CN102251224A - Device and method for depositing film on SiC fiber surface - Google Patents
Device and method for depositing film on SiC fiber surface Download PDFInfo
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- CN102251224A CN102251224A CN2011101930659A CN201110193065A CN102251224A CN 102251224 A CN102251224 A CN 102251224A CN 2011101930659 A CN2011101930659 A CN 2011101930659A CN 201110193065 A CN201110193065 A CN 201110193065A CN 102251224 A CN102251224 A CN 102251224A
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Abstract
The invention relates to vacuum coating magnetron sputtering deposition technology, and particularly a device and a method for depositing a film on a SiC fiber surface; on one hand, a film with a uniform thickness is deposited on a continuous SiC fiber surface; on the other hand, the problem of target material poisoning of compound film deposition is solved, and the continuity and stability of the deposition process is realized. The device is provided with a target material I, a target material II, a workpiece rotating shelf, an intermediate-frequency pulsed magnetron sputtering power supply, a magnetron sputtering vacuum chamber; the workpiece rotating shelf is disposed in the magnetron sputtering vacuum chamber; the target material I and the target material II are facingly disposed inside and outside the workpiece rotating shelf in the magnetron sputtering vacuum chamber; a cathode of the intermediate-frequency pulsed magnetron sputtering power supply is connected to the target material I; and an anode of the intermediate-frequency pulsed magnetron sputtering power supply is connected to the target material II. According to the invention, the gas flow, the reaction gas types, the sputtering time and the like in the vacuum chamber of the magnetron sputtering device are adjusted so as to realize the deposition of metals or compound films with different types and different thicknesses on a continuous SiC fiber surface, and to realize the surface modification of the SiC fiber.
Description
Technical field
The present invention relates to the vacuum plating magnetron sputtered deposition technology, more specifically, relate to a kind of on the continuous SiC fiber surface device and method of deposit film.
Background technology
Chemical vapor deposition (CVD) method continuous SiC fiber is owing to have excellent performance such as high specific strength, high specific stiffness, its high-temperature behavior can remain to 1200 ℃, it is the main enhancing body of metal (Ti alloy, Ni alloy) based composites, be applied to the Aeronautics and Astronautics field, can significantly reduce the density of material, improve mechanical property.
In order to reduce the surface residual stress of SiC fiber, improve the intensity of fiber, the SiC fiber surface generally has the thick carbon rich coating of about 2.5 μ m, but find that in metal (especially Ni alloy) based composites preparation process this carbon rich coating can not stop the reaction between SiC fiber and the matrix well, destroyed the integrity of fiber, made fiber lose reinforced effects.For the reaction between controlling fiber and the matrix effectively, improve the physical compatibility between fiber and the matrix simultaneously, need be in the new coating of SiC fiber surface deposition, the coating that meets above condition generally is a compound coat, as Al
2O
3, TiN, AlN etc.Simultaneously also can continue depositing the certain thickness metal level of continuous SiC fiber surface deposition of compound coat, difference according to metal targets, can form different metal levels at fiber surface, comprise Ti and alloy thereof, Ni and alloy thereof etc., with the compound precursor wire of preparation continuous SiC fiber/metal (alloy) based composites.
The physical vapor deposition (PVD) method is in a kind of main method of lower temperature condition preparing compound film, comprises arc ion plating, magnetron sputtering etc.Wherein arc ion plating method sedimentation rate is fast, but the macrobead phenomenon of film surface is more serious, has influenced the quality of film; Though the magnetron sputtering method sedimentation rate is lower, the film even compact of preparation does not have surperficial macrobead phenomenon, and film quality is better.
