CN110760934B - Lithium tantalate wafer blackening device and use method thereof - Google Patents
Lithium tantalate wafer blackening device and use method thereof Download PDFInfo
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- CN110760934B CN110760934B CN201911180646.1A CN201911180646A CN110760934B CN 110760934 B CN110760934 B CN 110760934B CN 201911180646 A CN201911180646 A CN 201911180646A CN 110760934 B CN110760934 B CN 110760934B
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- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 25
- 235000012431 wafers Nutrition 0.000 claims description 139
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 76
- 229910052757 nitrogen Inorganic materials 0.000 claims description 38
- 239000003638 chemical reducing agent Substances 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 abstract 2
- 238000006243 chemical reaction Methods 0.000 description 16
- 230000008569 process Effects 0.000 description 10
- 238000006722 reduction reaction Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000028161 membrane depolarization Effects 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a lithium tantalate wafer blackening device and a use method thereof. Including holding the pipe to and place at the inside wafer placer of holding the pipe, wafer placer includes bottom plate, apron and sets up a plurality of jigs between the two, wafer placer passes through the bottom plate level and places inside the holding the pipe, the tool is cyclic annular structure and all has seted up logical groove at its cyclic annular structure's two terminal surfaces, and a plurality of jigs overlap the level and place on the bottom plate, and the logical groove staggered arrangement between the adjacent tool, the apron still is provided with the pouring weight near one side of tool, the pouring weight is matchd with the tool inner ring that can imbed the tool inner ring. The invention improves the blackening uniformity of the lithium tantalate wafer.
Description
Technical Field
The invention relates to the field of wafer processing, in particular to a lithium tantalate wafer blackening device and a use method thereof.
Background
The lithium tantalate wafer is a typical multifunctional material, has good physical characteristics of piezoelectricity, ferroelectric electricity, pyroelectric electricity, acousto-optic, electro-optic, photorefractive, nonlinearity and the like, and is widely applied to the fields of surface acoustic wave devices, optical communication, laser and photoelectron. The lithium tantalate wafer has a large piezoelectric coefficient and is therefore suitable for manufacturing substrates for low insertion loss saw filters.
The lithium tantalate wafer has high pyroelectric coefficient, so that the temperature change can cause a large amount of static charges to be generated on the surface of the wafer, the static charges can be automatically released among the wafers, particularly between the interdigital electrodes, and the problems of cracking of the lithium tantalate wafer, burning of the interdigital electrodes and the like can occur to a certain extent. Because the lithium tantalate wafer is colorless and transparent, diffuse reflection can be generated when the photoetching process is carried out, so that the electrode line accuracy is reduced. The lithium tantalate wafer is subjected to reduction treatment, so that accumulation of static charge on the surface of the wafer can be effectively avoided, and the pyroelectric effect is obviously reduced. The lithium tantalate wafer after such reduction treatment is brown or even black, and is thus called blackened, while the accuracy of the photolithography process is improved.
At present, the blackening treatment mainly adopts a method that lithium tantalate wafers are buried in powder formed by reducing agents, the low-temperature treatment is carried out, nitrogen is filled to take away reaction products after the blackening reaction, the reducing agents comprise C, si, mg, al, fe, lithium carbonate, magnesium carbonate, calcium carbonate and the like, the reducing agents around the wafers are different in quantity, and the blackening effect and depolarization condition are obviously different due to the distribution of the nitrogen in a heat treatment furnace, so that the uniformity of the blackening reduction reaction is influenced. The patent CN205662628U adopts a device to place the wafer, which ensures that the periphery of the wafer is in the same reducing agent powder, but the part of the wafer placing frame contacting the wafer will generate uneven reaction in the blackening process, which results in uneven blackening of the wafer, and the blackening uniformity is very important in practical application and needs to be improved.
Disclosure of Invention
The invention aims at: the invention provides a lithium tantalate wafer blackening device and a use method thereof, which are used for controlling the blackening uniformity of a lithium tantalate wafer and solving the problem of non-uniformity in the blackening process of the lithium tantalate wafer.
