CN105862013B - A kind of high-temperature heating equipment applied to small-sized MOCVD systems - Google Patents

A kind of high-temperature heating equipment applied to small-sized MOCVD systems Download PDF

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Publication number
CN105862013B
CN105862013B CN201610439793.6A CN201610439793A CN105862013B CN 105862013 B CN105862013 B CN 105862013B CN 201610439793 A CN201610439793 A CN 201610439793A CN 105862013 B CN105862013 B CN 105862013B
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electric furnace
heating element
stainless steel
thermal insulation
insulation board
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CN105862013A (en
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朱顺明
刘松民
顾书林
叶建东
汤琨
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Nanjing University
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Nanjing University
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/48Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Resistance Heating (AREA)

Abstract

A kind of high-temperature heating equipment applied to small-sized MOCVD systems including heating element, electric furnace pan and electrode connecting line, is equipped with cover board, electric furnace tray bottom reserves several holes, and the electrode connecting line for connecting heating element has ceramic tube to be protected above heating element;It is closed outside heating unit by stainless steel outer cover; there is thermal insulation board below electric furnace pan; several and corresponding hole of electric furnace tray bottom is reserved on thermal insulation board; the side of outer cover is equipped with the stainless steel tube that can lead to protective gas above thermal insulation board; stainless steel tube pipe is passed through heating element top for the protection gas such as nitrogen, and duplicate protection is carried out to heating element;The high-temperature heating of small-sized MOCVD systems can be achieved in the present invention, and oxygen etc. can effectively be prevented under high-temperature condition to be aoxidized caused by heating element and corrosion impact, greatly improve heating element service life, the various releases of heating element under limitation hot conditions can also be shielded, are conducive to obtain the deposited thin film material haveing excellent performance.

