CN106521403B - A kind of method of tantalum item surface treatment - Google Patents
A kind of method of tantalum item surface treatment Download PDFInfo
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- CN106521403B CN106521403B CN201611260609.8A CN201611260609A CN106521403B CN 106521403 B CN106521403 B CN 106521403B CN 201611260609 A CN201611260609 A CN 201611260609A CN 106521403 B CN106521403 B CN 106521403B
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- 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
Abstract
The invention belongs to tantalum wire field of surface treatment, are related to one kind in tantalum wire production process, the processing method of tantalum surface oxidation treatment.Processing method using the present invention is surface-treated tantalum item, can control the surface oxide layer thickness of tantalum item, makes tantalum surface uniform alumina, controls the oxygen content of oxide layer, improves finished product tantalum wire surface smoothness.
Description
Technical field
The invention belongs to tantalum wire field of surface treatment, are related to one kind in tantalum wire production process, the surface treatment side of tantalum item
Method.
Background technology
Capacitor is widely used in the fields such as communication, computer, automobile, household electrical appliances, aerospace now, makees sun with tantalum powder
Pole, tantalum wire make the tantalum electrolytic capacitor of anode tap making, have small, and capacitance is big, chip type degree is high, reliability
The characteristics of excellent combination properties such as good, service life length, thus can be in many other capacitors such as ceramics, aluminium film capacitor
It is worked normally under incompetent harsh conditions.
Tantalum wire as tantalum capacitor anodes lead, it is desirable that chemical purity is high, and surface smoothness is good, accurate size, machine
Tool performance, chemical property meet the strict demand of capacitor.For example, being to the specific requirement of tantalum wire surface smoothness：60
Times or more microscopically observation surface without apparent groove, burr, hole point the defects of；The specific requirement of chemical property is leakproof
Stream, leakage current is smaller, and performance is better.
Tantalum wire to produce the technique since bar as follows：
Raw bar material → type rolls → and surface film process → intermediate annealing → drawing → cleaning → after-combustion → quality inspection → is packaged into
Library.
Surface membrane treatment process ensures tantalum wire surface smoothness during the drawing process mainly for the protection of tantalum wire surface.Table
Facial mask treatment process is mainly surface-treated by salt bath and is aoxidized benefit film surface processing and forms.
Salt bath furnace, which refers to, uses melting saline solution as heat medium, and workpiece is immersed to the industrial furnace heated in saline solution, usually uses chlorine
Change the salts such as sodium, potassium chloride, barium chloride, sodium hydride, potassium cyanide, sodium nitrate, potassium nitrate as heat medium.Salt bath furnace can be used for
The heat treatments such as the quenching of carbon steel, steel alloy, tool steel, mould steel and aluminium alloy etc., annealing, tempering, cyaniding, timeliness are heated,
It can also be used for slight oxidization heating when steel precision forging.Tantalum category refractory metal, 2996 DEG C of fusing point do not occur anti-with oxygen at room temperature
It answers；In 280 DEG C to 300 DEG C very slight surface oxidations；350 DEG C of slight oxidation surfaces from yellow to red, purpling, become blue；390℃
To 440 DEG C of blackening, 480 DEG C or so change dark gray, 500 DEG C gradually appear oxide white.The surface treatment of tantalum salt bath furnace is logical
The salts such as sodium chloride, potassium chloride, barium chloride, sodium nitrate, the potassium nitrate for the molten condition being sufficiently stirred are crossed as heat medium pair
Do oxidation processes in tantalum surface.Lead of the tantalum item for doing tantalum capacitor after drawing tantalum wire, it is desirable that chemical composition purity is high, tantalum wire
Middle oxygen content≤100ppm.Tantalum item is immersed in the time in salt bath furnace and must be strictly controlled, to ensure after salt bath furnace is handled
Tantalum oxygen content in controlled range.
