CN106676624B - A kind of guided mode processing method of flaky sapphire - Google Patents
A kind of guided mode processing method of flaky sapphire Download PDFInfo
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- CN106676624B CN106676624B CN201710208044.7A CN201710208044A CN106676624B CN 106676624 B CN106676624 B CN 106676624B CN 201710208044 A CN201710208044 A CN 201710208044A CN 106676624 B CN106676624 B CN 106676624B
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/34—Edge-defined film-fed crystal-growth using dies or slits
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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
- C30B29/20—Aluminium oxides
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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 present invention relates to sapphire processing technology fields, and in particular to a kind of guided mode processing method of flaky sapphire mainly includes step are as follows: (1) feedstock processing；(2) furnace body is cleared up；(3) raw material is filled；(4) furnace body vacuumizes；(5) high temperature seeding；(6) necking down；(7) expand shoulder；(8) isodiametric growth；(9) processes such as annealing cooling, on the one hand reduce the impurity in crystal growing process, crystal are avoided to be contaminated, and improve crystal purity；On the other hand, so that crystal is reduced the generation of bubble in fusion process, raw material is subjected to compacting filling according to a certain percentage, reduces the presence in raw material gap, so that the bubble for reducing growth crystal generates probability, improve crystal quality；In another aspect, by high temperature seeding, necking down, expanding shoulder, isodiametric growth and annealing cooling process, make to reduce cracking and the generation of dislocation, glass fragment striped and genetic defect in crystal growing process, to improve crystal quality.
Description
Technical field
The present invention relates to sapphire processing technology fields, and in particular to a kind of guided mode processing method of flaky sapphire.
Background technique
Sapphire English name is Sapphire, is derived from Latin Spphins, means blue；Belong to corundum race mineral,
Trigonal system.Assorted Gem Grade corundum except ruby is referred to as sapphire by jewel circle.Sapphire and ruby, emerald
Jinsui River bodhi tourmaline, smooth Sang Shi etc. belong to colored gemstone category.
Because containing the microelements such as iron (Fe) and titanium (Ti) in corundum, and the colors such as blue, sky blue, pale blue are presented, wherein with
Bright-coloured sky blue person is best.Sapphire mineral name is corundum, belongs to corundum race mineral.Jewel actually in nature
For grade corundum in addition to red title ruby, remaining various colors is such as blue, light blue, green, yellow, grey, colourless, claims
For sapphire.Sapphire chemical component (Al2O3), mainly with Fe, Ti, coloring.
Sapphire ingredient is aluminium oxide, because of (the Ti containing Trace Element Titanium4+) or iron (Fe2+) and it is blue.Belong to three prismatic crystals
System.Crystal habit is often cylindrical in shape, short cylinder, plate etc., and solid is mostly granular or compact massive.It is clear to translucent, glass
Gloss.Index of refraction 1.76~1.77, birefringence 0.008, dichroism is strong.Heterogeneous body.Sometimes there is special optical effect-
Asterism.Hardness is 9,3.95~4.1 grams/cc of density.It is cut in cabochon, inside is rich in parallel with bottom surface and fixed
To arrangement three groups of backpack bodies when, when can produce beautiful six-pointed star, referred to as " starlight sapphire ".
Existing sapphire crystal guided mode processing method is in specific production process, and there are the following problems: on the one hand, due to original
Material processing is not clean enough and furnace body cleaning is not thorough enough, causes crystal guided mode processing quality to be affected, there are crystals
Impurity reduces flat crystal purity；On the other hand, it is filled in crucible due to raw material not closely knit enough, causes to exist inside melt
Aeration crystal quality；In another aspect, the controlling of production process due to flat crystal is improper, cause under crystal production quality
Drop occurs being cracked or the deficiencies of crystal dislocation is serious.
Therefore, based on above-mentioned, the present invention provides a kind of guided mode processing method of flaky sapphire, is deposited with solving the prior art
The bad deficiency and defect of EFG technique production flat crystal quality.
