CN101074477B - Method for coating silicon nitride film in vacuum - Google Patents
Method for coating silicon nitride film in vacuum Download PDFInfo
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- CN101074477B CN101074477B CN200710101779.6A CN200710101779A CN101074477B CN 101074477 B CN101074477 B CN 101074477B CN 200710101779 A CN200710101779 A CN 200710101779A CN 101074477 B CN101074477 B CN 101074477B
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Abstract
Method for coating silicon nitride film in vacuum and its implementation case involving coating silicon nitride film field, and it can be used for encapsulating film OLED structure (organic luminescence diode) in vacuum. According to the first implementation, to feed working gas mixture: nitrogen and argon to vacuum box so as to form ion beam from at least a ion source; directional ion beam sputter silicon target, and to layered deposit on the substrate through scanning the surface sputtering material of the substrate, and to move relative to the substrate ion beam source; moreover, during each cycle of relative motion of the ion source and target, forming at least one layer which width is 2-10 nm and importing nitrogen to the mixture of the working gas. The method for protecting and its implementation case maintain the high sealed degree of the film structure and improve the density of the film, and reduce the hole ratio of the film and its inside stress, reduce the substrate temperature during the process of coating film on the substrate surface, which insure the high quality of the film coated.
Description
Technical field
The present invention relates to the field of coating silicon nitride film, and can be used for packaging film OLED structure (Organic Light Emitting Diode) in a vacuum.
Background technology
Become known for the device of applying coating in a vacuum, wherein by plasma treatment substrate surface, form coating thereon, and be combined with the ion beam source [1] of the difference in functionality that oriented energy stream is provided.
But, because the dissimilar ion beam source using in device operates under different conditions, structure and the phase composite of the coating conventionally forming are different, it is highly bonding quite complicated that this guarantees each layer of mutual coupling, so can not utilize in practice known devices to guarantee coated with multiple layer coating on substrate.In this case, thus because need to guarantee that the particular job condition in the source that each is independent has spent a large amount of time, so the productivity that applying coating is processed sharply reduces.
In addition, use the energy source of difference in functionality in known devices not allow deposited coatings on large-sized substrate.
The method of another kind of known applying coating is included in vacuum sputtering material and settling thereof on the surface of article, and wherein the surface of article is flowed and cleaned in advance and activate by inert gas ion.
In this case, clean, activated surface thereon deposition material, in the processing volume of vacuum chamber, keep residue invariablenes pressure of liquid simultaneously, and deposit sputter material to obtain a plurality of coatings by continuous sputtering target, wherein at least one target is made of metal, by pottery, made for one, sputter ceramic target at least 15 minutes is to form independent layer [2].
Approaching most of the present invention is vacuum module, in the specification sheets that uses this module, is not directly disclosed in the method for applying coating on substrate.
The method of applying coating on substrate has been described when explaining vacuum module operation, substrate is immovably arranged in vacuum chamber, be fed to wherein working gas mixture, the ion beam sputtering silicon target that use forms from ion source, when carrying out ion source and silicon target with respect to the relative movement of substrate, by scanning substrate surface with sputter material, sputter material stratified sedimentation is [3] to the surface of substrate.
But the method and apparatus known to technology [2,3] has serious common disadvantage:
The film being obtained by aforesaid method has following shortcoming:
-density is low;
-porosity is high, so film can not provide sufficient sealing, especially when the thickness of film is during at 0.1-0.3 μ m;
-internal stress is high;
If coating silicon nitride film on substrate, all these shortcomings manifest in can be on a large scale.
Above-mentioned shortcoming causes film cracking and distortion, and has reduced the sticking power of its sticking power (binding property of interlayer) and basal layer and metallic surface.If coating silicon nitride film on elastomeric polymer, as produced OLED structure, polymer breakage also comes off from basal layer or substrate.