In the prior art, tantalum salt bath furnace treatment process uses external heating type salt bath furnace, is that the tantalum item that will be tied is put into not
Rust steel material frame, is immersed in salt bath furnace, after reaction appropriate, layer oxide film can be formed on tantalum surface, in tantalum
Tantalum surface is formed in drawing process and is protected.However, this equipment and the processed tantalum item of process matching, surface forms oxygen
It is uneven to change layer thickness, local surfaces can be because form scratch and burr, Bu Nengyou without protective layer in tantalum drawing process
Effect ensures tantalum wire surface smoothness, and after drawing, oxygen content is higher than 100PPM in finished product tantalum wire, it is difficult to meet current tantalum capacitor institute
With the requirement of tantalum wire chemical purity.In addition, salt bath furnace fire door temperature is high, operating condition is severe, and the fused salt liquid of molten condition meets water
Splash phenomena then occurs, vigorous combustion and explosion can be occurred by meeting oil, charcoal and other organic matters.
Invention content
Present invention aims at a kind of rotation salt bath equipment is provided, it to be used for the salt bath surface oxidation treatment of tantalum item, the rotation
Salt bath equipment can make tantalum item when salt bath is handled, uniform to aoxidize, and form the uniform oxide layer of thickness, ensure tantalum wire after drawing
Finish and low oxygen content.
The present invention also aims to provide a kind of rotation salt bath equipment containing rotation rack.
The present invention also aims to provide a kind of method of tantalum item surface treatment.
The above-mentioned purpose of the present invention is realized by following technological means：
A kind of rotation salt bath equipment：The rotation salt bath equipment contains salt bath reacting furnace, and is located at salt bath reacting furnace
Interior salt bath reaction kettle, the salt bath reaction kettle can be equipped with the fused salt of melting, which is characterized in that further include rotation rack, institute
Stating rotation rack includes：
Electric rotating machine；
Rack；
Link；The link is for connecting electric rotating machine and rack.Further, one end of the link
It is connected with electric rotating machine, the other end is connect with rack.
The 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 and electric rotating machine of connecting rod.The other end of connecting rod
It is connected with linking arm.
The linking arm includes the first linking arm and the second linking arm.First linking arm and the second linking arm
One end is connected with the other end of connecting rod jointly.
The other end of first linking arm and the second linking arm and the both ends of rack are at least detachably to connect on one side
It connects.First linking arm and the second linking arm with the straight line where connecting rod axisymmetricly.
As preferred embodiment, it is provided with fixed link among first linking arm and the second linking arm, makes two
A linking arm and fixed link form triangular structure, enhance the stability of link.
The rack is for hanging tantalum item.As preferred embodiment, it is provided with insulated column on rack, for being isolated
Fixed tantalum item, entirely to rotate rack when rotated, tantalum item is stably fixed on rack, uniform to aoxidize.As more excellent
The embodiment of choosing is provided with multiple insulated columns on rack, and the spacing of each insulated column is identical.
In invention, the other end of first linking arm and the second linking arm is connect with rack both ends respectively, wherein
At least one linking arm is detachably connected with rack.It, can be by the coiled tantalum item of disk by dismantling linking arm and rack
Rack is hung up, and tantalum item is fixed by the insulated column of rack, then connects rack and linking arm, you can rotation liquid oxidizing.Salt
Linking arm and rack are dismantled after bath and cleaning, removes tantalum item.
In one embodiment of the invention, the detachable of one end of the other end and rack of first linking arm connects
It connects, the other end of the second linking arm is fixedly connected with the other end of rack.
In another embodiment of the invention, the other end of first linking arm and the second linking arm with rack
Both ends are detachably connected.
Further, being detachably connected for linking arm and rack is by being clamped or hinged or other detachably connect
Connect mode.
In the exemplary embodiment of the present invention, U is arranged in the other end of first linking arm and/or the second linking arm
Shape connector, U-shaped connector is for being removably secured rack.Further, having setting on U-shaped connector, there are two opposite
Lock-joint, the first lock-joint and the second lock-joint.The end of rack is provided with third lock-joint.First lock-joint, the second lock-joint and third pin
Mouth can be inserted into a movable pin on same straight line in lock-joint, rack and connection are kept away arm connection.When installation, it will expect
The end of frame is put into the U-shaped connector of linking arm, so that third lock-joint and the first, second lock-joint is aligned, is inserted into pin.U-shaped connection
A rotatable clamp is additionally provided on part, when rotate to block pin when, pin can be fixed, to linking arm and material
Frame.
