CN104726844B - A kind of method in the superpower light absorbs carbon nanotube coating of titanium alloy-based bottom growth - Google Patents
A kind of method in the superpower light absorbs carbon nanotube coating of titanium alloy-based bottom growth Download PDFInfo
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Abstract
A kind of method in the superpower light absorbs carbon nanotube coating of titanium alloy-based bottom growth, using growing surface micro-nanoization and increasing plating transition layer process, can cause that the firmness of growth CNT and serializing degree strengthen in metallic substrates (titanium alloy), overcome the problem of the insecure and direction of growth disorder being likely to result in metallic substrates growth CNT.The carbon nanotube coating for growing out in this way can be securely attached to titanium alloy surface, play a part of superabsorbent light radiation, suitable for various photoelectricity, optical instrumentation, uniform diffuse reflection surface etc., instrument and equipment particularly with signal detection is more powerful, such as the fixed star of spacecraft measures sensor, the mode for eliminating veiling glare pitch-dark relative to conventionally employed delustring, can significantly improve the ability for eliminating veiling glare.
Description
Technical field
The present invention relates to a kind of generation method of carbon nanotube coating, can be used for the frequency modulated light plate of titanium alloy substrate preparation, hide
The veiling glare of the optics such as light shield suppresses.
Background technology
Recent years, with the development of carbon nanotube technology, the characteristic of CNT blacker-than-black material is gradually recognized by people
Know.So-called blacker-than-black material, the absorptance for being exactly its almost full spectral coverage to light is attained by more than 99%.On a silicon substrate
The growth that having scholar carried out CNT is tested, and has delivered the paper of correlation, but for CNT in metallic substrates
On growth technique and the sessile nature of metallic substrates CNT also rarely have research.
Black light-absorbing coating technology is sprayed or grown on the metallic substrate can be applied to various occasions, such as space flight photoelectricity instrument
Area source, Homogeneouslly-radiating heat-absorbing material etc. are demarcated in the veiling glare baffle plate that disappears of device, diffusing radiation, wherein in the case of for light-absorbing coating most
Conventional is the veiling glare light shield that disappears of star sensor and camera, and this product typically can not, intensity frangible with fragility such as glass
Material not high, so existing CNT can not be used directly with the technology of growth in non metallic substrate, is needed as substrate
Study the new technology that CNT grows on the metallic substrate.And because carbon nano tube growth is generally required no less than 600 DEG C
Hot environment, accordingly, it would be desirable to study in dystectic metallic substrates such as titanium alloy grow CNT new technology.
, as light absorbing material, there are light absorbs using pitch-dark or black anodizing coating in the light shield in prior art
Than not high enough problem, thus result under the ability of the veiling glare that equally disappears, disappear veiling glare device, such as the volume weight of light shield compared with
Greatly.If the existing veiling glare black coating that disappears (pitch-dark or anodization nigrescence etc.) can be replaced using CNT, then receive with carbon
The blacker-than-black characteristic of mitron, its light absorbs can will significantly improve veiling glare inhibition considerably beyond material of the prior art.
The difficult point for growing superpower light absorbs CNT on the metallic substrate is, the directionality control that CNT grows in metallic substrates
System and adhesion-tight technique, current this process are rarely reported.
The content of the invention
Present invention solves the technical problem that being：Overcome the deficiencies in the prior art, there is provided one kind is raw in titanium alloy substrate
The method of the superpower light absorbs carbon nanotube coating of length, the carbon nanotube coating for growing out in this way can be firmly attached
In titanium alloy surface, play a part of superabsorbent light radiation, it is adaptable to various photoelectricity, optical instrumentation, uniform diffuse reflection
Surface etc., the instrument and equipment particularly with signal detection is more powerful, such as the fixed star measurement sensor of spacecraft,
The mode for eliminating veiling glare pitch-dark relative to conventionally employed delustring, can significantly improve the ability for eliminating veiling glare.
