CN206607315U - Multifunctional inductor coupled plasma strengthens chemical gas-phase deposition system - Google Patents
Multifunctional inductor coupled plasma strengthens chemical gas-phase deposition system Download PDFInfo
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- CN206607315U CN206607315U CN201720416429.8U CN201720416429U CN206607315U CN 206607315 U CN206607315 U CN 206607315U CN 201720416429 U CN201720416429 U CN 201720416429U CN 206607315 U CN206607315 U CN 206607315U
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Abstract
The utility model, which is related to a kind of Multifunctional inductor coupled plasma that can be used for growth two-dimensional material, strengthens chemical gas-phase deposition system.The film grower of prior art is not suitable for low-temperature epitaxy growth two-dimensional material, and complicated, and function is single, operation and maintenance inconvenience, expensive.System of the present utility model forms growth chamber using quartzy body, and by by plasma generating equipment in the upstream of growth chamber, and it is spaced a distance with deposition substrate, the intensity and density of plasma can effectively be controlled, the controllability of enhanced deposition process, realizes the high-quality two-dimensional material film of growth.Moreover, by using plasma device, two-dimensional material can not only be grown, but also two-dimensional material can be modified or etched, and body is cleaned using plasma, realize a variety of functions, and operation and maintenance is quite convenient to.It is prepared by depositing system cost savings of the present utility model, the two-dimensional material that factory and laboratory can be widely used in.
Description
Technical field
The utility model relates generally to field of material preparation, more specifically it relates to a kind of Multifunctional inductor coupling etc. from
Daughter strengthen chemical gas-phase deposition system, its can be used in such as growth of the two-dimensional material of graphene, molybdenum disulfide or the like,
Modification and etching.The system has relatively low cost, and operation and maintenance is all very convenient.
Background technology
In recent years, two-dimensional material increasingly attracts the interest of researcher due to its unique property.Two-dimensional material is
Refer to electronics only can in two non-nanos level dimensions (>100nm) material of free movement (plane motion), such as graphene, MoS2
Deng.Many new physical phenomenons are presented in two-dimensional material, thus new material, device etc. can be developed again.With two-dimentional material
Expect also to turn into study hotspot therewith for the hetero-junctions of base unit.
Traditionally, for grow the equipment of high-quality thin film material generally include molecular beam epitaxy deposition equipment (MBE) and
Chemical vapor depsotition equipment (CVD).Therefore, it is also preferred to consider to use these existing equipments when preparing two-dimensional material.However,
These equipment are typically dependent on ultrahigh vacuum growing environment, and equipment is huge and complexity, and cost is also very expensive, and film forming speed
Slowly, the maintenance of growth chamber is time-consuming and complicated.Therefore, the manufacturing cost of two-dimensional material is caused to remain high.
On the other hand, when being used to manufacture two-dimensional material by these conventional equipments, it can not play sometimes as deposition is conventional
Effect good like that during thin-film material.By taking chemical vapor depsotition equipment as an example, entitled " plasma activated chemical vapour deposition is filled
Put " Chinese invention patent application 201410503445.1 in disclose a kind of apparatus for plasma chemical vapor deposition, its wrap
Include the growth chamber for accommodating substrate and the inductively coupled plasma generating means being arranged on above substrate.By forming source gas
Plasma, promotes reaction using the activity of plasma, so as to deposit desired film on substrate.However,
When such plasma CVD device is used to deposit two-dimensional material, because energy of plasma is too high, growth
Excessive velocities, the more difficult control of growth parameter(s), therefore can not obtain with sufficiently large continuous surface product and high-quality enough
Two-dimensional material.
Another further aspect, traditional MBE and CVD equipment function is more single, is normally only used for deposited thin film material.And it is two-dimentional
The preparation of material and conventional pellicle materials are different, for example, very thin two-dimensional material is due to there was only monatomic structure, therefore pole
It is vulnerable to extraneous absorption or the destruction of active atomic, thus it is gentle to growth conditions requirement;And due to the ratio table of two-dimensional material
Area is very high, in order to be able to obtain good surface texture and marginal texture, it may be necessary to two dimension in deposition or after deposition
The surface of material is modified, or needs to carry out a certain degree of etching to two-dimensional material.Conventional MBE and CVD equipment are simultaneously
These functions can not be completed well.
Therefore, it is still necessary to a kind of equipment for depositing two-dimensional material, it can be used in preparing the two of high-quality large area
Material is tieed up, while operation and maintenance is convenient, there is the cost reduced relative to conventional MBE and CVD equipment.
