CN108456917A - A kind of preparation method of porous tantalum piece - Google Patents
A kind of preparation method of porous tantalum piece Download PDFInfo
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- CN108456917A CN108456917A CN201810354215.1A CN201810354215A CN108456917A CN 108456917 A CN108456917 A CN 108456917A CN 201810354215 A CN201810354215 A CN 201810354215A CN 108456917 A CN108456917 A CN 108456917A
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- tantalum piece
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- porous tantalum
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/08—Etching of refractory metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
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Abstract
The invention belongs to tantalum piece preparing technical fields, disclose a kind of preparation method of porous tantalum piece, and by the way of electrolytic etching, electrolyte solution is configured to absolute alcohol and etamon chloride；Be placed in electrolytic cell as cathode electrode, anode electrode and cathode electrode as anode electrode, stainless steel plate using tantalum piece and fix interpolar away from；Electrolyte solution is added in electrolytic cell, anode electrode, cathode electrode are respectively connected to the positive and negative anodes of DC power supply, starts electrolytic etching and prepares porous tantalum piece.Using this preparation method, indissoluble object will not be generated during electrolytic etching and is deposited on porous tantalum on piece, the porous tantalum piece ingredient of preparation gained is single, purity is higher, porosity is high, large specific surface area；Electrolyte solution ingredient is simple, easily controllable, and ingredient is not easily decomposed, and process stabilizing；Electrolytic cell is placed in vibration of ultrasonic wave device, electrolytic etching process is made to be completed under ultrasound-enhanced effect, the discharge for being electrolysed corrosion product on tantalum piece can be accelerated.
Description
Technical field
The present invention relates to tantalum piece preparing technical fields, and in particular, to a kind of preparation method of porous tantalum piece.
Background technology
Metal tantalum is high with fusing point, cold-forming property is good, chemical stability is high, anti-liquid metal corrosion ability is strong, surface
A series of excellent properties such as oxidation film dielectric constant is big, in electronics, metallurgy, steel, chemical industry, hard alloy, atomic energy, superconduction skill
The high-technology fields such as art, automotive electronics, aerospace, health care and scientific research have important application.But due to tantalum
High-melting-point characteristic, prepare material porosity it is relatively low, pore size is uneven and rate of closed hole is high, and the tantalum piece made by
Low in porosity, pore size is uneven, and specific surface area is small, influences normal use.
Currently, about including mainly in the preparation of porous tantalum piece：Two kinds of vapour deposition process, laser cladding.Wherein, gas phase
Porous tantalum piece prepared by sedimentation has high volume porosity rate, the characteristic of low elastic modulus and high skin-friction coefficient, but should
Process condition requirement is stringent, deposition velocity is slow, production cost is high, simultaneously because tantalum belongs to insoluble metal, evaporation is very
It is difficult.In addition, the manufacturing method of porous tantalum piece workpiece laser cladding has, energy-controllable is high, processing heat affected area is narrow, processing
The advantages that efficient, can preferably adapt to vibration monitoring, but it needs to be additionally carried out laser melting coating cutting, causes cost big
It is big to increase, limit its extensive use.
Invention content
Present invention solves the technical problem that be to overcome the deficiencies of existing technologies, provide it is a kind of it is simple and efficient to handle, of low cost,
The preparation method of readily available large specific surface area and the high porous tantalum piece of porosity.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of porous tantalum piece is configured to by the way of electrolytic etching with absolute alcohol and etamon chloride
Electrolyte solution；It is placed in as cathode electrode, anode electrode and cathode electrode as anode electrode, stainless steel plate using tantalum piece
In electrolytic cell and fix interpolar away from；Electrolyte solution is added in electrolytic cell, anode electrode, cathode electrode are respectively connected to
The positive and negative anodes of DC power supply start electrolytic etching and prepare porous tantalum piece（The sequencing of above step can be upset）.
Further, in electrolyte solution etamon chloride a concentration of 0.05~0.4mol/L.
Preferably, in electrolyte solution etamon chloride a concentration of 0.05~0.1mol/L.
It is further preferred that in electrolyte solution etamon chloride a concentration of 0.1mol/L.
Specifically, absolute alcohol purity is 95~99.7% in electrolyte solution.
Further, interpolar is away from for 1~5cm.
Further, the voltage that electrolytic etching uses is 10~40V；Or the electric current that electrolytic etching uses is 1~4A.
Further, the electrolytic etching time is 20s~30min, and the wherein electrolytic etching time is in anti-with electrolytic etching voltage
Correlation, i.e. voltage are smaller, then the electrolytic etching time need to be longer.
Further, tantalum piece and/or stainless steel plate need to carry out ultrasonic cleaning before being fixed in electrolytic cell.