In the film preparation process, if the target that adopts compound to make, not only target purity is limited, and the sputter insulating material is also very difficult.What therefore magnetron sputtering method prepared the general employing of compound film is the method for reaction magnetocontrol sputtering, and power supply can be divided into direct current, radio frequency and medium-frequency pulse.Adopt direct supply sputter meeting to cause the instability of target poisoning, sparking and sputter procedure, adopt the radio frequency sedimentation rate very low, and the medium-frequency pulse reactive sputtering can avoid target to poison, guarantee that the stable of sputter procedure carries out and higher sedimentation rate, in medium frequency reactive sputtering, when added voltage was in negative half period on the target, target surface was by the positive ion sputter; And when positive half cycle, the electronics in the plasma body is accelerated to target surface, the positive charge that has neutralized and accumulated on the target surface, thus suppressed sparking.But under the work field intensity of determining, supply frequency is high more, and the time that positive ion is accelerated in the plasma body is short more, and positive electric field is few more from the energy that external electric field absorbs, and the positive ion energy of bombardment target is low more, and the sputter rate of target also reduces.Because the range of frequency of sputtering voltage is in 5～80KHz scope, therefore make intermediate frequency shielding power supply, middle RF sputtering be usually used in two targets of sputter again, be generally two targets side by side, size is all identical with profile, so these two targets often are called target.To the target installation that in the sputter vacuum chamber, suspends, in sputter procedure, two targets had both suppressed sparking successively periodically in turn as negative electrode and anode, and,, the reaction magnetocontrol sputtering process carries out thereby being stablized owing to the anode extinction tests of having eliminated in the conventional DC reaction magnetocontrol sputtering.Owing to need deposit certain thickness metal level or chemical combination layer at successive SiC fiber surface, what especially consider in large-area coating film production to need special concern is sedimentation rate and target utilization, deposit film homogeneity question, and the problem of therefore controlling aspects such as substrate region plasma density and homogeneity is most important.
Summary of the invention
In order to satisfy demand at continuous SiC fiber surface deposition film, the invention provides a kind of device and method at SiC fiber surface deposit film, can go out the uniform film of thickness at the continuous SiC fiber surface deposition on the one hand; Solve the problem that deposited compound film target is poisoned on the one hand, to realize the continuity and the stability of deposition process.
Technical scheme of the present invention is:
A kind of device at SiC fiber surface deposit film, this device is provided with target I, target II, workpiece pivoted frame, middle frequency pulsed magnetron sputtering power supply, magnetron sputtering vacuum chamber, the workpiece pivoted frame places magnetron sputtering vacuum chamber, target I, target II are staggered relatively in magnetron sputtering vacuum chamber inside and outside the workpiece pivoted frame, the negative electrode of middle frequency pulsed magnetron sputtering power supply and target I join, and the anode of middle frequency pulsed magnetron sputtering power supply and target II join.
Described device at SiC fiber surface deposit film is provided with heating rod in the magnetron sputtering vacuum chamber, magnetron sputtering vacuum chamber is provided with vacuum orifice, reaction gas inlet and sputter gas inlet.
Described device at SiC fiber surface deposit film also is provided with grid bias power supply, and the anode of grid bias power supply is connected with vacuum chamber, and the negative electrode of grid bias power supply is connected with magnetron sputtering workpiece pivoted frame.
Described device at SiC fiber surface deposit film, target I, target II constitute nonequilibrium state magnetic field to target, nonequilibrium state magnetic field to target be set to a pair of or a pair of more than, between target I, the target II apart from 80mm～180mm.
Described device at SiC fiber surface deposit film, the workpiece pivoted frame comprises pallet under workpiece pivoted frame upper tray, the workpiece pivoted frame, has the support bar of cutting, the support bar that has cutting is connected with pallet under workpiece pivoted frame upper tray, the workpiece pivoted frame respectively, pallet is a disc under workpiece pivoted frame upper tray, the workpiece pivoted frame, the support bar that has cutting is along pallet circumference uniform distribution under workpiece pivoted frame upper tray, the workpiece pivoted frame, continuous SiC fiber is wrapped in the cutting of workpiece pivoted frame support bar, and groove depth is 0.5～4 millimeter.
Described device at SiC fiber surface deposit film is provided with permanent magnet at magnetic control to the target ectonexine, and the magneticstrength of internal layer permanent magnet is that the magneticstrength of the outer permanent magnet of 2800～3500 gaussian sums is 3800～5100 Gausses.
Described device at SiC fiber surface deposit film, target adopts pure metal targets: nickel target, titanium target, zinc target, chromium target, magnesium target, niobium target, tin target, aluminium target, iron target, zirconium target, copper target, silver-colored target, cobalt target, gold target, yttrium target, cerium target or molybdenum target.