Utility model content
Therefore, one side of the present utility model, which is that offer is a kind of, effectively can controllably grow setting for two-dimensional material
Standby, its is simple in construction, and operation and maintenance is convenient.Preferably, the equipment can also realize a variety of functions, such as to two-dimensional material
Modification and etching etc..
According to an exemplary embodiment, a kind of Multifunctional inductor coupled plasma enhancing chemical gas-phase deposition system can be wrapped
Include:Body for accommodating deposition substrate, the upstream end of the body is provided with least one gas access, and downstream is provided with
Vacuumize interface;Constant temperature oven, around the part for accommodating the deposition substrate of the body;And inductively coupled plasma
Generating means, around the part positioned at the constant temperature oven upstream of the body, so that in the direction of the axis along the body
It is upper to be spaced a distance with the deposition substrate.
In some instances, the distance can 10cm to 1.5m scope, the preferred scope in 20cm to 1.2m, more
Preferably in 30cm to 1m scope.
In some instances, the inductively coupled plasma generating means has 10 to 300 watts of operating power peace treaty
13.56MHz working frequency.
In some instances, the upstream end of the body has upstream flange, and it is sealingly engaged with close with upstream closure disk
The body is sealed, the gas access is formed on upstream closure disk.The downstream of the body has downstream flange, its
It is sealingly engaged with downstream closure disk to seal the body, it is described to vacuumize interface formation on downstream closure disk.
In some instances, the downstream closure disk also has the specimen holder interface being formed thereon to install sample
Support rod, the end extended in the body of the sample support rod is provided with the sample for supporting the deposition substrate
Sample platform, sample stage level height is in cavity cross-section center.
In some instances, the inductive coupling plasma generator includes:Around the coil of the body;And
Coil brace for fixing each coil turn in the coil.
In some instances, the constant temperature oven includes having on upper and lower part, the apparent surface of the upper and lower part
Depression is to accommodate the body, and the upper and lower part is connected through the hinge so as to which top energy around hinge axle is rotated to surround
Or the exposure body, refractory fibre and air cooling equipment are provided with constant temperature oven.
In some instances, the constant temperature oven includes one or more warm areas, and each warm area, which has, is arranged on the depression
In heating element heater and the temperature control equipment associated with the heating element heater.
In some instances, the body is quartzy body.
System of the present utility model can be used for the growth and etching of two-dimensional material, can be in the weaker environment of plasma energy
The chemical reaction of middle control two-dimensional material, so that the control of the growth and etching beneficial to two-dimensional material;And simple in construction, cost
Low, operation and maintenance is convenient, therefore with very high application value.
Brief description of the drawings
Fig. 1 shows the Multifunctional inductor coupled plasma enhancing chemical vapor deposition system of the embodiment of the utility model one
The structural representation of system.
Fig. 2 shows the schematic cross sectional views of the coil brace of an embodiment of the present utility model.
Fig. 3 shows the example being tightly connected between the closure disk of an embodiment of the present utility model and trip flange.
Fig. 4 shows the schematic diagram of closure disk, shows sample support rod mounted thereto and is supported by the sample
The sample stage of bar supporting.
Embodiment
Exemplary embodiment of the present utility model described below with reference to accompanying drawings.
Fig. 1 is shown strengthens chemical vapor deposition according to the Multifunctional inductor coupled plasma of the embodiment of the utility model one
The overall structure diagram of product system.As shown in figure 1, the system includes body 10, for example can be the quartz ampoule of drum,
It will be illustrated below as example, however, it is understood that body 10 can also be other high temperature resistants and have high leakproofness material
Body, and can have other shapes, such as square barrel shape, generally rectangular barrel shape, oval barrel shape.Quartz ampoule 10 has
There are upstream open and downstream opening, wherein, it is provided with upstream open at upstream flange 12, downstream opening and is provided with downstream flange 14,
Such as upstream flange 12 and downstream flange 14 can equally be made up of quartz material and be welded to quartz ampoule 10.Upstream flange 12
Can be in sealing contact with upstream closure disk 25, downstream flange 14 can be in sealing contact with downstream closure disk 15, specifically will be below
Reference picture 3 is described in detail, so as to the space in sealed silica envelope 10.Upstream blocks disk 25 and downstream closure disk 15 can be with
It is made up of such as stainless steel, one or more gas accesses 13 can be provided with its middle and upper reaches closure disk 25, for stone
Be passed through in English pipe 10 it is various such as source gas, carrier gas, reacting gas, etching gas or their mixed gas needed for gas.
