CN104862784B - A kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion - Google Patents
A kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion Download PDFInfo
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Abstract
The invention discloses a kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion, this method includes：The surface of original substrate is injected ions into by ion implantation, so as to form film layer, separating layer and remaining matter layer in original substrate；Make the thin film layer of target base plate and original substrate, and then original substrate and target base plate are bonded together using bonding chip method, to form bonding body；Para-linkage body is heated so that film layer and the separation of remaining matter layer；After film layer and the separation of remaining matter layer, film layer is heated with 200 DEG C~700 DEG C of temperature in the predetermined container equipped with diffusant, wherein, diffusant includes at least one of lithia and lithium nitrate.The present invention method, can be effectively prevented from monocrystal thin films missing lithium phase the problem of, produce nanometer grade thickness, uniform film thickness, component close to ideal stoichiometric than monocrystal thin films.
Description
Technical field
The present invention relates to a kind of method for manufacturing monocrystal thin films, specifically, it is equal to be related to a kind of nanometer grade thickness, thickness
Even, component close to ideal stoichiometric than monocrystal thin films manufacture method.
Background technology
Lithium niobate monocrystal film and monocrystalline lithium tantalate film (hereinafter referred to as film or monocrystal thin films) are in optical signal prosessing, letter
The field such as breath storage and electronic device tool has been widely used, and it can be used as backing material, can be used for making high frequency, height
Bandwidth, high integration, Large Copacity, high sensitivity, the optoelectronics device and integrated optical device of low-power consumption and stable performance,
For example, wave filter, waveguide modulator, optical waveguide switch, spatial light modulator, optical frequency doubler, surface acoustic wave generator, infrared
Detector and ferroelectric storage etc..The most frequently used lithium niobate monocrystal thin-film material generally can be divided into three kinds of structures, wherein, the
A kind of structure is followed successively by lithium niobate monocrystal film, silicon dioxide layer and lithium niobate substrate from top to bottom；Second of structure is from up to
Under be followed successively by lithium niobate monocrystal film, electrode, silicon dioxide layer and lithium niobate substrate；The third structure is followed successively by from top to bottom
Lithium niobate monocrystal film, silicon dioxide layer, electrode and lithium niobate substrate.The thickness of lithium niobate monocrystal film is typically at 50 nanometers
To between 3000 nanometers, the thickness of silicon dioxide layer is typically between 200 nanometers to 3000 nanometers.Monocrystalline lithium tantalate film has
With lithium niobate monocrystal film identical structure, therefore will not be repeated here.
, it is necessary to undergo annealing process to strengthen bonding force and eliminate ion note during lithium niobate monocrystal film is made
Enter caused damage, so as to improve the yield rate of finished films.Generally, annealing temperature need control 200 DEG C to 900 DEG C it
Between.For lithium niobate monocrystal film, when annealing temperature is more than 300 DEG C, phase transformation occurs in lithium niobate monocrystal film, very
To the phenomenon that decomposed occurs, that is, form LiNb3O8Mutually or with lithia (Li2O form) diffuses out lithium niobate monocrystal
Film, so as to cause lithium niobate monocrystal film to become the rich niobium structure of multiphase, it can be regarded as lithium niobate and five oxidations
Mixture (the LiNbO of two niobiums3+Nb2O5)。
In the presence of having rich niobium structure in lithium niobate monocrystal film, the optical property of lithium niobate monocrystal film can be had a strong impact on
And electrical properties, especially for the lithium niobate monocrystal film containing metal electrode.Connect in metal electrode with LiNbO_3 film layer
In the case of touching, metal electrode and lithium niobate are reacted near contact surface so that the lithium niobate monocrystal containing metal electrode is thin
The situation of film missing lithia is more serious.In the case where lithium niobate monocrystal film lacks lithia, its device can be had a strong impact on
The performance of part, makes index fall flat, or even can not use at all.
The content of the invention
It is an object of the present invention to provide a kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion, methods described
Can produce nanometer grade thickness, uniform film thickness, component close to ideal stoichiometric than monocrystal thin films.
