CN1414146A - Using induction heating molybdenium crucible in hydrogen atmosphere to make Czochralski grown sapphire crystal - Google Patents
Using induction heating molybdenium crucible in hydrogen atmosphere to make Czochralski grown sapphire crystal Download PDFInfo
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- CN1414146A CN1414146A CN 02134220 CN02134220A CN1414146A CN 1414146 A CN1414146 A CN 1414146A CN 02134220 CN02134220 CN 02134220 CN 02134220 A CN02134220 A CN 02134220A CN 1414146 A CN1414146 A CN 1414146A
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Abstract
A process for growing sapphite in molybdenum crucible by pull method is disclosed, which features that a crystal growing vacuum chamber is protected by high-and constant-temp environment, the crucible is heated by MF induction, the hydrogen is used as protecting gas, the pull device and electronic balance are used for isodiameter growth, and the purified Al2O3, is used as raw material.
Description
Technical field
Invention relates to crystal technique, ultra high vacuum technique, electron beam purification techniques, Magneticfluid Seal Technique, Computer Control Technology and sensor technology.
Background technology
At present, from melt growing crystal be the preparation crystal the most frequently used with most important a kind of method.Needed monocrystal material during modern technologies such as electronics, optics are used, major part prepares with the melt growth method.For example: Si, Ge, CaAs, GaP, LiNbO
3, Nd:YAG, Nd, Cr:GsGG, Al
2O
3Deng, and the halogen compound of some basic metal and alkaline-earth metal etc.Many crystal enter the suitability for industrialized production of different scales already.
Melt growth crystalline method at first is to introduce seed crystal to form a monocrystalline nuclear in melt, then, constantly carries out rearranging of atom or molecule on the boundary of nucleus melt, and the array of being piled up directly changes oldered array into and forms crystal.
The method of growing sapphire crystal comprises crystal pulling method and descent method in the melt, because the liquid level of descent method is difficult to control, now seldom adopts, and general at present crystal pulling method Medium frequency induction Iridium Crucible or the graphite resistance heating molybdenum crucible of using comes growing crystal.But these two kinds of methods have following problem:
1, the Frequency Induction Heating Iridium Crucible must be invested by great number, and as producing the iraurite that Φ 55mm * 150mm crystalline Iridium Crucible needs about 1,500,000 yuans, each in addition growing crystal process has the loss of 2～3% iraurites, and is with high costs.
2, graphite resistance heating molybdenum crucible can produce " molybdenum clothing " problem when the growing crystal process.
Summary of the invention
Purpose of the present invention is intended to overcome above-mentioned the deficiencies in the prior art, proposes a kind of Φ 2-3 inch Sapphire Substrate crystalline technology and equipment thereof of growing.
The technical scheme that realizes above-mentioned purpose is: by computer control, electron beam purification starting material, in nitrogen atmosphere, Frequency Induction Heating molybdenum crucible Czochralski grown sapphire substrate crystal, comprise the steps:
A, the protection of a high temperature, isoperibol is set and the crystal growth vacuum chamber of the gas atmosphere environment protection that adapts with crystal growth;
The warm field device of b, Frequency Induction Heating molybdenum crucible;
C, use reducing atmosphere shielding gas-hydrogen;
The pulling apparatus of d, crystal growth;
E, the isometrical electronic scales measuring system of control growing crystal;
Al after f, use are purified by electron beam
2O
3Starting material.