In addition, the process of coating silicon nitride film is accompanied by the significantly rising of underlayer temperature in many cases, up to 150-200 ℃ (423-473K), this functional element that wrapper is contained to fusible (to temperature sensitive) material is definitely unallowable.
Summary of the invention
Target of the present invention is to eliminate above-mentioned shortcoming, guarantee the stopping property of membrane structure, improve density of film, reduce the porosity of film and internal stress wherein, be reduced in substrate temperature in the process of substrate surface deposit film coating, and the high quality of guaranteeing coating.
By the method for coating silicon nitride film in a vacuum, realized the target of setting, wherein substrate is placed in work box regularly, to work box, be fed to working gas mixture: nitrogen and argon gas, from at least one ion source, form ionic fluid, by directed ion beam sputter silicon target, and by scanning substrate surface sputter material stratified sedimentation to substrate; And ion beam source and target are done relative movement with respect to substrate jointly; According to first embodiment of the method, each circulation at ion beam source with respect to the relative movement of substrate, forms thickness at least one deck in 2-10 nanometer range; And introduced helium in the mixture of working gas.
When implementing the method, in working gas mixture, the concentration of helium remains in the scope of 2-20%, and sputter material stream is given long linear; In this case, the sweep amplitude of sputter material stream and the length of linear portion surpass each linear dimension of substrate, and the operating pressure in the process raising middle flask of deposit film is no more than 10
-1handkerchief.
According to the second embodiment of the implementation method of coating silicon nitride film in a vacuum, substrate is placed in work box regularly, to work box, be fed to the mixture of working gas: nitrogen and argon gas, from at least two ion sources, form ionic fluid, by directed ion beam sputter silicon target, sputter material stratified sedimentation is to the surface of substrate, ion beam source and target are installed regularly with respect to the surface of substrate jointly, with pulse mode sputtering target, the interval between a last and rear pulse is at least 0.1 second by this way; In this case, in a pulse, form thickness at least one deck in 2-10 nanometer range, and introduce helium in working gas mixture.
As the first embodiment, in working gas mixture, the concentration of helium maintains in the scope of 2-20%, and the operating pressure in the process raising middle flask of deposit film is no more than 10
-1handkerchief.
Yet, can fixedly mount rotatably ion beam source around its axle.
Implement as follows the first embodiment of the method for coating silicon nitride film in a vacuum.
In vacuum chamber, be fixed for substrate and silicon target and one or more ion beam source of coated film, wherein during implementation process, pressure should not surpass 10
-1handkerchief.Substrate should maintain static, and with respect to pending substrate surface can carry out relative movement fixedly silicon target and one or more ion beam source.
With backward vacuum chamber, be fed to the mixture (nitrogen, argon gas and helium) of working gas, utilize one or more ion beam sources to form ionic fluid.Vacuum chamber can hold several ion sources, and in mixture, working gas content ratio is, for example, and nitrogen: argon gas: helium=70%: 20%: 10%.
By the ion beam sputtering silicon target obtaining from least one or more ion beam source.By scanning the surface of substrate during the relative movement with respect to substrate surface at ion beam source and target, the layers of material that sputtering target obtains is deposited on the substrate surface that needs to process, each cycle period with respect to the relative movement of substrate at ion beam source and target, is the film of 2-10 nanometer by forming a layer thickness by this way.
In implementing the process of the method, in working gas mixture, the concentration of helium maintains in the scope of 2-20%, and sputter material stream is given long linear; In this case, the sweep amplitude of sputter material stream and the length of linear portion surpass each linear dimension of substrate.
At ion beam source and silicon target, during the relative movement with respect to substrate surface, by the surface with sputter material scanning substrate, at fixed substrate surface higher slice deposition sputter material, can make the film of the desired thickness of generation there is low porosity.
One of reason that causes hole be before coated film and during the microdefect (hole, projection and particulate) that occurs on substrate surface.