The present invention provides a kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion, and methods described includes：Pass through ion
Injection method implants ions into the surface of original substrate, so as to form film layer, separating layer and remaining matter layer in original substrate, its
In, film layer is located at the surface of original substrate, and separating layer is located between film layer and remaining matter layer, and the ion distribution of injection is separating
In layer；Make the thin film layer of target base plate and original substrate, and then utilize bonding chip method by original substrate and target base plate
It is bonded together, to form bonding body；Para-linkage body is heated so that film layer and the separation of remaining matter layer；In film layer and remaining
After the separation of matter layer, film layer is heated with 200 DEG C~700 DEG C of temperature in the predetermined container equipped with diffusant, wherein, expand
Powder includes at least one of lithia and lithium nitrate.
According to an embodiment of the invention, diffusant is the lithia either mixture of lithia and lithium niobate.
According to an embodiment of the invention, in the step of being heated to film layer, oxygen is passed through to predetermined container, makes film layer
Lithia is heated so as at a temperature of 200 DEG C~700 DEG C to be diffused into film layer.
According to an embodiment of the invention, the predetermined container includes：For placing the first container of diffusant, hold first
One end of device is provided with air inlet；For placing the second container of film, one end of second container is provided with gas outlet；For
First container is connected to the pipeline of second container；The primary heater heated to the first container；And to second container
The secondary heater heated.
According to an embodiment of the invention, diffusant is lithium nitrate either at least one of sodium nitrate, potassium nitrate and nitre
The mixture of sour lithium.
According to an embodiment of the invention, in the step of being heated to film layer, film layer is immersed in molten condition
Diffusant in, film layer is heated so as to lithium ion at a temperature of 200 DEG C~700 DEG C and be diffused into film layer.
According to an embodiment of the invention, methods described is additionally included in after the step of para-linkage body is heated and to thin
Before the step of film layer heats, film layer is made annealing treatment under conditions of 300 DEG C~600 DEG C.
According to an embodiment of the invention, methods described is additionally included in before the step of being heated to film layer, and film layer is entered
The polishing of row surface, and/or after the step of being heated to film layer, surface polishing is carried out to film layer.
According to an embodiment of the invention, coated with silicon dioxide layer or coated with electrode layer and dioxy in target base plate
SiClx layer, and make the thin film layer of silicon dioxide layer and original substrate, to form bonding body；Or in the thin of original substrate
Electrode layer and silicon dioxide layer are coated with the surface of film layer, and silicon dioxide layer is contacted with target base plate, to form key
It is fit.
According to an embodiment of the invention, in the step of para-linkage body is heated, under vacuum or more than 1
Atmospheric pressure and carry out heating less than para-linkage body under the atmosphere of 300 atmospheric pressure and cause film layer and the separation of remaining matter layer.
According to an embodiment of the invention, the film is lithium niobate monocrystal film or monocrystalline lithium tantalate film.
According to the method for the monocrystal thin films of the manufacture near stoichiometric proportion of the present invention, film missing lithium can be effectively prevented from
The problem of phase, produce nanometer grade thickness, uniform film thickness, component close to ideal stoichiometric than monocrystal thin films.
Brief description of the drawings
By with reference to be exemplarily illustrated one accompanying drawing carry out description, above and other purpose of the invention and
Feature will become apparent, wherein：
Fig. 1 is the FB(flow block) for the method for showing the manufacture monocrystal thin films of the present invention；
Fig. 2 is the structural representation for showing disperser.
Embodiment
The method of the monocrystal thin films of the manufacture near stoichiometric proportion of the present invention is described in detail below in conjunction with the accompanying drawings.
The present invention provides a kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion, as shown in figure 1, the method for the present invention
Comprise the steps：By ion implantation, ion is injected against the surface of original substrate, formed film layer, separating layer and
Remaining matter layer；Original substrate and target base plate are bonded together to form into bonding body；Para-linkage body carries out heating and causes film layer and remaining matter layer
Separation；And film layer is transferred in target base plate, to film heating in disperser.
Specifically, by ion implantation, ion is injected against the surface of original substrate, film layer is formed, divides
In the step of absciss layer and remaining matter layer, using ion implantation, the upper table by ion (can be molecular ion) against original substrate
Face is injected, and forms separating layer, and original substrate is divided into upper and lower twoth area by separating layer：One is passed through for overwhelming majority injection ion
Region, referred to as film layer；Another for overwhelming majority injection ions without region, be referred to as remaining matter layer.The thickness of film layer
Degree is determined (for example, helium ion energy can be 10keV~2000keV, with the helium ion energy phase by the energy of ion implanting
The thickness of corresponding film layer is between 60 nanometers to 4500 nanometers).Wherein, ion implantation may include conventional ion implanters
The ion implantation of injection method, plasma immersion ion implantation and the segmentation injection using different implantation temperatures, wherein,
The ion injected in ion implantation can be at least one of hydrogen ion and helium ion.