Description

A kind of high-temperature heating equipment applied to small-sized MOCVD systems
Technical field
The present invention relates to film deposition techniques, particularly a kind of high-temperature heating equipment applied to small-sized MOCVD systems.
Background technology
Infrared radiation heating is the heating element higher to resistance by high current, it is made to generate very big heat, into And mainly conducted heat in a manner of radiation to graphite or metal base, it is one in commercial scale and scientific experiment research The very important heating means of kind, but the size of heating equipment, structure and use environment etc. differ its practical heating effect It is very big.
For tube furnace, furnace body has been generally designed certain thickness insulating layer and reflecting layer, and boiler tube is by heater strip It is wrapped up, the heat that heater strip generates can be made to concentrate on inside boiler tube, technological temperature inside boiler tube relatively heater strip Temperature, the temperature difference are usually no more than 200 DEG C, therefore are easier to realize 1100 DEG C or so even higher technological temperatures.
Different films are very big to the requirement difference of depositing operation and equipment, for MOCVD systems, generally require cavity The Cooling Design of wall surface, due to the needs of vacuum degree, the Spatial General 6 R of cavity is all than relatively limited, so the size of heating equipment It can be restricted, along with mechanical requirements such as substrate rotations, deposited samples are generally placed on above heating equipment, and and are added Hot equipment has a certain distance, and more than many factors cause the temperature difference of the technological temperature and heating element in MOCVD systems Very big, multiple theoretical calculations and measured data show that 1100 DEG C of the corresponding temp of heating element of technological temperature may reach 1700~2000 DEG C.For part semiconductor material, excellent quality of materials in order to obtain, be required in many cases by Silicon is accompanied by the oxidizing gas such as oxygen or chlorine, carbon dioxide to 1100 degree or so, at such high temperatures Work, heating element is easily aoxidized or is corroded by gas, so as to seriously affect the service life of heating equipment and stability;In addition, Under such hot conditions, heating element has been in red-hot state in itself, can discharge impurity or other unknown objects, these are to material Growth will bring adverse effect.
Invention content
The present invention seeks to propose a kind of high-temperature heating equipment applied to small-sized MOCVD systems, for the prior art Problem, provide it is a kind of be easily achieved the heating unit compared with high technology temperature, both can prevent heating element from being aoxidized, substantially extend The service life of electric furnace, and the various releases of limitation heating element in the case of a high temperature can be shielded, the environment of depositing system is purified, is made The performance of deposition materials is guaranteed.
The technical scheme is that a kind of high-temperature heating equipment applied to small-sized MOCVD systems, including heating element, Electric furnace pan and electrode connecting line, cover board is equipped with above heating element, and electric furnace tray bottom reserves several holes, connects heating element Electrode connecting line has ceramic tube to be protected;It is closed outside heating unit by stainless steel outer cover, has thermal insulation board below electric furnace pan, Several and corresponding hole of electric furnace tray bottom is reserved on thermal insulation board, the side of thermal insulation board top outer cover, which is equipped with, can lead to protective gas Stainless steel tube, stainless steel tube pipe for nitrogen etc. protection gas be passed through heating element top, to heating element carry out duplicate protection; Thermal insulation board is placed on the supporter in stainless steel outer cover, and electric furnace disk material is exhausted for aluminium oxide ceramics or silicon carbide or other high temperature resistants Edge fire proofing material;Electric furnace pan is designed with several grooves, and heating element is placed among groove, and depth of groove is slightly larger than heating element Height.
Heating element is resistive heater or heating resistor film, and material is tungsten, molybdenum or metal alloy etc..
Electric furnace tray bottom is fixed on by several they sup-ports, the other end of supporting rod on the pedestal of heating unit lower part.
Electric furnace disk shape is circle, size 6-12cm, according to the needs that substrate rotates, electric furnace disk center there are hole, Hole diameter 0.5-2.5cm.
Electric furnace tray bottom can reserve several holes, so that electrode connecting line or thermocouple assembly pass through.
Electric furnace pan outermost inner wall reserves the bayonet for placing quartz cover plate, and quartz cover plate is fixed when ensureing to use.
Cover plate materials are quartz or stainless steel above heating element, and according to the needs that substrate rotates, cover plate central can be there are Hole, hole diameter 0.5-1.5cm;To rotate by heating platform, that is, sample grown platform above cover board, reaction gas can be by spraying Head or the admission line of other forms are passed on example platform.
The stainless steel tube quantity of stainless steel outer cover side is 1-6 above thermal insulation board, pipe diameter size 0.3-1.5cm.
Thermal insulation board material below electric furnace pan is positioned over the branch in stainless steel outer cover for quartz or stainless steel, thermal insulation board On support body, the spacing of thermal insulation board and electric furnace pan is 0-1cm, several holes is reserved on thermal insulation board, for electrode connecting line or thermoelectricity Even device passes through, and according to the needs that substrate rotates, thermal insulation board center can there are holes.
Compared with prior art, the high-temperature heating of small-sized MOCVD systems can be achieved in beneficial effects of the present invention, the present invention, And oxygen etc. can effectively be prevented under high-temperature condition to be aoxidized caused by heating element and corrosion impact, greatly improve heating element Service life can also shield the various releases of heating element under limitation hot conditions, be conducive to obtain the deposition haveing excellent performance Thin-film material.Especially:
1st, the relatively high technology temperature of small-sized MOCVD systems can be achieved, prevent resistance wire under the high temperature conditions by reaction gas It aoxidizes or corrodes, substantially extend the service life of electric furnace;
2nd, the various releases of limiting resistance silk in the case of a high temperature can be shielded, purify the environment of depositing system;
3rd, processing technology difficulty is small, of low cost, highly practical, and good compatibility is easy to spread.
