CN200958115Y - Crystal-growth carbon-film coater for quartz crucible - Google Patents
Crystal-growth carbon-film coater for quartz crucible Download PDFInfo
- Publication number
- CN200958115Y CN200958115Y CN 200620035962 CN200620035962U CN200958115Y CN 200958115 Y CN200958115 Y CN 200958115Y CN 200620035962 CN200620035962 CN 200620035962 CN 200620035962 U CN200620035962 U CN 200620035962U CN 200958115 Y CN200958115 Y CN 200958115Y
- Authority
- CN
- China
- Prior art keywords
- pneumatic tube
- quartz crucible
- settling chamber
- valve
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Abstract
The utility model relates to a carbon film coating device for a crystalgrowing quartz crucible, which comprises a heating stove, a settling chamber for placing the quartz crucible to be coated and a gas supplying controller. The heating stove consists of a stove body, heating fittings arranged on the stove body and a temperature controller and detector. A supporting base for placing the settling chamber is arranged at the lower part of the hearth of the stove; the settling chamber consists of a tube shaped body with one end open and a stopper which encloses another end of the tube shaped body. An air intake pipe and an air outlet pipe which are communicated with the inner holes of the tube shaped body are arranged on the stopper; the gas supplying controller consists of a gas transmitting system and a control valve. The gas transmitting system consists of two gas transmitting pipes which are separately connected with the air intake pipe plugged into the tube shaped body in the settling chamber and into the air intake pipe plugged in the to be coated quartz crucible. A methane gas inlet and an inert shielding gas outlet are arranged on the gas transmitting pipe. The control valve is arranged on the pipeline of the gas transmitting system, to control the entry of the inert shielding gas into the tube shaped body in the settling chamber and the to be coated quartz crucible, and control the entry of the methane gas into the to be coated quartz crucible.
Description
Technical field
The utility model belongs to quartz container plated film field, particularly a kind of device that plates carbon film at the inner wall of quartz crucible of crystal growth.
Background technology
AgGaS
2, AgGaSe
2, AgGaSeS, AgGa
1-xIn
xSe
2Deng nonlinear optical material, have the infrared transparent wide ranges, outstanding advantages such as double refraction that nonlinear optical coefficients are big, suitable and low chromatic dispersion can be carried out and frequency, difference frequency, the adjustable infrared light parametric oscillation of three wave mixings and broadband.CdZnTe (CZT) crystal is the indoor temperature nucleus radiation detector material of excellent performance.The above-claimed cpd semiconductor material adopts Bridgman method (Brigdman method) growing single-crystal usually, the crystallization difficulty is big, contained Ga or Cd etc. are under hot conditions in the material, can faint chemical reaction take place with quartz crucible, cause melt and the adhesion of crucible inwall, not only cause crystal to pollute, can make that also melt crystallization is finished after, cause that crystal and growth ampoule break, and are difficult to obtain the good single crystal of integrity.Studies show that, on the inwall of quartz crucible, plate high-quality carbon film and not only can make the crucible inwall Paint Gloss, and can prevent the adhesion and the erosion of melt and crucible, reduce parasitic nucleation, help that integrity is good, the growth of high quality single crystal.
The quartz crucible of crystal growth generally is made up of seed crystal bag, shouldering section, isodiametric growth section and interface etc., is thin tube-like.Therefore, it is very big to plate the carbon film difficulty that meets the crystal growth requirement at the crucible inwall.Min Jiahua etc. have delivered " CdZnTe crystal growth with the plating carbon technical study of silica tube " and (have seen functional materials and device journal on " functional materials and device journal ", Vol.11, No.2,255,2005), the disclosed crystal growth of this article be carbon source with the silica tube carbon film coating method with " dehydrated alcohol ", and dehydrated alcohol is carried by high pure nitrogen after the water bath with thermostatic control heating is vaporized and enters by the plated film quartz crucible, and at high temperature dehydrated alcohol decomposites carbon and is attached on the inwall of quartz crucible.With the supporting film coating apparatus not full disclosure in above-mentioned paper of this method, only introduced the device of coating process and mainly formed by plating carbon stove, carbon source, water-bath device, breather and silica tube.
