CN106929916A - A kind of preparation method of lithium niobate black-film - Google Patents
A kind of preparation method of lithium niobate black-film Download PDFInfo
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- CN106929916A CN106929916A CN201710266783.1A CN201710266783A CN106929916A CN 106929916 A CN106929916 A CN 106929916A CN 201710266783 A CN201710266783 A CN 201710266783A CN 106929916 A CN106929916 A CN 106929916A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/30—Niobates; Vanadates; Tantalates
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The invention discloses a kind of preparation method of lithium niobate black-film, pending lithium niobate crystal chip is put into container A, reducing agent is put into container B simultaneously, then the container A and the container B equipped with reducing agent that will be equipped with lithium niobate crystal chip are positioned in heat-treatment furnace, in air atmosphere, in reduction treatment is carried out under reduction temperature, cooling obtains lithium niobate black-film.The present invention is simple to operate, safety, efficiency high, low cost and do not influence wafer surface crudy lithium niobate black-film preparation method, this method reduces the resistivity of chip on the premise of lithium niobate piezoelectric performance and single domain is not influenceed, weaken and even eliminate the pyroelectric effect that chip itself has, enhance the absorbability of visible region.
Description
Technical field
The present invention relates to crystalline material, particularly a kind of preparation method of lithium niobate black-film belongs to crystal post processing field.
Background technology
Lithium niobate monocrystal is a kind of excellent multifunction manual crystal, with good piezoelectric property, is made of the material
Surface acoustic wave（SAW）Device such as wave filter, resonator, oscillator etc., are widely applied to mobile communication, radar, electronics pair
It is anti-to wait civilian and military field.Because lithium columbate crystal has a wide range of application, consumption is big, and the production of lithium niobate in the world has had
Very big scale, annual yield is that IT industry Novel electronic devices develop indispensable functional material in terms of hundred tons.
Industrially, lithium columbate crystal is mainly grown using czochralski method, and generally using Platinum crucible, growth atmosphere is
Air atmosphere.Then it is annealed, polarization process, now crystal be in water white transparency or faint yellow.Eventually pass orientation, rolling
The processes such as circle, cutting, grinding, polishing, are fabricated to lithium niobate crystal chip.Chip after processing is visually presented white, is commonly called as " in vain
Piece ", resistivity is 1015Ω .cm or so.
Though lithium niobate white chip also has electrical property of heat releasing, its resistance high simultaneously with good piezo-electric effect
Rate prevents the electric charge that surface is produced by pyroelectric effect from being neutralized rapidly, is made to SAW device and application brings many difficulties
With the difficulty for avoiding.In the manufacturing process of wave filter, there is the treatment of lithium niobate substrate piece temperature change, such as in substrate surface
Form the front baking in electrode film, and photoetching and baking etc. afterwards.Due to lithium columbate crystal pyroelectric coefficient high, wafer surface is held very much
Easily because temperature change causes exhibiting high surface static charge accumulation, these electric charges can be between interdigital electrode, between chip, between chip and frock
Spontaneous release.When electrostatic field reaches to a certain degree, just occur that chip cracking, microdomain reversion and interdigital electrode are burnt etc. many
Problem, in particular with the development of mechanics of communication in recent years, the filter frequencies that communication product needs constantly are raised, interdigital electrode
Line width it is more and more narrow, the destruction that this electric discharge caused by pyroelectricity is caused also just more and more substantially, greatly increased device
The defect rate of part.Simultaneously as lithium niobate white tiles has light transmission rate high, in a photolithographic process, light is anti-at substrate slice back
Penetrate, produce graphics resolution the problems such as reduce.
Produced problem in being made for SAW device, new requirement is proposed to lithium niobate crystal chip, i.e., do not influenceing it to press
In the case of electrical property, the pyroelectric effect and light transmission rate of chip are reduced.It is main by lithium niobate crystal chip both at home and abroad at present
Reduction treatment is carried out, the pyroelectric effect and light transmission rate of substrate slice are reduced with this.By reduction treatment, the color of chip from
Water white transparency change grey, black are even almost opaque, therefore referred to as black-film.It is black compared with conventional lithium niobate " white tiles "
The resistivity of piece significantly declines（About 109~1012Ω .cm magnitudes）, so as to eliminate the defect that static discharge brings, finally carry
Rise the production efficiency of SAW device and reduce production cost.