The purpose for carrying out the ion implantation is in order to by the top layer of substantial amounts of ion implanting to original substrate, in separating layer
Injection ion played pendulum in original substrate, injection ion insertion lattice defect in, produce bulk strain, cause
Separating layer becomes area of stress concentration, so that the weak mechanical strength of original substrate part near separating layer.
In the step of original substrate and target base plate are bonded together to form into bonding body, using bonding chip method, make original base
Plate is bonded together with target base plate, forms bonding body.Wherein, can be applied on the surface of target base plate insulating layer coating (for example,
SiO2), the insulating barrier is combined face-to-face with the film layer of original substrate, be then bonded, so that the membrane structure made
Film layer, silicon dioxide layer and target base plate are followed successively by from top to bottom.Can also on the surface of target base plate electrode coated layer (example
Such as, metal electrode) and insulating barrier (for example, SiO2), insulating barrier is combined face-to-face with the film layer of original substrate, then carry out
Bonding, so that the membrane structure made is followed successively by film layer, insulating barrier, electrode layer and target base plate from top to bottom.Can also be
Coated with electrode layer and insulating barrier (for example, SiO on the surface of the film layer of original substrate2), make insulating barrier and target base plate face
Opposite combine, be then bonded so that make membrane structure be followed successively by from top to bottom film layer, electrode layer, insulating barrier and
Target base plate.
Bonding chip method can be selected from legal direct key, anode linkage method, low-temperature bonding method, vacuum bonding method, plasma
Strengthen bonding method and the one kind being bonded in bonding method etc..
In para-linkage body carries out the step of heating causes film layer and remaining matter layer to separate, bonding body is placed in heating container
It is interior, 150 DEG C~300 DEG C are then heated to, during heating, the ion of injection can become gas molecule or atom, be formed
Many small bubbles, with the extension of heat time or the rise of heating-up temperature, bubble can be more and more, and volume also gradually increases
Greatly, finally, bubble is connected with each other so that film layer and the separation of remaining matter layer.
In another embodiment of the invention, the step of heating of para-linkage body makes its separation can also be in more than 1 air
Press and carried out less than under the atmosphere of 300 atmospheric pressure or under vacuum condition.
It is transferred in film layer in target base plate, in the step of film heating in disperser, when film layer and mesh
After mark substrate separates with remaining matter layer, film layer has been transferred in target base plate, forms film.Film is placed in equipped with diffusant
In disperser, film is carried out under conditions of 200 DEG C~700 DEG C to be heated to certain time.
Diffusant includes at least one of lithia and lithium nitrate.Film is placed in the disperser equipped with diffusant
It is interior, heating less than 100 hours is carried out to film under conditions of 200 DEG C~700 DEG C, so that the diffusion with high chemical potential
Lithium in agent is mutually diffused into the film with low chemical potential, avoids the phenomenon of film missing lithium phase so that the group in film
Tap nearly ideal stoichiometric ratio.
In one embodiment of the invention, diffusant can be lithium nitrate either in sodium nitrate, potassium nitrate at least
A kind of and mixture of lithium nitrate.In order that the lithium ion obtained in diffusant is more fully diffused into film, it is preferable that can be incited somebody to action
It is thin film dipped that certain time is heated in the diffusant in molten condition.
In another embodiment of the present invention, diffusant can be the mixing of lithia either lithia and lithium niobate
Thing.In the disperser equipped with the lithia either mixture of lithia and lithium niobate, film is heated so that oxygen
Change lithium to be diffused into film.Wherein, in order that the lithia obtained in diffusant preferably can be diffused into film, it is preferable that
When being heated under conditions of 200 DEG C~700 DEG C to film, oxygen can be passed through into disperser.