Summary of the invention
The object of the invention is that: for presently, there are the above problem, the guided mode for providing a kind of flaky sapphire adds
Work method, to solve EFG technique production flat crystal quality of the existing technology bad deficiency and defect.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of guided mode processing method of flaky sapphire, includes the following steps:
(1) feedstock processing: alumina raw material is cleaned by ultrasonic 20min by acetone first, then clear with dehydrated alcohol ultrasound
10min is washed, then is cleaned by ultrasonic 10min with deionized water, raw material is subjected to cleaning treatment；Raw material is blown after having cleaned using nitrogen
It is dry, raw material is placed in drying 1h~1.5h, the concentrated hydrochloric acid for being then 36%-38% with mass fraction by raw material in 120 DEG C of baking ovens
26h~30h is impregnated, is placed in clear water reserviors and is rinsed to neutrality after immersion, places into and dries 1h~2h in silica crucible；
(2) furnace body is cleared up: before guided mode processes flaky sapphire, being endured strict scrutiny first to furnace body, by checking
Mode is understood furnace interior with the presence or absence of foreign matter or sundries, and is cleaned the sundries of furnace interior using cleaning agent, will be miscellaneous
Object or foreign matter are cleaned out；Then, furnace body heater switch is opened, furnace body is preheated using 80 DEG C of in-furnace temperatures, by furnace
The remaining moisture in internal portion is evaporated, and dries furnace interior；Impurity or foreign matter to effectively avoid furnace interior is to crystal
It pollutes, influences crystal quality, while also reducing a possibility that impurity is precipitated in furnace；
(3) raw material is filled: raw material is filled in crucible, raw material uses powder raw material and block stock quality proportioning for 3:
7 mode carries out dense packing effect；Crucible bottom first splices one layer of block stock of filling, and powder raw material is then filled in blocky original
The gap and upper surface of material, and be compacted；Then it is further continued for sprawling assembled block stock and powder raw material, makes to be formed in crucible
The raw material of compacting；So it can make melting sources speed faster, bubble existing for melt inside is less；
(4) furnace body vacuumizes: closing the gas vent of crystal growth equipment, opens mechanical pump pumping, and rise to furnace body
Temperature heating；After furnace body vacuumizes 1h-2h, argon gas switch valve is opened, applying argon gas is carried out to furnace body inner cavity, is made at furnace interior
In the state of argon gas protection；The purpose of argon atmosphere is vacuumized and is passed through, primarily to preventing molybdenum or iridium crucible and mould
Tool is oxidized under the high temperature conditions, while being prevented molybdenum or iridium and other residual gas from reacting and being generated volatile object
Matter impacts wafer quality；Argon gas, which is filled with, effectively to avoid melt from decomposing and evaporate under high-temperature low-pressure
Phenomenon occurs；
(5) high temperature seeding: the intermediate frequency power supply of furnace body being switched and is opened, and carries out furnace body heating heating；Heat up heating process are as follows:
Furnace body is risen to 300 DEG C with the heating rate of 5 DEG C/min first, keeps 5min~10min；Then use heating rate for 10
DEG C/heating method of min, furnace body temperature is risen to 1000 DEG C, keeps the temperature 10min-15min；Finally using 15 DEG C/min~20 DEG C/
The heating rate of min is heated to 2000 DEG C, and after keeping the temperature 5min, adjustment heating rate is 10 DEG C/min, and in-furnace temperature is risen to
2100 DEG C~2150 DEG C；After being completely melt to raw material, seed crystal is mounted on lifting rod, is moved down at a slow speed, seed crystal is made
Bottom end and mould upper surface are at a distance of 5mm~6mm；Furnace body temperature is dropped to 2050 DEG C, seed crystal is preheated, to prevent hot punching
It hits；It is 2~3 times that seed crystal, which preheats number, when fusing sign and then secondary cooling preheating, each preheating time occurs in seed crystal bottom end
It is spaced 1min~2min；After preheating is completed, seed crystal is lifted upwards, furnace body temperature is risen to 2100 DEG C~2150 DEG C again,
Start seeding；Seed crystal descending at slow speed is contacted with bath surface, makes the sheet-like melt and the abundant welding of seed crystal positioned at die surface,
