CN101560653A - Method for preparing gradient-index film - Google Patents
Method for preparing gradient-index film Download PDFInfo
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- CN101560653A CN101560653A CNA2009100987845A CN200910098784A CN101560653A CN 101560653 A CN101560653 A CN 101560653A CN A2009100987845 A CNA2009100987845 A CN A2009100987845A CN 200910098784 A CN200910098784 A CN 200910098784A CN 101560653 A CN101560653 A CN 101560653A
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Abstract
The invention discloses a method for preparing a gradient-index film. The method comprises the following steps: 1) putting a high-refractive-index material precursor and a low-refractive-index material precursor into a precursor reaction vessel respectively; 2) heating a substrate, performing vacuum pumping and turning on a coating machine; 3) depositing a low-refractive-index film; 4) depositing a high-refractive-index film; and 5) performing alternate deposition to form the gradient-index film. Compared with the prior art, the method has the following advantages that: 1) the method adopts an atomic-layer deposition technique and realizes sub-films different in refractive index by controlling the parameters of two material deposition processes; 2) the method adopts an alternate deposition mode, controls the number of cycles, and is simple in process control; 3) two film materials are a high-refractive-index film material and a low-refractive-index film material close in deposition temperature; 4) the refractive index of the deposited sub-films can be any value between a high refractive index and a low refractive index; and 5) the refractive-index sub-films are mixed films, and the refractive index can be controlled by controlling the deposition proportion of the two film materials alternately deposited.
Description
Technical field
The present invention relates to field of optical films, especially a kind of preparation method of gradient-index film.
Background technology
In field of optical films in order to realize the film structure of various requirement, usually require to have the coating materials of various specific refractory poweres, but it is very limited that occurring in nature can be used for the optics coating materials of optical thin film preparation, and, reason owing to humidity resistance and film hardness, the material that can be selective be used for the high quality rete still less, the present invention is by using technique for atomic layer deposition, use the height of various better performances, low two kinds of specific refractory power coating materials, adopt the method for alternating deposit, realize the material of different refractivity, by control of process condition, realize the size of different refractivity, and technology is simple, membranous layer stability is good, good reliability, specific refractory power is controlled, can regulate as required etc.
Gradient-index film, be called non-homogeneous film again, its principal character changes continuously for the normal direction specific refractory power along film surface, and specific refractory power remains unchanged on perpendicular to the horizontal direction of normal .... the traditional optical film is based on that the layered medium theoretical model designs, but, owing to have the interface, the jumping characteristic at interface and unstable thereof between the rete, make that some specific spectrum property is difficult to realize, and the interface between rete is the weak link that forms damage or performance degradation; But not uniform films had both been eliminated the interface between rete, had greatly increased the regulation and control degree of film system design again.
Though the research of gradient-index film starting early, but compare with uniform thin film, research be not a lot. its major cause is the complicated and difficult control of preparation process. in application, mainly be at present be used in antireflective coating, solar energy glass absorbing film, warble dielectric laser mirror and rugate spectral filter etc. the preparation method of non-uniform film can be divided into three major types: the one, multi-source steams method altogether; The 2nd, the reactive deposition method; The 3rd, the variation of deposition parameter (as depositing temperature, base reservoir temperature, air pressure) realizes change of refractive, but this only brings the minor alteration of specific refractory power. main research is that reactive deposition method and multi-source steam method altogether at present.
In the manufacturing of unicircuit, must deposition many pure and mixing material films have now been developed many technology and have been realized this class deposition.In recent years, the dominant technology of deposit film is ald (ALD) in this field, and its confirmation has excellent ability provides homogeneous smooth rete, and the uneven landform in plating through hole and the wafer well.ALD is called as a kind of method of atomic shell epitaxial at first, and its authoritative document is: Atomic Layer Epitaxy, and Blackie, Glasgo and London publishes (1990).
ALD is a kind of such method, and wherein the CVD method with routine is divided into two half-reaction steps, 4 steps of an ALD reaction cycle: (1) first kind of reaction precursor body enters reaction chamber and chemisorption at substrate surface in the mode of pulse; (2) treat that surface adsorption is saturated after, with rare gas element unnecessary reacting precursor purge is gone out reaction chamber; (3) then second kind of reaction precursor body enters reaction chamber in the mode of pulse, and reacts with last chemisorption precursor from the teeth outwards; (4) question response goes out reaction chamber with rare gas element with unnecessary reacting precursor and by product purge thereof after fully again.The basis of ALD film growth is to replace the reaction of saturated gas phase one solid phase surface, and after surface chemistry absorption was saturated, the quantity of surface reaction precursor increased no longer in time, and the film of therefore each cycling deposition all is a monoatomic layer.