Under constant mode of deposition, for example, when ion source () and target maintain static, and when sputter material stream deposits to substrate surface with the angle of constant (constant), the hole that field at micro-defect produces connects, therefore and grow into the outside surface of film, reduced the density of film and damaged the sealing characteristics of film.
If ion beam source and target are done relative movement with respect to the surface of substrate, sputter material deposits on the surface of substrate, each circulation with respect to the relative movement of substrate surface at ion beam source and target by this way, starts the thickness of every one deck subsequently in the scope of 2-10 nanometer from the first layer.
By this way, on the time, form discontinuously every one deck.
Within the timed interval, when there is no deposition of material on substrate time, on the thin film layer having deposited, absorb, diffusion and relaxation processes.These processing have improved the stoichiometry of film composition, have consolidated layer structure, and have reduced the internal stress grade of film.
In atom level, the layer thickness of 2-10 nanometer is corresponding to tens monoatomic layers, because the particle energy in ion beam sputtering process is very large, so be deposited on the atom of substrate surface, there is high mobility, thereby impel hole and the tiny crack occurring in the single lipostrat of effective sealing.
At ion beam source and target, during the relative movement with respect to substrate, according to the hole on sealing substrate surface and the degree of microdefect (hole, projection and particulate), change the angle of deposited coatings on substrate.
In addition,, even when atom level only applies one deck, due to the deposition of sputter material, also improved the degree of storage pore and microdefect.
The film being in this way deposited on substrate has high amorphous degree and low-crystallinity, thereby has improved the density of film and reduced the porosity of film.
Within the timed interval of the every thin film of deposition, on the surface of film, carry out the absorption of working gas atom and process.These atoms have not only been filled the interatomic hole forming in thin film layer, and prevent the further growth of crystal structure.
Therefore, the absorption of carrying out on the surface of each thin film layer is processed, and between the crystallite running through by inhibition, being formed with of passage helps the inhibition that crystal is grown, and between the crystallite running through, passage is potential perforation hole.
Because a large amount of crystal starts to form at the thickness of 2-10 nanometer, if the thickness of every one deck of deposition is within the scope of these, the most effective in lip-deep absorption processing and the crystal growth-inhibiting of deposit film.
In addition, due at substrate surface higher slice deposition material, wherein at ion beam source and target, with respect to each circulation of the relative movement of substrate, forming thickness is the thin film layer of 2-10 nanometer, is more conducive to the chance of heat radiation and does not reduce deposition intensity.
When reaching required film thickness,, during Multiple-Scan substrate surface, due to discontinuity, this processing becomes subzero treatment, and has this processing of highdensity feature and prevent that substrate surface is overheated owing to being deposited on the film of substrate surface.
Because the linear dimension of helium atom is little more a lot of than Siliciumatom and nitrogen-atoms, and when introducing helium atom in silicon nitride structure, reduced the internal stress level in film, so introduce helium in the component of working gas, can reduce internal stress 2.5-3 times in silicon nitride film.
During thin film deposition, sputter material stream is given long linear, and this can guarantee that the thickness at whole substrate surface upper film is uniform.
Realize this point and also due to the sweep amplitude of sputter material stream and the length of linear portion, surpass each linear dimension of substrate, its homogeneity of having eliminated sputter material stream in the size of pending substrate surface depends on the final condition over sputter material stream profile.
Due to technical progress of the present invention, if the concentration that can affirm helium in working gas mixture by experiment lower than 2%, the internal stress in film will be quite large.
If the concentration of helium surpasses 20% in working gas mixture, stress can further not reduce, and film deposition rate on substrate surface can decline.
Therefore the optimum percentage range that has been determined by experiment helium in working gas mixture is 2-20%.
The internal stress that this scope has been guaranteed to be deposited in the film on substrate surface is minimum, and this has improved the quality of applying coating undoubtedly.
Optimum pressure in vacuum chamber guarantees to be deposited on the essential quality of the film on substrate, and it is also determined by experiment.