Technical solution of the invention is：A kind of side in the superpower light absorbs carbon nanotube coating of titanium alloy-based bottom growth
Method, comprises the following steps：
(1) frosting treatment is carried out to titanium alloy sample surface using polishing mode so that by the titanium alloy exemplar of polishing
Surface has cut；
(2) the titanium alloy exemplar by polishing is cleaned, removes removal organic polluter；
(3) titanium alloy exemplar is put into drying baker drying；
(4) titanium alloy exemplar is taken out from drying baker, titanium alloy exemplar is cleaned with clear water after cooling；
(5) titanium alloy exemplar is put into drying baker drying again；
(6) treatment is electrochemically reacted to titanium alloy exemplar so that the surface of titanium alloy exemplar formed it is microcosmic quarter engrave it is micro-
Nanostructured；Or on the plated surface of titanium alloy exemplar aluminium nickel double metal intermediate buffer layer；
(7) the titanium alloy exemplar that step (6) is treated is inserted in CNT reacting furnace；
(8) toward argon gas is passed through in CNT reacting furnace, while CNT reacting furnace begins heat to CNT life
Temperature needed for long；
(9) after argon gas is full of CNT reacting furnace, argon flow amount is adjusted to 1000~2000mL/min, while being passed through
The hydrogen of 300~500mL/min；
(10) after hydrogen flowing quantity is stable and full of CNT reacting furnace, according to predetermined reaction speed to CNT
Gaseous carbon source is passed through in reacting furnace or vaporific liquid carbon source is introduced；
(11) the length setting reaction time according to needed for carbon nano pipe array, after completion of the reaction, hydrogen is cut off, stops adding
Heat, and the flow of argon gas is turned down to 100mL/min~150mL/min, take out titanium alloy exemplar after being cooled to room temperature；
(12) if being that treatment is electrochemically reacted to titanium alloy exemplar in step (6), carbon nanotube coating makes
Complete；If in step (6) being aluminium nickel double metal intermediate buffer layer on the plated surface to titanium alloy exemplar, the titanium that will be obtained is closed
Golden exemplar is put into high temperature furnace, is rapidly heated to 880 DEG C~920 DEG C, continues 1 minute to 10 minutes, and then high temperature furnace cooling, takes
Go out titanium alloy exemplar, thus complete the making of carbon nanotube coating.
Use in the step (6) electrochemical reaction treatment formed engrave at microcosmic quarter the method for micro nano structure for：Using electricity
Chemical reaction handling technique is surface-treated to titanium alloy exemplar, gets rid of the part metals on surface so that the part of residual
Fine texturing structure is showed on the surface.
The method of aluminium nickel double metal intermediate buffer layer is on the plated surface of titanium alloy exemplar in the step (6)：First
In titanium alloy sample surface evaporation or the aluminium nickel double metal of 3~10nm of sputtering sedimentation thickness, the pre-heat treatment is then carried out so that double
Metal intermediate buffer layer is changed into oxide coating and metal nanoparticle double-decker, preheating temperature scope 400 DEG C~600
℃。
Present invention advantage compared with prior art is：
1. the growing surface micro-nanoization and increasing plating transition layer process for being provided using the present invention, can cause in metallic substrates
Firmness and the serializing degree enhancing of CNT are grown on (titanium alloy), overcoming can in metallic substrates growth CNT
The problem of the insecure and direction of growth disorder that can be caused；
2. the metallic substrates carbon nanotube coating for being grown out using the inventive method has superelevation luminous absorptance, exceedes
The Limiting Level of light-absorbing coating light absorpting ability of the prior art, it is possible to achieve the application scenario of light absorbs requirement higher；
3. on absorption spectrum section width, ultraviolet, visible ray, near red can be absorbed using metallic substrates carbon nanotube coating
Outward, the all-wave spectral coverage such as far infrared, microwave, and existing most of light absorbent coating can only absorb visible ray and near-infrared spectral coverage,
It is decreased obviously in the absorbing ability of near-infrared spectral coverage；
4. because CNT blacker-than-black coating provided by the present invention is significantly larger than conventional material on absorbing ability, therefore
Allow that the appearance and size and weight of the veiling glare devices that disappear such as the light shield designed using the inventive method are greatly reduced.
