CN112578480A - Preparation method of multilayer film and multilayer film - Google Patents
Preparation method of multilayer film and multilayer film Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims description 11
- 239000000463 material Substances 0.000 claims abstract description 71
- 230000008021 deposition Effects 0.000 claims abstract description 63
- 238000000137 annealing Methods 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000010408 film Substances 0.000 claims description 192
- 238000000151 deposition Methods 0.000 claims description 65
- 230000007704 transition Effects 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- 239000012788 optical film Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000000758 substrate Substances 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
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- 239000011248 coating agent Substances 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 238000003384 imaging method Methods 0.000 description 1
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- G—PHYSICS
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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Abstract
本申请公开了一种多层膜的制备方法，通过将目标多层膜的材料厚度比例代入厚度应力关系式，得到所述目标多层膜在沉积温度时的沉积应力；将与所述目标多层膜的材料厚度比例相同的第一样品在第一温度下退火，并测量退火后的所述第一样品的应力；进行线性拟合得到温度应力关系式；其中，所述应力变化量为所述第一样品的应力与所述目标多层膜在沉积温度时的沉积应力的差值；通过所述温度应力关系式得到所述目标多层膜对应的目标退火温度；依据所述目标多层膜的材料厚度比例沉积多层膜，并在所述目标退火温度下对所述多层膜进行退火，得到所述目标多层膜。本申请减轻了计算量，操作简单，降低了生产成本。本申请还提供了一种具有上述有益效果的多层膜。
The present application discloses a method for preparing a multilayer film. By substituting the material thickness ratio of the target multilayer film into a thickness stress relationship, the deposition stress of the target multilayer film at the deposition temperature is obtained; The first samples with the same material thickness ratio of the layers are annealed at a first temperature, and the stress of the first sample after annealing is measured; a linear fitting is performed to obtain a temperature-stress relationship; wherein, the stress variation is the difference between the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature; the target annealing temperature corresponding to the target multilayer film is obtained through the temperature-stress relationship; Material thickness ratio of the target multilayer film Deposition of the multilayer film, and annealing the multilayer film at the target annealing temperature to obtain the target multilayer film. The application reduces the amount of calculation, the operation is simple, and the production cost is reduced. The present application also provides a multilayer film having the above-mentioned beneficial effects.
Description
Technical Field
The application relates to the field of film preparation, in particular to a preparation method of a multilayer film and the multilayer film.
Background
With the development of technology, more and more multilayer film materials are used in various fields, such as optical thin films capable of utilizing the interference effect of multilayer films to realize the function of selecting the required optical wavelength band. Generally, a multilayer film with a certain structure and material distribution is prepared on an optical substrate by a coating process.
In the deposition process of the film, the film has stress due to various reasons such as material growth defects, difference of thermal expansion coefficients of the substrate and the material, initial stress state and the like, and the film stretches or extrudes the substrate to deform the substrate. The surface shape change of the thin film device caused by the stress of the thin film material is different, and the thin film material is divided into tensile stress and compressive stress. Customarily, the former takes the positive sign and the latter takes the negative sign. However, both surface shape changes cause unnecessary aberration in the optical system, thereby affecting the imaging quality of the system. Therefore, the optical design often provides an index of surface shape for the optical coating. In addition, the high stresses can also lead to irreversible damage to the components. Under tensile stress, the film has a tendency to shrink, and when the tensile stress exceeds the elastic limit of the film, the film will crack, further causing the film to peel away from the substrate. In contrast, the compressive stress of the film causes the film to curl inward of the substrate, and further to crack, resulting in peeling of the film.
Therefore, in actual production, effective estimation of the stress of the multilayer film is a necessary process before film production, but the judgment of the influence of the process of improving the element surface shape by using the annealing process on the stress of the multilayer film is mainly based on experience, only qualitative deduction can be given, and quantitative analysis of the annealed stress is required, so that a large amount of simulation calculation is often needed, the time consumption is long, the cost is high, and the efficiency is low. In summary, finding a relatively simple, fast and efficient stress estimation method is an urgent problem to be solved by those skilled in the art.
Content of application
The application aims to provide a preparation method of a multilayer film and the multilayer film, so as to solve the problems that the multilayer film which is required to obtain the stress within the preset range in the prior art needs to be tested repeatedly, the cost is high, and the efficiency is low.