In an embodiment of the present invention, in order that the lithia obtained in diffusant can be sufficiently diffused in film, such as
Shown in Fig. 2, disperser may include the first container 10 for placing diffusant, and one end of the first container 10 is provided with air inlet
Mouth 11；For placing the second container 20 of film, one end of second container 20 is provided with gas outlet 21；For by the first container
10 are connected to the pipeline 30 of second container 20；The primary heater 40 that is heated to the first container 10 and to second container 20
The secondary heater 50 heated.Coagulated to prevent from entering the diffusant in second container 20 on the inwall of pipeline 30
Knot, disperser may also include the 3rd heater 60 heated to pipeline 30.
, can be by diffusant when being heated film so that lithia is diffused into film using above-mentioned disperser
(for example, lithia either mixture of lithia and lithium niobate) is placed in the first container 10；Film is placed in second container
In 20；By the temperature control of primary heater 40 to 400 DEG C~1200 DEG C, by the temperature control of secondary heater 50 to 200 DEG C
~700 DEG C；Oxygen is passed through into the first container 10 by air inlet 11, oxygen carries lithia steam and enters second container 20
It is interior, it is diffused into film, and flowed out by the gas outlet 21 of second container 20.
In addition, in order to provide production efficiency, the temperature in the first container 10 of placement diffusant can be made to be higher than second container
Temperature in 20, so that the saturated vapor pressure of lithia is higher, the concentration entered in second container 20 is larger, is advantageous to
The diffusion of lithia in the film.In this way, will can shorten to diffusion time 1 hour to 30 hours.
In another embodiment of the invention, can also be in order to strengthen bonding force and eliminate damage caused by ion implanting
After the step of para-linkage body heats and before to the step of film heating, film is entered under conditions of 300 DEG C to 600 DEG C
Row annealing.
The step of method of the present invention also includes being processed by shot blasting film, the step can be selected to film heating
The step of before, to film layer carry out surface polishing, or selection after to the step of film heating, film layer is entered
The polishing of row surface, also or selection is before to the step of film heating and after to the step of film heating, to thin
Film layer carries out surface polishing.
The monocrystal thin films of the method manufacture of the present invention can be lithium niobate monocrystal film or monocrystalline lithium tantalate film.
The method of the monocrystal thin films of the manufacture near stoichiometric proportion of the present invention, with traditional gas phase transmission balance method (VTE)
The method for manufacturing the lithium niobate crystal chip of near stoichiometric proportion is compared, and gross differences be present：Gas phase transmission balance method is one kind to thickness
Spend the method for the compensation of the lithia deficient phenomena progress of larger lithium niobate crystal chip (thickness is about in 0.5 millimeter).By
In the thickness of lithium niobate crystal chip, larger and diffusate diffusion coefficient has exponent relation with diffusion temperature, therefore, traditional
The diffusion temperature of gas phase transmission balance method needs to control more than 1000 DEG C.At this temperature, the vapour pressure of lithia is very high, mistake
The lithia of high concentration can react with lithium niobate crystal chip surface, cause to corrode, so, it can typically select to be rich in lithia
Polycrystalline lithium niobate ceramics are used as diffusant, but this diffusant preparation process is complicated, and diffusion time needs 100 hours left sides
It is right just to can guarantee that lithia spreads uniformly on lithium niobate crystal chip.But for lithium niobate monocrystal film or monocrystalline lithium tantalate film
For, if diffusion temperature is higher than 700 DEG C, there can be problems with.On the one hand, lithium niobate monocrystal film or monocrystalline lithium tantalate are thin
Film has generally comprised silicon dioxide layer, and because silica is different from the thermal coefficient of expansion of lithium niobate, too high temperature can make thin
There is larger internal stress inside film, cause film to damage；On the other hand, lithium niobate monocrystal film or monocrystalline lithium tantalate film one
As include electrode, too high temperature can make electrode easily be chemically reacted with the material around it, produce impurities phase, even
Cause electrode melting；Another further aspect, when being heated to 700 DEG C~900 DEG C, lithium niobate monocrystal film can be aggravated or monocrystalline lithium tantalate is thin
The phase transformation and thermal decomposition of film, substantial amounts of lithia can diffuse out from film, in the environment rich in lithia, by
In the reason such as thermo parameters method and air flow method oxidation lithium compensation can be caused uneven, eventually cause lithium niobate monocrystal film or tantalum
The component skewness of sour lithium monocrystal thin films.Therefore, traditional gas phase transmission balance method is not suitable for preparing lithium niobate monocrystal
Film or monocrystalline lithium tantalate film.