Described method at SiC fiber surface deposit film adopts the metal pair target at SiC fiber surface deposit film, and the negative electrode of middle frequency pulsed magnetron sputtering power supply and target I join, and anode and target II join; Continuous SiC fiber is wrapped on the workpiece pivoted frame, puts into magnetron sputtering vacuum chamber, be evacuated to vacuum tightness and reach (2～4) * 10
-3During Pa, feed sputter gas Ar gas and reactant gases O
2Gas to operating air pressure is 0.2～0.5Pa, Ar and O
2Throughput ratio is 1: (3～7), and the middle frequency pulsed magnetron sputtering power supply is started working, operating voltage 80～200V, working current 2～5A, dutycycle is 5～45%, and the shielding power supply frequency setting is 5～80kHz, and sputtering power is 400～500W, sputtering time is 0.5～10h, in the middle frequency pulsed magnetron sputtering power work, by grid bias power supply the workpiece pivoted frame is applied negative bias, voltage 100～200V, dutycycle is 10～45% final, obtains the film that thickness is 100～800nm.
The rotation in the middle of two relative magnetron sputtering targets of described method at SiC fiber surface deposit film, workpiece pivoted frame is passed through, the speed of rotation of workpiece pivoted frame be 1～10 rev/min adjustable, the workpiece pivoted frame also has forward to be changeed/reverse rotating function.
Described method at SiC fiber surface deposit film, the middle frequency pulsed magnetron sputtering power supply adopts the holohedry bipolar square wave way of output, and dutycycle is 5～45%, adjustable pulse-repetition scope 5～80kHz.
The device of the present invention's deposit film on the continuous SiC fiber surface, adopted the intermediate frequency power supply design to the target structure and the holohedry bipolar square wave way of output in nonequilibrium state magnetic field, two targets are staggered relatively inside and outside the workpiece pivoted frame, the target spacing is adjustable within the specific limits, makes that the film thickness that is deposited on the SiC fiber surface is even.
The SiC fiber is wrapped in can be on the workpiece pivoted frame that rotation between two targets is passed through, and it is simple and practical, and promptly workpiece pivoted frame sense of rotation is variable, adjustable-speed.The coiling magnetron sputtering workpiece pivoted frame that tension force is controlled, the support bar of workpiece pivoted frame has carried out the cutting processing, the fiber of adjacent like this winding can not be in contact with one another, and fiber can not drop in workpiece pivoted frame rotary course, and the staple length of winding can reach more than the 150m.
Because the sedimentary film of SiC fiber surface is a compound film, in order to guarantee that the stable of deposition process carries out, sputter procedure has adopted the middle frequency pulsed magnetron sputtering power supply, this power supply adopts bipolar pulse square wave out-put supply form, but alternation ground changes motion morphology and spatial distribution at magnetron sputtering deposition process ionic medium body.Parameters such as the dutycycle by changing power supply, amplitude, frequency, can moderately introduce the electronics in the plasma body in the target, the positive charge that the non-etched area insulation layer that neutralizes accumulates, suppress the matrix discharge, prevent the target poisoning, guaranteed the homogeneity of film forming processing quality stability of reactive sputtering and film.
Usually magnetic control is to two kinds of target Magnetic Field Design balance-dividing attitude and nonequilibrium state, outer magnet magnetic flux about equally in the equilibrium state magnetic controlling target, magnetic line of force is in magnetic control target surface closure, and plasma body (mainly being electronics) is constrained near the target surface, increases probability of collision, improved sputtering yield, thereby can be under lower operating air pressure and voltage just can the starting the arc and keep glow discharge, and reduce the bombardment of plasma body simultaneously to substrate, the suffered ion bombardment of substrate is little, saturation ion current density is little, usually about 10
-1MA/cm
2Magnitude helps realizing low temperature depositing; On the other hand, plated film need strengthen the plasma density of substrate region and the ionization level of reactant gases sometimes.In order to address that need, the present invention has adopted the non-balance magnetically controlled sputter technology, promptly allow the magnetic line of force on magnetic controlling target surface not closed, magnetic line of force can be along the border extended of target to substrate region, thereby portions of electronics and ion can expand to substrate along magnetic line of force, increased the specific ionization and the plasma density of substrate region, substrate place saturation ion current density is big, can reach 1～10mA/cm usually
2Magnitude.Controlled in order to increase substrate region specific ionization and plasma density, both having reached non-equilibrium degree regulates, along with changing the non-equilibrium degree of magnetic control to target, it both can strengthen or weaken ion bombardment intensity, the plasma density at substrate place, simultaneously also can improve target utilization in addition, improve and the thickness of control large-area film deposition and improve plasma body uneven distribution spatially, improve the homogeneity of deposit film.
