CN109650749A - Quartz boat surface treatment method, quartz boat and application - Google Patents
Quartz boat surface treatment method, quartz boat and application Download PDFInfo
- Publication number
- CN109650749A CN109650749A CN201811470987.8A CN201811470987A CN109650749A CN 109650749 A CN109650749 A CN 109650749A CN 201811470987 A CN201811470987 A CN 201811470987A CN 109650749 A CN109650749 A CN 109650749A
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- Prior art keywords
- quartz boat
- quartz
- gallium
- surface treatment
- gallium liquid
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/007—Other surface treatment of glass not in the form of fibres or filaments by thermal treatment
-
- 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
- C30B15/10—Crucibles or containers for supporting the melt
-
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/42—Gallium arsenide
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The embodiment of the invention discloses a kind of methods of quartz boat surface treatment, comprising the following steps: pours into quartz ampoule gallium liquid, is heated to 35 DEG C -40 DEG C, removes the oxidation film on gallium liquid surface；By several blasts, treated that quartz boat is immersed in gallium liquid；It vacuumizes 2-5 minutes；Protective gas is filled in the quartz ampoule, gallium liquid is warming up to 1230 DEG C -1260 DEG C, constant temperature keeps the 2-3 hours quartz boats for forming α-cristobalite spherocrystal body to get inner wall.Quartz boat after surface treatment is during drawing arsenide gallium monocrystal, it can effectively avoid the problem that infiltrating in GaAs and quartz boat inner surface, upper surface growth course, so that the arsenide gallium monocrystal back side has the identical bright luster with front, the bonding phenomenon for effectively avoiding quartz boat and arsenide gallium monocrystal avoids the influence that bonding grows arsenide gallium monocrystal.
Description
Technical field
The present embodiments relate to technical field of surface, in particular to a kind of quartz boat surface treatment method, quartz
Boat and application.
Background technique
Horizontal Bridgman method, abbreviation HB method are one of a kind of main methods for growing GaAs (GaAs) monocrystalline.HB method
Principle be to be placed on the raw material for growing monocrystalline in a kind of vessel, vessel are put into round tube, rear enclosed nozzle are vacuumized, using fixed
Monocrystalline is grown to zone-melting process.This vessel are commonly referred to as " boat ", and outer tube is referred to as growth tube.
The material that growth tube and boat use all selects quartz, and there are two reasons: (1) quartzy high temperature resistant.In GaAs fusing point
At a high temperature of 1238 DEG C, does not soften and certain steam pressure can be born.(2) quartzy transparency is good.In GaAs fusing point 1238
Its transparency is not lost at a high temperature of DEG C, the growth conditions of monocrystalline can be observed.During single crystal preparation, gallium arsenide and stone
Infiltration phenomenon occurs for English, in cooling procedure after solidification, because of the difference of the two thermal expansion coefficient, often makes gallium arsenide disconnected
It splits.In addition, more seriously the immersional wetting in GaAs crystallization process can enhance influence of the boat wall to melt, increase growth
Polycrystalline chance, makes crystal growth fail.
Currently in order to reducing GaAs melt " infiltration " quartz boat, it will usually following methods be taken to handle quartz boat:
(1) after quartz boat is fired into, compressor air or inert blowing gas band diamond dust are used using preceding, by its inner surface
" feather plucking " (is processed into hair side).After blast, under smelt surface tension effect, reduce contact area；
(2) liquid Ga high temperature refine boat: boat inner surface generate cristobalite spherulite, by quartz with GaAs melt every
From.Usual way is that first 80 mesh Buddha's warrior attendant sand blasting hairs of quartz boat inner wall are packed into gallium after cleaning, are loaded with it as much as possible,
It is subsequently placed in quartz ampoule and is evacuated to vacuum progress tube sealing, be put into high temperature furnace and kept for 10 hours at a temperature of about 1150 DEG C, it is natural
Gallium is removed after cooling once to be cleaned again, it is spare.This processing method is complicated, fills the quartz boat of gallium in push-in quartz ampoule
It is easy to cause gallium to outflow in the process, prevents in quartz boat that gallium is from being completely filled up, so that the upper surface of quartz boat and inner surface be made to lean on
The position of nearly top edge is not because reaching gallium liquid, poor processing effect；Meanwhile horizontal positioned quartz boat, the gallium liquid in boat is true
Heat-conductive characteristic is poor under dummy status, and the time to be treated is long, and treatment effect is bad；Quartz ampoule cannot repeat to make after vacuum sealing tube
With processing cost is high；And 1 quartz boat can only be handled simultaneously, treatment effeciency is low.