Further, stainless steel plate needs polishing removal surface oxidation film before carrying out ultrasonic cleaning.
Further, preparation can accommodate the vibration of ultrasonic wave device of electrolytic cell, and electrolytic cell is positioned in vibration of ultrasonic wave device
Ultrasound is carried out, electrolytic etching process is made to be carried out under ultrasound-enhanced effect.
Preferably, 350~450W of ultrasonic power, frequency are 35000~45000HZ.
It is further preferred that ultrasonic power 400W, frequency 40000HZ.
Further, electrolyte solution liquid level is at the 2/3 of electrolysis groove height.
Compared with prior art, the invention has the advantages that：
1）The porous tantalum piece porosity that is prepared is high, large specific surface area, and the excellent raw material that can be used as each related field uses；
2）Method using the present invention prepares porous tantalum piece, and indissoluble object will not be generated during electrolytic etching and is deposited on porous tantalum
On piece, the porous tantalum piece ingredient of preparation gained is single, purity is higher；
3）The electrolyte solution ingredient that the present invention prepares is simple, easily controllable, and ingredient is not easy to decompose, and process stabilizing；
4）Electrolytic cell is placed in vibration of ultrasonic wave device, electrolytic etching process is made to be completed under ultrasound-enhanced effect, tantalum can be accelerated
The discharge of on piece electrolytic etching product, while the supplement of fresh electrolyte can be promoted；
5）The porous tantalum piece preparation method preparation efficiency of the present invention is high, at low cost, should be widely promoted, can meet the market demand.
Description of the drawings
Fig. 1 is the preparation facilities schematic diagram used in the preparation method of porous tantalum piece described in embodiment；
Fig. 2 is the material phase analysis figure of porous tantalum piece obtained under concentration of electrolyte solutions different condition；
Fig. 3 is metallograph of the porous tantalum piece under 200um scales made from the preparation method of embodiment 1；
Fig. 4 is metallograph of the porous tantalum piece under 200um scales made from the preparation method of embodiment 2；
Fig. 5 is metallograph of the porous tantalum piece under 40um scales made from the preparation method of embodiment 5；
Fig. 6 is metallograph of the porous tantalum piece under 40um scales made from the preparation method of embodiment 6；
Fig. 7 is metallograph of the porous tantalum piece under 40um scales made from the preparation method of embodiment 7；
Fig. 8 is metallograph of the porous tantalum piece under 40um scales made from the preparation method of embodiment 8.
Specific implementation mode
The present invention is further illustrated With reference to embodiment, wherein attached drawing only for illustration,
What is indicated is only schematic diagram rather than pictorial diagram, should not be understood as the limitation to this patent；Reality in order to better illustrate the present invention
Example is applied, the certain components of attached drawing have omission, zoom in or out, and do not represent the size of actual product；To those skilled in the art
For, the omitting of some known structures and their instructions in the attached drawings are understandable.
Embodiment 1
It uses etamon chloride and the purity of a concentration of 0.4mol/L to prepare electrolyte solution for 95% absolute alcohol, prepares
Porous tantalum piece preparation facilities as shown in Figure 1, the device include adjustable DC power supply, the electrolysis for holding electrolyte solution
Slot is fixed on as cathode electrode in electrolytic cell using tantalum piece as anode electrode, stainless steel plate, and anode electrode and cathode electrode are logical
It crosses metal intermediate plate to fix with electrolytic cell, wherein anode electrode and cathode electrode are that one end is immersed into electrolyte solution, separately
Expose electrolyte solution liquid level for being connected with the positive and negative anodes of adjustable DC power supply in one end.Adjust the interpolar of tantalum piece and stainless steel plate
Spacing is 1cm, and electrolyte solution is added in electrolytic cell, and electrolyte solution liquid level is maintained at the 2/3 of electrolysis groove height（This
Sample facilitates ensuring that the amount of electrolyte solution is neither too much or too little）.
Tantalum piece needs to carry out ultrasonic cleaning, drying for standby after cleaning before being fixed in electrolytic cell.
Stainless steel plate needs to carry out polishing and ultrasonic cleaning before being fixed in electrolytic cell, to remove surface film oxide
Layer.
The cleaning solution of tantalum piece and stainless steel plate uses acetone or absolute alcohol.
Anode electrode and cathode electrode are connected with the anode and cathode of DC power supply respectively, open DC power supply switch,
The voltage of DC power supply is set as 10V（Electric current is 1A）, start electrolytic etching and prepare porous tantalum piece, electrolytic etching process continues
120s obtains the porous tantalum piece of different pore size size and distribution of pores.