The magneticstrength that the present invention is produced target ectonexine permanent magnet (magneticstrength of internal layer permanent magnet is that the magneticstrength of the outer permanent magnet of 2800～3500 gaussian sums is 3800～5100 Gausses) at magnetic control, implemented optimization design, reached the perfect closed of two target magnetic confining field magnetic line of force, effectively stoped the electronics escape, improve sputtering yield and ionization level, satisfied the different SiC fiber membranes of deposition, the magnetic control that may need different non-equilibrium degree is to target (being substrate region different plasma density) plated film needs.And with same fixedly magnetron sputtering to the target pattern, be difficult to satisfy actual requirement sometimes.
The present invention is used for SiC fiber surface thin film deposition device and has following characteristics:
1. can obtain high film deposition rate;
2. sputter procedure can be operated on the working point of setting to all-the-time stable.
3. owing to eliminated the spark phenomenon that target poisons in reactive sputtering, so film defects density is wanted little several magnitude than the conventional DC magnetron sputtering.
4. arrive the energy that the matrix atom on average obtains during owing to the intermediate frequency reaction magnetocontrol sputtering, it is higher than the value of dc reactive sputtering.Therefore substrate temperature is higher in deposition process, causes the deposit film can be finer and close, understands more firm with combine of matrix.
For this reason, optimization design of the present invention the ectonexine dynamic magnetic field the position shape, realized the perfect adaptation of non-equilibrium degree controllable pair target structure and medium frequency magnetron sputtering power supply.The length of considering continuous SiC fiber is more than rice up to a hundred, diameter is about 100 μ m, and it is to belong to stupalith, the special operation condition that shearing resistance is lower, in order to solve the inhomogeneity problem of deposit film on the continuous SiC fiber surface, designed a kind of simple and practically, promptly workpiece pivoted frame sense of rotation is variable, adjustable-speed.The coiling magnetron sputtering workpiece pivoted frame that tension force is controlled can guarantee the stably depositing of film to target structure in that workpiece pivoted frame configuration is inside and outside in addition, can realize that again sputtering particle is deposited on the surface of SiC fiber equably.
Innovative characteristics of the present invention is as follows:
1. magnetron sputtering equipment of the present invention adopts nonequilibrium state magnetic field that target is designed, and can be implemented in deposit film on the SiC fiber surface, makes that sedimentary film thickness is even.
The present invention to the setting of target be a pair of or a pair of more than, adopting purity is the above metallic target of 99.99wt%.Every pair of target adopts identical metallic target (each material to metallic target also can be different).By the sputter of control different metal target, not only can deposit a kind of coating like this, also can continue to deposit other coating on this basis, form the SiC fiber composite silk that has multiple coating at fiber surface.
3. magnetron sputtering equipment of the present invention can also can deposit uniform film with the continuous SiC fiber uniform winding on the workpiece pivoted frame.
4. adopt the medium-frequency pulse shielding power supply to carry out reactive sputtering, avoided the target poisoning, can guarantee that the stable of reaction process carries out.
5. the workpiece pivoted frame has the forwards/reverse function, has also designed adjustable-speed.The compatibility function of the coiling magnetron sputtering workpiece pivoted frame that tension force is controlled has solved batch process and the laboratory plated film needs to workpiece pivoted frame operation scheme.
6. the present invention adopts the optimization design to target ectonexine permanent magnet magnetic intensity of field, reached the closure of two target magnetic confining field magnetic line of force, satisfied deposit the different non-equilibrium degree of different film needs magnetic control to target (being substrate region different plasma density) plated film needs.