United States Patent (USP) US6319430B1 is proposed more than 500 DEG C, 1140 DEG C（Lithium niobate Curie temperature）Hereinafter, in nitrogen
Darkening process is carried out to lithium niobate crystal chip under the combination atmosphere of gas and hydrogen.This kind of process efficiency is higher, but reducing process process
In be related to hydrogen, the danger that easily set off an explosion, therefore higher to equipment requirement.
Granted patent 200410095073.X is proposed and lithium niobate crystal chip is embedded to by Al, Ti, Si, Ca, Mg, C, Zn
It is not enough more than 300 DEG C in vacuum or inert gas in container in the state of at least one element powders for constituting
Technology for Heating Processing is carried out at a temperature of 500 DEG C.United States Patent (USP) US20050265916 is proposed and is covered carbon on lithium niobate crystal chip surface
The reducing substances such as sour hydrogen sodium, lithium carbonate, magnesium carbonate, calcium hydride, lithium hydride, then in vacuum or reducing atmosphere, arrive at 250 DEG C
Darkening process is carried out in the range of lithium niobate Curie temperature.Although above-mentioned technique can obtain the LN black-films of low-resistivity, by
In burial mode is used, reducing agent is relatively contacted by force and directly with lithium niobate crystal chip, easily causes lithium niobate crystal chip over reduction.
Also require to vacuumize or fill reduction/inert atmosphere simultaneously, it is cumbersome, increased cost.And hydride is poisonous, security is not
Height, its waste material has harm to environment.
Chinese patent CN200910017339.1 is proposed using Fe and Li2CO3Mix according to a certain percentage, in nitrogen gas
The preparation of black-film is carried out under atmosphere to LN.Although obtaining the lithium niobate black-film of low-resistivity, due to the high activity of metal iron powder,
Lithium niobate crystal chip blackening degree is not easily controlled.Meanwhile, strong reproducibility is also easy to Li ion exchanges in a lithium niobate crystal chip
Go out, the piezoelectricity to chip is impacted.
Chinese patent CN201610660753.4 is proposed and led to using the mixing material of a kind of glue mixed carbonic acid lithium, Zn powder
Method for printing screen uniformly coating and pending lithium niobate substrate piece two sides are crossed, to it at flowing nitrogen, 400-600 DEG C of temperature
Darkening process.Similarly, since the strong oxidability of Zn powder, blackening degree is not easily controlled.Simultaneously by the way of coating, operation
Cumbersome, efficiency is low.
The content of the invention
Though the characteristics of having low-resistivity, low transmission for the lithium niobate black-film that existing reduction treatment makes, deposits
Complex process, low efficiency, over reduction, it is dangerous the shortcomings of, it is an object of the invention to propose a kind of simple to operate, peace
Entirely, efficiency high, low cost and do not influence wafer surface crudy lithium niobate black-film preparation method, this method do not influenceing
The resistivity of chip is reduced on the premise of lithium niobate piezoelectric performance and single domain, weakening or even eliminating chip itself has
Pyroelectric effect, enhance the absorbability of visible region.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of preparation method of lithium niobate black-film, pending lithium niobate crystal chip is put into container A, while reducing agent is put into
In container B, the container A and the container B equipped with reducing agent that then will be equipped with lithium niobate crystal chip are positioned in heat-treatment furnace, in air
Under atmosphere, in reduction treatment is carried out under reduction temperature, cooling obtains lithium niobate black-film.
Preferably, the reduction temperature is 400 DEG C to lithium niobate Curie temperature, recovery time 2-24 hours.
The container A and container B are quartz, the crucible that is made of aluminum oxide or zirconium oxide exotic material.
Preferably, the reducing agent is carbon dust or carbon block.
Heat-treatment furnace is heated to reduction temperature according to the heating rate of 100-300 DEG C/h.During cooling, heat-treatment furnace according to
The rate of temperature fall of 100-300 DEG C/h is down to room temperature.
Compared with prior art, the invention has the advantages that：
1）Lithium niobate black-film technique is prepared with conventional use hydrogen and nitrogen atmosphere to compare, the present invention is safe, to equipment
It is required that low.
2）Compared with the reduction mode of conventional use reducing agent embedding lithium niobate crystal chip, reducing agent of the present invention and lithium niobate
Chip uses cordless, and the crudy of wafer surface is not influenceed.
3）Reducing agent of the invention used is cheap, nontoxic, environmentally safe, the characteristics of with safety, low cost.
4）The making for directly carrying out black-film in atmosphere of the invention, without vacuumizing or filling reduction/inert atmosphere, operation letter
It is single quick, efficiency high.Wafers up to a hundred can be disposably processed simultaneously, is adapted to mass production.