In order to solve the above technical problem, the present application provides a method for preparing a multilayer film, including:
substituting the material thickness proportion of the target multilayer film into a thickness stress relational expression to obtain the deposition stress of the target multilayer film at the deposition temperature; the thickness stress relation is a linear relation expression of the material thickness proportion and the stress of the target multilayer film;
annealing a first sample having the same material thickness ratio as the target multilayer film at a first temperature, and measuring the stress of the annealed first sample; the first temperature is higher than the deposition temperature of the target multilayer film and lower than the phase transition temperature of the target multilayer film;
establishing a coordinate system of annealing temperature and stress variation, introducing the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature, and performing linear fitting to obtain a temperature stress relational expression; wherein the stress variation is a difference between the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature;
obtaining a target annealing temperature corresponding to the target multilayer film through the temperature stress relational expression;
depositing a multilayer film according to the material thickness proportion of the target multilayer film, and annealing the multilayer film at the target annealing temperature to obtain the target multilayer film.
Optionally, in the method for manufacturing a multilayer film, the thickness stress relation is obtained by:
preparing a plurality of second samples of the same different material thickness ratio as the target multilayer film material, and measuring a first stress of the second samples after deposition;
and establishing a coordinate system of the material thickness proportion and the first stress, and substituting the data of the second samples for linear fitting to obtain the thickness stress relational expression.
Optionally, in the method of manufacturing a multilayer film, the number of the second samples is 2.
The present application also provides a multilayer film obtained by the production method of any one of the above multilayer films.
Optionally, in the multilayer film, the target multilayer film is an optical film.
Optionally, in the multilayer film, the target multilayer film is an antireflection film.
Optionally, in the multilayer film, the target multilayer film is a multilayer film in which a high refractive index material and a low refractive index material are alternately arranged.
Optionally, in the multilayer film, the target multilayer film is a multilayer film in which a silicon dioxide layer and a niobium pentoxide layer are alternately arranged.
According to the preparation method of the multilayer film, the deposition stress of the target multilayer film at the deposition temperature is obtained by substituting the material thickness proportion of the target multilayer film into a thickness stress relational expression; the thickness stress relation is a linear relation expression of the material thickness proportion and the stress of the target multilayer film; annealing a first sample having the same material thickness ratio as the target multilayer film at a first temperature, and measuring the stress of the annealed first sample; the first temperature is higher than the deposition temperature of the target multilayer film and lower than the phase transition temperature of the target multilayer film; establishing a coordinate system of annealing temperature and stress variation, introducing the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature, and performing linear fitting to obtain a temperature stress relational expression; wherein the stress variation is a difference between the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature; obtaining a target annealing temperature corresponding to the target multilayer film through the temperature stress relational expression; depositing a multilayer film according to the material thickness proportion of the target multilayer film, and annealing the multilayer film at the target annealing temperature to obtain the target multilayer film. This application utilizes multilayer film when deposition temperature to phase transition temperature, annealing temperature and multilayer film stress variation are the linear correlation's characteristics, the multilayer film sample of getting the same material thickness proportion carries out linear fitting under different annealing temperature stress variation and obtains stress variation-annealing temperature's two-dimensional image, can know the material of this material thickness proportion and carry out the stress after annealing at the arbitrary temperature of the within range of annealing temperature, the method that this application provided only needs to prepare a small amount of samples can estimate the stress value, compare in current other techniques, the calculated amount has been alleviateed greatly, the operation is simple, and the production cost is reduced. The application also provides a multilayer film with the beneficial effects.
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For a clearer explanation of the embodiments or technical solutions of the prior art of the present application, the drawings needed for the description of the embodiments or prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic flow diagram of one embodiment of a method for making a multilayer film provided herein;
FIG. 2 is a schematic flow diagram of one embodiment of a method for making a multilayer film provided herein;
fig. 3 is a schematic structural view of an embodiment of a multilayer film provided herein.
Detailed Description
In order that those skilled in the art will better understand the disclosure, the following detailed description will be given with reference to the accompanying drawings. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The core of the present application is to provide a method for preparing a multilayer film, wherein a flow diagram of one embodiment of the method is shown in fig. 1, which is referred to as a first embodiment, and the method comprises the following steps:
step S101: substituting the material thickness proportion of the target multilayer film into a thickness stress relational expression to obtain the deposition stress of the target multilayer film at the deposition temperature; the thickness stress relation is a linear relation expression of the material thickness proportion and the stress of the target multilayer film.