Brief description of the drawings
Fig. 1 is the flow chart of the inventive method；
Fig. 2 is CNT reacting furnace structural representation.
Specific embodiment
As shown in figure 1, being the FB(flow block) of the inventive method, key step is as follows：
1) thick frosting treatment is carried out to titanium alloy sample surface using ultra-fine sand paper or similar polishing mode so that pass through
The titanium alloy sample surface of polishing has fine scratches, is grown for CNT (CNT, Carbon Nanometer Tube)
Favorably；
2) the titanium alloy exemplar by polishing is cleaned with alcohol or acetone and other organic solvent, organics removal is dirty
Dye thing, such as oil stain and incrustation with the reaction between the organic substance influence carbon source and catalyst that are evaporated under high temperature-proof, and are prevented
The quartzy tube wall of CNT reacting furnace (as shown in Figure 2) is polluted after cooling；
3) after the completion of organic washing, titanium alloy exemplar is put into drying baker drying, drying temperature is controlled below 150 DEG C,
It is clean to enable organic solvent to evaporate, while guaranteeing quick cooling；
4) titanium alloy exemplar is taken out from drying baker, is placed in 20 DEG C ± 5 DEG C of room temperature environment, after cooling, then use clear water
Titanium alloy exemplar is cleaned, removes surface floating dust and residue, it is ensured that what sequent surface was processed is normally carried out；
5) water cleaning after the completion of, again by titanium alloy exemplar be put into drying baker drying, drying temperature control 120 DEG C with
Under；This temperature can ensure that water is evaporated, while faster cooling velocity can be ensured, it is to avoid open-assembly time long causes in air
New pollution；
6) it is to strengthen CNT adhesive strength on the metallic substrate, growing surface can be carried out using two methods pre-
Treatment, one is to be electrochemically reacted treatment to titanium alloy exemplar so that the surface of titanium alloy exemplar is formed engraves micro-nano at microcosmic quarter
Rice structure；Two is the aluminium nickel double metal intermediate buffer layer on the plated surface of titanium alloy exemplar.Both approaches can strengthen carbon and receive
Pull-out capacity of the mitron coating in titanium alloy substrate, can be according to the technical equipment condition for being possessed using which kind of method.
Two methods are described respectively below.
A () is processed using electrochemical reaction makes growing surface produce micro-nano structure
First using electrochemical reaction handling process (in three-electrode electro Chemical system, by metallic substrates in acid solution
Carrying out cathodic polarization and anode etching carries out surface micro-nanoization treatment to it.By the suspicious acquisition of control electric current density and time not
Same surface micro-nano structure) titanium alloy exemplar is surface-treated, it is residual when the metallic element of table is reacted away a part face to face
The part stayed shows fine texturing structure on the surface of the substrate, such as sharp countless " mountain peaks ", due to this " mountain peak "
Height is very big (generally higher than 2) with the ratio of diameter, and actual diameter size is also in micron dimension, when the catalyst of growth response
Particle insertion " mountain peak " between when, after reaction CNT as from mountain valley borough chief out.Growing surface micro-nano texturing layer
Fusing point is relatively low, and well below metal fusing point in itself, after being rapidly heated, these micro-nano texturing structures are by under relatively low fusing point
Fusing, the root of CNT will be embedded in surface micro-nano struc-ture by the micro-nano structure of fusing, as hair is long in scalp
Equally, " soldering " of carbon nano pipe array and micro-nano texturing structure is realized, so as to enhance the adhesive strength of CNT.
B () plates bimetallic intermediate buffer layer
B1) in titanium alloy sample surface evaporation or the bimetal nano coating (such as Al/Ni) of 3~10nm of sputtering sedimentation thickness
(evaporated together in coating chamber, or successively evaporated, because film layer is very thin) as intermediate buffer layer；3~10nm this
Individual thickness range can make the firm binding force of metal oxide and titanium alloy surface, select both metals because they
Grain can be used as the catalyst of growth CNT, and other can be as catalyst and the metal being firmly combined with titanium alloy
As the pairing of double-metal layer.
