CN203049089U - Pulse injection type metal organic chemical vapor deposition system - Google Patents
Pulse injection type metal organic chemical vapor deposition system Download PDFInfo
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- CN203049089U CN203049089U CN 201320019409 CN201320019409U CN203049089U CN 203049089 U CN203049089 U CN 203049089U CN 201320019409 CN201320019409 CN 201320019409 CN 201320019409 U CN201320019409 U CN 201320019409U CN 203049089 U CN203049089 U CN 203049089U
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Abstract
The utility model relates to a pulse injection type metal organic chemical vapor deposition system which comprises a vacuum reaction chamber. The vacuum reaction chamber is internally provided with a hollow sample table which is closed at the bottom end and provided with an upper cover at the upper end. The hollow sample table is internally provided with an optical heater. A substrate is arranged at the lower side at the closed end of the hollow sample table. The vacuum reaction chamber is provided with a gas inlet communicated with a high-pressure gas bottle. A gas feed-in device is arranged outside the vacuum reaction chamber and is communicated with the vacuum reaction chamber through an injection opening. The gas feed-in device comprises an evaporator communicated with the injection opening. The inlet end of the evaporator is communicated with a micro-liquid feed-in device. The micro-liquid feed-in device consists of a steel tank for containing a precursor liquid and an electromagnetic spraying valve. The nozzle of the electromagnetic spraying valve is hermetically communicated with the inlet end of the evaporator. The steel tank is communicated with the high-pressure gas bottle. The electromagnetic spraying valve is electrically connected with a control device. The control device controls the liquid feed-in device to inject the precursor body into the evaporator by way of pulse.
Description
Technical field
The utility model is about a kind of metal organic chemical vapor deposition system, relates in particular to the pouring-in metal organic chemical vapor deposition film preparing system of a kind of pulse.
Background technology
Utilize the organometallics (Metal Organism) that easily decomposes under the low temperature and volatilize to be called metal organic chemical vapor deposition (MOCVD) as the method that substance source carries out chemical vapour deposition, metal organic chemical vapor deposition is a kind of novel vapor phase epitaxial growth technology that grows up on the basis of vapor phase epitaxial growth (VPE), it is with III family, organic compound and the V of II family element, the hydride of VI family element etc. are as the crystal growth starting material, in the pyrolysis mode at the enterprising promoting the circulation of qi phase epitaxy of substrate, the various III-V family of growing, the thin layer monocrystal material of II-VI compound semiconductor and their multivariate solid solution.Usually the crystal growth in the metal organic chemical vapor deposition system all is at normal pressure or the down logical H of low pressure (10-100Torr)
2Cold wall quartz (or stainless steel) reaction chamber in carry out, reaction chamber temperature is 500-1200 ℃,, H
2Fluid supply bubbling by Controllable Temperature carries metallorganics to the vitellarium.The characteristics of metal organic chemical vapor deposition technology are: (1) scope of application is extensive, almost can grow all compounds and alloy semiconductor; (2) the various heterogeneous structure materials that are very suitable for growing; (3) can the grow ultra-thin epitaxial film, and can obtain very steep interfaces transition; (4) growth is easy to control; (5) material with very high purity of can growing; (6) the epitaxial film large-area uniformity is good; (7) can carry out scale operation.
But, the structure of existing metal organic chemical vapor deposition system is to place substrate in quartz glass tube, the control out of true of the consumption of presoma and carrier gas, and the chemical stability of presoma before the uncontrollable reaction can not be controlled the thickness of speed of reaction and film well.
Thus, the inventor relies on experience and the practice of being engaged in relevant industries for many years, proposes the pouring-in metal organic chemical vapor deposition of a kind of pulse system, to overcome the defective of prior art.
The utility model content
The purpose of this utility model is to provide the pouring-in metal organic chemical vapor deposition of a kind of pulse system, can better control the chemical stability of the preceding presoma of metal organic chemical vapor deposition reaction, and consumption and the carrier gas of presoma accurately controlled, to realize the accurate control to speed of reaction and film thickness.
