CN106868595B - The manufacturing method of big thickness black lithium tantalate wafer - Google Patents
The manufacturing method of big thickness black lithium tantalate wafer Download PDFInfo
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- CN106868595B CN106868595B CN201710080781.3A CN201710080781A CN106868595B CN 106868595 B CN106868595 B CN 106868595B CN 201710080781 A CN201710080781 A CN 201710080781A CN 106868595 B CN106868595 B CN 106868595B
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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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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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
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Abstract
A kind of manufacturing method of big thickness black lithium tantalate wafer, comprising the following steps: lithium tantalate is first pressed into scheduled size well cutting, obtains several lithium tantalate wafers；The dirt on the surface of all lithium tantalate wafers is thoroughly removed, and lanthanum powder and lanthana powder are respectively put into vacuum drying oven drying by dry all lithium tantalate wafers, and mix the lanthanum powder of 5% ~ 15% mass into lanthana powder, and mixed to get reducing agent is arrived；Lithium tantalate wafer after the bottom of crucible alternating spreading reducing agent, placing cleaning, is put into vacuum reduction furnace for the crucible equipped with reducing agent and several lithium tantalate wafers；Burner hearth is vacuumized, the temperature in furnace is promoted with 1 DEG C/h ~ 50 DEG C/h rate, it is warming up to 550 DEG C ~ 600 DEG C, keep the temperature 20h ~ 40h, cooling stops vacuumizing when temperature is lower than 100 DEG C, crucible is taken out from the vacuum reduction furnace after the air pressure in furnace is equal with the external world, the lithium tantalate wafer after taking out reduction.
Description
Technical field
The present invention relates to a kind of manufacturing method of lithium tantalate wafer more particularly to a kind of big thickness black lithium tantalate wafers
Manufacturing method.
Background technique
In the prior art be usually using vertical pulling method produce lithium tantalate (LT) crystal, it may be assumed that so that LT crystal in air or
It is grown under anaerobic condition, crystal is usually at colourless or faint yellow, and resistivity is usually 1 × 1014Ω·cm~1×1015
Ω cm, due to needing to heat lithium tantalate wafer during making filter, because of the stronger heat of lithium tantalate wafer
Electrically, spark is generated in the aggregation of wafer surface so as to cause charge, causes the variation of surfacial pattern, can further cause
The micro-crack on surface leads to the reduction of yield rate.In addition, the light transmission rate high due to this LT crystal, in a photolithographic process, by
In light in the reflection of substrate backside, leads to the problem of and graphics resolution is caused to reduce.
For the these problems occurred in filter production, device puts forward new requirements LT crystal, reduces pyroelectricity
Effect reduces light transmission rate.For such a problem, reducing agent is generally used, the reducing agents such as aluminium, magnesium, carbon are to LT crystal
It is restored, makes LiTaO3In lose part oxygen, Ta+5Partially change into Ta+4Or Ta+3, LT crystal resistivity is from 1 × 1014Ω·cm
~1015Ω cm becomes 1 × 109Ω·cm~1012Ω cm, 1mm chip wavelength 532nm green light rate decline from 60% ~ 80%
To 10% ~ 20%, the thermoelectricity and the stronger disadvantage of light transmission rate of LT when making filter are substantially overcomed.
The reduction process of LT chip is in contact with it for reducing agent, is heated to certain temperature and starts to carry out reduction reaction, reaction
Since surface, the reaction of inner wafer is completed by thermal diffusion, gradually will form from wafer surface to inside in this way
Gradient distribution in one oxygen component, to form an internal stress distribution, existing reduction patented technology is generally used by force
Reducing agent is restored, and reduction process is very fast, and component gradient is bigger, and stress is obvious, and this stress is relatively thin in crystal wafer
When be unlikely to damage chip, when wafer thickness is larger, such as when more than 0.7mm, make chip in this strong reductant reduction process
The stress of generation is large enough to destroy the degree of chip, and causing internal structure after thick wafer reduction, there are crackle or latent cracks.