Summary of the invention
The embodiment of the present invention is designed to provide a kind of quartz boat surface treatment method, quartz boat and application, effectively keeps away
The bonding phenomenon for exempting from quartz boat and GaAs avoids the influence that bonding grows arsenide gallium monocrystal.
In order to solve the above technical problems, the embodiment provides a kind of methods of quartz boat surface treatment, including
Following steps:
Gallium liquid is poured into quartz ampoule, is heated to 35 DEG C -40 DEG C, removes the oxidation film on gallium liquid surface；
By several blasts, treated that quartz boat is immersed in gallium liquid；
It vacuumizes 2-5 minutes；Protective gas is filled in the quartz ampoule, gallium liquid is warming up to 1230 DEG C -1260 DEG C, perseverance
Temperature keeps the 2-3 hours quartz boats that α-cristobalite spherocrystal body is formed to get inner wall.
The embodiments of the present invention also provide a kind of quartz that the method being surface-treated by above-mentioned quartz boat is handled
Boat.
The embodiments of the present invention also provide application of the above-mentioned quartz boat in growth arsenide gallium monocrystal.
In terms of existing technologies, quartz boat is totally submerged in gallium liquid for the embodiment of the present invention, quartz boat inner surface,
Upper surface can be handled well, so that forming α-cristobalite spherocrystal body, treated quartz boat on the inner wall of quartz boat
During drawing arsenide gallium monocrystal, it can effectively avoid infiltrating in GaAs and quartz boat inner surface, upper surface growth course
The problem of, so that the arsenide gallium monocrystal back side has the identical bright luster with front, effectively avoid quartz boat and arsenide gallium monocrystal
Bonding phenomenon, avoid the influence that grows to arsenide gallium monocrystal of bonding.In addition, using upright method, quartz boat is complete
It is immersed in gallium liquid, is handled under the protection of protective gas, uniformity of temperature profile in gallium liquid, so that the guarantor of quartz boat inner wall
Cuticula is relatively uniform.And this method is easy to operate, treatment effeciency is high, can handle multiple quartz boats, the quartz equipped with gallium liquid simultaneously
Pipe can be used for multiple times, and reduce production cost.
In addition, by several blasts, that treated is further comprising the steps of before quartz boat is immersed in gallium liquid: will
Treated that quartz boat successively stacks to form class cylindrical body for several blasts.
In addition, further comprising the steps of after constant temperature is kept for 2-3 hours: coming out of the stove after being cooled to 60 DEG C -100 DEG C.
In addition, by several blasts, treated that quartz boat is immersed in gallium liquid the following steps are included: by several
Blast treated quartz boat is immersed in gallium liquid using upright method.
In addition, protective gas is selected from any one of helium, argon gas, nitrogen.
Detailed description of the invention
One or more embodiments are illustrated by the picture in corresponding attached drawing, these exemplary theorys
The bright restriction not constituted to embodiment, the element in attached drawing with same reference numbers label are expressed as similar element, remove
Non- to have special statement, composition does not limit the figure in attached drawing.
Fig. 1 is the quartz boat surface treatment method flow chart in the embodiment of the present invention 1.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with attached drawing to the present invention
Each embodiment be explained in detail.However, it will be understood by those skilled in the art that in various embodiments of the present invention
In, in order to make the reader understand this application better, many technical details are proposed.But even if without these technical details and
Based on the various changes and modifications of following embodiment, the application technical solution claimed also may be implemented.