As preferred embodiment, rotation rack of the invention also contains shaft coupling, for connecting electric rotating machine and company
Frame is connect, is allowed to rotate jointly.
The rotation salt bath equipment also contains the mobile motor being connected with the electric rotating machine of mobile rack, the movement
Motor is used to control moving up and down for rotation rack.
The rotation salt bath equipment also contains switch board, and the switch board is used to control the movement of mobile motor, rotation
The rotation of rotating motor and the temperature adjustment of salt bath furnace.
As preferred embodiment, rotation salt bath equipment of the invention also contains protection connection hanging scaffold, the protection
Connection hanging scaffold is for 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 reaction kettle of salt bath furnace is adjusted to
It is 500-530 DEG C, spare.Then the clamp for rotating rack is taken out, extracts pin, tantalum item is uniformly coiled in by insulated column
On rack, pin and clamp are installed, starts mobile motor, the rotation rack with tantalum item is hung in into salt bath by mobile motor
Reaction kettle adjusts switch board until tantalum item is completely immersed in fused salt, starts the electric rotating machine being fixed on protection connection hanging scaffold, presses
The speed of 50-100m/min rotates, in fused salt inside holding 120-300sec.
The present invention also provides a kind of methods of tantalum item surface treatment, and it includes following steps：
S1. tantalum item is coiled coiled；
S2. tantalum ultrasonic surface is cleaned；
S3. drying pretreatment is done to tantalum surface；
S4. tantalum item is put into the salt bath furnace of molten condition and does surface of revolution oxidation processes；
S5. removing surface is done to the processed tantalum item of salt bath.
In step S1, the coil diameter of tantalum item is Φ 200mm~Φ 300mm；Tantalum item coils curvature cannot be too big, otherwise tantalum
Generation is significantly bent by item on wire spool, cannot be satisfied requirement.
In step S3, when drying and processing, the temperature of baking oven is 120-150 DEG C, air quantity 30-50m3/min；
In step S4, the temperature of salt bath is 500-530 DEG C, and the time of salt bath is 120-300sec, the tantalum linear speed of rotation
Degree is 50-100m/min；
In step S5, to be rinsed using high-temperature high pressure water the step of removing surface, then boiling water impregnates；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 soaking time is 15-30min.
In an embodiment of the present invention, through rotate salt bath processing tantalum item, oxygen content in 200ppm hereinafter, it is preferred that
160ppm or less is more preferably in 140ppm or less, more preferably in 120ppm or less.Oxygen content after the surface treatment of national standard tantalum item
Generally in 300ppm or less.In the prior art, oxygen content oxygen generally after 200ppm or more, drawing after the surface treatment of tantalum salt bath
Content is generally in 100ppm or more.In an embodiment of the present invention, through rotating the tantalum item of salt bath processing, oxygen content exists after drawing
100ppm or less.
The advantageous effect that the present invention obtains：
1 present invention provides a kind of rotation salt bath equipment, which can be in tantalum item for the first time in tantalum wire field of surface treatment
When the film process of salt bath surface, by the rotation to tantalum item, make tantalum item uniformly oxidation filming, and is easy to control tantalum item film forming
Thickness.Through rotating the tantalum item of salt bath processing, oxygen content can even reach in 200ppm or less, even up to 160ppm or less, more
120ppm or less.The wire drawing die longevity can be effectively turned up in subsequent tantalum drawing process in tantalum item through rotating salt bath processing
Life, after tantalum item is drawn into tantalum wire, surface smoothness is high, and oxygen content in 100ppm hereinafter, disclosure satisfy that the chemistry of tantalum capacitor
Purity requirement.Before this, in the salt bath process field of tantalum item, never someone expected, also non-someone salt bath by the way of rotation
Tantalum item is handled, to improve the uniformity and chemical purity of tantalum oxidation filming, more nobody provides a kind of rotation salt bath equipment use
It is handled in the salt bath of tantalum item.