7. the inventive method is simple, and is easy for installation, simple to operate easy.
Description of drawings
Fig. 1 is apparatus of the present invention internal cross section synoptic diagram.Among the figure, 1 target I; 2 target II; 3 workpiece pivoted frames; 4 middle frequency pulsed magnetron sputtering power supplys; 5 grid bias power supplies; 6 heating rods; 7 magnetron sputtering vacuum chambers.
Fig. 2 is for being used to twine the workpiece pivoted frame schematic perspective view of SiC fiber in apparatus of the present invention.Among the figure, 31 workpiece pivoted frame upper tray; Pallet under the 32 workpiece pivoted frames; 33 support bars.
Fig. 3 is the workpiece pivoted frame that winds fiber.Among the figure, 31, workpiece pivoted frame upper tray; 32, pallet under the workpiece pivoted frame; 33, support bar; 8, SiC fiber.
Fig. 4 is a SiC fiber surface depositing Al
2O
3Surface topography behind the film.
Fig. 5 (a)-(b) is a SiC fiber surface depositing Al
2O
3The XPS spectrum figure of film.Wherein, Fig. 5 (a) is Al
2pThe peak; Fig. 5 (b) is O
1sThe peak.
Embodiment
As Figure 1-3, the device that the present invention is used for SiC fiber surface deposit film mainly comprises: target I 1, target II2, workpiece pivoted frame 3, middle frequency pulsed magnetron sputtering power supply 4, grid bias power supply 5, heating rod 6, magnetron sputtering vacuum chamber 7, workpiece pivoted frame 3 places magnetron sputtering vacuum chamber 7, two target (target I 1, target II2) inside and outside staggered relatively in magnetron sputtering vacuum chamber 7 at workpiece pivoted frame 3, the negative electrode of middle frequency pulsed magnetron sputtering power supply 4 and target I 1 join, the anode of middle frequency pulsed magnetron sputtering power supply 4 and target II2 join, heating rod 6 is set in the magnetron sputtering vacuum chamber 7, and magnetron sputtering vacuum chamber 7 is provided with vacuum orifice, reaction gas inlet and sputter gas inlet.The anode of grid bias power supply 5 is connected with vacuum chamber, and the negative electrode of grid bias power supply is connected with workpiece pivoted frame 3.
Target I1 of the present invention, target II2 constitute nonequilibrium state magnetic field to target, nonequilibrium state magnetic field to target be set to a pair of or a pair of more than, between target I 1, the target II2 apart from 80mm～180mm, the diameter of target I 1, target II2 is 60～100mm, workpiece pivoted frame 3 can pass through in the middle of two relative magnetron sputtering targets in rotation, and the speed of rotation that can realize positive and negative rotation and control workpiece pivoted frame 3 changes function (speed of rotation be 1～10 rev/min adjustable).And the compatibility function of having realized the coiling magnetron sputtering workpiece pivoted frame that constant speedpump, permanent tension force are controlled, solved batch process and laboratory plated film needs to workpiece pivoted frame operation scheme.
Shown in Fig. 2-3, workpiece pivoted frame 3 comprises pallet 32 under workpiece pivoted frame upper tray 31, the workpiece pivoted frame, has the support bar 33 of cutting, the support bar 33 that has cutting is connected with pallet 32 under workpiece pivoted frame upper tray 31, the workpiece pivoted frame respectively, pallet 32 is a disc under workpiece pivoted frame upper tray 31, the workpiece pivoted frame, the support bar 33 that has cutting is along pallet 32 circumference uniform distributions under workpiece pivoted frame upper tray 31, the workpiece pivoted frame, continuous SiC fiber 8 is wrapped in the cutting of workpiece pivoted frame 3 support bars 33, and groove depth is 0.5～4 millimeter.
The present invention is provided with permanent magnet at magnetic control to the target ectonexine, and the magneticstrength of internal layer permanent magnet is that the magneticstrength of the outer permanent magnet of 2800～3500 gaussian sums is 3800～5100 Gausses.The magneticstrength optimization design that the present invention is produced target ectonexine permanent magnet at magnetic control has realized that non-equilibrium degree effectively controls, reach the closure of two target magnetic confining field magnetic line of force, satisfied the different films of deposition, the magnetic control that may need different non-equilibrium degree is to target (being that substrate region needs different plasma density) plated film needs.