According to test, the pressure in vacuum chamber should not surpass 10
-1handkerchief.
Pressure surpasses 10
-1during handkerchief, the phenomenon that is called thermalization of deposition flow stream becomes very strong.This is the possibility increase due to sputtered atom in the drift space between target and substrate and working gas atomic collision, and the energy of the stream condensing sharply declines, thereby has greatly affected the density of coating.
In addition the saturation ratio that, has a silicon nitride film of working gas (nitrogen and argon gas) atom is also improved.Above-mentioned every bit has all caused film porosity to raise, and density reduces, and the internal stress in film increases, and has therefore reduced the quality that is deposited on the coating on substrate.
According to the second embodiment of implementation method, be different from the first embodiment, target and ion beam source (for example, single ion beam source) are placed in vacuum chamber regularly with respect to the substrate of fixed placement, guarantee layered coated coating in this case by pulse mode sputtering target.
In this case, for example the thickness range of the individual layer of a monopulse formation is in 2-10 nanometer, and the timed interval between a last and rear pulse is at least 0.1 second.
Therefore, in each pulse, form thickness corresponding to the layer of tens monoatomic layers of atom level.
Because the energy of particle in ion beam sputtering process is enough high, the atom that is deposited on the sputter material on substrate surface has high mobility, thus hole and microdefect that in single lipostrat, sealing occurs effectively.
In the timed interval without material, on the thin film layer of deposition, absorb, diffusion and relaxation processes, thereby improve the stoichiometry of film composition, consolidate a layer structure, and reduce the internal stress grade of film.
As the first situation, the deposit film obtaining with which has high amorphous degree and low-crystallinity, thereby has improved the density of film, has reduced porosity.
According to the timed interval between practical study strobe pulse.The time of having determined between pulse 0.1 second by test guarantees to obtain high-quality intensive film.Increasing this time can significantly not improve the quality of film, but can affect the production efficiency of processing, and productivity can reduce.
As the first embodiment, because the linear dimension of helium atom is little more a lot of than the linear dimension of silicon and nitrogen-atoms, and can reduce the internal stress in film while introducing helium atom in silicon nitride structure, so in the component of working gas, inject internal stress 2.5-3 that helium can reduce silicon nitride film doubly.
Therefore, being determined by experiment the optimum percentage range of helium in working gas mixture is 2-20%.
As the first embodiment, be determined by experiment the pressure in vacuum chamber in implementation method the second embodiment and should do not surpass 10
-1handkerchief.
In addition, around the ion beam source of its axle rotation can: the first, guarantee more completely to utilize target material; The second, the pattern of change material deposition during coating procedure; The 3rd, the more uniform film of coating thickness and porosity; The 4th, improve the productivity of processing.
Accompanying drawing explanation
Fig. 1 is according to the schematic diagram of the method for the coating silicon nitride film in a vacuum of first embodiment of the invention.
The layout of Fig. 2 for mutually locating according to the substrate of first embodiment of the invention, target and ion beam source.
Fig. 3 is according to the schematic diagram of the method for the coating silicon nitride film in a vacuum of second embodiment of the invention.
Fig. 4 is the layout that substrate, target and the ion beam source according to second embodiment of the invention located mutually.
Embodiment
The concrete enforcement of the first embodiment
Be fixed on and on substrate support 3, be of a size of the substrate 2 of 200 * 200 millimeters and be placed on regularly in vacuum chamber 1, as shown in Figure 1.Ion beam source (being 1 in this example) 4 and target 5 can be movable relatively and are placed in same vacuum chamber with respect to pending substrate surface.Utilize vacuum pump to deflate from vacuum chamber 1, residue pressure drops to 5 * 10
-4handkerchief.
With the mixture (argon gas and nitrogen) that is fed to working gas in backward vacuum chamber 1, and inject helium, make the per-cent of helium in working gas mixture in the scope of 2-20%, be not less than 2% and be not more than 20%.In the specific embodiment of the method, in mixture, the per-cent of working gas is 90% (nitrogen 70%, argon gas 20%), and the per-cent of helium is 10%.