Form an entirety；
(6) necking down: gradually promoting 1.5mm/h~2mm/h for pull rate, at the same melt temperature increased at a slow speed 15 DEG C~
20 DEG C, necking down is carried out to chip；The effect of necking down is: can reduce the genetic defect in seed crystal, pass through necking down process, crystal
Any non axial dislocation can be by successive elimination；The temperature of necking process is excessively high, the easy rapid melting of seed crystal；Necking down temperature
It is too low, then it is unobvious to will lead to necking down effect；
(7) expand shoulder: after necking down, the pull rate of guided mode equipment being subjected to reduction of speed adjustment, is reduced to pull rate
4.5mm/h~5mm/h starts to expand shoulder；Expand during shoulder, furnace body temperature drops at a slow speed according to 5 DEG C of h~10 DEG C/h cooling rates
Temperature expands shoulder process by low speed and is conducive to eliminate dislocation and grain boundary, until the width of chip and the width dimensions of mold mouth
When equal, expand shoulder and complete, expansion fillet degree is made to reach 115 °~120 °；When expansion shoulder temperature drops to 2000 DEG C, stop cooling operation,
To avoid crystal from setting off an explosion since temperature is too low；Take the purpose of cooling measure then can be avoided crystal temperature effect it is excessively high and
Caused crystal growth time extends；
(8) after expansion shoulder terminates, isodiametric growth isodiametric growth: is carried out to crystal；During isodiametric growth, by furnace body temperature
It gradually rises to 2050 DEG C, and be gradually increased to 2100 DEG C at a slow speed from 2050 DEG C, on the one hand can go out to avoid crystal in low temperature
On the other hand existing glass fragment shape striped then can be avoided the inside shrink defects of chip of high temperature appearance；By mentioning for lifting rod
Pulling rate degree is adjusted to 25mm/h, and is gradually risen from 25mm/h to 35mm/h；During isodiametric growth, if pull rate mistake
Fastly, blister interface is easily formed, leads to the half-cooked gas at trough, causes to generate bubble in the wafer；
(9) annealing cooling: after isodiametric growth is completed, crystal is separated with crucible；Then crystal is placed in furnace body and is delayed
Slow cooling down, cooling rate cool down according to the speed of 5 DEG C/min, the annealing of crystal are realized by cool down, is disappeared
Except the internal stress that crystal is accumulated during the growth process, the remaining internal stress of institute is avoided to cause crystal fracture；It is completely disengaged to crystal
When mold mouth, cooling rate is increased to 10 DEG C/min from 5 DEG C/min, so that furnace body temperature is down to 1500 DEG C and then improves drop
Warm speed turns off heating power supply after being down to 80 DEG C or less to furnace body temperature to 25 DEG C/min, continues cool to furnace body temperature
Room temperature；Finally cooling crystal is taken out.
The technical solution of the application makes in crystal growing process on the one hand by feedstock processing and furnace body cleaning technology
Impurity is reduced, and crystal is avoided to be contaminated, and improves crystal purity.
On the other hand, the present invention by raw material filling work procedure and vacuumizes process, can make crystal in fusion process
The generation for reducing bubble, carries out compacting filling for raw material, reduces the presence in raw material gap, according to a certain percentage to reduce life
The bubble of long crystal generates probability, improves crystal quality.
In another aspect, the present invention makes crystal by high temperature seeding, necking down, expansion shoulder, isodiametric growth and annealing cooling process
Cracking and the generation of dislocation, glass fragment striped and genetic defect are reduced in growth course, to improve crystal quality.
Preferably, the material of the mold is iridium or molybdenum, and the top surface of mold is provided with for accumulating sheet solution thin layer
Hydrops slot is provided with 5 pores in the hydrops slot, wherein 4 pores are separately positioned on 4 turnings of the hydrops slot
The geometric center position in hydrops groove top face is arranged in position, 1 pore.
Preferably, the pore is taper pore structure, and the top of pore is taper small end, and the bottom end of pore is cone
Shape big end.
Preferably, the inner wall of the pore is smooth inner wall.