The sputter mode that the present invention adopts is a reaction magnetocontrol sputtering, adopts pure metal targets, feeds reactant gases and sputter gas simultaneously, under the condition of different gas flow intrinsic standoff ratios, can deposit metal or compound individual layer, multilayer and graded composite coating film.
Among the present invention, metal targets adopts nickel target, titanium target, zinc target, chromium target, magnesium target, niobium target, tin target, aluminium target, iron target, zirconium target, copper target, silver-colored target, cobalt target, gold target, yttrium target, cerium target or molybdenum target etc.
Adopt the metal pair target at SiC fiber surface deposit film, continuous SiC fiber is wrapped on the workpiece pivoted frame, put into magnetron sputtering vacuum chamber, be evacuated to vacuum tightness and reach (2～4) * 10
-3During Pa, feed sputter gas Ar gas and reactant gases O
2Gas to operating air pressure is 0.2～0.5Pa, Ar and O
2Throughput ratio is 1: (3～7), the middle frequency pulsed magnetron sputtering power supply is started working, operating voltage 80～200V, working current 2～5A, dutycycle is 5～45%, and the shielding power supply pulse-repetition is set at 5～80kHz, and sputtering power is 400～500W, sputtering time is 0.5～10h, finally obtains the film that thickness is about 100～800nm.
Among the present invention, in 4 work of middle frequency pulsed magnetron sputtering power supply, apply the negative pulse bias voltage by 5 pairs of workpiece pivoted frames 3 of grid bias power supply, it can greatly improve the homogeneity and the sedimentation rate of film, grid bias power supply 5 adopts the pulsed negative bias power supply, voltage 100～200V, and dutycycle is 10～45%.
Consider that direct supply can cause unstable in target poisoning, sparking and the sputter procedure at reactive sputtering, adopt the radio frequency sedimentation rate very low, be unfavorable for the reason produced in batches, it is the middle frequency pulsed magnetron sputtering power supply that the present invention has adopted the magnetron sputtering power supply, designed and had holohedry bipolar square wave output mode, dutycycle is 5～45%, adjustable pulse-repetition scope 5～80kHz.
Embodiment 1
As Figure 1-3, adopt Al to target in SiC fiber surface depositing Al
2O
3Film, the purity of Al target is 99.99wt%, is of a size of 272 * 68 * 10mm.The negative electrode of middle frequency pulsed magnetron sputtering power supply 4 and target I 1 join, anode and target II2 join, between target I, the target II apart from 120mm, at magnetic control the target ectonexine is provided with permanent magnet, the magneticstrength of internal layer permanent magnet is that the magneticstrength of the outer permanent magnet of 3000 gaussian sums is 4500 Gausses.Continuous SiC fiber is wrapped in the cutting of workpiece pivoted frame 3 upper support bars, groove depth is 2 millimeters, puts into magnetron sputtering vacuum chamber 7, is evacuated to vacuum tightness and reaches 3 * 10
-3During Pa, feed bulk purity and be 99.999% sputter gas Ar gas and reactant gases O
2Gas to operating air pressure is 0.3Pa, Ar and O
2Throughput ratio is 1: 5, and the middle frequency pulsed magnetron sputtering power supply is started working, operating voltage 160V, and working current 3A, dutycycle is 45%, and the shielding power supply frequency setting is 30kHz, and sputtering power is 480W, and sputtering time is 8h, the speed of rotation of workpiece pivoted frame is 5 rev/mins; In the present embodiment, in middle frequency pulsed magnetron sputtering power supply 4 work, apply negative bias by 5 pairs of workpiece pivoted frames 3 of grid bias power supply, grid bias power supply 5 is the pulsed negative bias power supply, voltage 150V, and dutycycle is 20% final, obtains the Al that thickness is about 600nm
2O
3Film.The film surface appearance that obtains as shown in Figure 4, film even compact, no macrobead phenomenon.