Because ald (ALD) is a kind of surperficial control method, each cycle only deposits a monoatomic layer, and therefore sedimentary film thickness is that promptly thickness is along with the linearity of number of cycles increases by the supply cycle decision of reactant.
Adopt the rete as thin as a wafer of high low-refraction alternate combinations can be approximated to the middle refractive index film, as long as film thickness is more much smaller than reference wavelength, combined films just can be regarded successive as.Regulate the thickness proportion of two kinds of materials, just can synthesize the arbitrary refractive index between the high low-refraction.If the graded index rete is divided into a plurality of sublayers, make up with thin layer then and replace these sublayers, just can in very wide wavelength region, reach the effect of graded index.The outstanding advantage of ALD method is accurately to control the thickness of tunic as thin as a wafer, adopts this method just can realize the preparation of the graded index film that ordinary method is difficult to finish, as is used for chirped mirror that the very narrow thickness layer is arranged of femtosecond laser etc.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of gradient-index film is provided.
The preparation method of gradient-index film comprises the steps:
1) two kinds of low-index material reaction precursor bodies are put into the first reaction precursor body container and the 3rd reaction precursor body container of ald coating equipment, two kinds of high-index material reaction precursor bodies are put into the second reaction precursor body container and the 4th reaction precursor body container of ald coating equipment respectively;
2) substrate in the ald coating equipment is heated to 100 ℃～400 ℃, is evacuated to 0.1～1Torr, open the ald coating equipment;
3) the first valve P1 and the 3rd valve P3 of unlatching ald coating equipment feed the first reaction precursor body and the 3rd reaction precursor body respectively, and 1～100 circulation of deposition low-index film obtains the low refractive index film individual layer;
4) close the first valve P1 and the 3rd valve P3 of ald coating equipment, open the second valve P2 and the 4th valve P4 of ald coating equipment, feed the second reaction precursor body and the 4th reaction precursor body respectively, 1～100 circulation of deposition high refractive index layer obtains the high refractive index film individual layer;
5) high refractive index film individual layer and low refractive index film individual layer form the specific refractory power sublayer, and alternating deposit forms gradient-index film 10～100 times.
Described two kinds of high-index material presomas and two kinds of low-index material presomas are metal reactant and oxidizing gas; Metal reactant is titanium chloride or silicon chlorides, and oxidizing gas is water vapour, oxygen or ozone.Substrate is opticglass or semiconductor photoelectronic device chamber face.
The beneficial effect that the present invention compared with prior art has:
1) characteristics of the graded index rete technology of preparing of the present invention's proposition are: use technology is a technique for atomic layer deposition, realizes different refractivity film layers by two kinds of material deposition processes parameters of control deposition;
When 2) using technique for atomic layer deposition to prepare, the mode of employing is the mode of alternating deposit, and by the switching time of computer-controlled program by-pass valve control, technology controlling and process is simple;
3) two kinds of coating materials mentioning of the present invention are respectively the coating materials with high and low refractive index value, and their depositing temperature is close;
4) the thin-film refractive index size of the realization mentioned of the present invention can be the arbitrary refractive index value between the high and low refractive index;
5) the special specific refractory power individual layer mentioned of the present invention is a kind of mixing material rete, and the specific refractory power size can be by two kinds of coating materials deposition scale control of control alternating deposit.
Description of drawings
Fig. 1 is an ald coating equipment structural representation;
Fig. 2 is a process flow sheet of realizing the preparation method of gradient-index film.
Embodiment
The preparation method who realizes gradient-index film comprises the steps:
1) two kinds of low-index material reaction precursor bodies are put into the first reaction precursor body container and the 3rd reaction precursor body container of ald coating equipment, two kinds of high-index material reaction precursor bodies are put into the second reaction precursor body container and the 4th reaction precursor body container of ald coating equipment respectively;
2) substrate with the ald coating equipment is heated to 100 ℃～400 ℃, is evacuated to 0.1～1Torr, opens the ald coating equipment;
3) the first valve P1 and the 3rd valve P3 of unlatching ald coating equipment feed the first reaction precursor body and the 3rd reaction precursor body respectively, and 1～100 circulation of deposition low-index film obtains the low refractive index film individual layer;
4) close the first valve P1 and the 3rd valve P3 of ald coating equipment, open the second valve P2 and the 4th valve P4 of ald coating equipment, feed the second reaction precursor body and the 4th reaction precursor body respectively, 1～100 circulation of deposition high refractive index layer obtains the high refractive index film individual layer;
5) high refractive index film individual layer and low refractive index film individual layer form the specific refractory power sublayer, and alternating deposit forms gradient-index film 10～100 times.