Summary of the invention
In view of this, it is necessary to provide a kind of reduction process is more slow, can be avoided chip generated in reduction it is excessive
Internal stress big thickness black lithium tantalate wafer manufacturing method.
A kind of manufacturing method of big thickness black lithium tantalate wafer, comprising the following steps:
The preparation of lithium tantalate wafer: lithium tantalate is first pressed into scheduled size well cutting, obtains several lithium tantalate wafers；
Cleaning: thoroughly removing the dirt on the surface of all lithium tantalate wafers, and dry all lithium tantalate wafers,
Then all lithium tantalate wafers are placed in dustless environment for use；
The preparation of reducing agent: the lanthanum powder that purity is 90% ~ 99.99% is put into vacuum drying oven, in 120 DEG C of temperature condition
Lower drying 12 to 30 hours；The lanthana powder that purity is 90% ~ 99.99% is put into vacuum drying oven, in 120 DEG C of temperature condition
Lower drying 12 to 30 hours；The lanthanum powder is mixed into the lanthana powder after drying and is mixed to get reducing agent is arrived,
In, the incorporation of the lanthanum powder are as follows: the gross mass of the lanthanum powder accounts for the percentage of the gross mass of the lanthana powder are as follows: 5% ~
15%；Using preferable mobility under the higher fusing point of lanthana powder and high temperature, to keep lanthanum powder sufficiently to connect with lithium tantalate wafer
Touching；
Shove charge: the bottom of crucible equably one layer of spreading it is above-mentioned prepare resulting reducing agent, it is then that a piece of cleaning is dry
The lithium tantalate wafer after dry takes out from dustless environment, and be placed on immediately the bottom spreading of crucible reducing agent it is upper
Just, reduction effect is influenced to avoid the adsorption dust of the lithium tantalate wafer, then in the institute for being placed on crucible bottom
State the top of lithium tantalate wafer again equably one layer of spreading it is above-mentioned prepare resulting reducing agent, then spilt the tantalum of reducing agent in the paving
Another lithium tantalate wafer is placed in the top of sour lithium chip, and so on, it is brilliant that the lithium tantalate is placed in completion in the crucible
Piece and the reducing agent described in spreading between lithium tantalate wafer will be equipped with the reducing agent and several lithium tantalate wafers later
Crucible be put into vacuum reduction furnace；
Reduction: the burner hearth of the vacuum reduction furnace is vacuumized, by the pressure control in furnace in 20Pa hereinafter, with 1
DEG C/h ~ 50 DEG C/h rate promotes the temperature in furnace, it is warming up to 550 DEG C ~ 600 DEG C, 20h ~ 40h is kept the temperature, so that the lithium tantalate
Chip reacts under conditions of high temperature with the reducing agent, restores the lithium tantalate wafer equably, then with 1
DEG C/h ~ 50 DEG C/h rate reduces the temperature in furnace, when temperature is lower than 100 DEG C, stop vacuumizing, to air pressure in furnace and outer
The crucible is taken out from the vacuum reduction furnace after boundary is equal, the lithium tantalate wafer after taking out reduction in crucible.
Preferably, the thickness of the lithium tantalate wafer is at least 0.7mm.
Preferably, in the preparation of the reducing agent the step of, the partial size peak value of the reducing agent is no more than 150 μm, and
And the quantity of particle of the partial size less than 50 μm is greater than the quantity 50% of whole particles of the reducing agent in the reducing agent, it is described
The mobility of reducing agent is not less than 50g/40s.
Preferably, the crucible is cylindrical crucible, and the diameter of the crucible is greater than the diameter of the lithium tantalate wafer
20mm。
Preferably, the material of the crucible is silicon carbide, boron nitride, aluminium nitride, any one in aluminium oxide.
Preferably, in the shove charge the step of, the reducing agent of the lowest level spreading of the crucible with a thickness of 5mm, institute
State the reducing agent of spreading between lithium tantalate wafer with a thickness of 1mm, the thickness of the reducing agent of top layer's spreading of the crucible is big
In 15mm.