As shown in Figure 5, through XPS analysis as can be seen the composition of film be Al
2O
3
Embodiment 2
Present embodiment adopts Cr that target is deposited Cr at the SiC fiber surface
2O
3Film, the purity of Cr target is 99.99wt%, is of a size of 272 * 68 * 10mm.The negative electrode of middle frequency pulsed magnetron sputtering power supply 4 and target I 1 join, anode and target II2 join, between target I, the target II apart from 80mm, at magnetic control the target ectonexine is provided with permanent magnet, the magneticstrength of internal layer permanent magnet is that the magneticstrength of the outer permanent magnet of 2800 gaussian sums is 3800 Gausses.Continuous SiC fiber is wrapped in the cutting of workpiece pivoted frame 3 upper support bars, groove depth is 4 millimeters, puts into magnetron sputtering vacuum chamber 7, is evacuated to vacuum tightness and reaches 4 * 10
-3During Pa, feed bulk purity and be 99.999% sputter gas Ar gas and reactant gases O
2Gas to operating air pressure is 0.5Pa, Ar and O
2Throughput ratio is 1: 3, and the middle frequency pulsed magnetron sputtering power supply is started working, operating voltage 200V, working current 2.5A, dutycycle is 40%, the shielding power supply frequency setting is 80kHz, sputtering power is 500W, and sputtering time is 6h, and the speed of rotation of workpiece pivoted frame is 1 rev/min; In the present embodiment, in 4 work of middle frequency pulsed magnetron sputtering power supply, apply negative bias by 5 pairs of workpiece pivoted frames 3 of grid bias power supply, grid bias power supply 5 is the pulsed negative bias power supply, voltage 100V, and dutycycle is 10%, finally obtains the Cr that thickness is about 500nm
2O
3Film.The film even compact that obtains, no macrobead phenomenon, through XPS analysis as can be seen, the composition of film is Cr
2O
3
Embodiment 3
Present embodiment adopt Ti to target at SiC fiber surface depositing Ti O
2Film, the purity of Ti target is 99.99wt%, is of a size of 272 * 68 * 10mm.The negative electrode of middle frequency pulsed magnetron sputtering power supply 4 and target I1 join, anode and target II2 join, between target I, the target II apart from 180mm, at magnetic control the target ectonexine is provided with permanent magnet, the magneticstrength of internal layer permanent magnet is that the magneticstrength of the outer permanent magnet of 3500 gaussian sums is 5100 Gausses.Continuous SiC fiber is wrapped in the cutting of workpiece pivoted frame 3 upper support bars, groove depth is 0.5 millimeter, puts into magnetron sputtering vacuum chamber 7, is evacuated to vacuum tightness and reaches 2 * 10
-3During Pa, feed bulk purity and be 99.999% sputter gas Ar gas and reactant gases O
2Gas to operating air pressure is 0.2Pa, Ar and O
2Throughput ratio is 1: 7, and the middle frequency pulsed magnetron sputtering power supply is started working, operating voltage 80V, working current 5A, dutycycle is 20%, shielding power supply frequency setting frequency is 10kHz, sputtering power is 400W, and sputtering time is 10h, and the speed of rotation of workpiece pivoted frame is 10 rev/mins; In the present embodiment, in 4 work of middle frequency pulsed magnetron sputtering power supply, apply negative bias by 5 pairs of workpiece pivoted frames 3 of grid bias power supply, grid bias power supply 5 is the pulsed negative bias power supply, voltage 200V, and dutycycle is 30%.Finally obtain the TiO that thickness is about 800nm
2Film.The film even compact that obtains, no macrobead phenomenon, through XPS analysis as can be seen, the composition of film is TiO
2
Embodiment result shows, the present invention is by regulating the gas flow in the vacuum chamber in the magnetic control sputtering device, reactive gas species, sputtering time etc., can be implemented in the metal and the compound film of continuous SiC fiber surface deposition different sorts and different thickness, to reach the purpose of the SiC fiber being carried out surface modification.
