.
Claims (10)
1. a kind of rotation salt bath equipment, including salt bath reacting furnace, and the salt bath reactor in salt bath reacting furnace, its feature
It is that, also including rotation bin, the rotation bin includes：
Electric rotating machine；
Link, described link one end are connected with electric rotating machine；
Bin, described bin are connected with the other end of link.
2. it is as claimed in claim 1 to rotate salt bath equipment, it is characterised in that described link includes connecting rod and connection
Arm,
One end of connecting rod is connected with electric rotating machine, and the other end is connected with linking arm；
The linking arm includes the first linking arm and one end of the second linking arm, the first described linking arm and the second linking arm is common
It is connected with the other end with connecting rod；
The other end of the first described linking arm and the second linking arm is connected with the two ends of bin respectively, wherein at least one connection
Arm is detachably connected with bin.
3. it is as claimed in claim 2 to rotate salt bath equipment, it is characterised in that in described the first linking arm and the second linking arm
Between be provided with fix bar.
4. rotation salt bath equipment as claimed in claim 2, it is characterised in that the first linking arm and/or the second linking arm it is another
One end arranges U-shaped connector, for fixing bin；The first lock-joint and the second lock-joint are provided with U-shaped connector, bin end sets
The 3rd lock-joint is equipped with, first and third, two lock-joints are detachably connected by pin；Described U-shaped connector also has rotatable card
Son, for clasping pin.
5. it is as claimed in claim 1 to rotate salt bath equipment, it is characterised in that on described bin, to be provided with some insulated columns.
6. it is as claimed in claim 1 to rotate salt bath equipment, it is characterised in that also to set between described electric rotating machine and link
It is equipped with shaft coupling.
7. it is as claimed in claim 1 to rotate salt bath equipment, it is characterised in that also to include the mobile electricity being connected with electric rotating machine
Machine.
8. it is as claimed in claim 7 to rotate salt bath equipment, it is characterised in that also containing protection connection hanging scaffold, the electric rotating
Machine is connected by protecting connection hanging scaffold with mobile motor.
9. it is as claimed in claim 8 to rotate salt bath equipment, it is characterised in that the switch board for also containing.
10. a kind of method that tantalum bar is surface-treated, it is characterised in that comprise the steps of：
S1. tantalum bar is coiled into rolling；
S2. tantalum bar ultrasonic surface is cleaned；
S3. drying pretreatment is done to tantalum bar surface；
S4. tantalum bar is put in the salt bath furnace of molten condition and does surface of revolution oxidation processes
S5. the tantalum bar for processing to salt bath does removing surface；
Preferably, in step S1, the coil diameter of tantalum bar is Φ 200mm～Φ 300mm；
Preferably, in step S3, during drying and processing, the temperature of baking oven is 120-150 DEG C, and air quantity is 30-50m3/min；
Preferably, in step S4, the temperature of salt bath is 500-530 DEG C, and time of salt bath is 120-300sec, the tantalum bar line of rotation
Speed is 50-100m/min；
Preferably, in step S5, it is to be rinsed using high-temperature high pressure water the step of removing surface, then boiling water immersion；
Further, hydraulic pressure is 0.5-1.0MPa, and water temperature is 90 DEG C -100 DEG C, and washing time is to come out of the stove in 1-3min；Boiling water soaks
The bubble time is 15-30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611260609.8A CN106521403B (en) | 2016-12-30 | 2016-12-30 | A kind of method of tantalum item surface treatment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611260609.8A CN106521403B (en) | 2016-12-30 | 2016-12-30 | A kind of method of tantalum item surface treatment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106521403A true CN106521403A (en) | 2017-03-22 |
| CN106521403B CN106521403B (en) | 2018-09-14 |
Family
ID=58336202