The purpose of this utility model is to realize like this, the pouring-in metal organic chemical vapor deposition of a kind of pulse system, this metal organic chemical vapor deposition system includes the vacuum reaction chamber that sealing is communicated in vacuum pump, is provided with vacuumometer and thermo detector in the vacuum reaction chamber; Described vacuum reaction chamber upper end is provided with opening, constitutes sample and puts into end, and this vacuum reaction chamber is provided with the inlet mouth with the gas cylinder conducting; One gas feedthrough is arranged on the vacuum reaction chamber outside and passes through an inlet and vacuum reaction chamber conducting; Described gas feedthrough comprises the vaporizer that is communicated in inlet, the entrance end of vaporizer and the conducting of micro liquid feedthrough, and this micro liquid feedthrough is communicated in gas cylinder; This micro liquid feedthrough is made of cylinder of steel and an electromagnetic injection valve that holds precursor solution, and the spout of electromagnetic injection valve and the entrance end of vaporizer seal and conduct, and cylinder of steel is communicated in gas cylinder, and described electromagnetic injection valve is electrically connected with a control device; Put into a hollow sample table by its upper end open in the described vacuum reaction chamber, this hollow sample table bottom closed upper end is provided with loam cake, is provided with light heater in the hollow sample table; Hollow sample table upper end is tightly connected with the vacuum reaction chamber upper end open; This hollow sample table blind end downside is provided with substrate.
In a preferred embodiments of the present utility model, the entrance end of described vaporizer and the conducting of a plurality of micro liquid feedthrough.
In a preferred embodiments of the present utility model, described light heater is fixedly installed on loam cake; Described light heater is made of a plurality of bulbs.
In a preferred embodiments of the present utility model, described loam cake is fixedlyed connected with a Mechanical lifter, and this Mechanical lifter passes through actuator drives by motor.
In a preferred embodiments of the present utility model, the sidewall of described hollow sample table is the sandwich structure that is made of double-deck drum, and this mezzanine space is provided with prosopyle and posticum, is connected with water pump between prosopyle and the posticum and constitutes water-cooling circulating system.
In a preferred embodiments of the present utility model, described hollow sample table blind end downside fixedly has a hollow out specimen holder, and described substrate is placed on the hollow out place on the hollow out specimen holder; The inner edge of described hollow hole is provided with flange, and the edge of described substrate is set up on flange.
In a preferred embodiments of the present utility model, be covered with flexible baking heater on described gas feedthrough and the corresponding connecting tube thereof; This flexibility baking heater is made of the heating zone.
In a preferred embodiments of the present utility model, described light heater power is 8000-9000W, and maximum heating temperature is 800 ℃; Flexible baking heater total power is 1000W, and maximum heating temperature is 300 ℃.
In a preferred embodiments of the present utility model, described thermo detector is fixed in the vacuum reaction chamber blind end, and the probe height of thermo detector is consistent with substrate.
In a preferred embodiments of the present utility model, described vacuum reaction chamber upper end open place is provided with first flange; This vacuum reaction chamber is fixed on the housing by first flange; Hollow sample table upper end is provided with second flange, and this second flange is located at the first flange top; The bonding surface of described first flange and second flange is provided with sealing-ring.
From the above mentioned, the pouring-in metal organic chemical vapor deposition of the utility model pulse system, can keep the stability of presoma before chemical reaction, can accurately control simultaneously reaction meticulously carries out, be injected in the vaporizer with pulse mode with the accurate infinitesimal of the micro liquid feedthrough that links to each other with control device with precursor solution, atomizing is delivered to the high-temperature zone by carrier gas immediately, in substrate chemical transformation deposition film forming takes place; This system architecture is simple, cost of manufacture is low, easy to operate.
Description of drawings
The following drawings only is intended to the utility model done and schematically illustrates and explain, does not limit scope of the present utility model.Wherein:
Fig. 1: be the structural representation of the pouring-in metal organic chemical vapor deposition of the utility model pulse system;
Fig. 2: be the plan structure synoptic diagram of Fig. 1;
Fig. 3 A: be the structural representation of hollow out specimen holder in the utility model;
Fig. 3 B: be the side-looking structural representation of Fig. 3 A.
Embodiment
Understand for technical characterictic of the present utility model, purpose and effect being had more clearly, now contrast description of drawings embodiment of the present utility model.
