CN100575543C - A kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide - Google Patents
A kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide Download PDFInfo
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- CN100575543C CN100575543C CN200810137045A CN200810137045A CN100575543C CN 100575543 C CN100575543 C CN 100575543C CN 200810137045 A CN200810137045 A CN 200810137045A CN 200810137045 A CN200810137045 A CN 200810137045A CN 100575543 C CN100575543 C CN 100575543C
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Abstract
A kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide relates to a kind of processing method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide.Purpose is to solve adopting magnetically controlled sputter method commonly used to be difficult to realize the problem of good combination between coat of silicon carbide and the cobalt base superalloy.Realize the step that the inventive method comprises: one, with cobalt base superalloy hydrofluoric acid clean, acetone soln ultrasonic cleaning, spirituous solution ultrasonic cleaning and washed with de-ionized water; Two, the cobalt base superalloy after will handling is sent in the magnetron sputtering vacuum storehouse, and vacuumizes, to cobalt base superalloy heating and insulation; Three, will feed Ar gas in the storehouse, apply pulsed negative bias cobalt base superalloy surface reverse sputtering; Four: the sputtering power starter, to the pre-sputter of target material surface; Five, formal sputtering is carried out on the cobalt base superalloy surface, the high radiation coating of depositing silicon carbide; Six, close all power supplys, treat that temperature is reduced to room temperature in the storehouse, finish deposition.
Description
Technical field
The present invention relates to a kind of processing method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide.
Background technology
SiC (silicon carbide) has high temperature resistant, high radiation, wear-resistant and anti-particle impacting, and chemical stability is good, and mechanics and thermal property such as high strength.The emittance of SiC is more than 0.9, and this makes it become the preferred material of preparation high temperature resistance radiation coating.The SiC coatings applications after on the metallic substance, not only can significantly improve metallic substance high temperature resistance, resistance to wear and performance such as radioprotective, and all properties all can be designed within the specific limits, thereby is subjected to increasing attention.But its not seen widespread use still up to now, this mainly is because the preparation of coat of silicon carbide is carried out under excessive temperature usually, and complex process, cost are too high.Magnetron sputtering is a kind of highly effective membrane deposition method, can realize the low temperature and the high speed deposition of film.Adopt magnetron sputtering to prepare the important method that the SiC coating is a low-temperature epitaxy SiC coating., thermal expansivity approaching for substrate and coated material performance differs less and lattice mismatch differs less situation, the magnetically controlled sputter method that people adopt substrate not apply pulsed bias mostly prepares film, the effect of deposit film is more satisfactory, but for cobalt base superalloy substrate and coat of silicon carbide, the two material property differs bigger, it is also bigger that thermal expansivity of the two and lattice mismatch differ, easily have unrelieved stress and defective to produce at the interface, this has had a strong impact on coat of silicon carbide adhering on the cobalt base superalloy surface.As adopt magnetically controlled sputter method commonly used, be difficult to realize good binding between coat of silicon carbide and the cobalt base superalloy, thin film deposition weak effect.
Summary of the invention
The objective of the invention is to solve at cobalt base superalloy surface deposition coat of silicon carbide adopts magnetically controlled sputter method commonly used to be difficult to realize good binding between coat of silicon carbide and the cobalt base superalloy, the problem of thin film deposition weak effect designs a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide.
The method that the present invention is implemented in the high radiation coating of cobalt base superalloy surface deposition silicon carbide may further comprise the steps:
Step 1, with cobalt base superalloy with hydrofluoric acid clean 10～20 minutes; Put into acetone soln then, use ultrasonic cleaning 10～20 minutes; Put into spirituous solution again, use ultrasonic cleaning 10～20 minutes; Used washed with de-ionized water at last 10～20 minutes;
Step 2, the cobalt base superalloy after will handling are sent in the magnetron sputtering vacuum storehouse, and the magnetron sputtering vacuum chamber is vacuumized, and the vacuum tightness in magnetron sputtering vacuum storehouse reaches 10
-4During Pa, to the cobalt base superalloy heating, Heating temperature is 25～500 ℃, is incubated 10 minutes then～2 hours;
Step 3, with feeding Ar gas in the magnetron sputtering vacuum storehouse, when pressure reaches 4～6Pa in the magnetron sputtering vacuum storehouse, apply 300～500V pulsed negative bias and reverse sputtering is carried out on the cobalt base superalloy surface cleaned 10～20 minutes;
Step 4: apply the sputtering power starter, power is 60～200W, regulates the Ar airshed between 10sccm～50sccm, to the pre-sputter of target material surface 3～5 minutes;
Step 5, when regulating in the magnetron sputtering vacuum storehouse between gas pressure intensity to 0.1～2Pa, apply the pulsed negative bias of 40～200V on the cobalt base superalloy surface, sputtering power is 150W, the Ar airshed is between 10sccm～50sccm, carry out formal sputtering on the cobalt base superalloy surface, the high radiation coating of depositing silicon carbide;
Step 6, formal sputtering finish, and close all power supplys, treat that temperature is reduced to room temperature in the magnetron sputtering vacuum storehouse, finish the deposition to the high radiation coating of cobalt base superalloy surface carborundum.