Specimen holder 16 can be removably installed on downstream closure disk 15, its end being deep into quartz ampoule 10 can be provided with sample
Sample platform 17 is with the substrate of supporting such as such as wafer etc.Other interfaces are also provided with downstream closure disk 15, for example, are taken out
Gas interface 18 to quartz ampoule 10 for vacuumizing, and measurement interface 19 is for installing each of such as vacuum gauge etc
Plant measurement device.As shown in figure 1, downstream closure disk 15 can be supported in mounting bracket, in order to which downstream blocks disk 15
Install with dismantling, such as placing and taking out the growth substrates on sample stage 17.Quartz ampoule 10 can be supported on body branch
On frame 11, pipe body support 11 can be respectively arranged near the upstream and downstream two ends of quartz ampoule 10 it is one or more, for supporting stone
The whole machine balancing of English pipe 10.Pipe body support 11 can be telescopic, for adjusting the upper-lower height of quartz ampoule 10.It can manage
Solution, is also provided with damping device such as rubber blanket between the bottom of pipe body support 11 and operating desk table top.
Quartz ampoule 10 is provided with inductively coupled plasma generating means 20 at upstream open, and it includes surrounding quartz ampoule 10
Coil 21, and the coil brace 23 (as shown in Figure 2) for fixed coil 21, and being supported by support 22.Though
So it is not shown, inductive coupling plasma generator 20 may be also connected to corresponding high frequency electric source and control device, with
In control such as plasma power.When high frequency electric flowing through coil 21, electromagnetic field of high frequency can be produced, is made in quartz ampoule 10
Gas ionization, forms plasma.When the gas being imported into from gas access 13 in quartz ampoule 10 is such as growth gasses, its
Plasma can be used for depositing two-dimensional material on substrate;When the gas of importing is hydrogen or argon gas, its plasma can be used for
The two-dimensional material deposited is modified or etched, and can be also used for cleaning the inwall of quartz ampoule after etching has been completed
The material of upper deposition, therefore the operation and maintenance of device of the present utility model is quite convenient to.
It should be noted that in the utility model, inductively coupled plasma generating means 20 is located at the upstream end of quartz ampoule 10, from
Being located substantially at the sample stage 17 at the middle part of quartz ampoule 10 has a certain distance, and with plasma producing apparatus in the prior art and sample
Sample platform is located at different at the same position of growth chamber.So, the plasma that ionization is obtained needs to make by a segment distance
Use in the growth substrates on sample stage 17, be avoided that stronger plasma directly acts on substrate and Grown
Part film so that growth course can be carried out with gentler process so that the two-dimensional material film grown has more preferable
Characteristic, such as bigger continuous size and more flat surface.In the present embodiment, by the way that inductively coupled plasma is occurred
Device 20 is located at the upstream of quartz ampoule 10 so that the plasma generated can be naturally flow to air-flow positioned at relative
Sample stage 17 at downstream, so as to complete deposition or modification or etching process.Moreover, for example during cleaning, upstream
Such as Ar plasmas of generation can clean the inwall of whole quartz ampoule 10 with flow further downstream, so as to realize thoroughly
Cleaning.Therefore, equipment of the present utility model can not can realize abundant function to meet the growth needs of two-dimensional material, Er Qiecao
Make and safeguard all very simple and convenient.
The inventors discovered that, the distance between inductively coupled plasma generating means 20 and sample stage 17 can influence two-dimentional material
The growth course of material.In certain embodiments, on the axis direction of quartz ampoule 10, inductively coupled plasma generating means 20 with
The distance between sample stage 17 is in 10cm to 1.5m scope, the preferably scope in 20cm to 1.2m, more preferably in 30cm
To 1m scope.The power of inductively coupled plasma generating means 20 can be in such as 100 to 400 watts of scope.Preferably, example
Such as in deposited graphite alkene two-dimensional material, the power of inductively coupled plasma generating means 20 can in 10 to 300 watts of scope,
Its working frequency can be such as 13.56MHz, the inventors discovered that can prepare high-quality two-dimensional graphene under this condition
Material.
The present inventors have additionally discovered that, inductively coupled plasma generating means 20 can be generated substantial amounts of when producing plasma
Heat, and coil 21 can be deformed upon when heated, for example, cause the relative displacement between coil turn, so as to change the category of coil 21
Property, and then influence the generation of plasma and the deposition process of two-dimensional material.In the embodiment of the utility model one, coil 21 is also
It can be fixed by coil brace 23, to prevent the coil turn relative displacement produced because heated, so as to realize uniform plasma
Body and the two-dimensional material film well deposited.Fig. 2 is the schematic sectional of the coil brace 23 of an embodiment of the present utility model
Figure.As shown in Fig. 2 coil brace 23, which can have, has equidistant circular opening between two parts relative to each other, two parts, often
Individual hole can be accommodated and each circle in fixed coil 21, so that each coil turn in whole coil 21 can be consolidated
It is fixed.It can be fixed by screw together between two parts, and coil brace 23 can be further secured to inductance by screw
On the housing of coupling plasma generating means 20.Coil brace 23 can be made up of insulation heat proof material, for example can be by bakelite system
Into.