Realization by computer control, electron beam purification starting material, in nitrogen atmosphere, the method and the equipment thereof of Frequency Induction Heating molybdenum crucible Czochralski grown sapphire substrate crystal, form by electronic scales measuring system, computer temperature Controlling System and cooling system that warm field device, hydrogen flowing quantity Controlling System, the pulling apparatus of crystal growth, the control growing crystal of vacuum system, Frequency Induction Heating molybdenum crucible are isometrical, wherein:
(1) vacuum system comprises crystal growth vacuum chamber, direct connection sliding vane rotary vacuum pump, turbomolecular pump, vacuum valve and vacuum system pipeline, and the crystal growth vacuum chamber connects direct connection sliding vane rotary vacuum pump and turbomolecular pump through vacuum valve and vacuum system pipeline;
(2) Frequency Induction Heating temperature field device is fixed in the crystal growth vacuum chamber, by intermediate frequency power supply, Medium frequency induction coil, upper and lower annular zirconium white stay-warm case, the zirconium white thermal insulating seat, quartz socket tube, oxidation zircon sand thermal insulation layer, die casting mica thermal insulating seat, aluminum oxide stay-warm case and molybdenum crucible are formed, crystal starting material by in the Frequency Induction Heating fusing molybdenum crucible form the raw-material melt of crystal;
(3) the hydrogen flowing quantity Controlling System comprises the hydrogen inflation valve that is fixed on top in the crystal growth vacuum chamber, and inflation valve connects hydrogen quality under meter and sources of hydrogen successively by pressure piping;
(4) crystal growing and pulling device comprises the fixedly molybdenum matter anchor clamps seed rod of seed crystal, and seed rod is fixed on the ceramic lifting rod, and ceramic lifting rod is connected with the dynamo-electric pulling apparatus in outside, crystal growth vacuum chamber top; Seed rod is positioned at the top of crystal growth vacuum chamber crucible, controls crystalline growth velocity by rotation, vertical operation in attemperator;
(5) the isometrical electronic scales measuring system of control growing crystal is isometrical by being fixed in the crystal growth vacuum chamber pressure transmitter on the ceramic lifting rod and the computer temperature Controlling System control growing crystal that cooperatively interacts;
(6) be used to make the computer temperature Controlling System that produces high temperature temperature field in the crystal growth vacuum chamber to comprise feedback channel remote signal collection transport sector, temperature regulator and forward path temperature control topworks, the feedback channel remote signal is gathered the temperature signal input temp controller that transport sector is gathered the crystal growth vacuum chamber, computer is by the temperature signal of crystal growing furnace in the asynchronous communication interface timesharing receiving crystal growth vacuum chamber, every road temperature signal all passes through pid control algorithm, generates needed steering order and gives the crystal growth of forward path temperature control actuating mechanism controls;
(5) cooling system cools off the casing and the Medium frequency induction coil of turbomolecular pump, associated mode mechanical pump, cooling pit, crystal growth vacuum chamber.
Adopt technique scheme, the technical progress that the present invention gives prominence to is:
1, uses reducing atmosphere shielding gas-hydrogen; " molybdenum clothing " problem that the warm field device of Frequency Induction Heating molybdenum crucible is produced in the time of can avoiding with the molybdenum crucible growing sapphire fully; great number investment with the Frequency Induction Heating Iridium Crucible can obtain isometrical Φ 52.5 * 260mm fine sapphire crystal.Crystal stress is little, no slip band and twin defective, and dislocation desity is low, and perfection of crystal is good; The crystalline optical homogeneity is better; Can have certain industrial scale, commercially produce for industrial and science and technology field provide.
2, the present invention is by sensor monitoring crystal growing process such as photoelectricity temperature-sensitives, and carry out data processing and control by computer, control software is based upon under the Windows environment, form by two parts of Genie 2.0 figure control component platforms and the data management control module of utilizing VB 3.0 exploitations, by photoelectricity, air-sensitive, transmitter such as pressure-sensitive by computer control system to crystal growing process sample, analyze, add up, calculate, control and record, can carry out real-time monitoring, realize high-precision temperature control the crystal growth quality.