The rotation salt bath device structure of 2 present invention is simple, easy to use.
The rotation salt bath equipment safety of 3 present invention is reliable：It is provided with fixed link between two support arms, forms the steady of triangle
Determine structure, electric rotating machine is fixed on protection connection hanging scaffold；By using rotation salt bath equipment, salt bath table can be completed by switch board
Surface treatment does not need operator close to salt bath furnace.Because fire door temperature is high, operating condition is severe, the fused salt liquid of molten condition
It meets water and splash phenomena then occurs.
4 reduce the soaking time in salt bath processing procedure, improve treatment effeciency.
5 can effectively improve the wire drawing die service life to wire drawing die during the drawing process using the tantalum item of rotation salt bath processing,
Finished product φ 0.15mm tantalum wires, from originally often set can 2.4 myriametre of drawing be increased 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 rack 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
The exterior view of tantalum wire prepared by Fig. 4 embodiments 3 under an electron microscope
The exterior view of tantalum wire prepared by Fig. 5 comparative examples 1 under an electron microscope
The exterior view of tantalum wire prepared by Fig. 6 embodiments 4 under an electron microscope
The exterior view of tantalum wire prepared by Fig. 7 comparative examples 2 under an electron microscope
The exterior view of tantalum wire prepared by Fig. 8 embodiments 5 under an electron microscope
The exterior view of tantalum wire prepared by Fig. 9 comparative examples 3 under an electron microscope
Schema explanation：
1 mobile motor, 2 electric rotating machine
3. protection connection 4. shaft coupling of hanging scaffold
5. 6. link of salt bath reaction kettle
7. 8. salt bath furnace of rack
9 tantalum item, 10. switch board
61 connecting rod, 62 first linking arm
63 second linking arm, 64 fixed link
651 first lock-joint of 65U types connector
652 second lock-joint, 653 clamp
71 insulated column, 72 third lock-joint
73 pins
Specific implementation mode
Below by way of the technical solution that specific embodiment further illustrates the present invention, specific embodiment does not represent to this hair
The limitation of bright protection domain.Other people still fall within this hair 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 is reacted containing salt bath reacting furnace 8, and positioned at the salt bath of salt bath reacting furnace 8
Kettle 5.The salt bath reaction kettle 5 can be equipped with the fused salt of melting.
The rotation salt bath equipment also contains rotation rack (as illustrated in fig. 1 and 2).The rotation rack contains rotation
Motor 2 and rack 7.Between electric rotating machine 2 and rack 7, connected by link 6.
Link 6 contains connecting rod 61, the linking arm being connect with connecting rod.Linking arm contains the first linking arm 62 and second
Linking arm 63.One end of connecting rod 61 is connected with electric rotating machine 2 by shaft coupling 4, and the other end of connecting rod 61 is connect 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 where with connecting rod 61
Line, axisymmetricly.As preferred embodiment, fixation is provided among first linking arm 62 and the second linking arm 63
Bar 64 makes two linking arms and fixed link 64 form triangular structure, enhances the stability of link 6.
Both ends of the other end of first linking arm 62 and the second linking arm 63 respectively with rack 7 are detachably connected.More specifically
Ground, as shown in Figure 3 (by taking one side as an example), U-shaped connector 65 is arranged in the other end of the first linking arm 62 to the mode being detachably connected,
For fixing rack 7；The first lock-joint 651 and the second lock-joint 652 are provided on the U-shaped arm of U-shaped connector 65, the end of rack is set
It is equipped with third lock-joint 72, first and third, two lock-joints can run through pin 73, rack 7 is connect with the first linking arm 62；Described is U-shaped
Connector 65 also has rotatable clamp 653, for clasping pin 73,7 and first linking arm 62 of fixed rack.
Rack 7 is for hanging tantalum item 9.On rack 7, multiple insulated columns 71 are evenly provided with, so as to entirely rotate rack
When rotation, tantalum item 9 can be stably fixed on rack 7, uniform to aoxidize.