And the method for using the manufacture film of the present invention, it is thin at tens nanometers to 3,000 nanometers can to make to obtain thickness
Film, and the film is heated 1 hour to 60 hours under conditions of low temperature (200 DEG C~700 DEG C), you can make (the oxidation of lithium phase
Lithium or lithium ion) it is diffused into film.In addition, using the present invention disperser, will can shorten to diffusion time 1 hour~
30 hours, so as to improve production efficiency.Therefore, the method for manufacture film of the invention, can be effectively prevented from film missing
The problem of lithium phase, produce nanometer grade thickness, uniform film thickness, component close to ideal stoichiometric than film.
Illustrate that the present invention makes the detailed process of film exemplified by making lithium niobate monocrystal film below.
Embodiment 1
Original substrate is lithium niobate crystal chip, is 4 × 10 through overtreatment16ions/cm2Helium ion (He1+) injection, helium ion
Energy is 230keV.
Target base plate is lithium niobate crystal chip, and one is deposited in target base plate using plasma enhanced chemical vapor deposition method
Layer silica, and silicon dioxide layer is polished to 2 microns using chemical mechanical milling method.
It is legal using direct key, the silicon dioxide layer of target base plate is bonded to form bonding body with original substrate；
Bonding body is heated to 220 DEG C, and kept for 10 hours at such a temperature, makes bonding body separation that film be made.
Obtained film is put into closed container with oxidation lithium powder (solid) and heated, surrounding atmosphere is oxygen (O2),
Temperature is 500 DEG C, and the time is 50 hours, is taken out after film cooling.
Finally, the surface of film is polished, obtains lithium niobate monocrystal film.
Now the very optical index of lithium niobate monocrystal film is less than 2.202 (wavelength is 633 nanometers).In addition, lithium and niobium
Atomic ratio reach 0.95:More than 1, this shows the component of lithium niobate monocrystal film close to ideal stoichiometric than 1:1.
Embodiment 2
Original substrate is lithium niobate crystal chip, is 4 × 10 through overtreatment16ions/cm2Helium ion (He1+) injection, helium ion
Energy is 1000keV.
Target base plate is lithium niobate crystal chip, and one is deposited in target base plate using plasma enhanced chemical vapor deposition method
Layer silica, and silicon dioxide layer is polished to 2 microns using chemical mechanical milling method.
It is legal using direct key, the silicon dioxide layer of target base plate is bonded to form bonding body with original substrate；
Bonding body is heated to 220 DEG C, and kept for 10 hours at such a temperature, makes bonding body separation that film be made.
Film is made annealing treatment at 300~600 DEG C, then carries out surface polishing.
Film after polishing is put into closed container with oxidation lithium powder (solid) and heated, surrounding atmosphere is oxygen
(O2), temperature is 500 DEG C, and the time is 50 hours, is taken out after film cooling, and lithium niobate monocrystal film is obtained after cleaning.
Now the very optical index of lithium niobate monocrystal film is less than 2.202 (wavelength is 633 nanometers).In addition, lithium and niobium
Atomic ratio reach 0.95:More than 1, this shows the component of lithium niobate monocrystal film close to ideal stoichiometric than 1:1.
Embodiment 3
Original substrate is lithium niobate crystal chip, is 4 × 10 through overtreatment16ions/cm2Helium ion (He1+) injection, helium ion
Energy is 50keV.
Target base plate is lithium niobate crystal chip, the depositing electrode in target base plate, then utilizes plasma enhanced chemical gas
Phase sedimentation deposits layer of silicon dioxide in target base plate, and silicon dioxide layer is polished into 2 using chemical mechanical milling method
Micron.
It is legal using direct key, the silicon dioxide layer of target base plate is bonded to form bonding body with original substrate；
Bonding body is heated to 220 DEG C, and kept for 10 hours at such a temperature, makes bonding body separation that film be made.
Obtained film is put into closed container with oxidation lithium powder (solid) and heated, surrounding atmosphere is oxygen (O2),
Temperature is 500 DEG C, and the time is 50 hours, is taken out after film cooling.
Finally, the surface of film is polished, obtains electroded lithium niobate monocrystal film.