Description of the drawings
Fig. 1, semi-enclosed heating unit cross-sectional view of the present invention;
The MOCVD system cross-sectional views of heating unit described in Fig. 2, application drawing 1;
Fig. 3, totally enclosed type heating unit cross-sectional view.
Specific embodiment
The present invention is described in detail in the following with reference to the drawings and specific embodiments:
In the present invention, electric furnace disk material is aluminium oxide ceramics or silicon carbide or other resistance to height such as 99 porcelain, 95 porcelain, 90 porcelain Temperature insulation fire proofing material realizes that the relevant raw materials selection space of this heating unit is big, cheap.
In the present invention, electric furnace pan is designed with several grooves, and resistance wire is placed among groove, and depth of groove is slightly larger than electricity The height of silk is hindered, resistance wire can be avoided the situation of short circuit occur.
In the present invention, electric furnace tray bottom reserves several holes, is rotated for contact conductor or thermocouple assembly or substrate Support shaft passes through, and realizes the multifunctionality of depositing system.
In the present invention, heating has quartz or stainless steel cover board above, can prevent the oxidizing gas such as oxygen and resistance wire Contact, cover plate central also are available for substrate rotation support shaft there are hole and pass through.
In the present invention, it is closed outside Heating body by stainless steel outer cover, stainless steel outer cover is placed in below electric furnace pan Thermal insulation board on supporter can play shielding insulation effect, and there is stainless steel tube in outer cover side above this end baffle plate, for nitrogen It is passed through Deng protection gas, the small space that thermal insulation board and outer cover are formed is made to keep the positive pressure to chamber, avoids resistance wire and reaction gas The contact of body carries out duplicate protection to heating element.
In the present invention, limiting resistance silk can also effectively be shielded in height by heating the outer cover of cover board and Heating body above Various releases in the case of temperature purify the environment of depositing system.
Embodiment 1
As shown in Figure 1, a kind of high-temperature heating equipment applied to small-sized MOCVD systems of the present invention, including heating Main body has resistive heater 11, electrode connecting line 12 and electric furnace pan 13, in the present embodiment, resistance wire material in Heating body For tungsten filament, electric furnace pan is 95 porcelain, and shape is round, a diameter of 10cm, by the supporting rod 20 being fixed on the pedestal of inside cavity It is supported.There are hole 14 (while putting on diameter R), hole diameter 1.2cm among electric furnace pan to pass through, electrode for rotation axis Connecting line top first passes through the stainless steel sleeve pipe of long 2cm, diameter 0.4cm, and welds together, and has pottery outside stainless steel sleeve pipe Porcelain tube 15 is protected, and to prevent short circuit, lower part and a metal screws weld together, and screw diameter and stainless steel sleeve pipe are through phase When, and pass through that nut and binding post 16 are closely linked, ensure the good contact of electrode.Have on resistance wire outer diameter for 9.8cm, The quartz cover plate 17 of internal diameter 1.2cm, thickness 2mm in processing and fabricating electric furnace pan, are reserved and the comparable card of quartz cover plate size Mouthful, quartz cover plate can be positioned in bayonet by when use, ensure that quartz cover plate is fixed, while ensures the center of quartz cover plate Hole and resistance wire pallet hole aligning.It is closed outside Heating body by stainless steel outer cover 18, it is stainless right over electric furnace Steel deck-plate is annular, and internal diameter 9cm, more smaller than quartz cover plate outer diameter, quartz cover plate can be completely covered in guarantee stainless steel upper cover plate, Its outside and it is peripheral it is stainless steel welded together with.On the inside of stainless steel outer cover, supporter 19 is welded with, is placed on supporter Thermal insulation board 10, thermal insulation board and electric furnace pan spacing 0.5cm, the side of outer cover is welded with stainless steel tube 21 above thermal insulation board, for nitrogen The protection gas such as gas is passed through, and duplicate protection is carried out to resistance wire.It invents according to this embodiment, the highest underlayer temperature that we realize can Up to 1100 DEG C, resistance wire service life was up to 200 hours at this temperature, without cover board, thermal insulation board and stainless steel outer cover About 900 DEG C of the achievable maximum temperature of heating unit, service life at the maximum temperature only 30 hours.
41 be sample grown platform in Fig. 2, and 42 be sample, and 43 be inlet spray head, and 44 be rotary shaft
Embodiment 2
As shown in figure 3, a kind of high-temperature heating equipment of small-sized MOCVD systems of the present invention, including heater body, adds There are resistive heater 31, electrode connecting line 32, electric furnace pan 33 in hot ontology, by the supporting rod being fixed on the pedestal of inside cavity 30 are supported.In the present embodiment, resistance wire material is tungsten filament, and electric furnace pan is 95 porcelain, and shape is round, a diameter of 8cm.Electrode Lead top first passes through the stainless steel sleeve pipe of long 3cm, diameter 0.4cm, and welds together, and has ceramics outside stainless steel sleeve pipe Pipe 34 is protected, and to prevent short circuit, lower part and a metal screws weld together, and screw diameter and stainless steel sleeve pipe warp are suitable, And pass through that nut and binding post 35 are closely linked, ensure the good contact of electrode.By 36 institute of stainless steel outer cover outside Heating body Closing is completely covered and (can not be boxed out, for fixed sample stage structure) by stainless steel cover board 37 right over electric furnace, outside cover board Edge with periphery it is stainless steel welded together with.On the inside of stainless steel outer cover, be welded with supporter 38, on supporter place every Hot plate 39, thermal insulation board and electric furnace pan spacing 0.3cm, the side of outer cover is welded with stainless steel tube 40 above thermal insulation board, for nitrogen It is passed through Deng protection gas, duplicate protection is carried out to resistance wire.It invents according to this embodiment, the underlayer temperature that we realize is up to 1000 DEG C, resistance wire service life was up to 300 hours at this temperature.
For those skilled in the art, can technical solution according to the present invention and design, make various phases The change and deformation answered, and all these change and deform the protection domain for belonging to the claims in the present invention.