Step S102: annealing a first sample having the same material thickness ratio as the target multilayer film at a first temperature, and measuring the stress of the annealed first sample; the first temperature is greater than a deposition temperature of the target multilayer film and less than a phase transition temperature of the target multilayer film.
Step S103: establishing a coordinate system of annealing temperature and stress variation, introducing the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature, and performing linear fitting to obtain a temperature stress relational expression; wherein the stress variation is a difference between the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature.
Step S104: and obtaining the target annealing temperature corresponding to the target multilayer film through the temperature stress relational expression.
Step S105: depositing a multilayer film according to the material thickness proportion of the target multilayer film, and annealing the multilayer film at the target annealing temperature to obtain the target multilayer film.
The first temperature is any temperature between a deposition temperature of the target multilayer film and a phase transition temperature of the target multilayer film.
According to the preparation method of the multilayer film, the deposition stress of the target multilayer film at the deposition temperature is obtained by substituting the material thickness proportion of the target multilayer film into a thickness stress relational expression; the thickness stress relation is a linear relation expression of the material thickness proportion and the stress of the target multilayer film; annealing a first sample having the same material thickness ratio as the target multilayer film at a first temperature, and measuring the stress of the annealed first sample; the first temperature is higher than the deposition temperature of the target multilayer film and lower than the phase transition temperature of the target multilayer film; establishing a coordinate system of annealing temperature and stress variation, introducing the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature, and performing linear fitting to obtain a temperature stress relational expression; wherein the stress variation is a difference between the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature; obtaining a target annealing temperature corresponding to the target multilayer film through the temperature stress relational expression; depositing a multilayer film according to the material thickness proportion of the target multilayer film, and annealing the multilayer film at the target annealing temperature to obtain the target multilayer film. This application utilizes multilayer film when deposition temperature to phase transition temperature, annealing temperature and multilayer film stress variation are the linear correlation's characteristics, the multilayer film sample of getting the same material thickness proportion carries out linear fitting under different annealing temperature stress variation and obtains stress variation-annealing temperature's two-dimensional image, can know the material of this material thickness proportion and carry out the stress after annealing at the arbitrary temperature of the scope of annealing temperature, conveniently ask the annealing temperature range that the given stress range corresponds, the method that this application provided only needs to prepare a small amount of samples can estimate the stress value, compare in other prior art, the calculated amount has been alleviateed greatly, moreover, the steam generator is simple in operation, and production cost is reduced.
On the basis of the specific embodiment, a method for obtaining the thickness stress relational expression is further defined to obtain a second specific embodiment, a schematic flow chart of which is shown in fig. 2, and includes:
step S201, substituting the material thickness proportion of the target multilayer film into a thickness stress relational expression to obtain the deposition stress of the target multilayer film at the deposition temperature; the thickness stress relation is a linear relation expression of the material thickness proportion and the stress of the target multilayer film;
preparing a plurality of second samples with different material thickness ratios, which are the same as the target multilayer film material, and measuring the first stress of the second samples after deposition;
and establishing a coordinate system of the material thickness proportion and the first stress, and substituting the data of the second samples for linear fitting to obtain the thickness stress relational expression.
Still further, the number of the second samples is 2. Because the material thickness proportion is in linear relation with the first stress, a straight line in the graph can be determined by the two samples, the steps are further simplified, and the efficiency is improved.
Step S202: annealing a first sample having the same material thickness ratio as the target multilayer film at a first temperature, and measuring the stress of the annealed first sample; the first temperature is greater than a deposition temperature of the target multilayer film and less than a phase transition temperature of the target multilayer film.
Step S203: establishing a coordinate system of annealing temperature and stress variation, introducing the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature, and performing linear fitting to obtain a temperature stress relational expression; wherein the stress variation is a difference between the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature.
Step S204: and obtaining the target annealing temperature corresponding to the target multilayer film through the temperature stress relational expression.
Step S205: depositing a multilayer film according to the material thickness proportion of the target multilayer film, and annealing the multilayer film at the target annealing temperature to obtain the target multilayer film.
The difference between the present embodiment and the above embodiments is that the present embodiment specifically defines the origin of the thickness stress relationship, and the rest of the steps are the same as those of the above embodiments, and are not repeated herein.
By way of example, the following is derived from the formula for the preparation of the multilayer film provided herein:
it is known that film system stress in near ultraviolet, visible light, near infrared, infrared band and the like mainly comes from intrinsic stress of a thin film, and the stress at the interface between materials in the structure can be ignored, so that the stress of the multilayer film can be regarded as the superposition effect of the stress of each component layer:
σt＝Σσi(ti)ti
where i denotes the ith layer, σ denotes stress, and t denotes thickness.