Now the very optical index of lithium niobate monocrystal film is less than 2.202 (wavelength is 633 nanometers).In addition, lithium and niobium
Atomic ratio reach 0.95:More than 1, this shows the component of lithium niobate monocrystal film close to ideal stoichiometric than 1:1.
Embodiment 4
Original substrate is lithium niobate crystal chip, is 4 × 10 through overtreatment16ions/cm2Helium ion (He1+) injection, helium ion
Energy 230keV；Then, layer of metal electrode is deposited on the surface of injection helium ion；Finally, plasma enhanced chemical is utilized
Vapour deposition process deposits layer of silicon dioxide on electrode layer, and is polished to silicon dioxide layer using chemical mechanical polishing method
Target thickness.
Target base plate is lithium niobate crystal chip, is entered using the legal silicon dioxide layer by target base plate and original substrate of direct key
Line unit is closed to form bonding body；Bonding body is heated to 220 DEG C, and kept for 10 hours at such a temperature, separates bonding body
Film is made.
Obtained film is put into closed container with oxidation lithium powder (solid) and heated, surrounding atmosphere is oxygen (O2),
Temperature is 500 DEG C, and the time is 50 hours, is taken out after film cooling.
Finally, the surface of film is polished, obtains the lithium niobate monocrystal film with metal electrode.
Now the very optical index of lithium niobate monocrystal film is less than 2.202 (wavelength is 633 nanometers).In addition, lithium and niobium
Atomic ratio reach 0.95:More than 1, this shows the component of lithium niobate monocrystal film close to ideal stoichiometric than 1:1.
Embodiment 5
Original substrate is lithium niobate crystal chip, is 4 × 10 through overtreatment16ions/cm2Helium ion (He1+) injection, helium ion
Energy 230keV.
Target base plate is lithium niobate crystal chip, and one is deposited in target base plate using plasma enhanced chemical vapor deposition method
Layer silica, and silicon dioxide layer is polished to 2 microns using chemical mechanical milling method.
It is legal using direct key, the silicon dioxide layer of target base plate is bonded to form bonding body with original substrate；
Bonding body is heated to 220 DEG C, and kept for 10 hours at such a temperature, makes bonding body separation that film be made.
Film is made annealing treatment at 300 DEG C~600 DEG C, then carries out surface polishing.
Film after polishing is put into closed container with lithium nitrate and heated, temperature is 300 DEG C, and now lithium nitrate melts,
Thin film dipped in the lithium nitrate of molten condition in molten condition, setting time is 3 hours, after setting time reaches, by film
Take out.
Finally, the surface of film is polished, obtains lithium niobate monocrystal film.
Now the very optical index of lithium niobate monocrystal film is less than 2.202 (wavelength is 633 nanometers).In addition, lithium and niobium
Atomic ratio reach 0.95:More than 1, this shows the component of lithium niobate monocrystal film close to ideal stoichiometric than 1:1.
Embodiment 6
Original substrate is lithium niobate crystal chip, is 4 × 10 through overtreatment16ions/cm2Helium ion (He1+) injection, helium ion
Energy is 230keV.
Target base plate is lithium niobate crystal chip, and one is deposited in target base plate using plasma enhanced chemical vapor deposition method
Layer silica, and silicon dioxide layer is polished to 2 microns using chemical mechanical milling method.
It is legal using direct key, the silicon dioxide layer of target base plate is bonded to form bonding body with original substrate；
Bonding body is heated to 220 DEG C, and kept for 10 hours at such a temperature, makes bonding body separation that film be made.
Film is made annealing treatment at 300~600 DEG C, then carries out surface polishing.
Film after polishing is placed into second container 20 as shown in Figure 2, oxidation lithium powder is placed into such as Fig. 2
In the first shown container 10 in, be passed through oxygen (O from air inlet 112), oxygen flow is 1 liter/min, the first container 10
Temperature setting is 800 DEG C, and the temperature setting of second container 20 is 500 DEG C, and setting time is 20 hours, and setting time is treated after reaching
Taken out after film cooling, lithium niobate monocrystal film is obtained after cleaning.
Now the very optical index of lithium niobate monocrystal film is less than 2.202 (wavelength is 633 nanometers).In addition, lithium and niobium
Atomic ratio reach 0.95:More than 1, this shows the component of lithium niobate monocrystal film close to ideal stoichiometric than 1:1.