Now the total pressure in case is adjusted into 8 * 10
-2handkerchief.
To the anode of ion beam source 4, apply the positive potential of 4.0 kilovolts; Igniting electric discharge subsequently, wherein forming total current is 450 milliamperes of ionic fluids that point to target 5.Due to sputtering target 5, formed silicon nitride (Si
3n
4) stream.Then open scanning system, carry out ion source 4 and the common relative movement with respect to substrate 2 of target 5, substrate 2 is placed in vacuum chamber 1 jointly with substrate support 3.
Set the value of sweep velocity, thus can be to the layer of substrates coated 3 nanometer thickness during ion beam source 4 and target 5 are with respect to the single loop of the relative movement of substrate 2.In order to apply the film of 180 nanometer thickness, with respect to substrate 2 treatment unit, need to carry out 60 scan cycle.When complete on substrate 2 thin film deposition process time, ion beam source 4 is closed and is stopped being fed to working gas in vacuum chamber.To finishing dealing with of the surface-coated coating of substrate 2.
Therefore, the stress levels that is deposited on the silicon nitride film on substrate according to the first embodiment is low to moderate 383 MPas, and realizing this point is by the per-cent with respect to helium, to optimize the component of gaseous mixture.
Even at the thickness that surpasses 0.3 micron, film can resistance to fracture and is peeled off.
Meanwhile, use standard technique and the internal stress of the silicon nitride film that do not obtain to introducing helium in mixing gas component is 934 MPas, and easily break and from substrate desquamation at the thickness that surpasses 0.07 micron.
According to the first embodiment of this implementation method, the layout that substrate, target and ion beam source are located mutually as shown in Figure 2.
Be fixed on and on substrate support 3, be of a size of the substrate 2 of 620 * 375 millimeters and be placed on regularly in vacuum chamber 1.Ion beam source 4 (being in this case 1) and target 5 can be movable relatively with respect to pending substrate surface, and are placed in vacuum chamber with 45-60 degree angle.Utilize vacuum pump to deflate from vacuum chamber 1, residue pressure drops to 5 * 10
-4handkerchief.
With the mixture (argon gas and nitrogen) that is fed to working gas in backward vacuum chamber 1, and inject helium, make the per-cent of helium in working gas mixture in the scope of 2-20%, be not less than 2% and be not more than 20%.
In the specific embodiment of the method, in mixture, the per-cent of working gas is 85% (nitrogen 75%, argon gas 10%), and the per-cent of helium is 15%.
Now the total pressure in case 1 is adjusted into 7.5 * 10
-2handkerchief.
To the anode of ion beam source 4, apply the positive potential of 4.5 kilovolts; Igniting electric discharge subsequently, wherein forming total current is 550 milliamperes of ionic fluids that point to target 5.Due to sputtering target 5, formed silicon nitride (Si
3n
4) stream.Then open scanning system, carry out ion source 4 and the common relative movement with respect to substrate 2 of target 5.
Set the value of sweep velocity, thereby at ion beam source 4 and target 5 during the single loop with respect to the relative movement of substrate 2, can be to the layer of substrates coated 4.5 nanometer thickness.In order to apply the film of 225 nanometer thickness, with respect to substrate 2 treatment unit, need to carry out 50 scan cycle.When complete on substrate 2 thin film deposition process time, ion beam source 4 is closed and is stopped being fed to working gas in vacuum chamber 1.To finishing dealing with of the surface-coated coating of substrate.
The stress levels that is deposited on the silicon nitride film on substrate according to this embodiment is low to moderate 315 MPas, and realizing this point is to optimize the component of gaseous mixture and the low pressure of working gas by the per-cent with respect to helium.