Assuming again that the stress is independent of the film thickness, we can:
σt＝Σσiti＝ΣσHtH+ΣσLtL
σ＝(σH-σL)·r+σL＝kr+b
where subscript H represents a high refractive index material and subscript L represents a low refractive index material.
That is, the multilayer film stress σ is linear with the material ratio r. This linear relationship is temperature independent and therefore still applies after high temperature annealing.
At present, there is no formulaic summary result of the change relationship of the stress along with the annealing temperature, and other documents generally summarize in a qualitative description mode, but experimental results published in the documents all describe that the stress of the multilayer film changes monotonously along with the annealing temperature within a certain temperature range. Therefore, in this temperature range, the relationship between the amount of stress change of the multilayer film and the annealing temperature can be considered to be a linear relationship.
Δσ(r,T)＝KT+B
σ(r,T)-σ(r,150℃)＝KT+B
The above 150 ℃ represents the deposition temperature of the multilayer film in this example, and when other multilayer films are set, corresponding deposition temperatures are introduced, and the linear relationship obtained above is substituted to obtain the expression K, B (K, B, K, B are coefficients in the equation calculation process, and have no corresponding physical meanings):
the stress of the material in any material proportion and in a certain annealing temperature range can be estimated by the formula under the same process.
On the basis of the above-mentioned specific embodiment, the specific embodiment further utilizes a rule that the material thickness ratio of the multilayer film is linearly related to the stress of the annealed multilayer film within a certain temperature range, and the relationship between the material thickness ratio and the stress under a given material combination can be determined by preparing a plurality of (at least two) samples, so that the calculation amount is further reduced, the efficiency is improved, and the cost is reduced.
The present application further provides a multilayer film obtained by any one of the above methods for preparing a multilayer film, and a schematic structural diagram of an optical thin film according to a specific embodiment of the present application is shown in fig. 3, in which the optical unit layer includes a high refractive index unit layer and a low refractive index unit layer. According to the preparation method of the multilayer film, the deposition stress of the target multilayer film at the deposition temperature is obtained by substituting the material thickness proportion of the target multilayer film into a thickness stress relational expression; the thickness stress relation is a linear relation expression of the material thickness proportion and the stress of the target multilayer film; annealing a first sample having the same material thickness ratio as the target multilayer film at a first temperature, and measuring the stress of the annealed first sample; the first temperature is higher than the deposition temperature of the target multilayer film and lower than the phase transition temperature of the target multilayer film; establishing a coordinate system of annealing temperature and stress variation, introducing the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature, and performing linear fitting to obtain a temperature stress relational expression; wherein the stress variation is a difference between the stress of the first sample and the deposition stress of the target multilayer film at the deposition temperature; obtaining a target annealing temperature corresponding to the target multilayer film through the temperature stress relational expression; depositing a multilayer film according to the material thickness proportion of the target multilayer film, and annealing the multilayer film at the target annealing temperature to obtain the target multilayer film. This application utilizes multilayer film when deposition temperature to phase transition temperature, annealing temperature and multilayer film stress variation are the linear correlation's characteristics, the multilayer film sample of getting the same material thickness proportion carries out linear fitting under different annealing temperature stress variation and obtains stress variation-annealing temperature's two-dimensional image, can know the material of this material thickness proportion and carry out the stress after annealing at the arbitrary temperature of the within range of annealing temperature, the method that this application provided only needs to prepare a small amount of samples can estimate the stress value, compare in current other techniques, the calculated amount has been alleviateed greatly, the operation is simple, and the production cost is reduced.
In particular, the target multilayer film is an optical film; further, the target multilayer film is an antireflection film, and further, the target multilayer film is a multilayer film in which high refractive index materials and low refractive index materials are alternately arranged; specifically, the target multilayer film is a multilayer film in which a silicon dioxide layer and a niobium pentoxide layer are alternately arranged.
The embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same or similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
It is to be noted that, in the present specification, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The method for producing the multilayer film and the multilayer film provided by the present application are described in detail above. The principles and embodiments of the present application are explained herein using specific examples, which are provided only to help understand the method and the core idea of the present application. It should be noted that, for those skilled in the art, it is possible to make several improvements and modifications to the present application without departing from the principle of the present application, and such improvements and modifications also fall within the scope of the claims of the present application.
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