As shown in Figure 1 and Figure 2, the utility model proposes the pouring-in metal organic chemical vapor deposition of a kind of pulse system 100, this metal organic chemical vapor deposition system 100 includes the vacuum reaction chamber 1 that sealing is communicated in vacuum pump 12, be provided with extraction valve 121 between vacuum pump 12 and the vacuum reaction chamber 1, be provided with vacuumometer 13 and thermo detector 14 in the vacuum reaction chamber 1, both detector ends of vacuumometer 13 and thermo detector 14 be integrated into a tip, be used for measuring temperature and pressure in the vacuum reaction chamber 1, vacuumometer 13 is connected with the control device (not shown) with thermo detector 14; Described vacuum reaction chamber 1 upper end is provided with opening, puts into end to constitute sample, and described vacuum reaction chamber 1 upper end open place is provided with first flange 11; This vacuum reaction chamber 1 is fixed on the housing 15 by first flange 11; This vacuum reaction chamber 1 is provided with the inlet mouth 17 with gas cylinder 4 conductings, and inlet mouth 17 is provided with intake valve 171; One gas feedthrough is arranged on vacuum reaction chamber 1 outside and by an inlet 16 and vacuum reaction chamber 1 conducting, inlet 16 is provided with throttling valve 161; Described gas feedthrough comprises the vaporizer 5 that is communicated in inlet 16, the entrance end of vaporizer 5 and 6 conductings of micro liquid feedthrough, and this micro liquid feedthrough 6 is communicated in gas cylinder 4; This micro liquid feedthrough 6 constitutes (that is: constituting an injector) by cylinder of steel and an electromagnetic injection valve that holds precursor solution, the entrance end of the spout of electromagnetic injection valve and vaporizer 5 seals and conducts, cylinder of steel is communicated in gas cylinder 4, and described electromagnetic injection valve is electrically connected with a control device (not shown); Put into a hollow sample table 2 by its upper end open in the described vacuum reaction chamber 1, these hollow sample table 2 bottom closed upper ends are provided with loam cake, are provided with light heater 3 in the hollow sample table 2; Hollow sample table 2 upper ends are provided with second flange 21, and this second flange 21 is located at first flange, 11 tops; The bonding surface of described first flange 11 and second flange 21 is provided with sealing-ring; These hollow sample table 2 blind end downsides are provided with substrate, and described substrate is long film (that is: thin film deposition is in substrate).
Described presoma is the solution of the composition configuration of the film that generates as required, is generally organic solution in the metal organic chemical vapor deposition reaction, and it generates aimed thin film through heating, hydrolysis reaction.
In the present embodiment, micro liquid feedthrough (that is: injector) injects presoma with the pulse injection mode in vaporizer 5; Controlled the parameter such as frequency, pulsewidth, number of times (reaction times), flow of its pulse by control device.To have volatile presoma earlier incorporates in the suitable organic solvent and is contained in the cylinder of steel, be injected in the vaporizer with pulse mode at the accurate infinitesimal of using the micro liquid feedthrough (injector) that links to each other with control device with solution, atomizing immediately, deliver to the high-temperature zone by carrier gas, in substrate chemical transformation deposition film forming takes place.
From the above mentioned, the pouring-in metal organic chemical vapor deposition of the utility model pulse system, can keep the stability of presoma before chemical reaction, can accurately control simultaneously reaction meticulously carries out, be injected in the vaporizer with pulse mode with the accurate infinitesimal of the micro liquid feedthrough that links to each other with control device with precursor solution, atomizing is delivered to the high-temperature zone by carrier gas immediately, in substrate chemical transformation deposition film forming takes place; This system architecture is simple, cost of manufacture is low, easy to operate.
Further, shown in Fig. 3 A, Fig. 3 B, in the present embodiment, described hollow sample table 2 blind end downsides fixedly have a hollow out specimen holder 7, and described substrate 8 is placed on hollow hole 71 places on the hollow out specimen holder 7; The inner edge of described hollow hole 71 is provided with 711 flanges, and the reliable self gravitation in the edge of described substrate 8 is set up on flange, and this design both can make presoma be deposited on the lower surface of substrate 8, made things convenient for placement and the taking-up of substrate 8 in hollow hole again.The size of described substrate 8 can be 5X5mm, 5X10mm, and is perhaps circular.
Described thermo detector 14 is fixed in vacuum reaction chamber 1 blind end (that is: bottom), and the probe height of thermo detector 14 is consistent with the height of substrate 8, to measure base reservoir temperature the most accurately.
In the present embodiment, the entrance end of described vaporizer 5 can arrange a plurality of micro liquid feedthroughs 6, can add different presomas respectively.
Described light heater 3 can provide chemical reaction temperature required to substrate 8 heating; Described light heater 3 is fixedly installed on and covers, and described light heater 3 is made of a plurality of bulbs, a plurality of circular holes is set, bulb of each circular hole internal fixing covering that is:.