Described two kinds of high-index material presomas and two kinds of low-index material presomas are metal reactant and oxidizing gas; Metal reactant is titanium chloride or silicon chlorides, and oxidizing gas is water vapour, oxygen or ozone.Substrate is opticglass or semiconductor photoelectronic device chamber face.
Below with reference to accompanying drawings the present invention is described in detail.
Fig. 1 is that the present invention utilizes ald (ALD) method to form the device synoptic diagram of gradient-index film.This device comprises: reaction chamber M1, and it can be heated by external heater; Pedestal M2, it is installed in the bottom of reaction chamber M1, so that support base M3, this substrate is a silicon base; Shower nozzle M4, be installed in pedestal M2 above so that reactant gases can be injected in the reaction chamber M1; One vacuum pump M5, M1 links to each other with reaction chamber, so that the pressure in the control reaction chamber M1.
Two separated gas inlet A link to each other with shower nozzle M4 with B.The first reaction precursor body, the second reaction precursor body, rare gas element, the 3rd reaction precursor body and the 4th reaction precursor physical efficiency are injected in the shower nozzle M4.The first and second reaction precursor bodies are metal reactants.Rare gas element is nitrogen or argon gas.The third and fourth reaction precursor body is the oxidizing gas that does not comprise oxyhydroxide, for example O
2, O
3Or water vapour.In Fig. 1, the third and fourth reaction precursor body is separated to place, but they also can be positioned in together.R1 and R3 are the first reaction precursor body container and the 3rd reaction precursor body container.R2 and R4 are the second reaction precursor body container and the 4th reaction precursor body container.
The first reaction precursor body and the second reaction precursor body and rare gas element are injected into reaction formula M1 by gas inlet A, and the 3rd reaction precursor body and the 4th reaction precursor body are injected into reaction chamber M1 by gas inlet B.The first reaction precursor body, the second reaction precursor body, the 3rd reaction precursor body and the 4th reaction precursor body inject by valve separately to be controlled, and has different gas inletes, reacts to each other in a gas inlet to prevent them.
Embodiment
Fig. 2 is the technical process of the method for realization graded index rete of the present invention, and is specific as follows:
Preparation graded index rete, its specific refractory power distributes according to certain rules, can be divided into a plurality of sublayers, makes up with thin layer then to replace these sublayers, just can reach the effect of graded index in very wide wavelength region.
Substrate is packed into after the reaction chamber M1, utilize well heater that the treatment temp of reaction chamber is maintained between 100 ℃ and 400 ℃, preferred situation is to maintain between 200 ℃ and 350 ℃, the pressure of reaction chamber maintain 0.1 and 1Torr between.In consecutive steps, keep this treatment temp and processing pressure, still, if necessary, also can change temperature and pressure, for different process different deposition parameters is arranged.
By opening the first valve P1, keep treatment temp and pressure simultaneously, inject the first reaction precursor body by gas inlet A and shower nozzle M4 to reaction chamber M1, this example is silicon tetrachloride (SiCl
4), the injection length sufficiently long, for example 1ms to 10ms makes it cover the surface of substrate.Like this, the first reaction precursor body just by chemisorption in substrate.
By opening the 3rd valve P3, keep treatment temp and pressure simultaneously, utilize inert gas purge reaction chamber 0.01s to 0.1s, this example is a nitrogen.Like this, remove remaining first reaction precursor body and the by product thereof.
By opening the 4th valve P4, keep treatment temp and pressure simultaneously, inject the 3rd reaction precursor body by shower nozzle to reaction chamber, this example is H
2O.The first reaction precursor body is formed the atom tunic of metal-oxygen by chemical exchange.
Utilize inert gas purge reaction chamber 0.01s to 0.1s.Like this, remove residual reaction presoma and by product thereof, keep treatment temp and pressure simultaneously.
So just finished a circulation, formed low-index material on the matrix by being reflected between the first reaction precursor body and the 3rd reaction precursor body, this example is SiO
2Rete, thickness is between 0.1A and 0.4A.
SiCl
4+2H
2O＝SiO
2+4HCl (1)
Periodically repeat to inject the first reaction precursor body step to the second and purge reaction chamber step, cycle number N
SiO2By computer control, just can reach the pre-determined thickness of low-index material.