Claims (10)
1. device at SiC fiber surface deposit film, it is characterized in that, this device is provided with target I, target II, workpiece pivoted frame, middle frequency pulsed magnetron sputtering power supply, magnetron sputtering vacuum chamber, the workpiece pivoted frame places magnetron sputtering vacuum chamber, target I, target II are staggered relatively in magnetron sputtering vacuum chamber inside and outside the workpiece pivoted frame, the negative electrode of middle frequency pulsed magnetron sputtering power supply and target I join, and the anode of middle frequency pulsed magnetron sputtering power supply and target II join.
2. according to the described device at SiC fiber surface deposit film of claim 1, it is characterized in that, heating rod is set in the magnetron sputtering vacuum chamber, magnetron sputtering vacuum chamber is provided with vacuum orifice, reaction gas inlet and sputter gas inlet.
3. according to the described device at SiC fiber surface deposit film of claim 1, it is characterized in that also be provided with grid bias power supply, the anode of grid bias power supply is connected with vacuum chamber, the negative electrode of grid bias power supply is connected with magnetron sputtering workpiece pivoted frame.
4. according to the described device of claim 1 at SiC fiber surface deposit film, it is characterized in that, target I, target II constitute nonequilibrium state magnetic field to target, nonequilibrium state magnetic field to target be set to a pair of or a pair of more than, between target I, the target II apart from 80mm～180mm.
5. according to the described device of claim 1 at SiC fiber surface deposit film, it is characterized in that, the workpiece pivoted frame comprises pallet under workpiece pivoted frame upper tray, the workpiece pivoted frame, has the support bar of cutting, the support bar that has cutting is connected with pallet under workpiece pivoted frame upper tray, the workpiece pivoted frame respectively, pallet is a disc under workpiece pivoted frame upper tray, the workpiece pivoted frame, the support bar that has cutting is along pallet circumference uniform distribution under workpiece pivoted frame upper tray, the workpiece pivoted frame, continuous SiC fiber is wrapped in the cutting of workpiece pivoted frame support bar, and groove depth is 0.5～4 millimeter.
6. according to the described device of claim 1 at SiC fiber surface deposit film, it is characterized in that, at magnetic control the target ectonexine is provided with permanent magnet, the magneticstrength of internal layer permanent magnet is that the magneticstrength of the outer permanent magnet of 2800～3500 gaussian sums is 3800～5100 Gausses.
7. according to the described device of claim 1 at SiC fiber surface deposit film, it is characterized in that target adopts pure metal targets: nickel target, titanium target, zinc target, chromium target, magnesium target, niobium target, tin target, aluminium target, iron target, zirconium target, copper target, silver-colored target, cobalt target, gold target, yttrium target, cerium target or molybdenum target.
8. according to the described method at SiC fiber surface deposit film of claim 1, it is characterized in that adopt the metal pair target at SiC fiber surface deposit film, the negative electrode of middle frequency pulsed magnetron sputtering power supply and target I join, anode and target II join; Continuous SiC fiber is wrapped on the workpiece pivoted frame, puts into magnetron sputtering vacuum chamber, be evacuated to vacuum tightness and reach (2～4) * 10
-3During Pa, feed sputter gas Ar gas and reactant gases O
2Gas to operating air pressure is 0.2～0.5Pa, Ar and O
2Throughput ratio is 1: (3～7), and the middle frequency pulsed magnetron sputtering power supply is started working, operating voltage 80～200V, working current 2～5A, dutycycle is 5～45%, and the shielding power supply frequency setting is 5～80kHz, and sputtering power is 400～500W, sputtering time is 0.5～10h, in the middle frequency pulsed magnetron sputtering power work, by grid bias power supply the workpiece pivoted frame is applied negative bias, voltage 100～200V, dutycycle is 10～45% final, obtains the film that thickness is 100～800nm.
9. according to the described method of claim 8 at SiC fiber surface deposit film, it is characterized in that, the rotation in the middle of two relative magnetron sputtering targets of workpiece pivoted frame is passed through, the speed of rotation of workpiece pivoted frame be 1～10 rev/min adjustable, the workpiece pivoted frame also has forward to be changeed/reverse rotating function.
10. according to the described method at SiC fiber surface deposit film of claim 8, it is characterized in that the middle frequency pulsed magnetron sputtering power supply adopts the holohedry bipolar square wave way of output, dutycycle is 5～45%, adjustable pulse-repetition scope 5～80kHz.
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