Embodiment 1
A kind of method of quartz boat surface treatment, comprising the following steps: it is specific as shown in Figure 1,
1. gallium liquid is poured into the quartz ampoule in heating furnace and is heated to 35 degree, the oxidation film on removal gallium liquid surface；
2. the quartz boat after 5 2.0 inches of blasts cleanings is successively stacked after forming class cylindrical body, using upright
Method is put into the quartz ampoule equipped with gallium liquid (the 1st use), and quartz boat is immersed in gallium liquid；
It should be noted that quartz boat is semicircle in class, multiple quartz boats are sequentially overlapped to form class cylindrical body, in this way can be with
The accommodation space of quartz ampoule is utilized to greatest extent, to realize while handle the purpose of multiple quartz boats.
3. vacuumizing 2 points 38 seconds, applying argon gas is kept for constant temperature 2.5 hours after being warming up to 1240 DEG C；
It should be noted that the protective gas in the present embodiment is argon gas, naturally it is also possible to appointing in helium, nitrogen
One kind, details are not described herein for the present embodiment.
4. coming out of the stove at aeration-cooling to 78 DEG C；The quartz boat of α-cristobalite spherocrystal body is formed up to inner wall.
After the quartz boat cleaning that embodiment 1 is obtained, observation quartz boat inner wall forms uniform white α-cristobalite spherocrystal
Body.After the quartz boat crystal pulling in embodiment 1, the arsenide gallium monocrystal back side has identical bright luster, soap-free emulsion polymeization with front
Phenomenon is all avoided because bonding the influence to monocrystalline crystal forming rate.
Example example 2
A kind of method of quartz boat surface treatment, comprising the following steps:
1. gallium surface film oxide is pulled out after gallium liquid is warming up to 38 degree；
2. the quartz boat after 4 2.5 inches of blasts cleanings is successively stacked after forming class cylindrical body, using upright
Method is put into the quartz ampoule equipped with gallium liquid (the 8th use), and quartz boat is immersed in gallium liquid；
3. vacuumizing 30 seconds 3 minutes, after 1250 DEG C are warming up to after applying argon gas, kept for constant temperature 40 minutes 2 hours；
4. coming out of the stove at aeration-cooling to 68 DEG C；The quartz boat of α-cristobalite spherocrystal body is formed up to inner wall.
After the quartz boat that embodiment 2 is obtained takes out cleaning, observation quartz boat inner wall forms uniform white α-cristobalite
Spherocrystal body.After the quartz boat crystal pulling obtained with the present embodiment, the arsenide gallium monocrystal back side has and the identical bright luster in front, nothing
Bonding phenomenon is all avoided because bonding the influence to monocrystalline crystal forming rate.
Example example 3
A kind of method of quartz boat surface treatment, comprising the following steps:
1. gallium surface film oxide is pulled out after gallium liquid is warming up to 36 degree；
2. the quartz boat after 3 3.0 inches of blasts cleanings is successively stacked after forming class cylindrical body, using upright
Method is put into the quartz ampoule equipped with gallium liquid (the 15th use), and observation quartz boat is totally immersed into gallium liquid；
3. vacuumizing 3 points of 14 seconds applying argon gas, after being warming up to 1254 DEG C, kept for constant temperature 40 minutes 2 hours；
The quartz boat of α-cristobalite spherocrystal body is formed to get inner wall 4. coming out of the stove at aeration-cooling to 63 DEG C.
After the quartz boat that embodiment 3 is handled takes out cleaning, observation quartz boat inner wall forms uniform white α-cristobalite
Spherocrystal body, after the quartz boat crystal pulling with the processing of embodiment 3, the arsenide gallium monocrystal back side has and the identical bright luster in front, nothing
Bonding phenomenon is all avoided because bonding the influence to monocrystalline crystal forming rate.