Specific embodiment
The preparation method of lithium niobate black-film of the present invention, comprises the following steps that：
（1）Load：Pending lithium niobate crystal chip is sequentially placed into vessels crucible A, while carbon dust or carbon block are put into another
In individual vessels crucible B, the container A and the container B equipped with carbon dust or carbon block of lithium niobate crystal chip are then will be equipped with while being positioned over heat
In treatment furnace；Container A and container B are quartz, the crucible that is made of aluminum oxide or zirconium oxide exotic material.In order to ensure preferably
Reduction effect, all lithium niobate crystal chips can be put into vessels crucible A by support, by support make all lithium niobate crystal chips that
This is not in contact with each other, and be arranged in parallel as far as possible.
（2）Heat up：In air atmosphere, with the speed of 100-300 DEG C/h by lithium niobate crystal chip from be heated at room temperature also
Former temperature, reduction temperature is 400 to lithium niobate Curie temperature（Generally 1140 DEG C）.
（3）Insulation：2-24 hours is incubated under reduction temperature.
（4）Cooling：After insulation terminates, room temperature is down to the speed of 100-300 DEG C/h, lithium niobate crystal chip is taken out successively is
Can, black-film completes.
The reduction principle that chip of the present invention and reducing agent are not directly contacted with is：At high temperature, carbon source is remaining with reduction furnace
Oxygen reaction in air generates carbon monoxide, and then carbon monoxide diffuses whole burner hearth, is reduced with lithium niobate under high temperature
Reaction, chip color changes, that is, be made black-film.
Wherein, container A and container B can be placed side by side with front and rear placement or left and right.Container A and container B can be many simultaneously
Individual and arranged for interval, preferably container B container A are more one, and can so make the both sides of any one container A has container B to deposit
Chip can be made to reach faster reduction efficiency and more preferable reduction effect.
In theory, heating and cooling are faster, save time and power cost, but easily cause very much the larger stress of chip soon, hold
It is easy to crack, therefore need control in certain limit, research shows that the temperature rate of 100-300 DEG C/h can take into account time and power
Cost, it is also possible to reduce stress.
It is 10 to use TH2683A Type B Insulation Resistance Testers to measure its body resistivity the black-film for completing9~1013
Ω .cm, the lithium niobate black-film after treatment, can be directly used as the substrate of SAW filter.
Below in conjunction with several embodiments helping further understand the present invention.
Embodiment 1：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 4 hours of 500 DEG C of reduction treatments are warming up to the speed of 120 DEG C/h.After insulation terminates, with the speed of 120 DEG C/h
Room temperature is down to, lithium niobate crystal chip is taken out successively, black-film completes.Obtained lithium niobate black-film resistivity is about 7 × 1012Ω
.cm or so.
Embodiment 2：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 5 hours of 700 DEG C of reduction treatments are warming up to the speed of 200 DEG C/h.After insulation terminates, with the speed of 200 DEG C/h
Room temperature is down to, lithium niobate crystal chip is taken out successively, black-film completes.Obtained lithium niobate black-film resistivity is about 1 × 1012Ω
.cm or so.
Embodiment 3：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 10 hours of 700 DEG C of reduction treatments are warming up to the speed of 200 DEG C/h.After insulation terminates, with the speed of 200 DEG C/h
Rate is down to room temperature, and lithium niobate crystal chip is taken out successively, and black-film completes.Obtained lithium niobate black-film resistivity is about 5 × 1011
Ω .cm or so.
Embodiment 4：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 20 hours of 700 DEG C of reduction treatments are warming up to the speed of 300 DEG C/h.After insulation terminates, with the speed of 300 DEG C/h
Rate is down to room temperature, and lithium niobate crystal chip is taken out successively, and black-film completes.Obtained lithium niobate black-film resistivity is about 7 × 1010
Ω .cm or so.
Embodiment 5：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 20 hours of 800 DEG C of reduction treatments are warming up to the speed of 200 DEG C/h.After insulation terminates, with the speed of 200 DEG C/h
Rate is down to room temperature, and lithium niobate crystal chip is taken out successively, and black-film completes.Obtained lithium niobate black-film resistivity is about 4 × 1010
Ω .cm or so.
Embodiment 6：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 3 hours of 900 DEG C of reduction treatments are warming up to the speed of 300 DEG C/h.After insulation terminates, with the speed of 300 DEG C/h
Room temperature is down to, lithium niobate crystal chip is taken out successively, black-film completes.Obtained lithium niobate black-film resistivity is about 6 × 1011Ω
.cm or so.