Be covered with flexible baking heater (not shown) on described gas feedthrough 6 and the corresponding connecting tube thereof, to guarantee that presoma is fed in the vacuum reaction chamber with vaporific form, this flexibility baking heater can be made of the heating zone; In the present embodiment, the power of described light heater 3 is 8000-9000W, and maximum heating temperature is 800 ℃; Flexible baking heater total power is 1000W, and maximum heating temperature is 300 ℃.And the temperature regulation at each position and on-off control are to do to realize in the control panel drilling of control device.
As shown in Figure 2, in the present embodiment, described loam cake is fixedlyed connected with a Mechanical lifter 18, and this Mechanical lifter 18 by actuator drives, can be controlled 2 liftings of hollow sample table by motor, realizes opening a position and sealing of vacuum reaction chamber 1.
Further, as shown in Figure 1, in the present embodiment, the sidewall of described hollow sample table 2 is the sandwich structure that is made of double-deck drum, and this mezzanine space is provided with prosopyle and posticum, is connected with water pump between prosopyle and the posticum and constitutes water-cooling circulating system; This water-cooling circulating system can be used to reduce the temperature of sample table cavity except substrate, is mainly used to cool off filament.
As shown in Figure 1, also be horizontally arranged with a dividing plate 19 in the described vacuum reaction chamber 1, prevent that foreign material from falling at the bottom of the chamber.
When the preparation film, at first controlling Mechanical lifter 18 rises hollow sample table 2, with clean vacuum reaction chamber 1 and hollow out specimen holders 7 such as ethanol and acetone, handle the substrate 8 that needs use simultaneously, and substrate 8 put on the hollow out specimen holder 7, fall Mechanical lifter 18 (that is: substrate is put into vacuum reaction chamber 1), and will put air valve 171 into and be communicated with the gas cylinder 4 of carrier gas; The precursor solution that preparation is finished is put into injector and is sealed then; Start vacuum pump 12 and open extraction valve 121, by vacuum pump 12 gas in the vacuum reaction chamber 1 is extracted out, the registration of observing the air pressure display instrument simultaneously treats that vacuum reaction chamber 1 internal gas pressure is evacuated to 10
-1During handkerchief, can open intake valve 171 and put into carrier gas, treat that the air pressure registration is 10
5During handkerchief, close intake valve 171; Repeat this operation 3～5 times, finish and wash the chamber; Make vacuum reaction chamber 1 interior pressure be stabilized in the required numerical value of reaction at last; During growing film, injector by control device (or computer) control is injected into the form of precursor solution with pulse in the vaporizer 5 according to default parameter, through of short duration heating, the atomizing of presoma infinitesimal, delivered to the high-temperature zone of the hollow out specimen holder 7 in the vacuum reaction chamber 1 by carrier gas, chemical transformation takes place immediately, deposits film forming in substrate 8.Default pulse parameter is regulated by control device, reacts temperature required and also regulates and control by control device with each position temperature feedthrough.
The utility model compared with prior art has following advantage at least:
1. precursor solution infinitesimal (1-10mg) can evaporation fast in air pressure is about the vaporizer of 5Torr;
2. the mixture of presoma just has been heated the very short time, and it heats to realize chemical transformation fully not have when sufficient chien shih, so presoma can keep higher chemically stable state;
3. because the composition that the one-tenth of gas phase is grouped into the liquid phase precursor solution is consistent, so, be easy to control the composition of gas phase by changing the liquid phase composition;
4. by the air pressure of control reaction and the parameter of pulse, can control the characteristic of growth for Thin Film speed, growth repeatability and film at an easy rate;
5. change injector and can reach the purpose that changes the film composition easily, adopt multi-injector, can realize the growth in situ of multilayer film;
6. the setting pulse number of times can reach the purpose of control film thickness easily, and this point is very attractive for the growth of multilayer film.
The above only is the schematic embodiment of the utility model, is not in order to limit scope of the present utility model.Any those skilled in the art, the equivalent variations of having done under the prerequisite that does not break away from design of the present utility model and principle and modification all should belong to the scope that the utility model is protected.