Example example 4
A kind of method of quartz boat surface treatment, comprising the following steps:
1. gallium surface film oxide is pulled out after gallium liquid is warming up to 37 DEG C.
3. the quartz boat after 4 2.5 inches of blasts cleanings is successively stacked after forming class cylindrical body, using upright
Method is put into the quartz ampoule equipped with gallium liquid (the 7th use), and quartz boat is totally immersed into gallium liquid；
3. vacuumizing 3 points of 34 seconds applying argon gas, kept for constant temperature 20 minutes 2 hours after being warming up to 1259 DEG C；
The quartz boat of α-cristobalite spherocrystal body is formed to get inner wall 4. coming out of the stove at aeration-cooling to 75 DEG C.
After 4 quartz boats that embodiment 4 is handled take out cleaning, observation quartz boat inner wall forms uniform white α-ashlar
English spherocrystal body.The monocrystalline back side has identical bright luster, soap-free emulsion polymeization with front existing after the quartz boat crystal pulling handled with embodiment 4
As all avoiding because bonding the influence to monocrystalline crystal forming rate.
Comparative example 1
Examples 1 to 4 and comparative example 1 are kept for the time of constant temperature screen
Comparative example 1 is related to a kind of method of quartz boat surface treatment, comprising the following steps:
1. gallium surface film oxide is pulled out after gallium liquid is warming up to 36 degree；
2. the quartz boat after 5 2.0 inches of blasts cleanings is successively stacked after forming class cylindrical body, using upright
Method is put into the quartz ampoule of dress gallium liquid (the 15th use), and quartz boat is totally immersed into gallium liquid；
3. vacuumizing 3 points of 14 seconds applying argon gas, after being warming up to 1258 DEG C, kept for constant temperature 20 minutes 1 hour；
4. coming out of the stove at aeration-cooling to 63 DEG C.
After the quartz boat that comparative example 1 is handled takes out cleaning, the white α-cristobalite spherocrystal of observation quartz boat inner wall formation
Body film, the thin and uneven state of presentation.After quartz boat crystal pulling with the processing of comparative example 1, there are different journeys at the arsenide gallium monocrystal back side
The viscous profit phenomenon of degree, successful growth monocrystalline 1.6, monocrystalline crystal forming rate 32%.
Examples 1 to 4 and the quartz boat performance that the processing of comparative example 1 obtains are as shown in table 1:
Examples 1 to 4 and comparative example 1 handle obtained quartz boat performance
As seen from the above table, the quartz boat that the thermostatic hold-time used in Examples 1 to 4 is handled has white α-side
Quartz ball crystal, there is identical bright luster, soap-free emulsion polymeization phenomenon with front all to avoid at the arsenide gallium monocrystal back side after crystal pulling
Because bonding the influence to monocrystalline crystal forming rate.The quartz boat that the thermostatic hold-time that comparative example 1 uses is handled has white α-
Cristobalite ball crystal film, after crystal pulling, there is a different degrees of viscous profit phenomenon at the arsenide gallium monocrystal back side, and successful growth monocrystalline 1.6,
Monocrystalline crystal forming rate 32%.Therefore in the case where thermostatic hold-time is 2-3h, the quartz boat handled forms white α-ashlar
English spherocrystal body, after crystal pulling the arsenide gallium monocrystal back side have with the identical bright luster in front, soap-free emulsion polymeization phenomenon, all avoid because
Bond the influence to monocrystalline crystal forming rate.
It will be understood by those skilled in the art that the various embodiments described above are realization specific embodiments of the present invention, and
In practical applications, can to it, various changes can be made in the form and details, without departing from the spirit and scope of the present invention.
Claims (7)
1. a kind of method of quartz boat surface treatment, which comprises the following steps:
Gallium liquid is poured into quartz ampoule, is heated to 35 DEG C -40 DEG C, removes the oxidation film on the gallium liquid surface；
By several blasts, treated that quartz boat is immersed in the gallium liquid；
It vacuumizes 2-5 minutes；Protective gas is filled in the quartz ampoule, the gallium liquid is warming up to 1230 DEG C -1260 DEG C, perseverance
Temperature keeps the 2-3 hours quartz boats that α-cristobalite spherocrystal body is formed to get inner wall.
