CN102051634A - Titanium electrode material with porous titanium as substrate and preparation method of titanium electrode material - Google Patents
Titanium electrode material with porous titanium as substrate and preparation method of titanium electrode material Download PDFInfo
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Abstract
The invention discloses a titanium electrode material with porous titanium as a substrate, comprising a titanium substrate and a metal oxide coating on the surface of the titanium substrate, wherein the titanium substrate is a plate-like, tubular, strap-shaped or clubbed porous titanium substrate with porosity of 20%-50%; and the metal oxide coating is of a nano structure. The preparation method of the titanium electrode material comprises the following steps: 1, preparing the porous titanium substrate by vacuum-sintering and pretreating the surface of the porous titanium substrate; 2, preparing metal oxide coating masking liquid; 3, brushing the masking liquid on the porous titanium substrate, drying, and then carrying out thermal decomposition; and 4, repeating the step 3 until the required coating thickness is reached, and then carrying out thermal treatment to obtain the titanium electrode material with the porous titanium as the substrate. In the invention, the metal oxide coating with the nano structure is coated on the surface of the titanium electrode material. The titanium electrode material prepared by the preparation method has the advantages of excellent catalytic activity, good mass transfer effect and long service life.
Description
Technical field
The invention belongs to the electrode materials technical field, being specifically related to a kind of is the titanium electrode material and preparation method thereof of matrix with the POROUS TITANIUM.
Background technology
The titanium anode is with the goods of metal oxide containing precious metals for its reactive material, be widely used in chlorine industry, electroplating industry, oxymuriate industry, clorox production, the cathodic protection, begun in recent years to be applied to water electrolysis, sewage disposal and organism synthetic with field such as electrolysis.It is the core of electrochemical apparatus, play a part electric energy and be converted into chemical energy, so the quality of electrode is directly connected to the efficient of electrochemical apparatus.Good titanium anode must have high reactivity, high life and highly selective.
The titanium anode has had certain progress for electrocatalytic reaction and Study on Stability thereof between four more than ten years in the past, and the methods such as optimized coatings component, change preparation technology of coating and increase middle layer that at present research of titanium anodic mainly concentrated on improve anode performance.Want to obtain high performance electrode materials in electrochemical field, only depending on the raising coating performance is to be difficult to realize, must counter electrode matrix self structure improve.Counter electrode material, electrochemical activity mainly depend on active centre quantity and distribution thereof.The active centre of high dispersive not only has the effect that electrode activity is improved, and makes that the distribution of current of being on active service is even, and current density descends, and improves solidity to corrosion.
POROUS TITANIUM is a kind of novel product of titanium metal, has advantages such as good electrical conductivity, erosion resistance, superior biocompatibility and higher porosity, has been subjected to extensive studies and application.The powder metallurgy POROUS TITANIUM is to be raw material obtains honeycomb structure behind moulding, sintering POROUS TITANIUM with the metal-powder.POROUS TITANIUM as the electrode materials matrix has greater porosity, helps electrolytical transmission and circulation, improves the electrode catalyst speed of response; POROUS TITANIUM has flourishing specific surface area simultaneously, the dispersion that helps activated coating is with even, can obtain the activated coating of nanostructure, increased the active points quantity of electrocatalytic reaction, make that the distribution of current of being on active service is even, reduce the current density of electrode, improved the solidity to corrosion of electrode, prolonged the work-ing life of electrode.Therefore, the present invention is matrix with the POROUS TITANIUM, and surface-coated has the activated coating of nanostructure, can obtain the high-performance metal oxide coating titanium anode of catalytic activity height, long service life.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned the deficiencies in the prior art, and it is matrix that a kind of porosity height, POROUS TITANIUM that specific surface area is big are provided, and has excellent catalytic activity, good mass transfer effect and the titanium electrode material in long work-ing life.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of is the titanium electrode material of matrix with the POROUS TITANIUM, comprise the coating of metal oxides that titanium matrix and titanium matrix surface apply, it is characterized in that, described titanium matrix is that porosity is 20%～50% tabular, tubulose, band shape or bar-shaped POROUS TITANIUM matrix, and described coating of metal oxides has nanostructure.
Above-mentioned is the titanium electrode material of matrix with the POROUS TITANIUM, and described coating of metal oxides is the nanofeature pattern of nanocrystal or nano wire, and is evenly dispersed in POROUS TITANIUM outer surface of matrix and internal surface.