The rotation salt bath equipment also contains the mobile motor 1 being connected with electric rotating machine 2, and mobile motor 1 is for driving
Rotation rack moves up and down.
The rotation salt bath equipment also rotates salt bath equipment and contains switch board 10, and switch board 10 is for controlling mobile motor 1
Movement, the rotation of electric rotating machine 2 and the temperature adjustment of salt bath furnace 8.
It rotates salt bath equipment and also contains protection connection hanging scaffold 3, the protection connects hanging scaffold 3 for fixed and carrying rotation
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 reaction kettle 5 of salt bath furnace is adjusted to
It is 500-530 DEG C, spare.Then the clamp 653 for rotating rack is taken out, extracts pin 73, tantalum item 9 is uniform by insulated column 71
Be coiled on rack 7, install pin 73 and clamp 653, start mobile motor 1, the rotation rack with tantalum item 9 is passed through
Mobile motor 1 hangs in salt bath reaction kettle 5, until tantalum item 9 is completely immersed in fused salt, adjusts switch board 10, 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
Embodiment 1 is repeated, has following difference with embodiment 1：
The other end of first linking arm 62 and one end of rack 7 are detachably connected that (mode being detachably connected is shown in embodiment 1
Shown in Fig. 3), the other end of the second linking arm 63 is fixedly connected with the other end of rack 7.
A kind of method of 3 tantalum item of embodiment surface treatment
The length of side of roll forming is L=7.05mm regular hexahedron tantalum items, and disk is immersed in and is equipped at the volume of diameter 300mm
In the ultrasonic water tank of degreaser, behind water temperature >=60 DEG C, 120min is rinsed；Regular hexahedron tantalum item 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 item after cleaning carries out surface using cycle baking oven
Regular hexahedron tantalum item after cleaning, is first put into baking oven by pretreatment, starts cycle baking oven, is passed through by filtered air, rises
Temperature keeps the temperature 30min to 135 DEG C, carries out removing water process to tantalum surface.
Switch board 10 is adjusted, the temperature of molten salt in the reaction kettle 5 of salt bath furnace is adjusted to 520 DEG C, it is spare.It then will rotation
The clamp 653 of rack takes out, and extracts pin 73, regular hexahedron tantalum item 9 is uniformly coiled in by insulated column 71 on rack 7,
Pin 73 and clamp 653 are installed, starts mobile motor 1, the rotation rack with tantalum item 9 is hung in into salt by mobile motor 1
Reaction kettle 5 is bathed, until regular hexahedron tantalum item 9 is completely immersed in fused salt, adjusts switch board 10, 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.
210sec after rotation heat-insulation soaking, hangs out salt bath reaction kettle by regular hexahedron tantalum item 9 rapidly in salt bath reaction kettle
5, it is moved to designated position, 9 surface of regular hexahedron tantalum item is rinsed using giant, hydraulic pressure 0.8MPa, 90 DEG C of water temperature,
It rinses 2 minutes.Flushed regular hexahedron tantalum item 9 is soaked into boiling in boiling clear water, is taken out after twenty minutes.
By above-mentioned processed regular hexahedron tantalum item, make by processes, the operation of rolling such as secondary rolling and filament rolling
It is lubricated cooling with rolling white oil, is rolled into qualified tantalum capacitor anodes lead circle tantalum wire, tantalum wire diameter
A kind of method of 4 tantalum item of embodiment surface treatment
Embodiment 3 is repeated, there is following difference：
Raw material is regular hexahedron tantalum item, length of side L=6.05m.
The rotation of regular hexahedron tantalum item is immersed in salt bath reaction kettle, rotary speed 80m/min, and temperature of molten salt is 520 DEG C, is protected
Warm time 190sec.
By above-mentioned processed regular hexahedron tantalum item, make by processes, the operation of rolling such as secondary rolling and filament rolling
It is lubricated cooling with rolling white oil, is rolled into qualified tantalum capacitor anodes lead circle tantalum wire, tantalum wire diameter
A kind of surface treatment method of 5 tantalum item of embodiment
Embodiment 3 is repeated, there is following difference：
Raw material is regular hexahedron tantalum item, length of side L=5.05mm.