2. the method for quartz boat surface treatment according to claim 1, which is characterized in that play several sandblastings described
That treated is further comprising the steps of before quartz boat is immersed in the gallium liquid for hair:
By several blasts, treated that quartz boat successively stacks to form class cylindrical body.
3. the method for quartz boat surface treatment according to claim 1, which is characterized in that keep 2-3 small in the constant temperature
When after it is further comprising the steps of:
It comes out of the stove after being cooled to 60 DEG C -100 DEG C.
4. the method for quartz boat surface treatment according to claim 1, which is characterized in that handle several blasts
Quartz boat afterwards be immersed in the gallium liquid the following steps are included:
Several blasts treated quartz boat is immersed in the gallium liquid using upright method.
5. the method for quartz boat surface treatment according to claim 1, which is characterized in that the protective gas is selected from
Any one of helium, argon gas, nitrogen.
6. a kind of quartz boat that the method by the described in any item quartz boat surface treatments of Claims 1 to 5 is handled.
7. application of the quartz boat as claimed in claim 6 in growth arsenide gallium monocrystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811470987.8A CN109650749A (en) | 2018-12-04 | 2018-12-04 | Quartz boat surface treatment method, quartz boat and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811470987.8A CN109650749A (en) | 2018-12-04 | 2018-12-04 | Quartz boat surface treatment method, quartz boat and application |
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| CN109650749A true CN109650749A (en) | 2019-04-19 |
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| CN201811470987.8A Pending CN109650749A (en) | 2018-12-04 | 2018-12-04 | Quartz boat surface treatment method, quartz boat and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115609483A (en) * | 2022-09-30 | 2023-01-17 | 浙江浩锐石英科技有限公司 | Quartz boat sand blasting equipment |
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|---|---|---|---|---|
| JPS6317288A (en) * | 1986-07-03 | 1988-01-25 | Sumitomo Electric Ind Ltd | Production of gallium arsenide single crystal and quartz reaction tube |
| CN1657659A (en) * | 2004-12-15 | 2005-08-24 | 中国科学院上海光学精密机械研究所 | Growth method of gallium arsenide monocrystal |
| CN102677175A (en) * | 2012-05-28 | 2012-09-19 | 上海应用技术学院 | Gallium arsenide monocrystal growing method |
| CN103184339A (en) * | 2011-12-29 | 2013-07-03 | 广东先导稀材股份有限公司 | Gallium arsenide processing device and processing method |
| CN106319630A (en) * | 2015-07-02 | 2017-01-11 | 广东先导先进材料股份有限公司 | Growing method of gallium arsenide monocrystalline |
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2018
- 2018-12-04 CN CN201811470987.8A patent/CN109650749A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6317288A (en) * | 1986-07-03 | 1988-01-25 | Sumitomo Electric Ind Ltd | Production of gallium arsenide single crystal and quartz reaction tube |
| CN1657659A (en) * | 2004-12-15 | 2005-08-24 | 中国科学院上海光学精密机械研究所 | Growth method of gallium arsenide monocrystal |
| CN103184339A (en) * | 2011-12-29 | 2013-07-03 | 广东先导稀材股份有限公司 | Gallium arsenide processing device and processing method |
| CN102677175A (en) * | 2012-05-28 | 2012-09-19 | 上海应用技术学院 | Gallium arsenide monocrystal growing method |
| CN106319630A (en) * | 2015-07-02 | 2017-01-11 | 广东先导先进材料股份有限公司 | Growing method of gallium arsenide monocrystalline |
Non-Patent Citations (1)
| Title |
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| 余怀之: "《红外光学材料》", 31 January 2007, 国防工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115609483A (en) * | 2022-09-30 | 2023-01-17 | 浙江浩锐石英科技有限公司 | Quartz boat sand blasting equipment |
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