Preferably, the vacuum reduction furnace is tube type vacuum reduction furnace, and the temperature uniformity of the vacuum reduction furnace is ± 5
℃。
The present invention keeps the reducing agent being prepared into using preferable mobility under the higher fusing point of lanthana powder and high temperature
Mobility, avoid lanthanum powder from making to come into full contact with lithium tantalate wafer because agglomerating under the high temperature conditions, using week reduction
Lanthanum powder and lanthana powder as reducing agent, the lithium tantalate wafer for avoiding big thickness generates excessive internal stress in reduction, mentions
The high yield rate of the big thickness lithium tantalate wafer of production.
Detailed description of the invention
Fig. 1 is the manufacturing method flow chart of the big thickness lithium tantalate wafer of a better embodiment.
Fig. 2 is the schematic diagram for the mode that the lithium tantalate wafer after the reducing agent, cleaning is packed into the crucible.
In figure: manufacturing method step S100 ~ S104 of big thickness lithium tantalate wafer, crucible 20, lithium tantalate wafer 21, reduction
Agent 22.
Specific embodiment
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be apparent that, drawings in the following description are some embodiments of the invention, common for this field
For technical staff, without creative efforts, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is please referred to, is the manufacturing method of the big thickness lithium tantalate wafer of a better embodiment, including following step
It is rapid:
The preparation of lithium tantalate wafer: lithium tantalate is first pressed scheduled size well cutting, obtains several tantalums by step S100
Sour lithium chip 21, wherein the thickness of lithium tantalate wafer 21 is at least 0.7mm；
Cleaning: step S101 thoroughly removes the dirt on the surface of all lithium tantalate wafers 21, and dry all lithium tantalates are brilliant
Then all lithium tantalate wafers 21 are placed in dustless environment for use by piece 21；
The preparation of reducing agent: step S102 the lanthanum powder that purity is 90% ~ 99.99% is put into vacuum drying oven, at 120 DEG C
Temperature under the conditions of dry 12 to 30 hours, by purity be 90% ~ 99.99% lanthana powder be put into vacuum drying oven, at 120 DEG C
Temperature under the conditions of dry 12 to 30 hours, to remove moisture removal, prevent the moisture in the lanthanum powder or the lanthana powder from participating in
Reduction reaction and influence reduction effect；The lanthanum powder is mixed into the lanthana powder after drying and is mixed to get to also
Former agent 22, wherein the incorporation of the lanthanum powder are as follows: the gross mass of the lanthanum powder accounts for the percentage of the gross mass of the lanthana powder
Are as follows: 5% ~ 15%；Obtain reducing agent 22；
In one embodiment, lanthanum powder and lanthana powder can be put into the same vacuum drying oven simultaneously and is dried, it can also
With individually, be respectively dried.
In this step, by mixing lanthana powder into lanthanum powder, using under the higher fusing point of lanthana powder and high temperature
Preferable mobility keeps the mobility of reducing agent 22 being prepared into, and avoids lanthanum powder and agglomerates under the high temperature conditions and make lanthanum powder
It cannot be come into full contact with lithium tantalate wafer 21.
Step S103, shove charge: in the bottom of crucible 20 equably one layer of the spreading reducing agent 22, then by a piece of cleaning
Lithium tantalate wafer 21 after drying takes out from dustless environment, and is placed on the reducing agent 22 of the bottom spreading of crucible 20 immediately
Top, to avoid the lithium tantalate wafer 21 adsorption dust and influence reduction effect, be then placed on crucible 20
Bottom the lithium tantalate wafer 21 top equably one layer of the spreading reducing agent 22 again, then spilt reducing agent in the paving
Another lithium tantalate wafer 21 is placed in the top of 22 lithium tantalate wafer 21, and so on, completion places tantalic acid in crucible 20
Lithium chip 21 and the reducing agent 22 described in spreading between lithium tantalate wafer 21 will be equipped with reducing agent 22 and several lithium tantalates later
The crucible 20 of chip 21 is put into vacuum reduction furnace；
Reduction: step S104 vacuumizes the burner hearth of the vacuum reduction furnace, by the pressure control in furnace in 20Pa
Hereinafter, the temperature in furnace is promoted with 1 DEG C/h ~ 50 DEG C/h rate to avoid the progress of the oxygen interference reduction reaction in air,
550 DEG C ~ 600 DEG C are warming up to, 20h ~ 40h is kept the temperature, so that the lithium tantalate wafer is sent out under conditions of high temperature with the reducing agent
Raw reaction, restores the lithium tantalate wafer equably, then reduces the temperature in furnace with 1 DEG C/h ~ 50 DEG C/h rate, when
When temperature is lower than 100 DEG C, stop vacuumizing, takes out crucible from the vacuum reduction furnace after the air pressure in furnace is equal with the external world
20, the lithium tantalate wafer 21 after taking out reduction in crucible 20.