The porous tantalum piece for preparing gained is cleaned using acetone or absolute alcohol under the conditions of ultrasonic oscillation, it is this
Ultrasonic oscillation cleaning process can carry out repeatedly, being conducive to intrapore corrosion product being thoroughly discharged, metallographic being used after having cleaned
The pattern of micro- sem observation porous tantalum piece, Fig. 3 show the present embodiment prepare gained porous tantalum piece scale be 200um conditions
Under surface topography.
Embodiment 2
Vibration of ultrasonic wave device is introduced in the preparation method of the present embodiment, vibration of ultrasonic wave device makes tantalum piece for containing electrolytic cell
Electrolytic etching process carried out under ultrasound-enhanced effect, be discharged and promote fresh from tantalum piece convenient for accelerating electrolytic etching product
The supplement of electrolyte solution.
The present embodiment is to carry out the electrolytic etching process of embodiment 1 stage by stage, specifically, first according to the preparation of embodiment 1
Method makes tantalum piece corrode 60s, is then shut off DC power supply, DC power supply is opened again after electrolytic cell is placed in vibration of ultrasonic wave device
Switch, makes tantalum piece electrolytic etching 60s under ultrasound-enhanced effect.
Ultrasonic power 400W, frequency 40000HZ.
After the completion of entire electrolytic etching process, porous tantalum piece need to equally be cleaned in the way of embodiment 1, Fig. 4 shows
Go out the present embodiment and prepares surface topography of the porous tantalum piece of gained under the conditions of scale is 200um.
Embodiment 3
The present embodiment is a difference in that ultrasonic procedure parameter is different from embodiment 2：Ultrasonic power is 350W, and frequency is
35000HZ。
Embodiment 4
The present embodiment and the difference of embodiment 1 are as follows：Use etamon chloride and the purity of a concentration of 0.05mol/L for
99.7% absolute alcohol prepares electrolyte solution.
The interpolar spacing of tantalum piece and stainless steel plate is 1cm.
The voltage of DC power supply is set as 40V.
The electrolytic etching time is 20s.
Embodiment 5
The present embodiment and the difference of embodiment 1 are as follows：Use etamon chloride and the purity of a concentration of 0.1mol/L for 99.7%
Absolute alcohol prepare electrolyte solution.
The interpolar spacing of tantalum piece and stainless steel plate is 5cm, and the voltage of DC power supply is set as 20V, and the electrolytic etching time is
10min, Fig. 5 are that the present embodiment prepares surface topography of the porous tantalum piece of gained under the conditions of scale is 40um.
Embodiment 6
The difference of the present embodiment and embodiment 5 be 20min the electrolytic etching times, Fig. 6 is that the present embodiment prepares the porous of gained
Surface topography of tantalum piece under the conditions of scale is 40um.
Embodiment 7
The difference of the present embodiment and embodiment 5 be 30min the electrolytic etching times, Fig. 7 is that the present embodiment prepares the porous of gained
Surface topography of tantalum piece under the conditions of scale is 40um.
Embodiment 8
The present embodiment is that the electrolytic etching time is different, and has carried out repeatedly continuous corruption for same tantalum piece from the difference of embodiment 1
Erosion, respectively 20s, 30s, 40s, 50s, 60s, 70s, Fig. 8 show the porous tantalum piece under these electrolytic etchings time in scale
For the surface topography under the conditions of 40um, as can be seen from Figure 8, with the extension of electrolytic etching time, tantalum piece surface corrosion constantly adds
Play, the surface topography when etching time reaches 60s are even more some holes occur, hole showed increased when arriving 70s.
In addition, the present invention is directed to carries out material phase analysis using the porous tantalum that the electrolyte solution of various concentration is prepared,
Obtained material phase analysis figure as shown in Fig. 2, as seen from the figure, either using 0.05mol/L or 0.1mol/L or
Under electrolyte solution etching condition prepared by the etamon chloride of 0.4mol/L concentration, the diffraction maximum of porous tantalum piece is all very bright
Aobvious, consistent with the diffraction of metal tantalum, this has been absolutely proved, and the porous tantalum ingredient prepared by the preparation method of the present invention is single, purity
Higher, there is no generate indissoluble object to be deposited on porous tantalum on piece during electrolytic etching.
The preparation method of the present invention is easy to operate, of low cost, sample（Tantalum piece and stainless steel plate）It is convenient for disassembly and assembly flexible, it is right
Sample is harmless, and obtained porous tantalum piece large specific surface area, porosity is high, suits large area to popularize.
Obviously, above-described embodiment is only intended to clearly illustrate technical scheme of the present invention example, and is not
Restriction to embodiments of the present invention.For those of ordinary skill in the art, on the basis of the above description also
It can make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all
All any modification, equivalent and improvement made by within the spirit and principles in the present invention etc. should be included in right of the present invention and want
Within the protection domain asked.