Summary of the invention
The purpose of this utility model is to overcome the deficiencies in the prior art, a kind of quartz crucible plating carbon film device of crystal growth is provided, this kind device is not only simple in structure, easy to operate, with the supporting use of corresponding carbon film coating method, then can on inner wall of quartz crucible, deposit in the short period of time in conjunction with carbon film layer firm, even compact.
The quartz crucible plating carbon film device of crystal growth described in the utility model comprises process furnace, places by the settling chamber of plated film quartz crucible and air feed controller; Process furnace comprises body of heater, is installed in heating unit, temperature control thermoscope on the body of heater, and the lower furnace portion of body of heater is provided with the bearing that is used to lay the settling chamber; The settling chamber comprises the tubular body of an end opening and the stopper of closed tube body port, and the length of described tubular body and internal diameter are inserted with the inlet pipe and the vapor pipe that communicate with the tubular body endoporus greater than by the quartz crucible of plated film on the described stopper; The air feed controller comprises gas transmission piping and control valve; described gas transmission piping contains two pneumatic tubes that are connected by the inlet pipe of plated film quartz crucible with the inlet pipe of inserting settling chamber's tubular body and insertion respectively; be provided with methane gas import and inert protective gas import; described control valve is installed on the pipeline of gas transmission piping, and the control inert protective gas enters settling chamber's tubular body and entered by the plated film quartz crucible by plated film quartz crucible and control methane gas.
The temperature control thermoscope of said apparatus reaches the temperature control indicating instrument that is connected with thermopair by the thermopair that is installed in point for measuring temperature in the process furnace burner hearth and forms.
When said apparatus uses, about the assembling mode of parts or member is: the inlet pipe and the insertion of inserting settling chamber's tubular body are connected with corresponding pneumatic tube in the air feed controller by the inlet pipe of plated film quartz crucible, the settling chamber that quartz crucible is housed is placed on the bearing of process furnace burner hearth bottom, settling chamber's this body and function plug closes end is towards the process furnace fire door and stretch out outside the stove, and it stretches out the outer length of stove and does not exceed not produced carbon laydown by plated film quartz crucible closure part with upper segment.
As follows with the processing step of the carbon film coating method of plating carbon film matched with devices described in the utility model:
(1) processing of quartz crucible
The processing of quartz crucible comprises cleans and oven dry,
The cleaning of quartz crucible is followed successively by tap water flushing, dipping by lye, deionized water rinsing, K
2Cr
2O
7-H
2SO
4Washing lotion immersion, deionized water rinsing, acetone soak, deionized water rinsing,
Described dipping by lye, soak time were at least 30 minutes, described K
2Cr
2O
7-H
2SO
4Washing lotion is soaked, and soak time was at least 30 minutes, and described acetone soaks, and soak time was at least 24 hours,
After cleaning up, puts into by quartz crucible the drying plant dry for standby immediately;
(2) shove charge
From drying plant, take out silica crucible during plating carbon; And with the air inlet pipe insertion silica crucible Zhong that cleans; The silica crucible that will be inserted with then air inlet pipe is positioned over the body Zhong of tubular type mud chamber; The port plug closes of tubular type mud chamber body; During plug closes; The air inlet pipe of inserting silica crucible Zhong is passed stopper and is stretched out Yu the appendix for airgun controller and be connected; Also be inserted with air inlet pipe and the blast pipe logical Yu the body endoporus Xiang of mud chamber on the stopper of sealing mud chamber port; The air inlet pipe logical Yu the body endoporus Xiang of mud chamber is connected Yu the appendix that supplies airgun controller
After the assembling of quartz crucible and settling chamber, air feed controller finishes, the settling chamber that quartz crucible is housed is put into the burner hearth of process furnace, stretch out outside the stove with the plug closes end settling chamber;
(3) heating
After the settling chamber that quartz crucible is housed places in the burner hearth of process furnace, speed intensification with 2 ℃～3 ℃/minute under normal pressure is heated, to 1000 ℃～1060 ℃, be incubated and logical high purity inert gas eliminating residual air in quartz crucible and settling chamber in this temperature then, gas flow is 600～700ml/ minute, the time of logical high purity inert gas was at least 30 minutes
Described high purity inert gas is nitrogen or the argon gas of purity more than 99.99%;
(4) plated film
After settling chamber and the logical rare gas element end of quartz crucible, continuation is 1000 ℃～1060 ℃ insulations, and at flow to quartz crucible in the ventilating methane gas of this temperature with 50ml～60ml/ minute, the time of ventilating methane gas is 25 minutes～40 minutes, can make that sedimentary carbon film thickness meets the requirement of crystal growth on the inner wall of quartz crucible between 150nm to 230nm;
(5) rete annealing
After plated film finishes, continue, be cooled to room temperature with 1 ℃/minute～2 ℃/minute speed then 1000 ℃～1060 ℃ insulations 40 minutes～60 minutes.