Advantage of the present invention is: the present invention utilizes magnetron sputtering to realize the high radiation coating of low temperature depositing silicon carbide on the cobalt base superalloy surface.To adhere to unstable atom removing with the superalloy substrate by applying suitable pulsed bias, cleaning high-temp alloy substrate surface, make the sticking power of coat of silicon carbide and cobalt base superalloy substrate strengthen greatly, realize good binding between high radiation coating of silicon carbide and the cobalt base superalloy.With the common chemical vapour deposition, film preparing technologies such as molecular beam epitaxy are compared, and utilize by applying the coat of silicon carbide that certain pulsed bias is prepared: have good compactness; Eliminate cobalt base superalloy and SiC coating interface defective and unrelieved stress, realize good binding between coat of silicon carbide and the superalloy substrate; Have radiation characteristic preferably, emittance is higher.
Description of drawings
Fig. 1 is that institute's deposited coatings is made the Fourier infrared spectrum analysis chart on the cobalt base superalloy substrate.
Embodiment
Embodiment one: below in conjunction with Fig. 1 present embodiment is described, the method that present embodiment is implemented in the high radiation coating of cobalt base superalloy surface deposition silicon carbide may further comprise the steps:
Step 1, with cobalt base superalloy with hydrofluoric acid clean 10～20 minutes; Put into acetone soln then, use ultrasonic cleaning 10～20 minutes; Put into spirituous solution again, use ultrasonic cleaning 10～20 minutes; Used washed with de-ionized water at last 10～20 minutes;
Step 2, the cobalt base superalloy after will handling are sent in the magnetron sputtering vacuum storehouse, and the magnetron sputtering vacuum chamber is vacuumized, and the vacuum tightness in magnetron sputtering vacuum storehouse reaches 10
-4During Pa, to the cobalt base superalloy heating, Heating temperature is 25～500 ℃, is incubated 10 minutes then～2 hours;
Step 3, with feeding Ar gas in the magnetron sputtering vacuum storehouse, when pressure reaches 4～6Pa in the magnetron sputtering vacuum storehouse, apply 300～500V pulsed negative bias and reverse sputtering is carried out on the cobalt base superalloy surface cleaned 10～20 minutes;
With the ion bombardment solid surface that quickens, ion and solid surface atom exchange momentum make the atom of solid surface leave solid, and this process is called sputter.
We claim to impact target is sputter, and the impact substrate is a reverse sputtering.
Step 4: apply the sputtering power starter, power is 60～200W, regulates the Ar airshed between 10sccm～50sccm, to the pre-sputter of target material surface 3～5 minutes;
Energetic ion (Ar
+) acquisition be the key of sputtering technology, these energetic ions (Ar
+) in glow discharge, produce, therefore glow discharge is the basis of sputter, glow discharge is meant in vacuum tightness and is about in 1Pa～10Pa vacuum, the electric discharge phenomena that produced when adding high pressure between two electrodes, and we are simply referred to as " logical argon gas (Ar) starter " usually.
Before formal sputtering, oxide compound and other impurity in order to remove target material surface at first apply certain power and carry out starter, and present embodiment is selected 60～200W for use, makes energetic ion (Ar
+) target material surface being carried out pre-sputter, at this moment, between target and substrate, both are separated, so substrate surface can not form film, normally 3～5 minutes time with baffle plate.
Step 5, when regulating in the magnetron sputtering vacuum storehouse between gas pressure intensity to 0.1～2Pa, apply the pulsed negative bias of 40～200V on the cobalt base superalloy surface, sputtering power is 150W, the Ar airshed is between 10sccm～50sccm, carry out formal sputtering on the cobalt base superalloy surface, the high radiation coating of depositing silicon carbide;
Remove baffle plate during formal sputtering, at the substrate surface deposit film.