By adopting the above-described technical solution, the beneficial effects of the present invention are:
1, the technical solution of the application makes in crystal growing process on the one hand by feedstock processing and furnace body cleaning technology
Impurity reduce, avoid crystal from being contaminated, improve crystal purity.
2, on the other hand, the present invention by raw material filling work procedure and vacuumizes process, crystal can be made in fusion process
The middle generation for reducing bubble, carries out compacting filling for raw material, reduces the presence in raw material gap, according to a certain percentage to reduce
The bubble for growing crystal generates probability, improves crystal quality.
3, in another aspect, the present invention makes crystalline substance by high temperature seeding, necking down, expansion shoulder, isodiametric growth and annealing cooling process
Cracking and the generation of dislocation, glass fragment striped and genetic defect are reduced in body growth course, to improve crystal quality.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is mold structure diagram of the invention；
Fig. 3 is die cut view of the invention.
In figure: 1, hydrops slot；2, pore.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments, based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
Embodiment 1, as shown in Figs. 1-3:
A kind of guided mode processing method of flaky sapphire, includes the following steps:
(1) feedstock processing: raw material is cleaned by ultrasonic 20min by acetone first, is then cleaned by ultrasonic with dehydrated alcohol
10min, then it is cleaned by ultrasonic 10min with deionized water, raw material is subjected to cleaning treatment；Raw material is blown after having cleaned using nitrogen
It is dry, raw material is placed in drying 1h~1.5h, the concentrated hydrochloric acid for being then 36%-38% with mass fraction by raw material in 120 DEG C of baking ovens
26h~30h is impregnated, is placed in clear water reserviors and is rinsed to neutrality after immersion, places into and dries 1h~2h in silica crucible；
(2) furnace body is cleared up: before guided mode processes flaky sapphire, being endured strict scrutiny first to furnace body, by checking
Mode is understood furnace interior with the presence or absence of foreign matter or sundries, and is cleaned the sundries of furnace interior using cleaning agent, will be miscellaneous
Object or foreign matter are cleaned out；Then, furnace body heater switch is opened, furnace body is preheated using 80 DEG C of in-furnace temperatures, by furnace
The remaining moisture in internal portion is evaporated, and dries furnace interior；Impurity or foreign matter to effectively avoid furnace interior is to crystal
It pollutes, influences crystal quality, while also reducing a possibility that impurity is precipitated in furnace；
(3) raw material is filled: raw material is filled in crucible, raw material uses powder raw material and block stock quality proportioning for 3:
7 mode carries out dense packing effect；Crucible bottom first splices one layer of block stock of filling, and powder raw material is then filled in blocky original
The gap and upper surface of material, and be compacted；Then it is further continued for sprawling assembled block stock and powder raw material, makes to be formed in crucible
The raw material of compacting；So it can make melting sources speed faster, bubble existing for melt inside is less；
(4) furnace body vacuumizes: closing the gas vent of crystal growth equipment, opens mechanical pump pumping, and rise to furnace body
Temperature heating；After furnace body vacuumizes 1h-2h, argon gas switch valve is opened, applying argon gas is carried out to furnace body inner cavity, is made at furnace interior
In the state of argon gas protection；The purpose of argon atmosphere is vacuumized and is passed through, primarily to preventing molybdenum or iridium crucible and mould
Tool is oxidized under the high temperature conditions, while being prevented molybdenum or iridium and other residual gas from reacting and being generated volatile object
Matter impacts wafer quality；Argon gas, which is filled with, effectively to avoid melt from decomposing and evaporate under high-temperature low-pressure
Phenomenon occurs；
(5) high temperature seeding: the intermediate frequency power supply of furnace body being switched and is opened, and carries out furnace body heating heating；Heat up heating process are as follows:
Furnace body is risen to 300 DEG C with the heating rate of 5 DEG C/min first, keeps 5min~10min；Then use heating rate for 10
DEG C/heating method of min, furnace body temperature is risen to 1000 DEG C, keeps the temperature 10min-15min；Finally using 15 DEG C/min~20 DEG C/
The heating rate of min is heated to 2000 DEG C, and after keeping the temperature 5min, adjustment heating rate is 10 DEG C/min, and in-furnace temperature is risen to
2100 DEG C~2150 DEG C；After being completely melt to raw material, seed crystal is mounted on lifting rod, is moved down at a slow speed, seed crystal is made
Bottom end and mould upper surface are at a distance of 5mm~6mm；Furnace body temperature is dropped to 2050 DEG C, seed crystal is preheated, to prevent hot punching
It hits；It is 2~3 times that seed crystal, which preheats number, when fusing sign and then secondary cooling preheating, each preheating time occurs in seed crystal bottom end
It is spaced 1min~2min；After preheating is completed, seed crystal is lifted upwards, furnace body temperature is risen to 2100 DEG C~2150 DEG C again,
Start seeding；Seed crystal descending at slow speed is contacted with bath surface, makes the sheet-like melt and the abundant welding of seed crystal positioned at die surface,
Form an entirety；
(6) necking down: gradually promoting 1.5mm/h~2mm/h for pull rate, at the same melt temperature increased at a slow speed 15 DEG C~
20 DEG C, necking down is carried out to chip；The effect of necking down is: can reduce the genetic defect in seed crystal, pass through necking down process, crystal
Any non axial dislocation can be by successive elimination；The temperature of necking process is excessively high, the easy rapid melting of seed crystal；Necking down temperature
It is too low, then it is unobvious to will lead to necking down effect；
(7) expand shoulder: after necking down, the pull rate of guided mode equipment being subjected to reduction of speed adjustment, is reduced to pull rate
4.5mm/h~5mm/h starts to expand shoulder；Expand during shoulder, furnace body temperature drops at a slow speed according to 5 DEG C of h~10 DEG C/h cooling rates
Temperature expands shoulder process by low speed and is conducive to eliminate dislocation and grain boundary, until the width of chip and the width dimensions of mold mouth
When equal, expand shoulder and complete, expansion fillet degree is made to reach 115 °~120 °；When expansion shoulder temperature drops to 2000 DEG C, stop cooling operation,
To avoid crystal from setting off an explosion since temperature is too low；Take the purpose of cooling measure then can be avoided crystal temperature effect it is excessively high and
Caused crystal growth time extends；
(8) after expansion shoulder terminates, isodiametric growth isodiametric growth: is carried out to crystal；During isodiametric growth, by furnace body temperature
It gradually rises to 2050 DEG C, and be gradually increased to 2100 DEG C at a slow speed from 2050 DEG C, on the one hand can go out to avoid crystal in low temperature
On the other hand existing glass fragment shape striped then can be avoided the inside shrink defects of chip of high temperature appearance；By mentioning for lifting rod
Pulling rate degree is adjusted to 25mm/h, and is gradually risen from 25mm/h to 35mm/h；During isodiametric growth, if pull rate mistake
Fastly, blister interface is easily formed, leads to the half-cooked gas at trough, causes to generate bubble in the wafer；
(9) annealing cooling: after isodiametric growth is completed, crystal is separated with crucible；Then crystal is placed in furnace body and is delayed
Slow cooling down, cooling rate cool down according to the speed of 5 DEG C/min, the annealing of crystal are realized by cool down, is disappeared
Except the internal stress that crystal is accumulated during the growth process, the remaining internal stress of institute is avoided to cause crystal fracture；It is completely disengaged to crystal
When mold mouth, cooling rate is increased to 10 DEG C/min from 5 DEG C/min, so that furnace body temperature is down to 1500 DEG C and then improves drop
Warm speed turns off heating power supply after being down to 80 DEG C or less to furnace body temperature to 25 DEG C/min, continues cool to furnace body temperature
Room temperature；Finally cooling crystal is taken out.
The technical solution of the application makes in crystal growing process on the one hand by feedstock processing and furnace body cleaning technology
Impurity is reduced, and crystal is avoided to be contaminated, and improves crystal purity.