Above-mentioned is the titanium electrode material of matrix with the POROUS TITANIUM, and described coating of metal oxides is precious metal oxide coating or non-noble metal oxide coating.
Above-mentioned is the titanium electrode material of matrix with the POROUS TITANIUM, and described precious metal oxide coating is the binary mixed metal oxide coating that iridium and tantalum are formed, and described non-noble metal oxide coating is the binary mixed metal oxide coating that tin and antimony are formed.
The present invention also provide a kind of simple for process be the method for the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that this method may further comprise the steps:
(1) vacuum sintering prepares POROUS TITANIUM, and POROUS TITANIUM is carried out surface preparation, removes the oxide film on degreasing and surface, forms the fresh titanium matrix of pitted skin;
(2) by the formulated coating of metal oxides masking liquid of common titanium anode masking liquid, described coating of metal oxides masking liquid is precious metal oxide coating masking liquid or non-noble metal oxide coating masking liquid;
(3) coating of metal oxides masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 450 ℃～550 ℃ thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and will brush titanium matrix behind the coating of metal oxides masking liquid then and in temperature be thermal treatment 0.5h～1h under 450 ℃～550 ℃ the condition, the titanium electrode material that formation has the nanostructured metal oxides coating.
The method of surface preparation is an etching method described in the above-mentioned steps (1).
That above-mentioned is the preparation method of the titanium electrode material of matrix with the POROUS TITANIUM, and the etching solution in the described etching method is that mass concentration is not more than 10% oxalic acid, and etching time is not more than 1h.
Described in the above-mentioned steps (2) in the precious metal oxide coating masking liquid mass ratio of iridium, tantalum and organic solvent be 1: 0.67: 10～50, the mass ratio of tin, antimony and organic solvent is 1: 0.3: 10～50 in the described non-noble metal oxide coating masking liquid.
That above-mentioned is the preparation method of the titanium electrode material of matrix with the POROUS TITANIUM, and described organic solvent is propyl carbinol, Virahol or ethanol.
The present invention compared with prior art has the following advantages: the present invention is a matrix with porosity height, powder metallurgy POROUS TITANIUM that specific surface area is big, adopt simple technology, apply coating of metal oxides with nanostructure at the POROUS TITANIUM matrix surface, this oxide coating not only is evenly dispersed in the POROUS TITANIUM outer surface of matrix, also comprises POROUS TITANIUM matrix hole internal surface.The titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the coating of metal oxides shape appearance figure of the titanium electrode material of the embodiment of the invention 1 preparation.
Fig. 2 is the coating of metal oxides shape appearance figure of the titanium electrode material of the embodiment of the invention 7 preparations.
Embodiment
Embodiment 1
(1) to prepare porosity be 50% POROUS TITANIUM PLATE in vacuum sintering, adopt etching method that POROUS TITANIUM PLATE is carried out surface preparation, remove the oxide film on degreasing and surface, residual dirt settling in the POROUS TITANIUM matrix hole is fully removed in ultrasonic cleaning, forms the fresh titanium matrix of pitted skin; Etching solution in the described etching method is the oxalic acid of mass concentration 8%, and etching time is 30min;
(2) by the formulated precious metal oxide coating masking liquid of common titanium anode masking liquid, the mass ratio of iridium, tantalum and organic solvent is 1: 0.67: 10 in the precious metal oxide coating masking liquid; Described organic solvent is a Virahol;
(3) precious metal oxide coating masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 500 ℃ of thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and the titanium matrix that will brush the coating masking liquid then is thermal treatment 1h under 500 ℃ the condition in temperature, and formation has the titanium electrode material of nano thread structure coating of metal oxides.