Apply the plus earth (position at zero point) that pulsed negative bias is meant bias voltage on the cobalt base superalloy surface, negative pole connects cobalt base superalloy (substrate).
Substrate is applied certain pulsed negative bias, make coating surface in deposition process constantly be subjected to the cleaning of electric field, eliminate at any time and may enter electronics or other impurity of coating, help improving the purity of film, make film compactness better.
The time of this step deposition film is determined by deposit thickness.
Step 6, formal sputtering finish, and close all power supplys, treat that temperature is reduced to room temperature in the magnetron sputtering vacuum storehouse, finish the deposition to the high radiation coating of cobalt base superalloy surface carborundum.
Magnetron sputtering generally is to load onto permanent magnet or electro-magnet in cathode targets, and makes the path of the magnetic line of force that passes target cathode vertical with direction of an electric field, so that the constraint charging particle movement.What add mounted permanent magnet is called the permanent magnetism target, and what install electro-magnet additional is called the electromagnetism target.Its principle is that the charged particle at target material surface place not only is subjected to electric field action, simultaneously also is subjected to the target the action of a magnetic field, but in low-intensity magnetic field, and the quality electronics more much smaller than ion is influenced bigger.The target material surface electronics is subjected to the crossed electric and magnetic field effect, and its direction of motion constantly changes, and constantly does cyclotron motion around the target cathode surface.In the motion of substrate anode direction, prolonged the path of motion in fact greatly, the collision frequency of electronics and neutral gas molecule is increased, and its ionized number of times is significantly increased.Energy significantly descends when the electronics of repeatedly collision arrives the substrate anode, and this not only improves sputtering yield, guarantees again not cause that the substrate temperature rise is too high, has realized low temperature and high speed sputter effect.
Fig. 1 is that institute's deposited coatings is made the Fourier infrared spectrum analysis chart on the cobalt base superalloy substrate, utilizes magnetically controlled sputter method can realize the low temperature depositing coat of silicon carbide as seen from the figure.
According to the combine situation of standard GB/T 5210-1985 coating adhesion assay method mensuration cobalt base superalloy substrate with coat of silicon carbide.Adopt the adhesion condition of adhesive tape method test coat of silicon carbide, coating does not come off after tested, shows that cobalt base superalloy combines well with coat of silicon carbide.
Based on People's Republic of China's GJB " infrared emittance measuring method ", adopt the emittance of shooting method test coat of silicon carbide.Under the room temperature, the average emitted rate of SiC coating is 0.85, and its spectral emittance maximum value surpasses 0.9.Sedimentary coat of silicon carbide has thermal radiation property preferably on the cobalt base superalloy substrate, and emittance is higher, satisfies the requirement as the high radiation coating in metallic surface.
Embodiment two: the difference of present embodiment and embodiment one is in the step 1 cobalt base superalloy to be used hydrofluoric acid clean 15～20 minutes; Put into acetone soln then, use ultrasonic cleaning 15～20 minutes; Put into spirituous solution again, use ultrasonic cleaning 15～20 minutes; Used washed with de-ionized water at last 15～20 minutes.Other is identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one is that Heating temperature is 25～200 ℃ in the step 2, is incubated 40～80 minutes then.Other is identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is that Heating temperature is 100 ℃ in the step 2, is incubated 1 hour then.Other is identical with embodiment one.
Embodiment five: the difference of present embodiment and embodiment one is to apply in the step 3 450V pulsed negative bias reverse sputtering cleaning 15～20 minutes is carried out on the cobalt base superalloy surface.Other is identical with embodiment one.
Embodiment six: the difference of present embodiment and embodiment one was to apply in the step 4 sputtering power starter, and power is 60～150W, regulates the Ar airshed between 20sccm～30sccm, to the pre-sputter in coat of silicon carbide surface 3～5 minutes.Other is identical with embodiment one.
Embodiment seven: the difference of present embodiment and embodiment one is to apply on the cobalt base superalloy surface in the step 5 pulsed negative bias of 40～120V.Other is identical with embodiment one.
Embodiment eight: the difference of present embodiment and embodiment one is to apply on the cobalt base superalloy surface in the step 5 pulsed negative bias of 80V.Other is identical with embodiment one.
Embodiment nine: the difference of present embodiment and embodiment one is that the Ar airshed is between 20sccm～30sccm in the step 5.Other is identical with embodiment one.