Further, in the preparation of the reducing agent the step of, the partial size peak value of reducing agent 22 is no more than 150 μm, and
The quantity of particle of the partial size less than 50 μm is greater than the 50% of the quantity of whole particles in reducing agent 22, reducing agent in reducing agent 22
22 mobility is not less than 50g/40s, so that reducing agent 22 can come into full contact in reduction process with lithium tantalate wafer 21；
In the present embodiment, crucible 20 is cylindrical crucible, and the diameter of crucible 20 is greater than the diameter of lithium tantalate wafer 21
20mm, so that the reducing agent 22 in crucible 20 can bury lithium tantalate wafer 21 completely, the material of crucible 20 is silicon carbide, nitridation
Boron, aluminium nitride, any one in aluminium oxide, occur to avoid the material and reducing agent 22 or lithium tantalate that crucible 20 is made
Reaction, also makes crucible 20 be resistant to high temperature.
Further, in the shove charge the step of, the reducing agent 22 of the lowest level spreading of crucible 20 with a thickness of 5mm, tantalum
Between sour lithium chip 21 reducing agent 22 of spreading with a thickness of 1mm, the thickness of the reducing agent 22 of top layer's spreading of crucible 20 is big
In 15mm, thicker one layer of reducing agent 22 is covered by spreading, can not only guarantee that the lithium tantalate wafer 21 of top layer restores completely,
Moreover, the lithium tantalate wafer 21 of top layer can also be protected, compared with the reducing agent 22 of thick-layer to avoid the lithium tantalate wafer of top layer
21 temperature rises too fast and cracks, and the vacuum reduction furnace is tube type vacuum reduction furnace, the furnace of the vacuum reduction furnace
Warm uniformity is ± 5 DEG C.In this step, by improving the vacuum degree in reduction furnace, the oxygen pair in air is effectively reduced
The interference of reduction reaction.
The manufacturing method of big thickness black lithium tantalate wafer provided by the invention utilizes the higher fusing point of lanthana powder and height
Preferable mobility under temperature, keeps the mobility of reducing agent being prepared into, and lanthanum powder is avoided to make not because agglomerating under the high temperature conditions
It can be come into full contact with lithium tantalate wafer, using the lanthanum powder and lanthana powder of week reduction as reducing agent, avoid big thickness
Lithium tantalate wafer generates excessive internal stress in reduction, improves the yield rate for producing big thickness lithium tantalate wafer.