Embodiment 7：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 20 hours of 900 DEG C of reduction treatments are warming up to the speed of 100 DEG C/h.After insulation terminates, with the speed of 100 DEG C/h
Rate is down to room temperature, and lithium niobate crystal chip is taken out successively, and black-film completes.Obtained lithium niobate black-film resistivity is about 5 × 109
Ω .cm or so.
Embodiment 8：Pending lithium niobate crystal chip is sequentially placed into vessels crucible, while carbon dust or carbon block are put into separately
In one vessels crucible, then it is loaded into the container of lithium niobate crystal chip and loads the container of carbon dust or carbon block while being positioned over hot place
In reason stove, then 24 hours of 1000 DEG C of reduction treatments are warming up to the speed of 200 DEG C/h.After insulation terminates, with the speed of 200 DEG C/h
Rate is down to room temperature, and lithium niobate crystal chip is taken out successively, and black-film completes.Obtained lithium niobate black-film resistivity is about 2 × 109
Ω .cm or so.
Using black-film preparation method of the invention, on the premise of lithium niobate piezoelectric performance and single domain is not influenceed significantly
Degree reduces the resistivity of chip, weakens and even eliminates the pyroelectric effect that chip itself has, and reduces visible region
Transmitance, improves lithographic accuracy in device fabrication processes.Only need to suitably adjust reduction treatment temperature and time, it is possible to reduction
Degree is controlled.In theory, reduction temperature is higher, and the time is more long, and chip color is deeper, and resistivity is smaller.But there may be
Transition is reduced, and transition reduction chip easily ftractures when processing, while the size of resistivity is determined by back end device manufacturer, typically
1011~1012Ω .cm magnitudes are relatively adapted to, so control temperature and time makes the resistivity and color of chip satisfaction needs i.e.
Can.Simultaneously because the uniformity of lithium niobate crystal chip surrounding environment ensure that the wafer uniformity of reduction Darkening process, at utmost
Avoid and cause the inconsistent problem of performance of filter because chip melanism is uncontrollable.
The above embodiment of the present invention is only example to illustrate the invention, and is not to implementation of the invention
The restriction of mode.For those of ordinary skill in the field, other can also be made not on the basis of the above description
With the change and variation of form.Here all of implementation method cannot be exhaustive.It is every to belong to technical scheme
The obvious change amplified out changes row still in protection scope of the present invention.
Claims (6)
1. a kind of preparation method of lithium niobate black-film, it is characterised in that：Pending lithium niobate crystal chip is put into container A, together
When reducing agent is put into container B, the container A and the container B equipped with reducing agent that then will be equipped with lithium niobate crystal chip are positioned over heat
In treatment furnace, in air atmosphere, in reduction treatment is carried out under reduction temperature, cooling obtains lithium niobate black-film.
2. the preparation method of lithium niobate black-film according to claim 1, it is characterised in that：The reduction temperature is 400 DEG C
To lithium niobate Curie temperature, recovery time 2-24 hours.
3. the preparation method of lithium niobate black-film according to claim 1, it is characterised in that：The container A and container B are stone
The crucible that English, aluminum oxide or zirconium oxide exotic material are made.
4. the preparation method of lithium niobate black-film according to claim 1, it is characterised in that：The reducing agent is carbon dust or carbon
Block.
5. the preparation method of lithium niobate black-film according to claim 1, it is characterised in that：Heat-treatment furnace is according to 100-300
DEG C/heating rate of h is heated to reduction temperature.
6. the preparation method of lithium niobate black-film according to claim 1, it is characterised in that：During cooling, heat-treatment furnace according to
The rate of temperature fall of 100-300 DEG C/h is down to room temperature.
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Cited By (3)
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| CN107620125A (en) * | 2017-09-30 | 2018-01-23 | 中电科技德清华莹电子有限公司 | A kind of Darkening process method of lithium tantalate or lithium niobate crystal chip |
| WO2019149074A1 (en) * | 2018-02-02 | 2019-08-08 | 福建晶安光电有限公司 | Blackening method for wafer and blackened wafer |
| CN111230598A (en) * | 2019-10-30 | 2020-06-05 | 德清晶辉光电科技股份有限公司 | Preparation method of 8-inch lithium niobate wafer |
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| CN111230598B (en) * | 2019-10-30 | 2022-05-06 | 德清晶辉光电科技股份有限公司 | Preparation method of 8-inch lithium niobate wafer |
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