The technical scheme adopted by the invention is as follows:
the invention discloses a lithium tantalate wafer blackening device which comprises a containing tube and a wafer placing device placed in the containing tube, wherein the wafer placing device comprises a bottom plate, a cover plate and a plurality of jigs arranged between the bottom plate and the cover plate, the wafer placing device is horizontally placed in the containing tube through the bottom plate, the jigs are of annular structures, through grooves are formed in two end faces of the annular structures of the jigs, the jigs are horizontally placed on the bottom plate in an overlapping mode, the through grooves between the adjacent jigs are staggered, a weight is further arranged on one side of the cover plate, close to the jigs, and the weight is matched with the inner ring of the jigs and can be embedded into the inner ring of the jigs.
In the prior art, for wafer blackening, a device for containing a wafer is needed, but a part of the device for containing the wafer, which contacts the wafer, can generate a blackening uneven reaction in the blackening process, while the invention comprises a containing tube and a wafer placing device, wherein Cheng Zhuangguan is a container of the wafer placing device used for containing the wafer on a heat treatment furnace, a plurality of devices for placing lithium tantalate wafers and embedding reducing agent powder wafers can be placed in the containing tube, the wafer placing device comprises a bottom plate, a cover plate and a plurality of annular-structure jigs, reducing agent powder is paved in the jigs, the lithium tantalate wafers are paved at the same position of the jigs, the jigs are overlapped together, the surrounding of the lithium tantalate wafers is in the reducing agent powder environment with the same mass, and the thickness of the reducing agent is equal among the lithium tantalate wafers. The jig is provided with the through grooves, so that gaps are formed between the adjacent jigs, nitrogen can enter the reducing agent in the jig from the through grooves to take away reaction products in the blackening reaction process, the through grooves between the adjacent jigs are staggered and are not overlapped with each other, so that the gaps of the nitrogen entering the inside of the jig are more, the nitrogen is dispersed, and the uniform passing of the nitrogen among the lithium tantalate wafers is ensured. The weight is embedded in the inner ring of the jig at the uppermost end, and the cover plate is covered on the weight to strengthen the powdery reducing agent, so that the thickness and the shape of the reducing powder are consistent, the reducing agent powder is prevented from being fluffy and deformed in the blackening reaction process of the lithium tantalate wafer, and the blackening reduction reaction of the lithium tantalate wafer is uniform.
Further, the upper end face and the lower end face of the jig are provided with at least 2 through grooves, and the through grooves of the upper end face of the jig correspond to the through grooves of the lower end face one by one. By adopting the structure, the through grooves on the upper end face and the lower end face of the jig enable gaps to be formed between the jig and the adjacent jigs stacked on the two end faces of the jig, so that the jigs can be randomly selected to be stacked, and the front side and the back side of the jigs during stacking do not need to be considered.
Furthermore, both end faces of the jig are of a plane structure. By adopting the structure, the jig is convenient to stack stably with the adjacent jigs.
Further, the bottom plate is a rectangular plane plate. By adopting the structure, the wafer placement devices are horizontally placed in the containing tubes through the rectangular plane plates, and the adjacent wafer placement devices are compactly arranged and placed in the containing tubes.
Further, the jig is made of stainless steel materials. The stainless steel jig is heat-resistant, corrosion-resistant and long in service life, and is suitable for the wafer blackening reaction environment.
Further, the end surfaces at the two ends of the containing tube are also provided with heat insulation pads matched with the tube orifice. In the blackening reaction process of the wafer, the lithium tantalate wafer in the accommodating tube is required to be heated, and the heat insulation pad is arranged at the two ends of the accommodating tube, so that heat is prevented from being dissipated from the two ends of the accommodating tube, and the energy consumption of the heating device is reduced.
Further, the inner wall of the holding tube is also provided with fins.
Further, the fins are spiral and extend to two ends of the containing tube. The adoption of the spiral fin makes the heat insulation pad not contact with the inner wall of the containing tube, the inner wall of the containing tube forms a spiral airflow channel, nitrogen enters the spiral channel inside the containing tube from the spiral channel through the periphery of the heat insulation pad, the spiral channel surrounds the inner wall of the containing tube, nitrogen entering the containing tube diffuses from the inner wall of the containing tube to the center, the jig is ensured to be in a full and uniform nitrogen atmosphere, compared with the nitrogen which is introduced into the center, the upper part and the lower part, the nitrogen is introduced into the containing tube through the structure, the blackening uniformity of the lithium tantalate wafer is further improved, the nitrogen continues to flow towards the other end of the containing tube and flows out through the spiral airflow channel at the other end of the containing tube, and reaction products of the blackening reduction reaction are taken away.