On the other hand, the present invention by raw material filling work procedure and vacuumizes process, can make crystal in fusion process
The generation for reducing bubble, carries out compacting filling for raw material, reduces the presence in raw material gap, according to a certain percentage to reduce life
The bubble of long crystal generates probability, improves crystal quality.
In another aspect, the present invention makes crystal by high temperature seeding, necking down, expansion shoulder, isodiametric growth and annealing cooling process
Cracking and the generation of dislocation, glass fragment striped and genetic defect are reduced in growth course, to improve crystal quality.
Preferably, the material of the mold is iridium or molybdenum, and the top surface of mold is provided with for accumulating sheet solution thin layer
Hydrops slot 1 is provided with 5 pores 2 in the hydrops slot 1, wherein 4 pores 2 are separately positioned on the 4 of the hydrops slot 1
The geometric center position of 1 top surface of hydrops slot is arranged in a corner location, 1 pore 2.
Preferably, the pore 2 is taper pore structure, and the top of pore 2 is taper small end, the bottom end of pore 2
For taper big end.
Preferably, the inner wall of the pore 2 is smooth inner wall.
For the present invention by the way that mold to be placed in crucible, the melt in crucible passes through the capillary action of pore 2, makes to melt
Body gradually accumulates in vector product liquid bath 2, and then seed crystal is declined to by lifting rod the melt of contact die surface, make melt and seed crystal
Between realize the welding of solid-liquid interface, and being controled and operated by czochralski process, realizing the molding of flaky sapphire crystals.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art within the technical scope of the present disclosure, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be subject to the protection scope in claims.
Claims (1)
1. a kind of guided mode processing method of flaky sapphire, characterized by the following steps:
(1) feedstock processing: alumina raw material is cleaned by ultrasonic 20min by acetone first, is then cleaned by ultrasonic with dehydrated alcohol
10min, then it is cleaned by ultrasonic 10min with deionized water, raw material is subjected to cleaning treatment；Raw material is blown after having cleaned using nitrogen
It is dry, raw material is placed in drying 1h~1.5h, the concentrated hydrochloric acid for being then 36%-38% with mass fraction by raw material in 120 DEG C of baking ovens
26h~30h is impregnated, is placed in clear water reserviors and is rinsed to neutrality after immersion, places into and dries 1h~2h in silica crucible；
(2) furnace body is cleared up: before guided mode processes flaky sapphire, being endured strict scrutiny first to furnace body, is passed through the mode of checking
Understanding furnace interior whether there is foreign matter or sundries, and be cleaned the sundries of furnace interior using cleaning agent, by sundries or
Foreign matter is cleaned out；Then, furnace body heater switch is opened, furnace body is preheated using 80 DEG C of in-furnace temperatures, it will be in furnace body
The remaining moisture in portion is evaporated, and dries furnace interior；To effectively avoid the impurity of furnace interior or foreign matter from causing crystal
Pollution, influences crystal quality, while also reducing a possibility that impurity is precipitated in furnace；
(3) raw material is filled: raw material being filled in crucible, raw material uses powder raw material and block stock quality proportioning for 3:7's
Mode carries out dense packing effect；Crucible bottom first splices one layer of block stock of filling, and powder raw material is then filled in block stock
Gap and upper surface, and be compacted；Then it is further continued for sprawling assembled block stock and powder raw material, makes to form pressure in crucible
Real raw material；So it can make melting sources speed faster, bubble existing for melt inside is less；
(4) furnace body vacuumizes: closing the gas vent of crystal growth equipment, opens mechanical pump pumping, and carry out heating to furnace body and add
Heat；After furnace body vacuumizes 1h-2h, argon gas switch valve is opened, applying argon gas is carried out to furnace body inner cavity, furnace interior is made to be in argon
The state of gas shielded；The purpose of argon atmosphere is vacuumized and is passed through, primarily to preventing molybdenum or iridium crucible and mold from existing
It is oxidized under hot conditions, while preventing molybdenum or iridium and other residual gas from reacting and generating volatile substance, it is right
Wafer quality impacts；Argon gas is filled with the phenomenon that can also effectively avoiding melt from decomposing and evaporate under high-temperature low-pressure hair
It is raw；
(5) high temperature seeding: the intermediate frequency power supply of furnace body being switched and is opened, and carries out furnace body heating heating；Heat up heating process are as follows: first