The diameter of embodiment one, lithium tantalate wafer is 100mm, with a thickness of 0.8mm, lanthanum powder and lanthana in the reducing agent
The mass ratio of powder is 5:95, and the material of crucible is silicon carbide, and it is highly 140mm that the diameter of crucible, which is 120mm, vacuum reduction furnace
Interior air pressure is 18Pa, the temperature adjustment step in the vacuum reduction furnace are as follows: by room temperature to 550 DEG C, the speed of heating is 50
DEG C/h, 20h is kept the temperature, is cooled to 100 DEG C, the speed of cooling is 50 DEG C/h, and the vacuum reduction furnace is made after stopping vacuumizing certainly
So cooling, temperature is cooled to room temperature, comes out of the stove, state when lithium tantalate wafer is come out of the stove are as follows: brown is presented, color is uniform, does not split
The generation of line, resistivity are 2.8 × 1012Ω·cm。
The diameter of embodiment two, lithium tantalate wafer is 100mm, with a thickness of 0.8mm, lanthanum powder and lanthana in the reducing agent
The mass ratio of powder is 10:90, and the material of crucible is silicon carbide, and it is highly 140mm that the diameter of crucible, which is 120mm, vacuum reduction furnace
Interior air pressure is 15Pa, the temperature adjustment step in the vacuum reduction furnace are as follows: by room temperature to 580 DEG C, the speed of heating is 50
DEG C/h, 40h is kept the temperature, is cooled to 100 DEG C, the speed of cooling is 50 DEG C/h, and the vacuum reduction furnace is made after stopping vacuumizing certainly
So cooling, temperature is cooled to room temperature, comes out of the stove, state when lithium tantalate wafer is come out of the stove are as follows: brownish black is presented, color is uniform, does not have
The generation of crackle, resistivity are 1.4 × 1011Ω·cm。
The diameter of embodiment three, lithium tantalate wafer is 100mm, with a thickness of 0.8mm, lanthanum powder and lanthana in the reducing agent
The mass ratio of powder is 15:85, and the material of crucible is silicon carbide, and it is highly 140mm that the diameter of crucible, which is 120mm, vacuum reduction furnace
Interior air pressure is 15Pa, the temperature adjustment step in the vacuum reduction furnace are as follows: by room temperature to 570 DEG C, the speed of heating is 50
DEG C/h, 40h is kept the temperature, is cooled to 100 DEG C, the speed of cooling is 50 DEG C/h, and the vacuum reduction furnace is made after stopping vacuumizing certainly
So cooling, temperature is cooled to room temperature, comes out of the stove, state when lithium tantalate wafer is come out of the stove are as follows: brownish black is presented, color is uniform, does not have
The generation of crackle, resistivity are 3.9 × 1010Ω·cm。
In the embodiment above, by adjusting the mass ratio of lanthanum powder and lanthana powder, at the same control the temperature in reduction furnace,
Vacuum degree, to control the resistivity of the big thickness lithium tantalate wafer after reduction, and, the results showed that, after being restored using this method
Big thickness lithium tantalate wafer color it is uniform, the not generation of crackle, and resistivity and light transmission rate are significantly reduced, we
Method effectively prevents the big internal stress that the lithium tantalate wafer of big thickness was generated in reduction under the premise of guaranteeing also proper mass
And it damages.
Claims (7)
1. a kind of manufacturing method of big thickness black lithium tantalate wafer, it is characterised in that the following steps are included:
The preparation of lithium tantalate wafer: lithium tantalate is first pressed into scheduled size well cutting, obtains several lithium tantalate wafers；
Cleaning: the dirt on the surface of all lithium tantalate wafers, and dry all lithium tantalate wafers are thoroughly removed, then
All lithium tantalate wafers are placed in dustless environment for use；
The preparation of reducing agent: the lanthanum powder that purity is 90% ~ 99.99% is put into vacuum drying oven, is dried under the conditions of 120 DEG C of temperature
It is 12 to 30 hours dry；The lanthana powder that purity is 90% ~ 99.99% is put into vacuum drying oven, is dried under the conditions of 120 DEG C of temperature
It is 12 to 30 hours dry；The lanthanum powder is mixed into the lanthana powder after drying and is mixed to get reducing agent is arrived, wherein institute
State the incorporation of lanthanum powder are as follows: the gross mass of the lanthanum powder accounts for the percentage of the gross mass of the lanthana powder are as follows: 5% ~ 15%；It utilizes
Preferable mobility under the higher fusing point of lanthana powder and high temperature, to keep lanthanum powder and lithium tantalate wafer to come into full contact with；