Claims (9)
1, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide is characterized in that realizing that this bag method may further comprise the steps:
Step 1, with cobalt base superalloy with hydrofluoric acid clean 10～20 minutes; Put into acetone soln then, use ultrasonic cleaning 10～20 minutes; Put into spirituous solution again, use ultrasonic cleaning 10～20 minutes; Used washed with de-ionized water at last 10～20 minutes;
Step 2, the cobalt base superalloy after will handling are sent in the magnetron sputtering vacuum storehouse, and the magnetron sputtering vacuum chamber is vacuumized, and the vacuum tightness in magnetron sputtering vacuum storehouse reaches 10
-4During Pa, to the cobalt base superalloy heating, Heating temperature is 25～500 ℃, is incubated 10 minutes then～2 hours;
Step 3, with feeding Ar gas in the magnetron sputtering vacuum storehouse, when pressure reaches 4～6Pa in the magnetron sputtering vacuum storehouse, apply 300～500V pulsed negative bias and reverse sputtering is carried out on the cobalt base superalloy surface cleaned 10～20 minutes;
Step 4: apply the sputtering power starter, power is 60～200W, regulates the Ar airshed between 10sccm～50sccm, to the pre-sputter of target material surface 3～5 minutes;
Step 5, when regulating in the magnetron sputtering vacuum storehouse between gas pressure intensity to 0.1～2Pa, apply the pulsed negative bias of 40～200V on the cobalt base superalloy surface, sputtering power is 150W, the Ar airshed is between 10sccm～50sccm, carry out formal sputtering on the cobalt base superalloy surface, the high radiation coating of depositing silicon carbide;
Step 6, formal sputtering finish, and close all power supplys, treat that temperature is reduced to room temperature in the magnetron sputtering vacuum storehouse, finish the deposition to the high radiation coating of cobalt base superalloy surface carborundum.
2, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide according to claim 1 is characterized in that in the step 1 cobalt base superalloy being used hydrofluoric acid clean 15～20 minutes; Put into acetone soln then, use ultrasonic cleaning 15～20 minutes; Put into spirituous solution again, use ultrasonic cleaning 15～20 minutes; Used washed with de-ionized water at last 15～20 minutes.
3, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide according to claim 1 is characterized in that Heating temperature is 25～200 ℃ in the step 2, is incubated 40～80 minutes then.
4, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide according to claim 1 is characterized in that Heating temperature is 100 ℃ in the step 2, is incubated 1 hour then.
5, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide according to claim 1 is characterized in that applying in the step 3 450V pulsed negative bias reverse sputtering cleaning 15～20 minutes is carried out on the cobalt base superalloy surface.
6, a kind of method according to claim 1 at the high radiation coating of cobalt base superalloy surface deposition silicon carbide, it is characterized in that applying in the step 4 sputtering power starter, power is 60～150W, regulate the Ar airshed between 20sccm～30sccm, to the pre-sputter in sedimentary coat of silicon carbide surface 3～5 minutes.
7, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide according to claim 1 is characterized in that applying on the cobalt base superalloy surface in the step 5 pulsed negative bias of 40～120V.
8, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide according to claim 1 is characterized in that applying on the cobalt base superalloy surface in the step 5 pulsed negative bias of 80V.
9, a kind of method at the high radiation coating of cobalt base superalloy surface deposition silicon carbide according to claim 1 is characterized in that the Ar airshed is between 20sccm～30sccm in the step 5.
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| CN103014645A (en) * | 2012-12-26 | 2013-04-03 | 哈尔滨工业大学 | Method for simply reinforcing large-size magneto-controlled sputter coating |
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| CN102051589B (en) * | 2010-11-25 | 2013-01-02 | 南京理工大学 | Method for preparing amorphous silicon carbide film and epitaxial film at low temperature |
| CN102080212A (en) * | 2011-02-25 | 2011-06-01 | 上海太阳能电池研究与发展中心 | Low-temperature manufacturing method and special target of ZnO transparent conductive film |
| CN103796346A (en) * | 2014-02-27 | 2014-05-14 | 上海理工大学 | High-temperature nano-electrothermal film of double-film structure and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103014645A (en) * | 2012-12-26 | 2013-04-03 | 哈尔滨工业大学 | Method for simply reinforcing large-size magneto-controlled sputter coating |
| CN103014645B (en) * | 2012-12-26 | 2015-04-08 | 哈尔滨工业大学 | Method for simply reinforcing large-size magneto-controlled sputter coating |
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