Process 6 is as follows：The rotation of regular hexahedron tantalum item is immersed in salt bath reaction kettle, rotary speed 80m/min, temperature of molten salt
It is 520 DEG C, soaking time 170sec.
By above-mentioned processed regular hexahedron tantalum item, make by processes, the operation of rolling such as secondary rolling and filament rolling
It is lubricated cooling with rolling white oil, is rolled into qualified tantalum capacitor anodes lead circle tantalum wire, tantalum wire diameter
Comparative example 1：
Embodiment 3 is repeated, there is following difference：
Do not start electric rotating machine when tantalum salt bath, impregnates in salt bath furnace, holding time to 240sec.Due to not stirring
Pattern is mixed, tantalum item is stationary state when impregnating, the contact of tantalum surface in the case of the time is insufficient, especially tantalum item and rack
More close place is contacted between position and tantalum item and tantalum item, has that selective oxidation is incomplete or oxidated layer thickness is inadequate,
Once there is part not aoxidize, in follow-up drawing process can direct fracture of wire, can not drawing, once there is continuous fracture of wire, whole
Silk can be scrapped, and only keep enough soaking times, just can guarantee that whole tantalum surface oxidation is complete.Therefore compared to embodiment
3 increase extension soaking time.
Comparative example 2：
Embodiment 4 is repeated, there is following difference：
Do not start electric rotating machine when tantalum salt bath.
Comparative example 3：
Embodiment 5 is repeated, there is following difference：
Tantalum salt bath does not start electric rotating machine.
The measurement of embodiment 6 tantalum item and tantalum wire oxygen content
To embodiment 3-5, tantalum material oxygen content and surface smoothness are measured under three states in comparative example 1-3,
It is before 1. tantalum salt baths are handled respectively
2. after the processing of tantalum salt bath
3. the tantalum wire after drawing
Determination of oxygen content method：According to National Standard of the People's Republic of China《GB3463-1995 tantalum wires》Defined method
It carries out.
Measurement result see the table below 1.
Table 1
Finish sensing equipment：It is measured under SEM electron microscopes X200
The test result of finish is shown in Figure of description 4-9.
Experimental result：As shown in Table 1, treated that tantalum surface oxygen content is far below for the rotation salt bath equipment through the present invention
Tantalum surface oxygen content without rotation processing.Tantalum wire after drawing, rotation processing cross tantalum wire oxygen content and are less than 100ppm, energy
Enough meet tantalum wire chemical purity requirement used in current tantalum capacitor, and the then up to 200ppm of the tantalum wire oxygen content after comparative example drawing
More than.
Treated that tantalum wire surface smoothness is good for rotation salt bath equipment through the present invention, without apparent scratch and burr,
And then scratch is more and apparent for comparative example.
Claims (5)
1. a kind of method of tantalum item surface treatment, which is characterized in that comprise the steps of：
S1. tantalum item is coiled coiled；
S2. tantalum ultrasonic surface is cleaned；
S3. drying pretreatment is done to tantalum surface；
S4. tantalum item is put into the salt bath furnace of molten condition and does surface of revolution oxidation processes；
Wherein, in step S4, the temperature of salt bath is 500-530 DEG C, and the time of salt bath is 120-300sec, the tantalum linear speed of rotation
Degree is 50-100m/min；
S5. removing surface is done to the processed tantalum item of salt bath.
2. according to the method described in claim 1, it is characterized in that, in step S1, the coil diameter of tantalum item is Φ 200mm~Φ
300mm。
3. according to the method described in claim 1, it is characterized in that, in step S3, when drying pre-processes, the temperature of baking oven is
120-150 DEG C, air quantity 30-50m3/min。
4. according to the method described in claim 1, it is characterized in that, in step S5, for using high temperature height the step of removing surface
Blow wash, then boiling water impregnate.
5. according to the method described in claim 4, it is characterized in that, hydraulic pressure is 0.5-1.0MPa, water temperature is 90 DEG C -100 DEG C, punching
It is to come out of the stove in 1-3min to wash the time；Boiling water soaking time is 15-30min.
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