In summary, the method for manufacture monocrystal thin films of the invention due to after being transferred to target base plate in film layer containing
Have in the environment of diffusant to film heating so that the lithium in monocrystal thin films is mutually effectively compensated, so as to avoid monocrystalline
Film lacks the problem of lithium phase.
In addition, the method for the present invention can produce nanometer grade thickness, uniform film thickness, component close to ideal stoichiometric ratio
Monocrystal thin films.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, technical scheme can be carried out a variety of simple variants and
Combination, these simple variants belong to protection scope of the present invention.
Claims (8)
1. a kind of method for the monocrystal thin films for manufacturing near stoichiometric proportion, methods described comprise the steps：
The surface of original substrate is implanted ions into by ion implantation, so as to form film layer, separation in original substrate
Layer and remaining matter layer, wherein, film layer is located at the surface of original substrate, and separating layer is located between film layer and remaining matter layer, injection
Ion distribution is in separating layer；
Make the thin film layer of target base plate and original substrate, and then utilize bonding chip method by original substrate and target base plate key
It is combined, to form bonding body；
Para-linkage body is heated so that film layer and the separation of remaining matter layer；
The film layer after separation is made annealing treatment under conditions of 300 DEG C~600 DEG C；
Film layer is heated with 200 DEG C~700 DEG C of temperature in the predetermined container equipped with diffusant, wherein, diffusant includes
At least one of lithia and lithium nitrate,
Wherein, in the step of being heated to film layer, oxygen is passed through to predetermined container, makes temperature of the film layer at 200 DEG C~700 DEG C
Lithia is heated so as under degree to be diffused into film layer.
2. according to the method for claim 1, wherein, diffusant is the mixing of lithia either lithia and lithium niobate
Thing.
3. according to the method for claim 1, wherein, the predetermined container includes：For placing the first container of diffusant,
One end of first container is provided with air inlet；For placing the second container of film, it is provided with out in one end of second container
Gas port；For the first container to be connected to the pipeline of second container；The primary heater heated to the first container；It is and right
The secondary heater that second container is heated.
4. according to the method for claim 1, wherein, diffusant be lithium nitrate either in sodium nitrate, potassium nitrate at least
A kind of and mixture of lithium nitrate.
5. according to the method for claim 4, wherein, in the step of being heated to film layer, film layer is immersed in and is in
In the diffusant of molten condition, film layer is heated so as to lithium ion at a temperature of 200 DEG C~700 DEG C and be diffused into film layer
In.
6. according to the method for claim 1, wherein, methods described is additionally included in before the step of being heated to film layer, right
Film layer carries out surface polishing, and/or after the step of being heated to film layer, film layer is carried out at the polishing of surface
Reason.
7. according to the method for claim 1, wherein, silicon dioxide layer is coated with target base plate or coated with electrode
Layer and silicon dioxide layer, and make the thin film layer of silicon dioxide layer and original substrate, to form bonding body；Or original
Electrode layer and silicon dioxide layer are coated with the surface of the film layer of substrate, and silicon dioxide layer is contacted with target base plate,
To form bonding body.
8. according to the method for claim 1, wherein, in the step of para-linkage body is heated, under vacuum or
Para-linkage body carries out heating and causes film layer and remaining matter layer point under the atmosphere more than 1 atmospheric pressure and less than 300 atmospheric pressure
From.
Priority Applications (1)
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| KR20180038369A (en) * | 2016-10-06 | 2018-04-16 | 신에쓰 가가꾸 고교 가부시끼가이샤 | Composite substrate manufacturing method |
| CN108565211A (en) * | 2018-06-21 | 2018-09-21 | 济南晶正电子科技有限公司 | Composite single crystal film |
| CN110764185B (en) * | 2019-10-12 | 2021-01-01 | 天津大学 | Preparation method of low-loss lithium niobate thin film optical waveguide |
| CN112410885A (en) * | 2020-11-10 | 2021-02-26 | 珠海光库科技股份有限公司 | Lithium niobate single crystal film and manufacturing method thereof |
| CN112382563A (en) * | 2020-11-13 | 2021-02-19 | 济南晶正电子科技有限公司 | Ion implantation thin film wafer separation method, single crystal thin film, and electronic component |
| CN115207206B (en) * | 2022-09-16 | 2022-12-06 | 济南晶正电子科技有限公司 | Near-stoichiometric composite film and preparation method thereof |
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