The application method of the lithium tantalate wafer blackening device comprises the following application steps:
s1, placing a jig on a bottom plate, adding reducing agent powder with a fixed mass ratio into the jig, and compacting after strickling;
s2, placing the lithium tantalate wafer on the pressed reducer powder in the jig;
s3, adding reducing agent powder with a fixed mass ratio to cover the lithium tantalate wafer, and compacting after strickling;
s4, repeating the steps S1-S3, and stacking a plurality of jigs and lithium tantalate wafers on the jigs;
s5, embedding a weight into the inner ring of the jig at the uppermost end, covering a cover plate on the weight, and reinforcing and compacting the reducer powder;
s6, placing the whole wafer placing device into a containing tube, filling 2-4L/min of nitrogen, performing heat treatment at the constant temperature of 480-550 ℃ for 3-10h, naturally cooling to room temperature, and taking out the lithium tantalate wafer.
Further, in the step S2, the lithium tantalate wafer is placed in the center of the jig. The distance between the edge of the lithium tantalate wafer and the jig is consistent, and the contact gas quantity of each part of the wafer is ensured to be the same.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
1. the invention relates to a lithium tantalate wafer blackening device, which is characterized in that gaps are formed between adjacent jigs through grooves on the jigs, the through grooves between the adjacent jigs are staggered, so that nitrogen enters the inside of the jigs to be dispersed, the uniform passing of nitrogen among the lithium tantalate wafers is ensured, the passing rate of the nitrogen is ensured, the lithium tantalate wafers are in a reducing agent powder environment with the same quality, the thickness consistency of the reducing agent powder among the lithium tantalate wafers is ensured, the reaction of the lithium tantalate wafers is uniform and sufficient, and the blackening uniformity is ensured.
2. The invention relates to a lithium tantalate wafer blackening device, which is characterized in that a weight is embedded in an inner ring of a jig at the uppermost end, and a cover plate is covered on the weight to strengthen powdery reducing agent, so that the thickness and the shape of reducing powder are consistent, and the blackening reduction reaction of the lithium tantalate wafer is uniform.
3. The invention relates to a lithium tantalate wafer blackening device, which is characterized in that spiral fins are arranged on the inner wall of a containing tube, and heat insulation pads matched with tube orifices are arranged on the end surfaces of two ends of the spiral fins, so that a jig is in a full and uniform nitrogen atmosphere, nitrogen can be more uniformly in the containing tube, and the blackening uniformity of the lithium tantalate wafer is improved.
4. The invention relates to a use method of a lithium tantalate wafer blackening device, wherein a lithium tantalate wafer is placed in the center of a jig, the distance between the edge of the lithium tantalate wafer and the jig is consistent, and the contact gas quantity of each part of the lithium tantalate wafer is ensured to be the same.
Drawings
For a clearer description of the technical solutions of embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and should not be considered limiting in scope, and other related drawings can be obtained according to these drawings without inventive effort for a person skilled in the art, wherein:
FIG. 1 is a schematic view of a wafer placement apparatus of the present invention;
FIG. 2 is a schematic view of the structure of the loading tube of the present invention;
FIG. 3 is a schematic view of the end face of the containment tube of the present invention;
FIG. 4 is a schematic diagram of the flow of nitrogen within Cheng Zhuangguan of the present invention;
FIG. 5 is a schematic diagram of a prior art lithium tantalate wafer after blackening;
fig. 6 is a schematic representation of a lithium tantalate wafer employing the present invention and after blackening.
Reference numerals illustrate: 1-filling tube, 11-fin, 2-wafer placement device, 21-bottom plate, 22-jig, 2201-through groove, 23-cover plate, 24-weight and 3-heat insulation pad.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the particular embodiments described herein are illustrative only and are not intended to limit the invention, i.e., the embodiments described are merely some, but not all, of the embodiments of the invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
It is noted that relational terms such as "first" and "second", and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present invention.
All of the features disclosed in this specification, or all of the steps of a method or process disclosed, may be combined in any combination, except combinations of mutually exclusive features.
The present invention will be described in detail with reference to the accompanying drawings.