Claims (5)

1. a kind of high-temperature heating equipment applied to small-sized MOCVD systems, including heating element, electric furnace pan and electrode connecting line, Cover board is equipped with above heating element, electric furnace tray bottom reserves several holes, and the electrode connecting line for connecting heating element has ceramic tube It is protected;Closed outside heating unit by stainless steel outer cover, there is thermal insulation board below electric furnace pan, reserved on thermal insulation board it is several and The corresponding hole of electric furnace tray bottom, the side of thermal insulation board top outer cover are equipped with the stainless steel tube that can lead to protective gas, stainless steel Pipe is passed through heating element top for nitrogen protection gas, and duplicate protection is carried out to heating element;Thermal insulation board is placed in stainless steel outer cover Supporter on, electric furnace disk material be aluminium oxide ceramics, silicon carbide or other high-temperature insulation fire proofing materials;Electric furnace pan is designed with Several grooves, heating element are placed among groove, and depth of groove is slightly larger than the height of heating element;
Electric furnace disk shape is circle, and size 6-12cm, according to the needs that substrate rotates, there are hole, holes for electric furnace disk center Diameter 0.5-2.5cm;Electric furnace pan outermost inner wall reserves the bayonet for placing quartz cover plate, and quartz cover plate is fixed not when ensureing to use It is dynamic;Cover plate materials are quartz or stainless steel above heating element, and according to the needs that substrate rotates, there are hole, holes for cover plate central Hole dia 0.5-1.5cm;To rotate by heating platform, that is, sample grown platform above cover board, reaction gas is by spray head admission line It is passed on example platform;
The stainless steel tube quantity of stainless steel outer cover side is 1-6 above thermal insulation board, pipe diameter size 0.3-1.5cm.
2. high-temperature heating equipment according to claim 1, it is characterized in that heating element is resistive heater or adding thermal resistance Piece, material are tungsten, molybdenum or metal alloy.
3. high-temperature heating equipment according to claim 1, it is characterized in that electric furnace tray bottom is by several they sup-ports, support The other end of bar is fixed on the pedestal of heating unit lower part.
4. high-temperature heating equipment according to claim 1, it is characterized in that electric furnace tray bottom reserves several holes, with power pole Connecting line or thermocouple assembly pass through.
5. high-temperature heating equipment according to claim 1, it is characterized in that the thermal insulation board material below electric furnace pan is stone English or stainless steel, thermal insulation board are positioned on the supporter in stainless steel outer cover, and the spacing of thermal insulation board and electric furnace pan is 0-1cm, every Several holes are reserved on hot plate, so that electrode connecting line or thermocouple assembly pass through, according to the needs that substrate rotates, in thermal insulation board There are holes for the heart.
CN201610439793.6A 2016-06-17 2016-06-17 A kind of high-temperature heating equipment applied to small-sized MOCVD systems Active CN105862013B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113637944B (en) * 2021-10-14 2022-01-07 中国科学院沈阳科学仪器股份有限公司 Button type high temperature heating ware

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05195220A (en) * 1992-01-23 1993-08-03 Anelva Corp Substrate heating mechanism
CN101063195A (en) * 2006-04-25 2007-10-31 马塞尔-布加蒂股份有限公司 Process furnance or the like
CN101191202A (en) * 2006-12-01 2008-06-04 甘志银 Heating system for metal organic substance chemical gaseous phase deposition device reaction cavity
CN201670873U (en) * 2010-04-30 2010-12-15 苏州索乐机电设备有限公司 Substrate heating furnace for MOCVD
CN104046965A (en) * 2014-05-27 2014-09-17 中国电子科技集团公司第四十八研究所 Radiant heating element, radiant heater and MOCVD reactor
CN105420693A (en) * 2015-11-30 2016-03-23 中国电子科技集团公司第四十八研究所 Heating device for MOCVD reactor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05195220A (en) * 1992-01-23 1993-08-03 Anelva Corp Substrate heating mechanism
CN101063195A (en) * 2006-04-25 2007-10-31 马塞尔-布加蒂股份有限公司 Process furnance or the like
CN101191202A (en) * 2006-12-01 2008-06-04 甘志银 Heating system for metal organic substance chemical gaseous phase deposition device reaction cavity
CN201670873U (en) * 2010-04-30 2010-12-15 苏州索乐机电设备有限公司 Substrate heating furnace for MOCVD
CN104046965A (en) * 2014-05-27 2014-09-17 中国电子科技集团公司第四十八研究所 Radiant heating element, radiant heater and MOCVD reactor
CN105420693A (en) * 2015-11-30 2016-03-23 中国电子科技集团公司第四十八研究所 Heating device for MOCVD reactor

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