Claims (10)
1. a kind of preparation method of porous tantalum piece, which is characterized in that by the way of electrolytic etching, with absolute alcohol and tetraethyl
Ammonium chloride is configured to electrolyte solution；Using tantalum piece as anode electrode, stainless steel plate as cathode electrode, anode electrode and the moon
Pole electrode be placed in electrolytic cell and fix interpolar away from；Electrolyte solution is added in electrolytic cell, by anode electrode, cathode electricity
Pole is respectively connected to the positive and negative anodes of DC power supply, starts electrolytic etching and prepares porous tantalum piece.
2. the preparation method of porous tantalum piece according to claim 1, which is characterized in that tetraethyl chlorination in electrolyte solution
A concentration of 0.05~0.4mol/L of ammonium.
3. the preparation method of porous tantalum piece according to claim 2, which is characterized in that tetraethyl chlorination in electrolyte solution
Ammonium concentration is 0.05~0.1mol/L.
4. the preparation method of porous tantalum piece according to claim 1, which is characterized in that interpolar is away from for 1~5cm.
5. the preparation method of porous tantalum piece according to claim 1, which is characterized in that the voltage that electrolytic etching uses is 10
~40V；Or the electric current that electrolytic etching uses is 1~4A.
6. the preparation method of porous tantalum piece according to claim 1, which is characterized in that the electrolytic etching time be 20s~
30min。
7. the preparation method of porous tantalum piece according to claim 1, which is characterized in that tantalum piece and/or stainless steel plate are solid
Determine to need to carry out ultrasonic cleaning before into electrolytic cell.
8. the preparation method of porous tantalum piece according to claim 7, which is characterized in that stainless steel plate is clear in progress ultrasonic wave
Polishing removal surface oxidation film is needed before washing.
9. the preparation method of porous tantalum piece according to claim 1, which is characterized in that electrolytic cell is positioned over ultrasonic wave shake
Ultrasound is carried out in dynamic device；Preferably, electrolytic etching process carries out under ultrasound-enhanced effect, 350~450W of ultrasonic power, frequency
For 35000~45000HZ.
10. the preparation method of porous tantalum piece according to claim 9, which is characterized in that ultrasonic power 400W, frequency are
40000HZ。
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| CN201810354215.1A CN108456917A (en) | 2018-04-19 | 2018-04-19 | A kind of preparation method of porous tantalum piece |
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| CN201810354215.1A CN108456917A (en) | 2018-04-19 | 2018-04-19 | A kind of preparation method of porous tantalum piece |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440179A (en) * | 2019-01-04 | 2019-03-08 | 中南大学 | A kind of metal tantalum matrix of roughing in surface and preparation method thereof |
| CN111185600A (en) * | 2020-02-25 | 2020-05-22 | 大连理工大学 | Preparation method of fine metal mesh structure |
| CN113077987A (en) * | 2020-01-03 | 2021-07-06 | 深圳先进电子材料国际创新研究院 | Chip tantalum electrolytic capacitor and preparation method thereof |
| CN113445117A (en) * | 2021-06-29 | 2021-09-28 | 中国地质大学（武汉） | Electrolytic method and device for removing metallic cobalt in polycrystalline diamond compact |
| CN116288636A (en) * | 2023-02-06 | 2023-06-23 | 安徽格兰科新材料技术有限公司 | High-pressure-resistant ordered porous tantalum foil and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109440179A (en) * | 2019-01-04 | 2019-03-08 | 中南大学 | A kind of metal tantalum matrix of roughing in surface and preparation method thereof |
| CN113077987A (en) * | 2020-01-03 | 2021-07-06 | 深圳先进电子材料国际创新研究院 | Chip tantalum electrolytic capacitor and preparation method thereof |
| CN113077987B (en) * | 2020-01-03 | 2022-07-22 | 深圳先进电子材料国际创新研究院 | Chip tantalum electrolytic capacitor and preparation method thereof |
| CN111185600A (en) * | 2020-02-25 | 2020-05-22 | 大连理工大学 | Preparation method of fine metal mesh structure |
| CN113445117A (en) * | 2021-06-29 | 2021-09-28 | 中国地质大学（武汉） | Electrolytic method and device for removing metallic cobalt in polycrystalline diamond compact |
| CN116288636A (en) * | 2023-02-06 | 2023-06-23 | 安徽格兰科新材料技术有限公司 | High-pressure-resistant ordered porous tantalum foil and preparation method and application thereof |
| CN116288636B (en) * | 2023-02-06 | 2024-05-03 | 安徽格兰科新材料技术有限公司 | High-pressure-resistant ordered porous tantalum foil and preparation method and application thereof |
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Application publication date: 20180828 |