B2 after) plating double-metal layer with vacuum evaporation or sputtering equipment in titanium alloy substrate, the pre-heat treatment is carried out,
So that bimetallic intermediate buffer layer is changed into oxide coating/metal nanoparticle double-decker；Different coating material combinations
The preheating temperature scope of use is different, and 400 DEG C -600 DEG C this scopes are used for aluminium nickel dam, to ensure that bimetallic is aoxidized
It is moderate, it is unlikely to excessive.Metal nanoparticle is used to grow CNT as catalyst, and oxide coating is used as CNT
Articulamentum between titanium alloy substrate, realizes the effective connection of the two, strengthens bond strength.
7) by step 6) treated titanium alloy exemplar is equipped on quartz boat, then quartz boat is slowly pushed into CNT
The middle part of reacting furnace, the two ends of closed quartz tube；
8) argon gas (can be other inert gases) is passed through toward quartz ampoule, flow is 100~200mL/min, and heating is anti-
Temperature needed for device to carbon nano tube growth is answered, typically at 650 DEG C~850 DEG C.The selection of above flow is on the basis of experiment
What analysis determined, flow selection can ensure that the air in quartz ampoule is thoroughly excluded.In the selection of temperature range, 650 DEG C is fixed
Near the temperature requirement lower limit of carbon nano tube growth, and 850 DEG C of determination is to be unlikely to make titanium alloy that crystalline phase metamorphosis to occur, with
Keep the mechanical property of titanium alloy.
9) in order to empty the air in quartz ampoule with argon gas, it is necessary to the argon gas filling time of practical experience determination, works as the time
When reaching, argon flow amount is adjusted in quartz ampoule to 1000~2000mL/min, while being passed through the hydrogen of 300~500mL/min；
The security when range of flow of argon gas ensure that hydrogen is passed through, the range of flow of hydrogen makes CNT both obtain
Growth rate can guarantee that directionality again faster.
10) it is true according to designed reaction speed when hydrogen flowing quantity stabilization, and when ensuring that hydrogen is uniformly filled in quartz ampoule
Fixed flow is passed through gaseous carbon source (such as methane, ethene) or introduces vaporific liquid carbon source (such as dimethylbenzene) with delicate flow pump, enters
In entering quartz ampoule；
11) the length setting reaction time according to needed for carbon nano pipe array, the setting in reaction time according to growth length with
The relation curve in reaction time, this curve is got from experiment, typically with catalyst type and concentration, carbon source kind and dense
Degree, the species of reducing agent and concentration have relation.General length of carbon nanotube is increased as the reaction time increases.
After completion of the reaction, hydrogen is cut off, is stopped substrate and is heated.Turn down the flow of argon gas to 100mL/min~
150mL/min.Treat that quartz ampoule is cooled to room temperature, take out titanium alloy exemplar.
The flow in this stage mainly considers the security after disconnected hydrogen and saves argon gas determination, and the range of flow of use is
For the reacting furnace of diameter 100mm, should increase according to diameter square ratio when growth furnace increases or reduces and reduce.
If 12) using the adhesion-tight surface treatment method of bimetallic transition zone, take out titanium alloy exemplar, thus
Complete.If using electrochemical reaction micro-nano texturing surface treatment method, by step 11) the titanium alloy exemplar that obtains is put into height
In warm stove, it is rapidly heated to 880 DEG C~920 DEG C, continues 1 minute to 10 minutes, realizes " the weldering of catalyst granules and micro-nano structure
Close " effect.The selection of this temperature is that the fusing for both having considered macro structure considers that titanium alloy crystalline phase does not make a variation simultaneously.It is then high
Warm stove cooling, takes out titanium alloy exemplar, thus completes.
The content not being described in detail in description of the invention belongs to the known technology of those skilled in the art.