The concrete enforcement of the second embodiment
Be fixed on and on substrate support 3, be of a size of the substrate 2 of 200 * 200 millimeters and be placed on regularly in vacuum chamber 1.Target 5 and two can be around the ion beam sources 4 and 4 of its axle rotation ' be placed in same case.With synchronizing pulse mode operate ion beam source 4 and 4 ', to be spaced apart at least 0.1 second between the last and rear pulse of which.Layering obtains the film of desired thickness, is similar to according to the method for the first embodiment, as shown in Figure 3.
Utilize vacuum pump to deflate from vacuum chamber 1, residue pressure drops to 4.5 * 10
-4handkerchief.
Mixture (argon gas and nitrogen) to being fed to working gas in vacuum chamber 1, wherein also injects helium.In working gas mixture, the per-cent of helium should be in the scope of 2-20%, is not less than 2% and be not more than 20%.In the specific embodiment of present method, in mixture, the per-cent of working gas is 92% (nitrogen 75%, argon gas 17%), and the per-cent of helium is 8%.
Now the total pressure in case 1 is adjusted into 6.5 * 10
-2handkerchief.
To ion beam source 4 and 4 ' anode apply the positive potential of 5.0 kilovolts; Igniting electric discharge subsequently, wherein forming total current is 950 milliamperes of ionic fluids that point to silicon target 5.
Due to sputtering target 5, formed silicon nitride (Si
3n
4) stream.
Set ion beam source 4 and 4 ' the time value of pulse persistance operation, therebetween sputtering target 5 and on the surface of substrate cvd nitride silicon film, thereby during individual pulse, apply the layer of 5 nanometer thickness.
In order to apply the film of 200 nanometer thickness on the surface at substrate 2, with 40 pulses of recurrent interval generation of 0.2 second.In this interval, film is relaxed and desorption processing.These processing can obtain intensive imporous silicon nitride film, and film internal stress grade is low.
When thin film deposition process completes, ion beam source 4 and 4 ' close and stop being fed to working gas in vacuum chamber 1.To finishing dealing with of substrate 2 applying coatings.
The stress levels of the silicon nitride film obtaining on substrate surface according to the second embodiment is low to moderate 395 MPas, realizes this point and be the component of optimizing gaseous mixture by the per-cent with respect to helium, and thickness surpass the film of 0.3 micron can resistance to fracture and peel off.
Fig. 4 is the layout of mutually locating according to this implementation method second embodiment substrate, target and ion beam source.
Be fixed on and on substrate support 3, be of a size of the substrate 2 of 620 * 375 millimeters and be placed on regularly in vacuum chamber 1.Target 5 and four can around the ion beam source 4,4 of its axle rotation ', 4 " and 4 ' " are arranged in same case.With synchronizing pulse mode operate ion beam source 4,4 ', 4 " and 4 ' ", with which, can obtain discontinuously the layered film of desired thickness, be similar to according to the method for the first embodiment.
Utilize vacuum pump to deflate from vacuum chamber 1, residue pressure drops to 4.0 * 10
-4handkerchief.
In vacuum chamber 1, be fed to the mixture (argon gas and nitrogen) of working gas, and inject helium.In working gas mixture, the per-cent of helium should be in the scope of 2-20%, is not less than 2% and be not more than 20%.In the specific embodiment of present method, in mixture, the per-cent of working gas is 85% (nitrogen 70%, argon gas 15%), and the per-cent of helium is 15%.
Now the total pressure in vacuum chamber is adjusted into 8.5 * 10
-2handkerchief.
To ion beam source 4,4 ', the anode of 4 " and 4 " ' applies the positive potential of 5.2 kilovolts; Igniting electric discharge subsequently, wherein forming total current is 1850 milliamperes of ionic fluids that point to silicon target 5.
Due to sputtering target 5, formed silicon nitride (Si
3n
4) stream.
Set ion beam source 4,4 ', 4 " and 4 " ' the value in pulse duration, therebetween sputtering target 5 and on the surface of substrate 2 cvd nitride silicon film, thereby during individual pulse, apply the layer of 15 nanometer thickness.