Furnace body is risen to 300 DEG C with the heating rate of 5 DEG C/min, keeps 5min~10min；Then use heating rate for 10 DEG C/min
Heating method, furnace body temperature is risen to 1000 DEG C, keeps the temperature 10min-15min；Finally use 15 DEG C/min~20 DEG C/min
Heating rate is heated to 2000 DEG C, and after keeping the temperature 5min, adjustment heating rate is 10 DEG C/min, and in-furnace temperature is risen to 2100 DEG C
~2150 DEG C；After being completely melt to raw material, seed crystal is mounted on lifting rod, is moved down at a slow speed, make the bottom end of seed crystal with
Mould upper surface is at a distance of 5mm~6mm；Furnace body temperature is dropped to 2050 DEG C, seed crystal is preheated, to prevent thermal shock；Seed
Crystalline substance preheating number is 2~3 times, when fusing sign and then secondary cooling preheating, each preweld interval occurs in seed crystal bottom end
1min~2min；After preheating is completed, seed crystal is lifted upwards, furnace body temperature is risen to 2100 DEG C~2150 DEG C again, started
Seeding；Seed crystal descending at slow speed is contacted with bath surface, makes the sheet-like melt and the abundant welding of seed crystal positioned at die surface, is formed
One entirety；
(6) necking down: pull rate is gradually promoted into 1.5mm/h~2mm/h, while melt temperature being increased at a slow speed to 15 DEG C~20
DEG C, necking down is carried out to chip；The effect of necking down is: the genetic defect in seed crystal can be reduced, by necking down process, crystal
Any non axial dislocation can be by successive elimination；The temperature of necking process is excessively high, the easy rapid melting of seed crystal；Necking down temperature mistake
It is low, then it is unobvious to will lead to necking down effect；
(7) expand shoulder: after necking down, the pull rate of guided mode equipment being subjected to reduction of speed adjustment, pull rate is made to be reduced to 4.5mm/h
~5mm/h starts to expand shoulder；Expand during shoulder, furnace body temperature cools down at a slow speed according to 5 DEG C of h~10 DEG C/h cooling rates, by low
Speed expands shoulder process and is conducive to eliminate dislocation and grain boundary, until expanding when the width of chip and the equal width dimensions of mold mouth
Shoulder is completed, and expansion fillet degree is made to reach 115 °~120 °；When expansion shoulder temperature drops to 2000 DEG C, stop cooling operation, to avoid
Crystal sets off an explosion since temperature is too low；Take the purpose of cooling measure then can be avoided crystal temperature effect it is excessively high caused by crystalline substance
Body growth time extends；
(8) after expansion shoulder terminates, isodiametric growth isodiametric growth: is carried out to crystal；During isodiametric growth, gradually by furnace body temperature
2050 DEG C are increased to, and is gradually increased to 2100 DEG C at a slow speed from 2050 DEG C, on the one hand can be occurred to avoid crystal in low temperature
On the other hand glass fragment shape striped then can be avoided the inside shrink defects of chip of high temperature appearance；By the lifting speed of lifting rod
Degree is adjusted to 25mm/h, and is gradually risen from 25mm/h to 35mm/h；During isodiametric growth, if pull rate is too fast,
Blister interface is easily formed, leads to the half-cooked gas at trough, causes to generate bubble in the wafer；
(9) annealing cooling: after isodiametric growth is completed, crystal is separated with crucible；Then crystal is placed in furnace body and is slowly dropped
Temperature is cooling, and cooling rate cools down according to the speed of 5 DEG C/min, and the annealing of crystal is realized by cool down, eliminates brilliant
The internal stress that body is accumulated during the growth process avoids the remaining internal stress of institute from causing crystal fracture；Mold is completely disengaged to crystal
When mouth, cooling rate is increased to 10 DEG C/min from 5 DEG C/min, so that furnace body temperature is down to 1500 DEG C and then improves cooling speed
Degree turns off heating power supply after being down to 80 DEG C or less to furnace body temperature to 25 DEG C/min, and furnace body temperature is made to continue cool to room
Temperature；Finally cooling crystal is taken out；The material of the mold is iridium or molybdenum, and die top is provided with for accumulating sheet solution
The hydrops slot (1) of thin layer, the hydrops slot (1) is interior to be provided with 5 pores (2), wherein 4 pores (2) are separately positioned on
4 corner locations of the hydrops slot (1), geometric center position of 1 pore (2) setting in hydrops slot (1) top surface；
The pore (2) is taper pore structure, and the top of pore (2) is taper small end, and the bottom end of pore (2) is that taper is big
End；The inner wall of the pore (2) is smooth inner wall.