Shove charge: the bottom of crucible equably one layer of spreading it is above-mentioned prepare resulting reducing agent, then will be after a piece of cleaning-drying
The lithium tantalate wafer taken out from dustless environment, and be placed on the top of the reducing agent of the bottom spreading of crucible immediately,
To avoid the lithium tantalate wafer adsorption dust and influence reduction effect, then in the tantalum for being placed on crucible bottom
The top of sour lithium chip again equably one layer of spreading it is above-mentioned prepare resulting reducing agent, then spilt the lithium tantalate of reducing agent in the paving
Another lithium tantalate wafer is placed in the top of chip, and so on, the lithium tantalate wafer, simultaneously is placed in completion in the crucible
The reducing agent described in spreading between lithium tantalate wafer will be equipped with the crucible of the reducing agent and several lithium tantalate wafers later
It is put into vacuum reduction furnace；
Reduction: the burner hearth of the vacuum reduction furnace is vacuumized, by the pressure control in furnace in 20Pa hereinafter, with 1 DEG C/h ~
The rate of 50 DEG C/h promotes the temperature in furnace, is warming up to 550 DEG C ~ 600 DEG C, 20h ~ 40h is kept the temperature, so that the lithium tantalate wafer exists
It reacts under conditions of high temperature with the reducing agent, restores the lithium tantalate wafer equably, then with 1 DEG C/h ~ 50
DEG C/rate of h reduces the temperature in furnace, when temperature is lower than 100 DEG C, stops vacuumizing, it is equal with the external world to the air pressure in furnace
The crucible is taken out from the vacuum reduction furnace afterwards, the lithium tantalate wafer after taking out reduction in crucible.
2. the manufacturing method of big thickness black lithium tantalate wafer as described in claim 1, it is characterised in that: the lithium tantalate is brilliant
The thickness of piece is at least 0.7mm.
3. the manufacturing method of big thickness black lithium tantalate wafer as described in claim 1, it is characterised in that: in the reducing agent
Preparation the step of in, the partial size peak value of the reducing agent is no more than 150 μm, and in the reducing agent partial size less than 50 μm
The quantity of particle is greater than the quantity 50% of whole particles of the reducing agent, and the mobility of the reducing agent is not less than 50g/40s.
4. the manufacturing method of big thickness black lithium tantalate wafer as described in claim 1, it is characterised in that: the crucible is circle
Skittele pot, the diameter of the crucible are greater than the diameter 20mm of the lithium tantalate wafer.
5. the manufacturing method of big thickness black lithium tantalate wafer as described in claim 1, it is characterised in that: the material of the crucible
Matter is silicon carbide, boron nitride, aluminium nitride, any one in aluminium oxide.
6. the manufacturing method of big thickness black lithium tantalate wafer as described in claim 1, it is characterised in that: in the shove charge
In step, the reducing agent of the lowest level spreading of the crucible with a thickness of 5mm, the reducing agent of spreading between the lithium tantalate wafer
With a thickness of 1mm, the thickness of the reducing agent of top layer's spreading of the crucible is greater than 15mm.
7. the manufacturing method of big thickness black lithium tantalate wafer as described in claim 1, it is characterised in that: the vacuum reduction
Furnace is tube type vacuum reduction furnace, and the temperature uniformity of the vacuum reduction furnace is ± 5 DEG C.
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| JP3938147B2 (en) * | 2003-04-08 | 2007-06-27 | 住友金属鉱山株式会社 | Lithium tantalate substrate and manufacturing method thereof |
| US7374612B2 (en) * | 2003-09-26 | 2008-05-20 | Shin-Etsu Chemical Co., Ltd. | Method of producing single-polarized lithium tantalate crystal and single-polarized lithium tantalate crystal |
| JP4063190B2 (en) * | 2003-10-16 | 2008-03-19 | 住友金属鉱山株式会社 | Method for producing lithium tantalate substrate |
| JP2005119907A (en) * | 2003-10-16 | 2005-05-12 | Sumitomo Metal Mining Co Ltd | Lithium tantalate substrate and its producing method |
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| CN101574741B (en) * | 2009-06-25 | 2011-05-18 | 宁夏东方钽业股份有限公司 | Preparation method of tantalum powder for capacitor |
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| CN105463581B (en) * | 2015-11-30 | 2018-02-13 | 上海召业申凯电子材料有限公司 | The Darkening process method of lithium tantalate substrate |
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