In order to apply the film of 0.30 micron thickness on the surface at substrate 2, with the interval of 0.3 second, produce 20 pulses.In this interval, film is relaxed and desorption processing.These processing can obtain intensive imporous silicon nitride film, and film internal stress grade is low.
When thin film deposition process completes, ion beam source 4,4 ', 4 " and 4 " ' close and stop being fed to working gas in vacuum chamber 1.To finishing dealing with of substrates coated coating.
The stress levels of the silicon nitride film obtaining on the surface of substrate 2 according to the second embodiment is low to moderate 285 MPas, and realizing this point is by the per-cent with respect to helium, to optimize the component of gaseous mixture and the thickness of optimizing pulse sputtering mode and settled layer.
The method of coating silicon nitride film in a vacuum and the embodiment that propose can be applicable to industrial production, have guaranteed to be coated in the high quality of the coating on substrate, and the high productivity of processing.
Open source
1, No. 2095467th, Russ P; C23C is open on November 10th, 14/34,1997;
2, No. 2037563rd, Russ P; C23C 14/46, and 06 month 19 days nineteen ninety-five is open;
3, No. 003148th, Eurasian patent; C23C 14/54; 14/56; 14/34; Be disclosed in EAB20301.
Claims (8)
1. in a vacuum to the method for coating silicon nitride film on the substrate of fixed placement, wherein to the mixture that is fed to working gas in vacuum chamber: nitrogen and argon gas, from at least one ion source, form ionic fluid, by directed ion beam sputter silicon target, and the surface sputtering material stratified sedimentation that passes through scanning substrate is to substrate; And ion source and target are done relative movement with respect to substrate jointly, it is characterized in that each circulation with respect to the relative movement of substrate at ion source, form thickness at least one deck in 2-10 nanometer range, and introduce helium in the mixture of working gas.
2. method according to claim 1, is characterized in that the volume percent of helium in the mixture of working gas remains in the scope of 2-20%.
3. method according to claim 1 and 2, is characterized in that sputter material stream is given long linear; The sweep amplitude of sputter material stream and the length of linear portion surpass each linear dimension of substrate in this case.
4. method according to claim 3, is characterized in that the operating pressure in the process raising middle flask of deposit film is no more than 10
-1handkerchief.
5. in a vacuum to the method for cvd nitride silicon film on the substrate of fixed placement, wherein to the mixture that is fed to working gas in vacuum chamber: nitrogen and argon gas, from at least two ion sources, form ionic fluid, by directed ion beam sputter silicon target, and sputter material stratified sedimentation is to the surface of substrate, it is characterized in that ion source and target are jointly with respect to the surface fixed installation of substrate, with pulse mode sputtering target, to be spaced apart at least 0.1 second between the last and rear pulse of which; In a pulse, form in this case thickness at least one deck in 2-10 nanometer range, and introduce helium in the mixture of working gas.
6. method according to claim 5, is characterized in that the volume percent of helium in the mixture of working gas remains in the scope of 2-20%.
7. according to the method described in claim 5 or 6, it is characterized in that ion source being installed rotatably around its axle.