Example 1
As shown in fig. 1, 2 and 4, the invention relates to a lithium tantalate wafer blackening device, which comprises a containing tube 1 and a wafer placing device 2 placed in the containing tube 1, wherein the wafer placing device 2 comprises a bottom plate 21, a cover plate 23 and a plurality of jigs 22 arranged between the bottom plate 21 and the cover plate, the wafer placing device 2 is horizontally placed in the containing tube 1 through the bottom plate 21, the jigs 22 are of annular structures, through grooves 2201 are formed in two end faces of the annular structures, the jigs 22 are horizontally placed on the bottom plate 21 in an overlapping mode, the through grooves 2201 between the adjacent jigs 22 are staggered, a weight 24 is further arranged on one side of the cover plate 23, which is close to the jigs 22, and the weight 24 is matched with the inner ring of the jigs 22 and can be embedded into the inner ring of the jigs 22.
In the prior art, for blackening lithium tantalate wafers, a device for containing lithium tantalate wafers is needed, however, blackening non-uniform reaction is generated at the position where the device for containing lithium tantalate wafers contacts the wafers in the blackening process, while the invention comprises a containing tube 1 and a wafer placing device 2, wherein the containing tube 1 is a container for containing the wafer placing device 2 on a heat treatment furnace, in this embodiment, the containing tube 1 is a circular tube, a plurality of tools 22 for containing lithium tantalate wafers and embedding reducing agent powder are contained in the containing tube 1, the wafer placing device 2 comprises a bottom plate 21, a cover plate 23 and a plurality of annular structures, the plurality of tools 22 in this embodiment are of the same specification, reducing agent powder is paved in the tools 22 of the tools, lithium tantalate wafers are paved at the same position of the tools 22, each tool 22 in this embodiment places one lithium tantalate wafer, the plurality of tools 22 are overlapped together, the periphery of lithium tantalate wafers is in the reducing agent powder environment of the same quality, the thickness of the lithium tantalate wafers is equal, and the uppermost tools 22 of the lithium tantalate wafers are placed at the same end. The jig 22 of the invention is provided with the through grooves 2201, so that gaps are formed between the adjacent jigs 22, nitrogen can enter the reducing agent in the jig 22 from the through grooves 2201 to take away reaction products in the blackening reaction process, the through grooves 2201 between the adjacent jigs are staggered and are not overlapped with each other, so that the gaps for entering the inside of the jig 22 by the nitrogen are more, the nitrogen is more dispersed, and the uniform passing of the nitrogen among the lithium tantalate wafers is ensured. The weight 24 is embedded in the inner ring of the jig 22 at the uppermost end, and the cover plate 23 is covered on the weight 24 to strengthen the powdery reducing agent, so that the thickness and the shape of the reducing powder are consistent, the reducing agent powder is prevented from being fluffy and deformed in the blackening reaction process of the lithium tantalate wafer, and the blackening reduction reaction of the lithium tantalate wafer is uniform. The thickness consistency of the reducer powder among the lithium tantalate wafers and the gaps among the jigs ensure the passing rate of gas, the reaction of the lithium tantalate wafers is uniform and sufficient, and the blackening uniformity is ensured.
Example 2
This example is a further illustration of the invention.
As shown in fig. 1, in this embodiment, in a preferred embodiment of the present invention, at least 2 through slots 2201 are disposed on the upper and lower end surfaces of the jig 22, and the through slots 2201 on the upper end surface of the jig 22 and the through slots 2201 on the lower end surface are in one-to-one correspondence. By adopting the structure, the through grooves 2201 on the upper end face and the lower end face of the jig 22 enable gaps to be formed between the jig 22 and the adjacent jigs 22 stacked on the two end faces of the jig 22, so that the jig 22 can be randomly selected to be stacked without considering the front side and the back side of the jig 22 when being stacked.
Example 3
This example is a further illustration of the invention.
In the preferred embodiment of the present invention, the two end surfaces of the jig 22 are both planar structures. By adopting the structure, the jig 22 and the adjacent jigs 22 can be stacked stably.
Example 4
This example is a further illustration of the invention.
This embodiment is based on the above embodiment, and in a preferred embodiment of the present invention, the bottom plate 21 is a rectangular flat plate. By adopting the structure, the wafer placement device 2 is conveniently placed in the accommodating tube 1 horizontally through the rectangular plane plate, and the adjacent wafer placement devices 2 are conveniently placed in the accommodating tube 1 in a compact arrangement.
Example 5
This example is a further illustration of the invention.