By opening the second valve P2, keep treatment temp and pressure simultaneously, inject the second reaction precursor body by shower nozzle to reaction chamber, this example is TiCl
4, the injection length sufficiently long, for example 1ms to 10ms makes it cover the surface of substrate.Like this, the second reaction precursor body just by chemisorption in substrate.
Utilize inert gas purge reaction chamber 0.01s to 0.1s.Like this, remove residual reaction presoma and by product thereof, keep treatment temp and pressure simultaneously.
By opening the 5th valve P5, keep treatment temp and pressure simultaneously, inject the 4th reaction precursor body by shower nozzle to reaction chamber, this example is H
2O.The 3rd reaction precursor body is formed the atom tunic of metal-oxygen by chemical exchange.
Utilize inert gas purge reaction chamber 0.01s to 0.1s.Like this, remove residual reaction presoma and by product thereof, keep treatment temp and pressure simultaneously.
So just finished a circulation, formed high-index material on the matrix by being reflected between the second reaction precursor body and the 4th reaction precursor body, this example is TiO
2Rete, thickness is between 0.2A and 0.5A.
TiCl
4+2H
2O＝TiO
2+4HCl (2)
Periodically repeat to inject the second reaction precursor body step to the four and purge reaction chamber step, cycle number N
TiO2By computer control, just can reach the pre-determined thickness of high-index material.
Like this, adopt the rete as thin as a wafer of two kinds of specific refractory power alternating deposits of height to be similar to the middle refractive index film, wherein the very thin films layer thickness is more much smaller than reference wavelength, and combined films can be regarded successive as.The specific refractory power of this deposited seed layer is by the thickness proportion decision of regulating two kinds of materials.By computer control, repeated deposition high and low refractive index rete step is controlled two kinds of material thickness ratios like this, and the specific refractory power that obtains setting is finished a plurality of sublayers as thin as a wafer, realizes the preparation of gradient-index film.
Claims (3)
1. the preparation method of a gradient-index film is characterized in that comprising the steps:
1) two kinds of low-index material reaction precursor bodies are put into the first reaction precursor body container and the 3rd reaction precursor body container of ald coating equipment, two kinds of high-index material reaction precursor bodies are put into the second reaction precursor body container and the 4th reaction precursor body container of ald coating equipment respectively;
2) substrate in the ald coating equipment is heated to 100 ℃～400 ℃, is evacuated to 0.1～1Torr, open the ald coating equipment;
3) the first valve P1 and the 3rd valve P3 of unlatching ald coating equipment feed the first reaction precursor body and the 3rd reaction precursor body respectively, and 1～100 circulation of deposition low-index film obtains the low refractive index film individual layer;
4) close the first valve P1 and the 3rd valve P3 of ald coating equipment, open the second valve P2 and the 4th valve P4 of ald coating equipment, feed the second reaction precursor body and the 4th reaction precursor body respectively, 1～100 circulation of deposition high refractive index layer obtains the high refractive index film individual layer;
5) high refractive index film individual layer and low refractive index film individual layer form the specific refractory power sublayer, and alternating deposit forms gradient-index film 10～100 times.
2. the making method of a kind of graded index rete according to claim 1 is characterized in that, described two kinds of high-index material presomas and two kinds of low-index material presomas are metal reactant and oxidizing gas; Metal reactant is titanium chloride or silicon chlorides, and oxidizing gas is water vapour, oxygen or ozone.
3. the making method of a kind of graded index rete according to claim 1 is characterized in that, described substrate is opticglass or semiconductor photoelectronic device chamber face.
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| CN102910835A (en) * | 2012-10-25 | 2013-02-06 | 中国科学院宁波材料技术与工程研究所 | Method for forming durable dual-layer antireflection film on surface of soda-lime glass |
| CN103635838A (en) * | 2011-06-24 | 2014-03-12 | 柯尼卡美能达株式会社 | Optical reflective film |
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| CN103635838A (en) * | 2011-06-24 | 2014-03-12 | 柯尼卡美能达株式会社 | Optical reflective film |
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| CN103773083B (en) * | 2012-10-18 | 2015-04-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Optical interference color change pigment and its preparation method and application |
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| KR20210053809A (en) * | 2019-11-01 | 2021-05-12 | 항저우 엠디케이 옵토 일렉트로닉스 컴퍼니 리미티드 | ALD manufacturing method for reducing dot defects in camera modules and products thereof |
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| JP7390296B2 (en) | 2019-11-01 | 2023-12-01 | 杭州美迪凱光電科技股▲分▼有限公司 | ALD manufacturing method and its product to eliminate particle defects in imaging module |
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Open date: 20091021 |