Claims (3)
1. a kind of method in the superpower light absorbs carbon nanotube coating of titanium alloy-based bottom growth, it is characterised in that including following step
Suddenly：
(1) frosting treatment is carried out to titanium alloy sample surface using polishing mode so that by the titanium alloy sample surface of polishing
With cut；
(2) the titanium alloy exemplar by polishing is cleaned, removes removal organic polluter；
(3) titanium alloy exemplar is put into drying baker drying；
(4) titanium alloy exemplar is taken out from drying baker, titanium alloy exemplar is cleaned with clear water after cooling；
(5) titanium alloy exemplar is put into drying baker drying again；
(6) treatment is electrochemically reacted to titanium alloy exemplar so that the surface of titanium alloy exemplar formed it is microcosmic quarter engrave it is micro-nano
Structure；Or on the plated surface of titanium alloy exemplar aluminium nickel double metal intermediate buffer layer；
(7) the titanium alloy exemplar that step (6) is treated is inserted in CNT reacting furnace；
(8) toward argon gas is passed through in CNT reacting furnace, while CNT reacting furnace begins heat to carbon nano tube growth institute
Need temperature；
(9) after argon gas is full of CNT reacting furnace, argon flow amount is adjusted to 1000~2000mL/min, while being passed through 300
The hydrogen of~500mL/min；
(10) after hydrogen flowing quantity is stable and full of CNT reacting furnace, reacted to CNT according to predetermined reaction speed
Gaseous carbon source is passed through in stove or vaporific liquid carbon source is introduced；
(11) the length setting reaction time according to needed for carbon nano pipe array, after completion of the reaction, hydrogen is cut off, stops heating, and
The flow of argon gas is turned down to 100mL/min~150mL/min, titanium alloy exemplar is taken out after being cooled to room temperature；
(12) if in step (6) being aluminium nickel double metal intermediate buffer layer, CNT on the plated surface to titanium alloy exemplar
Coating completes；If being to be electrochemically reacted treatment to titanium alloy exemplar in step (6), the titanium alloy sample that will be obtained
Part is put into high temperature furnace, is rapidly heated to 880 DEG C~920 DEG C, continues 1 minute to 10 minutes, then high temperature furnace cooling, takes out titanium
Alloy exemplar, thus completes the making of carbon nanotube coating.
2. a kind of method in the superpower light absorbs carbon nanotube coating of titanium alloy-based bottom growth according to claim 1, its
It is characterised by：Use in the step (6) electrochemical reaction treatment formed engrave at microcosmic quarter the method for micro nano structure for：Using electricity
Chemical reaction handling technique is surface-treated to titanium alloy exemplar, gets rid of the part metals on surface so that the part of residual
Fine texturing structure is showed on the surface.
3. a kind of method in the superpower light absorbs carbon nanotube coating of titanium alloy-based bottom growth according to claim 1, its
It is characterised by：The method of aluminium nickel double metal intermediate buffer layer is on the plated surface of titanium alloy exemplar in the step (6)：First
In titanium alloy sample surface evaporation or the aluminium nickel double metal of 3~10nm of sputtering sedimentation thickness, the pre-heat treatment is then carried out so that double
Metal intermediate buffer layer is changed into oxide coating and metal nanoparticle double-decker, preheating temperature scope 400 DEG C~600
℃。
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| CN105154846A (en) * | 2015-09-11 | 2015-12-16 | 兰州空间技术物理研究所 | Method for manufacturing stray light eliminating surface with ultra high absorptivity |
| CN105549297B (en) * | 2015-12-23 | 2017-12-22 | 北京控制工程研究所 | A kind of preparation method of CNT light shield |
| CN105776173B (en) * | 2016-02-04 | 2018-07-24 | 北京控制工程研究所 | A method of growing carbon nano pipe array on substrate |
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| CN107400928B (en) * | 2017-07-25 | 2019-08-06 | 东北石油大学 | A kind of simple and easy method directly growing carbon nano pipe array on metal and application |
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| CN113564559B (en) * | 2021-07-28 | 2022-08-16 | 福州大学 | Rapid in-situ preparation method of CNTs @ TC4 composite powder |
| CN114836783B (en) * | 2022-04-07 | 2024-02-06 | 福州城建设计研究院有限公司 | Preparation method and application based on nano ruthenium dioxide/carbon composite array |
| CN116908265B (en) * | 2023-09-11 | 2023-12-12 | 常州先趋医疗科技有限公司 | Preparation method of electrochemical biosensor for detecting LAMP amplification products of nucleic acids |
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