In this embodiment, based on the foregoing embodiment, in a preferred embodiment of the present invention, the jig 22 is made of stainless steel. The stainless steel jig 22 is heat-resistant, corrosion-resistant, long in service life and suitable for the blackening reaction environment of lithium tantalate wafers.
Example 6
This example is a further illustration of the invention.
As shown in fig. 2-4, in this embodiment, on the basis of the above embodiment, in a preferred embodiment of the present invention, the end surfaces of the two ends of the containing tube 1 are further provided with heat insulation pads 3 matched with the tube orifice. In the blackening reaction process of the lithium tantalate wafer, the lithium tantalate wafer in the accommodating tube 1 is required to be heated, and in the invention, the lithium tantalate wafer is subjected to heat treatment at the constant temperature of 480-550 ℃, and the heat insulation pads 3 are arranged at the two ends of the accommodating tube 1, so that heat is prevented from being dissipated from the two ends of the accommodating tube 1, and the energy consumption of a heating device is reduced.
In a preferred embodiment of the present invention, the inner wall of the holding tube 1 is further provided with fins 11.
In a preferred embodiment of the present invention, the fins 11 are spiral and extend to both ends of the tube 1. The adoption of the spiral fins 11 ensures that the heat insulation pad 3 is not in contact with the inner wall of the containing tube 1, the inner wall of the containing tube 1 forms a spiral airflow channel, nitrogen enters the spiral channel inside the containing tube 1 from the spiral channel through the periphery of the heat insulation pad 3, the spiral channel surrounds the inner wall of the containing tube 1, the nitrogen entering the containing tube 1 diffuses from the inner wall of the containing tube 1 to the center, the jig 22 is ensured to be in a full and uniform nitrogen atmosphere, compared with the nitrogen which is introduced in the center, the upper part and the lower part, the nitrogen is filled in the structure, the nitrogen can be more uniform in the containing tube 1, the blackening uniformity of lithium tantalate wafers is further improved, the nitrogen continues to flow towards the other end of the containing tube, and flows out through the spiral airflow channel at the other end of the containing tube 1 so as to take away reaction products of the blackening reduction reaction.
In the invention, the flow rate of nitrogen is 2-4L/min, and the preferred flow rate of nitrogen is 2.5L/min, so that the uniformity of the blackening reaction of the lithium tantalate wafer contacted with nitrogen is ensured, and the cost of nitrogen can be saved.
Example 7
This example is a further illustration of the invention.
The embodiment is based on the foregoing embodiment, and in a preferred embodiment of the present invention, a method for using a lithium tantalate wafer blackening apparatus includes the foregoing lithium tantalate wafer blackening apparatus, and further includes the following steps:
s1, placing a jig 22 on a bottom plate 21, adding reducing agent powder with a fixed mass ratio into the jig 22, and compacting after strickling;
s2, placing the lithium tantalate wafer on the compacted reducer powder in the jig 22;
s3, adding reducing agent powder with a fixed mass ratio to cover the lithium tantalate wafer, and compacting after strickling;
s4, repeating the steps S1-S3, and stacking a plurality of jigs 22 and lithium tantalate wafers on the jigs 22;
s5, embedding a weight 24 into the inner ring of the jig 22 at the uppermost end, covering a cover plate 23 on the weight 24, and reinforcing and compacting the reducer powder;
s6, placing the whole wafer placing device 2 into the containing tube 1, filling 3L/min of nitrogen, performing heat treatment at the constant temperature of 500 ℃ for 7 hours, naturally cooling to room temperature, and taking out the lithium tantalate wafer.
The nitrogen amount in the embodiment not only ensures the uniformity of the contact nitrogen in the blackening reaction of the lithium tantalate wafer, but also can save the cost of the nitrogen.
In a preferred embodiment of the present invention, in the step S2, the lithium tantalate wafer is placed in the center of the jig 22. The distance between the edge of the lithium tantalate wafer and the jig 22 is consistent, so that the contact gas quantity of each part of the lithium tantalate wafer is ensured to be the same.
Example 8
This example is a further illustration of the invention.
The difference between this embodiment and embodiment 7 is that in step S6, the whole wafer placement device 2 is placed in the holding tube 1, 2L/min nitrogen is filled, heat treatment is performed at a constant temperature of 480 ℃ for 3 hours, and the lithium tantalate wafer is taken out after the temperature naturally drops to room temperature.
Example 9
This example is a further illustration of the invention.