As shown in Figure 1, the coating of metal oxides of the titanium electrode material of present embodiment preparation has nano thread structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 2
Present embodiment is identical with embodiment 1 preparation method, and wherein difference is: described organic solvent is propyl carbinol or ethanol.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has nano thread structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 3
(1) to prepare porosity be 20% POROUS TITANIUM pipe in vacuum sintering, adopt etching method that the POROUS TITANIUM pipe is carried out surface preparation, remove the oxide film on degreasing and surface, residual dirt settling in the POROUS TITANIUM matrix hole is fully removed in ultrasonic cleaning, forms the fresh titanium matrix of pitted skin; Etching solution in the described etching method is the oxalic acid of mass concentration 3%, and etching time is 1h;
(2) by the formulated precious metal oxide coating masking liquid of common titanium anode masking liquid, the mass ratio of iridium, tantalum and organic solvent is 1: 0.67: 50 in the precious metal oxide coating masking liquid; Described organic solvent is an ethanol;
(3) precious metal oxide coating masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 550 ℃ of thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and the titanium matrix that will brush the coating masking liquid then is thermal treatment 0.8h under 550 ℃ the condition in temperature, and formation has the titanium electrode material of nano thread structure coating of metal oxides.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has nano thread structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 4
Present embodiment is identical with embodiment 3 preparation methods, and wherein difference is: described organic solvent is propyl carbinol or Virahol.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has nano thread structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 5
(1) to prepare porosity be 40% banded POROUS TITANIUM in vacuum sintering, adopt etching method that banded POROUS TITANIUM is carried out surface preparation, remove the oxide film on degreasing and surface, residual dirt settling in the POROUS TITANIUM matrix hole is fully removed in ultrasonic cleaning, forms the fresh titanium matrix of pitted skin; Etching solution in the described etching method is the oxalic acid of mass concentration 10%, and etching time is 20min;
(2) by the formulated precious metal oxide coating masking liquid of common titanium anode masking liquid, the mass ratio of iridium, tantalum and organic solvent is 1: 0.67: 30 in the precious metal oxide coating masking liquid; Described organic solvent is a propyl carbinol;
(3) precious metal oxide coating masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 550 ℃ of thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and the titanium matrix that will brush the coating masking liquid then is thermal treatment 1h under 550 ℃ the condition in temperature, and formation has the titanium electrode material of nano thread structure coating of metal oxides.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has nano thread structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 6
Present embodiment is identical with embodiment 5 preparation methods, and wherein difference is: described organic solvent is ethanol or Virahol.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has nano thread structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 7
(1) to prepare porosity be 20% POROUS TITANIUM rod in vacuum sintering, adopt etching method that the POROUS TITANIUM rod is carried out surface preparation, remove the oxide film on degreasing and surface, residual dirt settling in the POROUS TITANIUM matrix hole is fully removed in ultrasonic cleaning, forms the fresh titanium matrix of pitted skin; Etching solution in the described etching method is the oxalic acid of mass concentration 5%, and etching time is 1h;
(2) by the formulated non-noble metal oxide coating masking liquid of common titanium anode masking liquid, the mass ratio of tin, antimony and organic solvent is 1: 0.3: 10 in the non-noble metal oxide coating masking liquid; Described organic solvent is an ethanol;
(3) non-noble metal oxide coating masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 500 ℃ of thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and the titanium matrix that will brush the coating masking liquid then is thermal treatment 1h under 500 ℃ the condition in temperature, and formation has the titanium electrode material of nanocrystal structural metal oxide coating.
As shown in Figure 2, the coating of metal oxides of the titanium electrode material of present embodiment preparation has the nanocrystal structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 8
Present embodiment is identical with embodiment 7 preparation methods, and wherein difference is: described organic solvent is propyl carbinol or Virahol.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has the nanocrystal structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 9
(1) to prepare porosity be 50% POROUS TITANIUM pipe in vacuum sintering, adopts etching method that POROUS TITANIUM is carried out surface preparation, removes the oxide film on degreasing and surface, and residual dirt settling in the POROUS TITANIUM matrix hole is fully removed in ultrasonic cleaning, forms the fresh titanium matrix of pitted skin; Etching solution in the described etching method is the oxalic acid of mass concentration 8%, and etching time is 1h;
(2) by the formulated non-noble metal oxide coating masking liquid of common titanium anode masking liquid, the mass ratio of tin, antimony and organic solvent is 1: 0.3: 30 in the non-noble metal oxide coating masking liquid; Described organic solvent is a propyl carbinol;
(3) non-noble metal oxide coating masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 450 ℃ of thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and the titanium matrix that will brush the coating masking liquid then is thermal treatment 1h under 450 ℃ the condition in temperature, and formation has the titanium electrode material of nanocrystal structural metal oxide coating.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has the nanocrystal structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 10
Present embodiment is identical with embodiment 9 preparation methods, and wherein difference is: described organic solvent is ethanol or Virahol.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has the nanocrystal structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 11
(1) to prepare porosity be 30% POROUS TITANIUM PLATE in vacuum sintering, adopt etching method that POROUS TITANIUM PLATE is carried out surface preparation, remove the oxide film on degreasing and surface, residual dirt settling in the POROUS TITANIUM matrix hole is fully removed in ultrasonic cleaning, forms the fresh titanium matrix of pitted skin; Etching solution in the described etching method is the oxalic acid of mass concentration 5%, and etching time is 50min;
(2) by the formulated non-noble metal oxide coating masking liquid of common titanium anode masking liquid, the mass ratio of tin, antimony and organic solvent is 1: 0.3: 50 in the non-noble metal oxide coating masking liquid; Described organic solvent is a Virahol;
(3) non-noble metal oxide coating masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 500 ℃ of thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and the titanium matrix that will brush the coating masking liquid then is thermal treatment 0.5h under 500 ℃ the condition in temperature, and formation has the titanium electrode material of nanocrystal structural metal oxide coating.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has the nanocrystal structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
Embodiment 12
Present embodiment is identical with embodiment 11 preparation methods, and wherein difference is: described organic solvent is propyl carbinol or ethanol.
The coating of metal oxides of the titanium electrode material of present embodiment preparation has the nanocrystal structure, this coating of metal oxides is scattered in POROUS TITANIUM outer surface of matrix and internal surface equably, the titanium electrode material of preparation has the catalytic activity of excellence, good mass transfer effect and long work-ing life, is a kind of high-performance, highly active coating titanium anode.
The above; it only is preferred embodiment of the present invention; be not that the present invention is imposed any restrictions, everyly any simple modification that above embodiment did, change and equivalence changed, all still belong in the protection domain of technical solution of the present invention according to the technology of the present invention essence.
Claims (9)
1. one kind is the titanium electrode material of matrix with the POROUS TITANIUM, comprise the coating of metal oxides that titanium matrix and titanium matrix surface apply, it is characterized in that, described titanium matrix is that porosity is 20%～50% tabular, tubulose, band shape or bar-shaped POROUS TITANIUM matrix, and described coating of metal oxides has nanostructure.
2. according to claim 1 is the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that, described coating of metal oxides is the nanofeature pattern of nanocrystal or nano wire, and is evenly dispersed in POROUS TITANIUM outer surface of matrix and internal surface.
3. according to claim 1 is the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that, described coating of metal oxides is precious metal oxide coating or non-noble metal oxide coating.
4. according to claim 3 is the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that, described precious metal oxide coating is the binary mixed metal oxide coating that iridium and tantalum are formed, and described non-noble metal oxide coating is the binary mixed metal oxide coating that tin and antimony are formed.
5. preparing as claimed in claim 1 is the method for the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that this method may further comprise the steps:
(1) vacuum sintering prepares POROUS TITANIUM, and POROUS TITANIUM is carried out surface preparation, removes the oxide film on degreasing and surface, forms the fresh titanium matrix of pitted skin;
(2) by the formulated coating of metal oxides masking liquid of common titanium anode masking liquid, described coating of metal oxides masking liquid is precious metal oxide coating masking liquid or non-noble metal oxide coating masking liquid;
(3) coating of metal oxides masking liquid described in the step (2) is brushed on the fresh titanium matrix of pitted skin described in the step (1), the oven dry back is cooled to room temperature in 450 ℃～550 ℃ thermolysis 10min;
(4) repeating step (3) is to the coat-thickness that needs, and will brush titanium matrix behind the coating of metal oxides masking liquid then and in temperature be thermal treatment 0.5h～1h under 450 ℃～550 ℃ the condition, the titanium electrode material that formation has the nanostructured metal oxides coating.
6. according to claim 5 is the preparation method of the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that, the method for surface preparation is an etching method described in the step (1).
7. according to claim 6 is the preparation method of the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that, the etching solution in the described etching method is that mass concentration is not more than 10% oxalic acid, and etching time is not more than 1h.
8. according to claim 5 is the preparation method of the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that, described in the step (2) in the precious metal oxide coating masking liquid mass ratio of iridium, tantalum and organic solvent be 1: 0.67: 10～50, the mass ratio of tin, antimony and organic solvent is 1: 0.3: 10～50 in the described non-noble metal oxide coating masking liquid.
9. according to claim 8 is the preparation method of the titanium electrode material of matrix with the POROUS TITANIUM, it is characterized in that, described organic solvent is propyl carbinol, Virahol or ethanol.
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