Claims (10)
1. the pouring-in metal organic chemical vapor deposition of pulse system, this metal organic chemical vapor deposition system include the vacuum reaction chamber that sealing is communicated in vacuum pump, are provided with vacuumometer and thermo detector in the vacuum reaction chamber; It is characterized in that: described vacuum reaction chamber upper end is provided with opening, constitutes sample and puts into end, and this vacuum reaction chamber is provided with the inlet mouth with the gas cylinder conducting; One gas feedthrough is arranged on the vacuum reaction chamber outside and passes through an inlet and vacuum reaction chamber conducting; Described gas feedthrough comprises the vaporizer that is communicated in inlet, the entrance end of vaporizer and the conducting of micro liquid feedthrough, and this micro liquid feedthrough is communicated in gas cylinder; This micro liquid feedthrough is made of cylinder of steel and an electromagnetic injection valve that holds precursor solution, and the spout of electromagnetic injection valve and the entrance end of vaporizer seal and conduct, and cylinder of steel is communicated in gas cylinder, and described electromagnetic injection valve is electrically connected with a control device; Put into a hollow sample table by its upper end open in the described vacuum reaction chamber, this hollow sample table bottom closed upper end is provided with loam cake, is provided with light heater in the hollow sample table; Hollow sample table upper end is tightly connected with the vacuum reaction chamber upper end open; This hollow sample table blind end downside is provided with substrate.
2. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 1 system is characterized in that: the entrance end of described vaporizer and the conducting of a plurality of micro liquid feedthrough.
3. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 1 system, it is characterized in that: described light heater is fixedly installed on loam cake; Described light heater is made of a plurality of bulbs.
4. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 1 system, it is characterized in that: described loam cake is fixedlyed connected with a Mechanical lifter, and this Mechanical lifter passes through actuator drives by motor.
5. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 4 system, it is characterized in that: the sidewall of described hollow sample table is the sandwich structure that is made of double-deck drum, this mezzanine space is provided with prosopyle and posticum, is connected with water pump between prosopyle and the posticum and constitutes water-cooling circulating system.
6. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 1 system, it is characterized in that: described hollow sample table blind end downside fixedly has a hollow out specimen holder, and described substrate is placed on the hollow out place on the hollow out specimen holder; Described hollow hole is identical with shapes of substrates; The inner edge of described hollow hole is provided with flange, and the edge of described substrate is set up on flange.
7. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 1 system is characterized in that: be covered with flexible baking heater on described gas feedthrough and the corresponding connecting tube thereof; This flexibility baking heater is made of the heating zone.
8. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 7 system, it is characterized in that: described light heater power is 8000-9000W, maximum heating temperature is 800 ℃; Flexible baking heater total power is 1000W, and maximum heating temperature is 300 ℃.
9. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 1 system, it is characterized in that: described thermo detector is fixed in the vacuum reaction chamber blind end, and the probe height of thermo detector is consistent with substrate.
10. the pouring-in metal organic chemical vapor deposition of pulse as claimed in claim 1 system, it is characterized in that: described vacuum reaction chamber upper end open place is provided with first flange; This vacuum reaction chamber is fixed on the housing by first flange; Hollow sample table upper end is provided with second flange, and this second flange is located at the first flange top; The bonding surface of described first flange and second flange is provided with sealing-ring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320019409 CN203049089U (en) | 2013-01-15 | 2013-01-15 | Pulse injection type metal organic chemical vapor deposition system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320019409 CN203049089U (en) | 2013-01-15 | 2013-01-15 | Pulse injection type metal organic chemical vapor deposition system |
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| CN203049089U true CN203049089U (en) | 2013-07-10 |
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| CN 201320019409 Expired - Fee Related CN203049089U (en) | 2013-01-15 | 2013-01-15 | Pulse injection type metal organic chemical vapor deposition system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607125A (en) * | 2014-12-24 | 2015-05-13 | 宁波英飞迈材料科技有限公司 | Preparation equipment and preparation method of high-flux combined material |
| CN105734528A (en) * | 2016-03-09 | 2016-07-06 | 无锡盈芯半导体科技有限公司 | Growth method for layered molybdenum disulfide films on basis of pulse airflow method |
-
2013
- 2013-01-15 CN CN 201320019409 patent/CN203049089U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607125A (en) * | 2014-12-24 | 2015-05-13 | 宁波英飞迈材料科技有限公司 | Preparation equipment and preparation method of high-flux combined material |
| CN105734528A (en) * | 2016-03-09 | 2016-07-06 | 无锡盈芯半导体科技有限公司 | Growth method for layered molybdenum disulfide films on basis of pulse airflow method |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130710 Termination date: 20190115 |
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| CF01 | Termination of patent right due to non-payment of annual fee |