In the aforesaid method, the employed alkali lye of dipping by lye is the NaOH or the NaCO of mass concentration 8%～10%
3The aqueous solution.
In the aforesaid method, K
2Cr
2O
7-H
2SO
4The component that washing lotion is soaked the washing lotion of using is K
2Cr
2O
7, dense H
2SO
4And deionized water, K
2Cr
2O
7With gram or kilogram metering, dense H
2SO
4Measure with milliliter or liter with deionized water, proportioning is:
K
2Cr
2O
7Quality: dense H
2SO
4Volume: deionized water volume=1: 16: 2.
In the aforesaid method, settling chamber's this body and function plug closes end stretches out the outer length of stove and does not produce carbon laydown with the quartz crucible closure part with outer portion part and exceed.
The utlity model has following beneficial effect:
1, meets the requirement of plating carbon technology, with the supporting use of carbon film coating method, (25 minutes～40 minutes) can make and form the level and smooth carbon film layer of the macroscopic view that is evenly distributed on the whole inner wall of quartz crucible at short notice, and also can plate the carbon film layer of even compact for complex-shaped quartz crucible.
2, simple in structure, be easy to make, control is convenient.
Description of drawings
Fig. 1 is a kind of shape structural map of quartz crucible;
Fig. 2 is a kind of structure diagram of the quartz crucible plating carbon film device of crystal growth described in the utility model, and this figure has also shown the mounting means of quartz crucible in the settling chamber;
Fig. 3 is a kind of structure iron of air feed controller.
Among the figure, 1-body of heater, 2-thermopair, 3-temperature control indicator, 4-heating unit, 5-burner hearth, 6-quartz crucible, 7-bearing, 8-settling chamber, 9-stopper, 10-vapor pipe, 11-air feed controller, 12-settling chamber inlet pipe, 13-quartz crucible inlet pipe, 14-T-valve, 15-stopping valve k
3, 16-stopping valve k
2, 17-stopping valve k
1, 18-pneumatic tube I, 19-pneumatic tube II.
Embodiment
Embodiment:
Present embodiment is to the inner wall of quartz crucible plating carbon film of crystal growth shown in Figure 1, and the structure of film coating apparatus and the mounting means of quartz crucible are as shown in Figure 2.Film coating apparatus comprises process furnace, places by the settling chamber 8 of plated film quartz crucible and air feed controller 11; Process furnace is a mono temperature area resistance furnace, comprise body of heater 1, be installed in heating unit 4, temperature control thermoscope on the body of heater, heating unit 4 is along the body of heater axial distribution, the temperature control thermoscope reaches the FP93 temperature control indicating instrument 3 that is connected with thermopair by the thermopair 2 that is installed in point for measuring temperature in the process furnace burner hearth and forms (temperature-controlled precision is 1 ℃), and burner hearth 5 bottoms of body of heater are provided with two bearings 7 that are used to lay the settling chamber; Settling chamber 8 comprises the tubular body of an end opening and the stopper 9 of closed tube body port, described tubular body is a silica tube, its length and internal diameter get final product can place by the quartz crucible of plated film and plug-in mounting inlet pipe, are inserted with the inlet pipe 12 and the vapor pipe 10 that communicate with the tubular body endoporus on the described stopper; Air feed controller 11 comprises gas transmission piping and control valve, as shown in Figure 3, described gas transmission piping contains the pneumatic tube I18 that is connected with the inlet pipe 12 of inserting settling chamber's tubular body, with insert the pneumatic tube II19 that is connected by the inlet pipe 13 of plated film quartz crucible, pneumatic tube I links to each other by pipe fitting with pneumatic tube II, described control valve is three stopping valve and a T-valve, stopping valve k
117 are installed in the exit end of pneumatic tube II19, stopping valve k
216 are installed in the entrance end of pneumatic tube II19, stopping valve k
315 are installed on the connecting tube of pneumatic tube I and pneumatic tube II, and T-valve 14 is installed on the pneumatic tube I18, and the inlet mouth of pneumatic tube II is connected with the methane gas pneumatic tube, and T-valve 14 links to each other with the inert protective gas pneumatic tube.
During use, the mounting means of quartz crucible and film coating apparatus: be positioned at settling chamber's tubular body by plated film quartz crucible 6, inserting the inlet pipe 12 of settling chamber's tubular body and insertion is connected with pneumatic tube II by corresponding pneumatic tube I in the inlet pipe 13 of plated film quartz crucible and the air feed controller, the settling chamber 8 that quartz crucible is housed is placed on the bearing 7 of process furnace burner hearth bottom, settling chamber's this body and function stopper 9 blind ends are towards the process furnace fire door and stretch out outside the stove, it stretches out the outer length of stove should make that to be stretched out the outer length l of stove by plated film quartz crucible sealing end be 10cm, to guarantee not produced carbon laydown by plated film quartz crucible closure part with upper segment.
Claims (6)
1, a kind of quartz crucible of crystal growth plating carbon film device is characterized in that comprising process furnace, places by the settling chamber of plated film quartz crucible (8) and air feed controller (11),
Process furnace comprises body of heater (1), is installed in heating unit (4), thermostat on the body of heater, and the burner hearth of body of heater (5) bottom is provided with the bearing (7) that is used to lay the settling chamber,
Settling chamber (8) comprises the tubular body of an end opening and the stopper (9) of closed tube body port, is inserted with the inlet pipe (12) and the vapor pipe (10) that communicate with the tubular body endoporus on the described stopper,
Air feed controller (11) comprises gas transmission piping and the control valve that is installed on the gas transmission piping pipeline.
2, the quartz crucible of crystal growth according to claim 1 plating carbon film device, assembling mode when it is characterized in that using is: the inlet pipe (12) of inserting settling chamber's tubular body is connected with corresponding pneumatic tube in the air feed controller by the inlet pipe of plated film quartz crucible (13) with inserting, the settling chamber (8) that quartz crucible is housed is placed on the bearing (7) of process furnace burner hearth bottom, and settling chamber's this body and function stopper (9) blind end is towards the process furnace fire door and stretch out outside the stove.
3, the quartz crucible of crystal growth according to claim 2 plating carbon film device is characterized in that settling chamber's this body and function stopper (9) blind end stretches out the outer length of stove and do not exceed not produced carbon laydown by plated film quartz crucible closure part with upper segment.
4,, it is characterized in that the temperature control thermoscope reaches the temperature control indicating instrument (3) that is connected with thermopair by the thermopair that is installed in point for measuring temperature in the process furnace burner hearth (2) and forms according to the quartz crucible plating carbon film device of claim 1 or 2 or 3 described crystal growths.
5, the quartz crucible according to claim 1 or 2 or 3 described crystal growths plates the carbon film device, it is characterized in that described gas transmission piping contains the pneumatic tube I (18) that is connected with the inlet pipe (12) of inserting settling chamber's tubular body, with insert the pneumatic tube II (19) that is connected by the inlet pipe of plated film quartz crucible (13), pneumatic tube I links to each other by pipe fitting with pneumatic tube II, described control valve is three stopping valve and a T-valve, stopping valve k
1(17) be installed in the exit end of pneumatic tube II (19), stopping valve k
2(16) be installed in the entrance end of pneumatic tube II (19), stopping valve k
3(15) be installed on the connecting tube of pneumatic tube I and pneumatic tube II, T-valve (14) is installed on the pneumatic tube I (18), and the inlet mouth of pneumatic tube II is connected with the methane gas pneumatic tube, and T-valve links to each other with the inert protective gas pneumatic tube.
6, the quartz crucible of crystal growth according to claim 4 plating carbon film device, it is characterized in that described gas transmission piping contains the pneumatic tube I (18) that is connected with the inlet pipe (12) of inserting settling chamber's tubular body, with insert the pneumatic tube II (19) that is connected by the inlet pipe of plated film quartz crucible (13), pneumatic tube I links to each other by pipe fitting with pneumatic tube II, described control valve is three stopping valve and a T-valve, stopping valve k
1(17) be installed in the exit end of pneumatic tube II (19), stopping valve k
2(16) be installed in the entrance end of pneumatic tube II (19), stopping valve k
3(15) be installed on the connecting tube of pneumatic tube I and pneumatic tube II, T-valve (14) is installed on the pneumatic tube I (18), and the inlet mouth of pneumatic tube II is connected with the methane gas pneumatic tube, and T-valve links to each other with the inert protective gas pneumatic tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200620035962 CN200958115Y (en) | 2006-10-23 | 2006-10-23 | Crystal-growth carbon-film coater for quartz crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200620035962 CN200958115Y (en) | 2006-10-23 | 2006-10-23 | Crystal-growth carbon-film coater for quartz crucible |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN200958115Y true CN200958115Y (en) | 2007-10-10 |
Family
ID=38784990
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200620035962 Expired - Fee Related CN200958115Y (en) | 2006-10-23 | 2006-10-23 | Crystal-growth carbon-film coater for quartz crucible |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN200958115Y (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110819960A (en) * | 2019-12-19 | 2020-02-21 | 苏州凯利昂光电科技有限公司 | Continuous gas supply device for sputtering coating |
-
2006
- 2006-10-23 CN CN 200620035962 patent/CN200958115Y/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110819960A (en) * | 2019-12-19 | 2020-02-21 | 苏州凯利昂光电科技有限公司 | Continuous gas supply device for sputtering coating |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100489154C (en) | Carbon film coating method and device for quartz crucible for use in crystal growth | |
| CN105063741B (en) | The preparation method of ZnTe monocrystal | |
| CN207552442U (en) | A kind of large area HF CVD diamond film growth device | |
| CN113026106B (en) | Growth process of silicon carbide crystal | |
| CA1179213A (en) | Process for producing an optical fiber preform and apparatus therefor | |
| CN200958115Y (en) | Crystal-growth carbon-film coater for quartz crucible | |
| CN208472105U (en) | Examine microbiological incubator | |
| CN106319618A (en) | Equipment and method for manufacturing czochralski silicon rod from silane | |
| CN108531981A (en) | A method of preparing two-dimentional indium trisulfide monocrystalline in mica substrate | |
| CN101397651A (en) | Method for plating carbon film on ampoule internal wall for CdZnTe crystal growth and apparatus thereof | |
| CN201190120Y (en) | Automatic monitoring apparatus for purification and re-use of recirculated cooling water | |
| CN203187688U (en) | Algae cultivation box | |
| CN108502873B (en) | Preparation method of high-quality graphene with few defects and uniform structure | |
| CN101834233A (en) | Method for rapidly depositing hydrogenated amorphous silicon solar battery thin film at low temperature | |
| CN107099782A (en) | A kind of chemical vapor deposition unit for preparing the thin-film materials such as graphene, hexagonal boron nitride | |
| CN112851138A (en) | Smoked carbon device of quartz ampoule wall | |
| CN106435519A (en) | Method for improving uniformity of tungsten coating prepared on inner wall of long pipe through CVD method | |
| CN108676710B (en) | Method and device for simulating influence of blue algae decomposition on generation and release of greenhouse gases | |
| CN103489749B (en) | The method of many circulations rapid thermal annealing assistant metal inducing crystallization of amorphous silicon thin film | |
| CN111486795B (en) | Experimental device and method for researching growth and deposition of natural gas hydrate film in gas transmission pipeline | |
| CN113322522B (en) | Preparation method of large-single-domain large-area single-layer tungsten disulfide film by epitaxy | |
| CN107541714B (en) | Rapid growth method of large-size graphene glass | |
| CN105177533A (en) | Method for washing MWCVD cabin in situ by using plasma | |
| CN1699236A (en) | Glass coated with titanium nitride and preparation method thereof | |
| US5232855A (en) | Apparatus for use in a axenic mass culture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20071010 Termination date: 20091123 |