8. method according to claim 7, is characterized in that the operating pressure in the process raising middle flask of deposit film is no more than 10
-1handkerchief.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EA200601327A EA009303B1 (en) | 2006-05-15 | 2006-05-15 | Method of application of silicon nitride films under vacuum (embodiments) |
| EA200601327 | 2006-05-15 |
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| Publication Number | Publication Date |
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| CN101074477A CN101074477A (en) | 2007-11-21 |
| CN101074477B true CN101074477B (en) | 2014-10-01 |
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| CN200710101779.6A Expired - Fee Related CN101074477B (en) | 2006-05-15 | 2007-05-15 | Method for coating silicon nitride film in vacuum |
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| JP (1) | JP5079388B2 (en) |
| CN (1) | CN101074477B (en) |
| EA (1) | EA009303B1 (en) |
| TW (1) | TWI434350B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103147055A (en) * | 2013-03-04 | 2013-06-12 | 电子科技大学 | In-line multi-target magnetron sputtering coating device |
| CN104480428A (en) * | 2014-12-02 | 2015-04-01 | 中国航天科工集团第三研究院第八三五八研究所 | Method for regulating and controlling ion beam sputtered silicon dioxide optical membrane stress |
| CN106191770B (en) * | 2015-05-05 | 2019-03-01 | 中国科学院宁波材料技术与工程研究所 | Porous silicon nitride based sealing coating and the preparation method and application thereof |
| CN108441838B (en) * | 2018-03-21 | 2020-04-17 | 中国兵器科学研究院宁波分院 | Method for ion beam sputtering deposition of film on surface of medium-large diameter optical element |
| EP3591090A1 (en) * | 2018-07-05 | 2020-01-08 | Justus-Liebig-Universität Gießen | Method and device for sputter deposition coating of an object of arbitrary geometry |
| CN110983279B (en) * | 2019-11-21 | 2022-04-01 | 天津津航技术物理研究所 | Preparation method of high-hardness low-absorption silicon nitride film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1617947A (en) * | 2000-07-05 | 2005-05-18 | 伊佐瓦克有限责任公司 | Vacuum module (variants thereof) and system of modules for applying coatings to a substrate |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6462456A (en) * | 1987-08-29 | 1989-03-08 | Nissin Electric Co Ltd | Formation of thin silicon nitride film |
| JPH0222198A (en) * | 1988-07-12 | 1990-01-25 | Kyoto Semiconductor Kk | Production of single crystal |
| JPH06151421A (en) * | 1992-11-02 | 1994-05-31 | Nippon Telegr & Teleph Corp <Ntt> | Formation of silicon nitride thin film |
| RU2052538C1 (en) * | 1993-04-08 | 1996-01-20 | Сергей Николаевич Кучанов | Method for vacuum deposition of metallized coating on dielectric substrates |
| JP3627273B2 (en) * | 1994-02-21 | 2005-03-09 | 旭硝子株式会社 | Resin substrate with transparent conductive film and method for producing the same |
| JPH08127869A (en) * | 1994-10-27 | 1996-05-21 | Japan Aviation Electron Ind Ltd | Ion beam sputtering device |
| JPH11279756A (en) * | 1998-03-26 | 1999-10-12 | Okura Ind Co Ltd | Formation of transparent conductive film |
| JP2000293901A (en) * | 1999-04-02 | 2000-10-20 | Canon Inc | Information recording medium and its production |
| RU2204179C1 (en) * | 2002-08-19 | 2003-05-10 | Общество с ограниченной ответственностью "Агентство маркетинга научных разработок" | Method for shaping nanotopography on film surface |
| JPWO2006049022A1 (en) * | 2004-11-04 | 2008-05-29 | 旭硝子株式会社 | Ion beam sputtering apparatus and method for forming multilayer film of reflective mask blank for EUV lithography |
-
2006
- 2006-05-15 EA EA200601327A patent/EA009303B1/en not_active IP Right Cessation
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2007
- 2007-05-14 JP JP2007128090A patent/JP5079388B2/en not_active Expired - Fee Related
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1617947A (en) * | 2000-07-05 | 2005-05-18 | 伊佐瓦克有限责任公司 | Vacuum module (variants thereof) and system of modules for applying coatings to a substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI434350B (en) | 2014-04-11 |
| EA200601327A1 (en) | 2007-12-28 |
| JP5079388B2 (en) | 2012-11-21 |
| TW200845217A (en) | 2008-11-16 |
| JP2007308799A (en) | 2007-11-29 |
| EA009303B1 (en) | 2007-12-28 |
| CN101074477A (en) | 2007-11-21 |
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