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611260609.8A Active CN106521403B (en) | 2016-12-30 | 2016-12-30 | A kind of method of tantalum item surface treatment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106521403B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150259A (en) * | 2021-12-08 | 2022-03-08 | 宁夏大学 | Nitriding heat treatment device for blind hole characteristic parts |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050223976A1 (en) * | 2002-06-21 | 2005-10-13 | Band-Zink Gmbh | Coating device |
| CN204111848U (en) * | 2014-09-26 | 2015-01-21 | 扬州市派莱斯塑胶电器有限公司 | A kind of bolt heat galvanizing rig |
| CN105861790A (en) * | 2016-04-20 | 2016-08-17 | 太仓宝达齿条有限公司 | Electrothermal treatment device for helical rack |
| CN206359601U (en) * | 2016-12-30 | 2017-07-28 | 江门富祥电子材料有限公司 | A kind of rotation salt bath equipment of tantalum material surface treatment |
-
2016
- 2016-12-30 CN CN201611260609.8A patent/CN106521403B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050223976A1 (en) * | 2002-06-21 | 2005-10-13 | Band-Zink Gmbh | Coating device |
| CN204111848U (en) * | 2014-09-26 | 2015-01-21 | 扬州市派莱斯塑胶电器有限公司 | A kind of bolt heat galvanizing rig |
| CN105861790A (en) * | 2016-04-20 | 2016-08-17 | 太仓宝达齿条有限公司 | Electrothermal treatment device for helical rack |
| CN206359601U (en) * | 2016-12-30 | 2017-07-28 | 江门富祥电子材料有限公司 | A kind of rotation salt bath equipment of tantalum material surface treatment |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150259A (en) * | 2021-12-08 | 2022-03-08 | 宁夏大学 | Nitriding heat treatment device for blind hole characteristic parts |
| CN114150259B (en) * | 2021-12-08 | 2023-09-29 | 宁夏大学 | Nitriding heat treatment device for blind hole characteristic parts |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106521403B (en) | 2018-09-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6788097B2 (en) | Method for producing reduced titanium powder by multi-step strong reduction | |
| CN106653373B (en) | A kind of aluminium electrolutic capacitor Waste Acid From Hua Cheng Foil and its production technology | |
| CN104630633B (en) | Preparation method of anti-carburizing electrothermal alloy | |
| JP6922090B2 (en) | Manufacturing method of medium-high pressure corrosive foil for aluminum electrolytic capacitors | |
| CN105331913B (en) | Method for thermally extruding and deforming high-temperature alloy Inconel 625 pipe through short process | |
| CN109652627B (en) | Annealing processing technology for producing high-performance metal wire | |
| CN109277429B (en) | Preparation method of high-purity vanadium wire | |
| CN106086865B (en) | A kind of magnesia coating processes improving orientation silicon steel bottom | |
| CN206359601U (en) | A kind of rotation salt bath equipment of tantalum material surface treatment | |
| CN112064043A (en) | Method for removing oxide film on surface of iron-chromium-aluminum wire rod and heating container | |
| CN106521403B (en) | A kind of method of tantalum item surface treatment | |
| CN104308461A (en) | Titanium alloy tube and production method thereof | |
| CN109786113A (en) | A kind of aluminium electrolutic capacitor Waste Acid From Hua Cheng Foil and its production technology | |
| CN106782849A (en) | One kind compound hard state copper busbar and its preparation technology | |
| CN107699928A (en) | The preparation method of black rhenium coating | |
| CN110644025A (en) | Ultrathin nickel-copper alloy foil and preparation method thereof | |
| CN207828380U (en) | A kind of copper wire annealing device | |
| CN104562088A (en) | Electrolytic aluminum cathode conductive rod and preparation method thereof | |
| CN104616898B (en) | A kind of method that additional annealing treatment improves aluminium foil hair engaging aperture performance | |
| CN107902888A (en) | A kind of processing method for improving glass fibre electric conductivity | |
| CN106757236A (en) | Improve the method and palladium film layer of stainless steel surfaces palladium film layer decay resistance | |
| CN114709026B (en) | Copper-clad steel processing technology without acid and alkali participation | |
| CN106191731A (en) | Copper covered steel wire vertical Jin Tong mechanism | |
| CN105321625A (en) | Production process of soft copper-clad steel wire | |
| CN104722771A (en) | Preparation method of molybdenum powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |