CN108039497A - One kind has the preparation method of the tungsten coating of high { 110 } crystal face share - Google Patents
One kind has the preparation method of the tungsten coating of high { 110 } crystal face share Download PDFInfo
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- CN108039497A CN108039497A CN201711379423.9A CN201711379423A CN108039497A CN 108039497 A CN108039497 A CN 108039497A CN 201711379423 A CN201711379423 A CN 201711379423A CN 108039497 A CN108039497 A CN 108039497A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The present invention proposes a kind of preparation method with high { 110 } crystal face share chemical vapor deposition tungsten coating.Using tungsten { 110 } crystal face with it<100>The characteristics of preferred orientation is in 45 °, processed on Copper substrate raised in 45 ° of zigzag with original surface, after aumospheric pressure cvd, outer surface is polished according to intended size, { 110 } crystal face of abundant exposed tungsten, and then improve the crystal face share on tungsten surface { 110 }.This technique can effectively improve { 110 } crystal face share of tungsten coating to more than 33%, and the stabilization of crystal face share can be kept in hot environment.
Description
Technical field
The present invention relates to a kind of preparation method of the tungsten coating with high { 110 } crystal face share, belong to thermion type fuel
Battery technology field, can particularly instruct the raising of thermion type operation of fuel cells efficiency, the height { 110 } crystal face part
Volume refers to that tungsten coating surface { 110 } crystal face share is more than 33%.
Background technology
Thermion type fuel cell is presently the most successful high-power space nuclear power form, its critical piece for heat from
Sub- energy converter, the electronic work function of converter emission pole material will directly affect its output voltage, carrying load ability and heat
Photoelectric transformation efficiency.Although the electronic work function of tungsten is higher, the work function of different crystal faces still has different, and { 110 } of tungsten are brilliant
Face has highest electronic work function, and secondly, { 111 } crystal face is minimum for { 112 } and { 100 } crystal face.
The electronic work function of 1 tungsten difference crystal face of table
The output voltage of thermionic energy converters can be represented with following formula：
Wherein, VoutFor output voltage, V；Be respectively emitter and absorb pole electronic work function,
eV；eVdFor energy loss of the electronics in electrode space plasma；VωFor emitter, receiving pole with line resistance it
Between voltage drop.As it can be seen that the tungsten with higher { 110 } crystal face share can be improved into Thermionic energy as emitter coating material
The output voltage of converter, and then improve the carrying load ability and conversion efficiency of thermoelectric of thermion type fuel cell.
The method of { 110 } the crystal face share for the raising thermionic energy converters tungsten emitter being currently known, which mainly has, to be passed through
Etching process tungsten monocrystalline is so as to exposure { 110 } crystal face, the molybdenum single crystal matrix deposition of utilization { 110 } orientation<110>Tungsten preferentially,
Its preferred orientation is changed into doping during deposits tungsten<110>Direction.Wherein tungsten monocrystalline etching method can prepare { 110 } crystal face part
Volume reaches 60% tungsten monocrystalline, but etches rear surface out-of-flatness, during hot operation surface tungsten atom volatilization seriously cause { 110 } crystalline substance
Face share declines to a great extent, and single-crystal tungsten manufacture cost and its molybdenum single crystal matrix cost used are very high.Utilize<110>The molybdenum of orientation
Single crystal substrate deposits<110>Tungsten preferentially can prepare the tungsten that { 110 } crystal face share reaches 60%~80%, but this method applies
Layer thickness is maximum to be no more than 60 μm, it is difficult to meets the needs of practical application, molybdenum single crystal matrix cost used is higher.This is very big
Limit the raising of emitter conversion efficiency of thermoelectric and the application of thermion type fuel cell.
The content of the invention
The purpose of the invention is to propose a kind of preparation with high { 110 } crystal face share chemical vapor deposition tungsten coating
Method, particularly a kind of method of { 110 } the crystal face share that can improve chemical vapor deposition tungsten coating simple and stable.The present invention
Method using tungsten { 110 } crystal face with it<100>The characteristics of preferred orientation is in 45 °, processes on Copper substrate and is in original surface
45 ° of zigzag is raised, after aumospheric pressure cvd, polishes outer surface according to intended size, { 110 } of abundant exposed tungsten are brilliant
Face, to achieve the purpose that to improve tungsten surface { 110 } crystal face share.This technique can effectively improve { 110 } crystal face part of tungsten coating
Volume, and the stabilization of crystal face share can be kept in hot environment.
The purpose of the present invention is what is be achieved through the following technical solutions.
There is one kind of the present invention the step of preparation method of the tungsten coating of high { 110 } crystal face share, this method to include：
(1) Copper substrate is processed；
Processing Copper substrate method be：Process several continuous grooves on Copper substrate surface, the cross section of groove for etc.
Waist is trapezoidal or isosceles triangle；The trapezoidal waist and the surface of Copper substrate are in two waists and copper of 45 ° or described of triangle
The surface of matrix is in 45 °；
(2) the Copper substrate surface deposits tungsten with several grooves obtained in step (1), obtains tungsten coating；
(3) tungsten coating obtained to step (2) is processed, and obtains the tungsten coating with high { 110 } crystal face share.
In the step (1), the groove processed is cleaned, when cleaning uses deionized water and/or anhydrous second
Alcohol is cleaned.
In the step (1), the shape of the Copper substrate is tabular or cylindric.
In the step (1), the bottom side length of triangle of the trapezoidal upper bottom width no more than 500 μm or described is not
More than 500 μm.
It is described it is trapezoidal be isosceles trapezoid, upper bottom width is 466 μm, and lower bottom width is 166 μm, 150 μm high.
The triangle is isosceles triangle, and a length of 466 μm of base is 233 μm high.
In the step (2), using the method for chemical vapor deposition during deposits tungsten, H is used2Reduce WF6Method.
Carried out during deposits tungsten in normal pressure cold wall chemical vapor deposition room.
The thickness of tungsten coating is：The distance at the trapezoidal upper bottom of the surface distance of tungsten coating is not less than 250 μm；Either tungsten applies
The distance at the bottom of the surface distance triangle of layer is not less than 250 μm.
In the step (3), the tungsten coating of deposition is cut and polished by the way of grinding and Electrolyzed Processing.
Beneficial effect
(1) present invention includes three processing of copper matrix, the deposition of tungsten coating and processing key steps, has cost
It is low, deposition is fast, purity is high, { 110 } crystal face share is obviously improved, high-temperature stable, it is simple and practicable the advantages that；
(2) chemical vapor deposition tungsten coating is organized as in the present invention<100>Column crystal preferentially, theoretical calculation (Fig. 3)
Show { 110 } crystal face in column crystal<100>Share can reach 48% on section 45 ° axial；EBSD test results (Fig. 4) are aobvious
Show { 110 } crystal face in column crystal<100>Share can reach 41.5% on section 45 ° axial, close with the calculated results,
Therefore matrix is processed the zigzag protrusion that same original surface is in 45 ° can greatly improve the share of { 110 } crystal face.
(3) matrix in the present invention and coating according to Fig. 1, Fig. 2 requirement processing can farthest (about 80%) it is sudden and violent
Dew with<100>Axial is in 45 ° of crystal face.{ 110 } crystal face share of chemical vapor deposition tungsten is brought up to more than 33% by 0%；
(4) with etching process single-crystal tungsten exposure { 110 } crystal face method compared with, the present invention in tungsten coating by grinding,
Electrolyzed Processing rear surface is smooth, and in hot operation, surface tungsten atom is not volatile, and crystal face share can keep stablizing simultaneously
And cost is relatively low.With utilization<110>The monocrystalline Mo substrate deposition of orientation<110>Preferentially the method for tungsten is compared, and tungsten applies in the present invention
Layer deposition velocity is fast, thickness is adjustable, cost is relatively low.The present invention is with cost is low, deposition is fast, purity is high, { 110 } crystal face share carries
High obvious, high-temperature stable, it is simple and practicable the advantages that.
(5) method for obtaining tungsten by aumospheric pressure cvd on Copper substrate being used in the present invention has cost
Relatively low, the advantages that sedimentation rate is fast, product purity is high.However, the tungsten prepared under these conditions is height<100>Select
Excellent, its surface { 100 } crystal face share is high, and { 110 } crystal face share is very low.Changed so as to significantly reduce material as energy
The effect that device emitter uses.Therefore, the key that prepared by material is how to ensure that this method cost is low, deposition is fast, purity
Surface { 110 } crystal face share is improved while high advantage as far as possible.To solve the problems, such as that surface { 110 } crystal face share improves, this
Invention utilizes { 110 } crystal face same<100>The characteristics of being in preferentially 45 °, employ and a kind of matrix surface is processed into special pattern
The method deposited again, exposure simultaneously improve the share of surface { 110 } crystal face.
Brief description of the drawings
Fig. 1 is the first machining sketch chart；
Fig. 2 is second of machining sketch chart；
Fig. 3 is calculated<100>The share of { 110 } crystal face on 45 ° of directions of crystal orientation, its value are 48%；
Fig. 4 is what EBSD was measured<100>The share of { 110 } crystal face on 45 ° of directions of crystal orientation, its value are 41.5%；
Embodiment
One kind has the preparation method of the tungsten coating of high { 110 } crystal face share, comprises the following steps：
(1) processing of Copper substrate：It can make tungsten coating by being processed for the tabular of deposition or columned Copper substrate
Surface, which is tried one's best, exposes the given shape of { 110 } crystal face, and with deionized water and washes of absolute alcohol, it is spare；Described is specific
Shape refers to that several are continuous trapezoidal in Copper substrate skin cut, and trapezoidal is isosceles trapezoid, and upper bottom width is 466 μm, lower bottom width
It is 150 μm high for 166 μm；
The given shape can also be that triangle is isosceles in several continuous triangles of Copper substrate skin cut
Triangle, a length of 466 μm of base are 233 μm high；
(2) chemical vapor deposition of tungsten coating：In normal pressure cold wall chemical vapor deposition room, H is used2Reduce WF6Method is in step
Suddenly the given shape surface deposition tungsten coating for the Copper substrate that (1) obtains；The thickness of tungsten coating is：The surface distance of tungsten coating is trapezoidal
Upper bottom distance be not less than 250 μm；Either the distance at the bottom of the surface distance triangle of tungsten coating is not less than 250 μm；
(3) processing of coating：The tungsten coating surface of deposition in step (2) is cut successively, is polished, obtains that there is height
{ 110 } tungsten coating of crystal face share, according to the thickness for being actually needed the tungsten coating determined.
When being cut, being polished in the step (3) by the way of grinding and Electrolyzed Processing.
The present invention uses H2Reduce WF6It is prepared by method<100>The tungsten coating of preferred orientation, by processing base according to certain method
Body and coating achieve the purpose that to improve surface { 110 } crystal face share.
With reference to specific embodiment, the present invention is described in detail.Following embodiments will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, present inventive concept is not being departed from --- matrix surface is processed into special pattern to improve { 110 } share premise
Under, some deformations and change (including changing shape, angle, size and processing method etc.) can also be made, these are belonged to
Protection scope of the present invention.
Embodiment 1
(1) processing of Copper substrate：By size after outer circle finish turning(outside diameter × height × thickness)
Tool sharpening of the hollow copper matrix blank by numerically-controlled precise grinding machine or respective shapes go out same former table as shown in Fig. 1
Face is trapezoidal in 45 °, it is preferable that sawtooth spacing is 466 μm, and sawtooth highly is 150 μm.And with deionized water and alcohol washes,
It is spare.
(2) chemical vapor deposition of tungsten coating：In the vertical cold wall chemical vapor deposition room of normal pressure, H is used2Reduce WF6
Method is deposited.Preferably, depositing temperature is 550 DEG C, and deposit thickness is 250 μm (from trapezoidal upper bottom).
(3) processing of coating：The ready tungsten coating with matrix in step (2) is used into precision grinder grinding or electricity
Solution lathe Electrolyzed Processing removes surface and polishes smooth bright and clean.Preferably, the thickness for removing material should be 200 μm.So it there are about
80% surface is all same<100>Preferred orientation is in 45 °, wherein the crystal face for having 41. 5%~48% again is { 110 } crystal face, therefore can
{ 110 } the crystal face share on tungsten surface is brought up to more than 33% by 0%.
Implementation result：By the processing of the above method, { 110 } the crystal face share on chemical vapor deposition tungsten surface is brought up to
33.2%~37%；Tungsten coating is smooth by grinding, Electrolyzed Processing rear surface, and in hot operation, surface tungsten atom is not easy
Volatilization, crystal face share can keep stable；Present invention employs on common copper matrix use to working equipment requirement compared with
The method that low aumospheric pressure cvd prepares tungsten coating, therefore cost is relatively low.
As shown in figure 3, the high preferred orientation of 45 ° of { 100 } crystal face angle is calculated, the ratio of { 110 } crystal face is
48%.As shown in figure 4, carrying out EBSD analyses in 45 ° of section to tungsten coating { 100 } crystal face, the ratio for obtaining { 110 } crystal face is
41.5%.
Embodiment 2
For the implementation of the present embodiment with embodiment 1, difference is depositing base shape.By size after outer circle finish turningCutter of the hollow copper matrix blank of (outside diameter × height × thickness) Jing Guo number respective shapes adds
Work goes out the triangle that same original surface as shown in Figure 2 is in 45 °, it is preferable that sawtooth spacing is 466 μm, and sawtooth is highly 233 μm.
Subsequent step is the same as example 1.
Implementation result：With example 1.
In conclusion the method for the present invention improves the crystal face share on tungsten surface { 110 }.Using tungsten { 110 } crystal face with it<
100>The characteristics of preferred orientation is in 45 °, processes with original surface on Copper substrate in 45 ° of zigzag protrusion, normal pressure chemical gas
After mutually depositing, outer surface, { 110 } crystal face of abundant exposed tungsten are polished according to intended size.This technique can effectively improve tungsten painting
{ 110 } crystal face share of layer, and the stabilization of crystal face share can be kept in hot environment.
Claims (10)
1. one kind has the preparation method of the tungsten coating of high { 110 } crystal face share, it is characterised in that the step of this method includes：
(1) Copper substrate is processed；
Processing Copper substrate method be：Process several continuous grooves on Copper substrate surface, the cross section of groove to be trapezoidal or
Triangle；The trapezoidal waist and the surface of Copper substrate are in 45 ° or described of hypotenuse and the surface of Copper substrate
45°；
(2) the Copper substrate surface deposits tungsten with several grooves obtained in step (1), obtains tungsten coating；
(3) tungsten coating obtained to step (2) is processed, and obtains the tungsten coating with high { 110 } crystal face share.
2. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 1, its feature exist
In：In the step (1), the groove processed is cleaned, is carried out using deionized water and/or absolute ethyl alcohol during cleaning
Cleaning.
3. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 1, its feature exist
In：In the step (1), the shape of the Copper substrate is tabular or cylindric.
4. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 1, its feature exist
In：In the step (1), the bottom side length of triangle of the trapezoidal upper bottom width no more than 500 μm or described is not more than
500μm。
5. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 4, its feature exist
In：It is described it is trapezoidal be isosceles trapezoid, upper bottom width is 466 μm, and lower bottom width is 166 μm, 150 μm high.
6. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 4, its feature exist
In：The triangle is isosceles triangle, and a length of 466 μm of base is 233 μm high.
7. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 1, its feature exist
In：In the step (2), using the method for chemical vapor deposition during deposits tungsten, H is used2Reduce WF6Method.
8. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 7, its feature exist
In：Carried out during deposits tungsten in normal pressure cold wall chemical vapor deposition room.
9. one kind according to claim 1,7 or 8 has the preparation method of the tungsten coating of high { 110 } crystal face share, it is special
Sign is：The thickness of tungsten coating is：The distance at the trapezoidal upper bottom of the surface distance of tungsten coating is not less than 250 μm；Either tungsten applies
The distance at the bottom of the surface distance triangle of layer is not less than 250 μm.
10. a kind of preparation method of tungsten coating with high { 110 } crystal face share according to claim 1, its feature exist
In：In the step (3), the tungsten coating of deposition is cut and polished by the way of grinding and Electrolyzed Processing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114481101A (en) * | 2021-12-15 | 2022-05-13 | 中南大学 | Metal material obtained by method for regulating crystal face orientation of metal coating and application |
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2017
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| EP1055746A1 (en) * | 1999-05-24 | 2000-11-29 | Lucent Technologies Inc. | Method of chemical vapor depositing tungsten films |
| CN104025225A (en) * | 2011-11-03 | 2014-09-03 | 英特尔公司 | Energy Storage Structure, Method Of Manufacturing A Support Structure For Same, And Microelectronic Assembly And System Containing Same |
| CN103484830A (en) * | 2012-06-12 | 2014-01-01 | 核工业西南物理研究院 | Preparation method of thick tungsten coating material and tungsten coating material |
| CN105842038A (en) * | 2016-03-21 | 2016-08-10 | 北京理工大学 | Tungsten single crystal coating layer {110} crystal plane recognition and surface portion statistical method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114481101A (en) * | 2021-12-15 | 2022-05-13 | 中南大学 | Metal material obtained by method for regulating crystal face orientation of metal coating and application |
| CN114481101B (en) * | 2021-12-15 | 2023-09-29 | 中南大学 | Metal material obtained by method for regulating and controlling crystal face orientation of metal coating and application |
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