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| CN109048626B (en) * | 2018-07-31 | 2020-12-11 | 江西伟嘉创展企业管理有限公司 | Method for preparing mobile phone rear cover by EFG (edge-defined film) guide mold method |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586866A (en) * | 2012-02-09 | 2012-07-18 | 上海施科特光电材料有限公司 | Method for restraining bulbs in process of growing slice-shaped sapphire in guiding mold mode |
| CN102943303A (en) * | 2012-11-14 | 2013-02-27 | 上海施科特光电材料有限公司 | Method to restrain bubbles in process of growing sapphire by using kyropoulos method |
| CN103184518A (en) * | 2011-12-27 | 2013-07-03 | 中国科学院上海硅酸盐研究所 | Treatment method for sapphire raw materials |
| CN103243388A (en) * | 2013-04-02 | 2013-08-14 | 苏州海铂晶体有限公司 | Method for heating and melting precast shaped filler in sapphire crystal growth |
| CN103726101A (en) * | 2014-01-20 | 2014-04-16 | 江苏苏博瑞光电设备科技有限公司 | Ending method for reducing fracture of edge-defined film-fed crystal growth tubular sapphire crystal |
| CN103849928A (en) * | 2014-03-19 | 2014-06-11 | 江苏苏博瑞光电设备科技有限公司 | Multiple-piece guided mode method growth technology for sapphire wafer |
| CN103866378A (en) * | 2014-04-04 | 2014-06-18 | 玉溪市明珠晶体材料有限公司 | Method for growing accessory-grade demantoid single crystal |
| CN104047049A (en) * | 2014-06-30 | 2014-09-17 | 南京航空航天大学 | Preparation method for growing crack-free sapphire crystals by edge-defined film-fed growth process |
-
2017
- 2017-03-31 CN CN201710208044.7A patent/CN106676624B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184518A (en) * | 2011-12-27 | 2013-07-03 | 中国科学院上海硅酸盐研究所 | Treatment method for sapphire raw materials |
| CN102586866A (en) * | 2012-02-09 | 2012-07-18 | 上海施科特光电材料有限公司 | Method for restraining bulbs in process of growing slice-shaped sapphire in guiding mold mode |
| CN102943303A (en) * | 2012-11-14 | 2013-02-27 | 上海施科特光电材料有限公司 | Method to restrain bubbles in process of growing sapphire by using kyropoulos method |
| CN103243388A (en) * | 2013-04-02 | 2013-08-14 | 苏州海铂晶体有限公司 | Method for heating and melting precast shaped filler in sapphire crystal growth |
| CN103726101A (en) * | 2014-01-20 | 2014-04-16 | 江苏苏博瑞光电设备科技有限公司 | Ending method for reducing fracture of edge-defined film-fed crystal growth tubular sapphire crystal |
| CN103849928A (en) * | 2014-03-19 | 2014-06-11 | 江苏苏博瑞光电设备科技有限公司 | Multiple-piece guided mode method growth technology for sapphire wafer |
| CN103866378A (en) * | 2014-04-04 | 2014-06-18 | 玉溪市明珠晶体材料有限公司 | Method for growing accessory-grade demantoid single crystal |
| CN104047049A (en) * | 2014-06-30 | 2014-09-17 | 南京航空航天大学 | Preparation method for growing crack-free sapphire crystals by edge-defined film-fed growth process |
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