The difference between this embodiment and embodiment 7 is that in step S6, the whole wafer placement device 2 is placed in the holding tube 1, 4L/min nitrogen is filled, heat treatment is performed at a constant temperature of 550 ℃ for 10 hours, and the lithium tantalate wafer is taken out after the temperature naturally drops to room temperature.
In the prior art, the uniformity after blackening the lithium tantalate wafer is shown in fig. 5, and the volume resistivity of the test area 1 is as follows: 2 x 10e+14Ω x cm, volume resistivity of test zone 2: 5×10e+13 Ω×cm, volume resistivity of test zone 3: 9×10e+14Ω×cm, volume resistivity of test zone 4: 8×10e+13 Ω×cm, volume resistivity of test zones 5, 6, 7, 8, 9: 2 x 10E+12Ω x cm, and the blackening degree was uneven. After the blackening reduction reaction of the lithium tantalate wafer using the apparatus of the present invention and using the apparatus of the present invention according to any one of examples 7 to 9, the blackening uniformity was as shown in fig. 6, and volume resistivity of test areas 1 to 9: 4.10E+12Ω.cm, and uniform blackening degree.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not creatively contemplated by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope defined by the claims.
Claims (8)
1. A lithium tantalate wafer blackening device, comprising Cheng Zhuangguan (1) and a wafer placing device (2) placed inside a containing tube (1), characterized in that: the wafer placement device (2) comprises a bottom plate (21), a cover plate (23) and a plurality of jigs (22) arranged between the bottom plate and the cover plate, the wafer placement device (2) is horizontally placed inside a containing tube (1) through the bottom plate (21), the jigs (22) are of annular structures, through grooves (2201) are formed in two end faces of the annular structures, the jigs (22) are horizontally placed on the bottom plate (21) in an overlapping mode, the through grooves (2201) between the adjacent jigs (22) are staggered, a weight (24) is further arranged on one side, close to the jigs (22), of the cover plate (23), and the weight (24) can be embedded into the inner ring of the jigs (22) in a matching mode with the inner ring of the jigs (22);
fins (11) are further arranged on the inner wall of the containing tube (1);
the fins (11) are spiral and extend to two ends of the containing tube (1).
2. The lithium tantalate wafer blackening apparatus of claim 1, characterized in that: at least 2 through grooves (2201) are formed in the upper end face and the lower end face of the jig (22), and the through grooves (2201) of the upper end face of the jig (22) correspond to the through grooves (2201) of the lower end face one by one.
3. The lithium tantalate wafer blackening apparatus of claim 1, characterized in that: both end faces of the jig (22) are of a plane structure.
4. The lithium tantalate wafer blackening apparatus of claim 1, characterized in that: the bottom plate (21) is a rectangular plane plate.
5. The lithium tantalate wafer blackening apparatus of claim 1, characterized in that: the jig (22) is made of stainless steel materials.
6. A lithium tantalate wafer blackening apparatus as claimed in claim 2, characterized in that: the end surfaces of the two ends of the containing tube (1) are also provided with heat insulation pads (3) matched with the tube orifice.
7. A method of using a lithium tantalate wafer blackening apparatus comprising the lithium tantalate wafer blackening apparatus of any of claims 1 to 6, characterized by further comprising the steps of:
s1, placing a jig (22) on a bottom plate (21), adding reducing agent powder with a fixed mass ratio into the jig (22), and compacting after strickling;
s2, placing the lithium tantalate wafer on the compacted reducer powder in a jig (22);
s3, adding reducing agent powder with a fixed mass ratio to cover the lithium tantalate wafer, and compacting after strickling;
s4, repeating the steps S1-S3, and stacking a plurality of jigs (22) and lithium tantalate wafers on the jigs (22);
s5, embedding a weight (24) into the inner ring of the jig (22) at the uppermost end, and covering a cover plate (23) on the weight (24) to strengthen and compact the reducer powder;
s6, placing the whole wafer placing device (2) into a containing tube (1), filling 2-4L/min of nitrogen, performing heat treatment at the constant temperature of 480-550 ℃ for 3-10h, naturally cooling to the room temperature, and taking out the lithium tantalate wafer.
8. The method of using a lithium tantalate wafer blackening apparatus of claim 7, characterized in that: in the step S2, the lithium tantalate wafer is placed in the center of the jig (22).
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