3, the present invention is applicable to the growth of Φ 2-3 inch, Sapphire Substrate crystal and laser crystals.Below by embodiment also in conjunction with the accompanying drawings, the present invention is further detailed explanation:
Description of drawings
Fig. 1 is the present invention by computer control, electron beam purification starting material, in nitrogen atmosphere, Frequency Induction Heating molybdenum crucible, the method for Czochralski grown sapphire crystal growth and the structural representation of equipment thereof;
Fig. 2 is the structure for amplifying synoptic diagram of the Frequency Induction Heating molybdenum crucible temperature field device among the present invention;
Fig. 3 is the control electricity cabinet block diagram among the present invention;
Fig. 4 is the medium frequency induction power supply control electricity cabinet block diagram among the present invention.
The drawing explanation:
The explanation of Fig. 1 crystal growth equipment1, hydrogen venting port and valve 2, crystal growing chamber door 3, crystal growing chamber 4, viewing window 5, temperature field device 6, seed chuck 7, pottery lifting rod 8, pressure transmitter 9, hydrogen inlet and valve 10, vacuum test pipe 11, vacuum pipe 12, ruhmkorff coil electrode 13, low vacuum valve 14, high vacuum valve 15, cooling pit 16, turbomolecular pump 17, low vacuum valve 18, associated mode mechanical pump 19, anistree measuring seat 20, anistree measuring seat 21, temperature sensor
Fig. 2 temperature schematic view illustrating1, stay-warm case 8, refractory brick cover (1) 9, refractory brick cover (2) 10, quartz socket tube 11, molybdenum crucible lid 12, molybdenum crucible on stay-warm case 7, the zirconium white under Medium frequency induction coil 2, die casting mica base 3, zirconium white collet 4, zirconium white insulation sand 5, zirconium white insulation base 6, the zirconium white
Fig. 3 control electricity cabinet block diagram illustrations1, display screen 2, equipment operation control panel 3, computer temperature system 4, crystal growth control panel 5, vacuscope control panel 6, turbo-molecular pumping source
Fig. 4 intermediate frequency power supply control electricity cabinet block diagram illustrations1. instrument display screen 2. trip switchs
Embodiment
A kind ofly in nitrogen atmosphere, use induction heating molybdenum crucible Czochralski grown sapphire crystal to comprise the steps: a, the protection of a high temperature, isoperibol be set and the crystal growth vacuum chamber of the gas atmosphere environment protection that adapts with crystal growth; The warm field device of b, Frequency Induction Heating molybdenum crucible; C, use reducing atmosphere shielding gas-hydrogen; The pulling apparatus of d, crystal growth; E, the isometrical electronic scales measuring system of control growing crystal; Al after f, use are purified by electron beam
2O
3Starting material; Form a monocrystalline nuclear by introduce seed crystal in melt, then, constantly carry out rearranging of molecule on the boundary of nucleus melt, the array of being piled up directly changes oldered array into and forms crystal.
In conjunction with Fig. 1～4, this equipment is made up of warm field device, hydrogen flowing quantity Controlling System, the pulling apparatus of crystal growth, the control growing crystal of vacuum system, Frequency Induction Heating molybdenum crucible isometrical electronic scales measuring system, computer temperature Controlling System and cooling system, wherein:
The crystal growth equipment mainframe box divides levels, the top section setting: crystal growing chamber door [1-1], crystal growing chamber [1-3], viewing window [1-4], warm field device [1-5], seed chuck [1-6], ceramic lifting rod [1-7], pressure transmitter [1-8], hydrogen inlet and valve [1-9]; The setting of lower floor's cabinet is made up of hydrogen venting port and valve [1-1], and isolate steel plate is set between the levels, and crystal growth vacuum chamber casing [1-3] is fixed on the isolate steel plate of the portion of combining between the higher and lower levels, and makes the cabinet top and the bottom be integrated into firm integral body.
(1) vacuum system comprises crystal growth vacuum chamber [1-3], direct connection sliding vane rotary vacuum pump [1-18], turbomolecular pump [1-16], high vacuum valve [1-14] and vacuum system pipeline [1-11], and crystal growth vacuum chamber [1-3] connects direct connection sliding vane rotary vacuum pump [1-18] and turbomolecular pump [1-16] through low vacuum valve [1-17] and vacuum system pipeline [1-11];
(2) Frequency Induction Heating temperature field device is fixed in the crystal growth vacuum chamber, by intermediate frequency power supply [4-1], Medium frequency induction coil [2-1], die casting mica base [2-2], zirconium white collet [2-3], zirconium white insulation sand [2-4], zirconium white insulation base [2-5], stay-warm case under the zirconium white [2-6], stay-warm case on the zirconium white [2-7], refractory brick cover (1) [2-8], refractory brick cover (2) [2-9], quartz socket tube [2-10], molybdenum crucible lid [2-11], molybdenum crucible [2-12] is formed, crystal starting material by in the Frequency Induction Heating fusing molybdenum crucible form the raw-material melt of crystal;
(3) shielding gas-hydrogen and the hydrogen flowing quantity Controlling System of use reducing atmosphere: comprise the hydrogen inlet and the valve [1-9] that are fixed on crystal growth vacuum chamber [1-3] top, inflation valve connects hydrogen quality under meter and sources of hydrogen successively by pressure piping;
(4) crystal growing and pulling device comprises the fixedly molybdenum matter seed chuck [1-6] of seed crystal, and seed chuck is fixed on the ceramic lifting rod [1-7], and ceramic lifting rod [1-7] is connected with the dynamo-electric pulling apparatus in outside, crystal growth vacuum chamber top; Seed rod is positioned at the top of crystal growth vacuum chamber temperature field device [1-5] molybdenum crucible [2-12], controls crystalline growth velocity by rotation, vertical operation;
(5) the isometrical electronic scales measuring system of control growing crystal, the pressure transmitter [1-8] on the ceramic lifting rod [1-7] and computer temperature Controlling System [3-3] the control growing crystal that cooperatively interacts is isometrical by being fixed in the crystal growth vacuum chamber;
(6) be used to make the computer temperature Controlling System [3-3] that produces high temperature temperature field in the crystal growth vacuum chamber to comprise feedback channel remote signal collection transport sector, temperature regulator and forward path temperature control topworks, the feedback channel remote signal is gathered the temperature signal input temp controller that transport sector is gathered the crystal growth vacuum chamber, computer is by the temperature signal of crystal growing furnace in the asynchronous communication interface timesharing receiving crystal growth vacuum chamber, every road temperature signal all passes through pid control algorithm, generates needed steering order and gives the crystal growth of forward path temperature control actuating mechanism controls;
(7) cooling system cools off the casing and the ruhmkorff coil [2-1] of the sub-pump of turbo-molecular [1-16], associated mode mechanical pump [1-18], cooling pit [1-15], crystal growth vacuum chamber.
The crystal growth technique process:
1, the Al after the use electron beam is purified
2O
3Starting material;
Open the crystal growth door for vacuum chamber when 2, equipment uses, clean crystal growth vacuum chamber, and the crystal growth raw material put into molybdenum crucible, and seed crystal is installed on seed chuck, and is closed the crystal growth door for vacuum chamber, open total water source;
3, open general supply, and startup robot calculator execution trace routine is carried out system's detection to equipment;
4, behind the startup associated mode mechanical pump, take out rough vacuum;
5, start the vacuum test instrument, when the system vacuum degree reaches 3Pa, start turbomolecular pump, crystal growth vacuum chamber pumping high vacuum;
6, the vacuum tightness when the crystal growth vacuum chamber reaches 3 * 10
-4During Pa, can carry out crystal growth and prepare;
7, charge into shielding gas hydrogen or keep the certain vacuum degree according to processing requirement;
8, adjust the computer temperature Controlling System, with per hour 300 ℃ speed intensification; Reach 2150 ℃ of processing requirements; Crystal starting material by in the Frequency Induction Heating fusing molybdenum crucible form the raw-material melt of crystal;
9, seeding: start crystal growing and pulling device, seed crystal is fallen in the molybdenum crucible in the raw-material melt, it is molten that seed crystal and melt are soaked mutually, induces by seed crystal that molecule is rearranged for oldered array on solid-liquid body interface, the formation crystal; Control crystalline growth velocity by crystal growing and pulling device rotation, vertical operation;
10, crystal growth: use cooling shouldering method, per hour lower the temperature 3 ℃,, begin constant temperature then and grow to required length, per hour heat up again 5 ℃ and receive shoulder until reaching the diameter that needs; Perhaps use the isometrical electronic scales measuring system of control growing crystal, by being fixed in the crystal growth vacuum chamber control crystal growth that cooperatively interacts of the pressure transmitter on the ceramic lifting rod and computer temperature Controlling System;
11, after finishing crystal growth, adjust the computer temperature Controlling System, with per hour 120 ℃ speed cooling;
12, after reaching room temperature in the crystal growth vacuum chamber, close the vacuum test instrument, close each vacuum valve and vacuum pump;
13, close the heating in medium frequency power supply, close cooling water valve;
14, start crystal growth vacuum chamber button, the crystal growth vacuum chamber is inflated;
15, open the crystal growth door for vacuum chamber, clean crystal growth vacuum chamber takes out crystal, closes the crystal growth door for vacuum chamber then;
16, the crystal growth vacuum chamber is taken out rough vacuum.
As proceeding crystal growth, then repeat above-mentioned 1-15 program;
If shutdown is shut down computer, carry out trace routine; Close general supply, close total water source.
Claims (6)
1, use induction heating molybdenum crucible Czochralski grown sapphire crystal it is characterized in that in the nitrogen atmosphere:
A, the protection of a high temperature, isoperibol is set and the crystal growth vacuum chamber of the gas atmosphere environment protection that adapts with crystal growth;
The warm field device of b, Frequency Induction Heating molybdenum crucible;
C, use reducing atmosphere shielding gas-hydrogen;
The pulling apparatus of d, crystal growth;
E, the isometrical electronic scales measuring system of control growing crystal;
Al after f, use are purified by electron beam
2O
3Starting material
2, according to using induction heating molybdenum crucible Czochralski grown sapphire crystal method in the described nitrogen atmosphere of claim 1, it is characterized in that: adopt the warm field device of Frequency Induction Heating molybdenum crucible in the atmosphere of using reducing gas-hydrogen, the crystal starting material of molybdenum crucible are melt in the heat fused crystal growth vacuum chamber; Introduce seed crystal and form a monocrystalline nuclear in melt, then, constantly carry out rearranging of atom or molecule on the boundary of nucleus melt, the array of being piled up directly changes oldered array into and forms crystal.
3, according to the warm field device of the described use Frequency Induction Heating of claim 1 molybdenum crucible, it is characterized in that: warm field device is made up of intermediate frequency power supply, heating unit and attemperator respectively; Heating unit provides electric current by intermediate frequency power supply to the Medium frequency induction coil, and the induced current that ruhmkorff coil produced makes molybdenum crucible produce high temperature, thereby makes the crystal starting material Al in the molybdenum crucible
2O
3Fusing forms Al
2O
3Melt; Attemperator is by upper and lower annular zirconium white stay-warm case, the zirconium white thermal insulating seat, and quartz socket tube, oxidation zircon sand thermal insulation layer, compositions such as die casting mica thermal insulating seat, aluminum oxide stay-warm case are to guarantee crystal starting material Al in the molybdenum crucible
2O
3Melt be under high temperature, the isoperibol state.
4, according to the described use reducing atmosphere of claim 1 shielding gas-hydrogen, it is characterized in that: eliminate and use molybdenum crucible and Al in the Frequency Induction Heating process
2O
3" molybdenum clothing " that reaction is produced and protection molybdenum crucible are difficult for oxidation in the condition of high temperature;
5, according to the Al after the described use electron beam purification of claim 1
2O
3Starting material is characterized in that: at the indoor purification crucible that is provided with of ultrahigh vacuum(HHV),, evaporate after making metal or nonmetallic impurity reach its vaporization temperature being carried out indirect heating by the purification material in the crucible by electron beam gun emission high power density electronic beam current.
6, be implemented in use induction heating molybdenum crucible Czochralski grown sapphire crystal in the nitrogen atmosphere, it is characterized in that: realize computer control, electron beam purification starting material, in nitrogen atmosphere, the method and the equipment thereof of Frequency Induction Heating molybdenum crucible Czochralski grown sapphire substrate crystal technology, form by electronic scales measuring system, computer temperature Controlling System and cooling system that warm field device, hydrogen flowing quantity Controlling System, the pulling apparatus of crystal growth, the control growing crystal of vacuum system, Frequency Induction Heating molybdenum crucible are isometrical, wherein:
(1) vacuum system comprises crystal growth vacuum chamber, direct connection sliding vane rotary vacuum pump, turbomolecular pump, vacuum valve and vacuum system pipeline composition, and the crystal growth vacuum chamber is connected direct connection sliding vane rotary vacuum pump and turbomolecular pump through vacuum valve respectively with the vacuum system pipeline;
(2) Frequency Induction Heating temperature field device is made up of intermediate frequency power supply, heating unit and attemperator; Heating unit is fixed in the crystal growth vacuum chamber, form by Medium frequency induction coil and molybdenum crucible, attemperator is by upper and lower annular zirconium white stay-warm case, the zirconium white thermal insulating seat, quartz socket tube, oxidation zircon sand thermal insulation layer, die casting mica thermal insulating seat, compositions such as aluminum oxide stay-warm case, the crystal starting material by in the Frequency Induction Heating fusing molybdenum crucible form the raw-material melt of crystal;
(3) shielding gas-hydrogen and the hydrogen flowing quantity Controlling System of use reducing atmosphere comprise the hydrogen inflation valve that is fixed on top in the crystal growth vacuum chamber, and inflation valve connects hydrogen quality under meter and sources of hydrogen successively by pressure piping;
(4) crystal growing and pulling device comprises: the fixing molybdenum matter anchor clamps seed rod of seed crystal, and seed rod is fixed on the ceramic lifting rod, and ceramic lifting rod is connected with the dynamo-electric pulling apparatus in outside, crystal growth vacuum chamber top; Seed rod is positioned at the top of crystal growth vacuum chamber crucible, in attemperator, by rotating, vertically moving and control crystalline growth velocity;
(5) the isometrical electronic scales measuring system of control growing crystal, the pressure transmitter on the ceramic lifting rod and the computer temperature Controlling System control growing crystal that cooperatively interacts is isometrical by being fixed in the crystal growth vacuum chamber;
(6) be used to make the computer temperature Controlling System that produces high temperature temperature field in the crystal growth vacuum chamber to comprise feedback channel remote signal collection transport sector, temperature regulator and forward path temperature control topworks, the feedback channel remote signal is gathered the temperature signal input temp controller that transport sector is gathered the crystal growth vacuum chamber, computer is by the temperature signal of crystal growing furnace in the asynchronous communication interface timesharing receiving crystal growth vacuum chamber, every road temperature signal all passes through pid control algorithm, generates needed steering order and gives the crystal growth of forward path temperature control actuating mechanism controls;
(7) cooling system cools off the casing and the Medium frequency induction coil of turbomolecular pump, associated mode mechanical pump, cooling pit, crystal growth vacuum chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02134220 CN1228477C (en) | 2002-06-21 | 2002-06-21 | Using induction heating molybdenium crucible in hydrogen atmosphere to make Czochralski grown sapphire crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02134220 CN1228477C (en) | 2002-06-21 | 2002-06-21 | Using induction heating molybdenium crucible in hydrogen atmosphere to make Czochralski grown sapphire crystal |
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| CN1228477C CN1228477C (en) | 2005-11-23 |
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