With continued reference to Fig. 1, chemical vapor deposition system is strengthened according to Multifunctional inductor coupled plasma of the present utility model
System also includes constant temperature oven 30, and it can be around the sample area in quartz ampoule 10 and heated quarty tube 10.As shown in figure 1, permanent
Warm stove 30 may include to be provided with heat-insulating heat-preserving material in constant temperature furnace shell 31 and constant temperature furnace base 32, constant temperature furnace shell 31, its example
It is such as micro- for senior fire resisting.Although it is not shown, constant temperature furnace shell 31 and insulation material can be divided into above and below two parts, and
Connected up and down between two parts by hinge (such as loose-leaf) so as to which upper part can the rotation of around hinge axle.It is two-part relative up and down
Surface on can have semicircular depression so that when upper part is buckled on lower part, formation circular channel is to accommodate quartz
Pipe 10.Heating element heater, such as resistance wire can be provided with the inwall of semi-cylindrical canyon, with heated quarty tube 10.Although not showing
Go out, but air cooling equipment is also provided with constant temperature oven, in order to be cooled down.Constant temperature furnace base 32 is arranged on constant temperature oven 30
Bottom, in the present embodiment, constant temperature furnace base 32 and constant temperature oven 30 are set to one, and it can be placed on operating desk table top, use
The quartz ampoule 10 in constant temperature oven 30 is arranged in support constant temperature oven 30 and a part.In certain embodiments, constant temperature furnace base
32 can be set to adjustable base, for the height of regulating thermostatic stove 30, on the one hand be easy to operating personnel to be grasped in suitable height
Make, be on the other hand easy to keep on the same axis with inductive coupling plasma generator.Although constant temperature oven 30 in Fig. 1
A warm area is only included, but in further embodiments, constant temperature oven 30 can be also arranged on provided with many sub- warm areas, heating element heater
In many sub- warm areas of constant temperature oven 30, every sub- warm area can have a single heating element heater, such as resistance wire, and can be independent
Temperature control equipment control, such as with single thermocouple, so as to realize different temperature.The constant temperature oven of the structure is resistance to
Fiery good heat preservation performance, and without obvious heat radiation around stove, security performance is high.
Fig. 3 shows the example being tightly connected between downstream closure disk 15 and downstream flange 14.It should be understood that Fig. 3's is close
The sealing that seal structure may be equally applied between upstream flange 12 and upstream closure disk 25.As shown in figure 3, downstream closure disk 15
Recess R is could be formed with the surface of downstream flange 14, O-ring (being shown as in Fig. 3 " O ") can be entrapped in the recess R, O
Vacuum grease can be scribbled between type circle and downstream flange 14.When being evacuated in quartz ampoule 10, external atmosphere pressure can seal downstream
It is stifled to be compressed between disk 15 and downstream flange 14, so as to play sealed effect.In further embodiments, can also be using such as
Downstream closure disk 15 is fastened on downstream flange 14 by the fastener of fixture etc.
Fig. 4 is the schematic diagram that disk 15 is blocked according to the downstream of the embodiment of the utility model one, is shown mounted thereto
Sample support rod 16 and the sample stage 17 supported by the sample support rod 16, sample stage 17 include shank and are connected to shank
The wafer for depositing two-dimensional material can be placed on round plate, round plate.As shown in figure 4, solderable on downstream closure disk 15
Vacuumize interface 18, measurement interface 19 and specimen holder interface 41.It can for example mark to vacuumize interface 18 and measurement interface 19
Quasi- KF interfaces, such as KF interfaces, can be attached or be sealed by standard clip, joint, blind plate etc..Vacuumizing interface 18 can
To be connected to vaccum-pumping equipment, such as vavuum pump for example, by bellows, butterfly valve can also be connected, for controlling and adjusting stone
Air pressure in English pipe 10.Measurement interface 19 can connect various measuring apparatus, such as measuring vacuum in quartz ampoule 10
Vacuum gauge etc..Specimen holder interface 41 can be clamping interface, and sample support rod 16 can be clamped installed in specimen holder interface 41
In and extend in quartz ampoule 10.Sample support rod 16 can be quartz ampoule or quartz rod, and it is deep into quartz ampoule 10
One end can have frosted male plug head 40, and it, which may be inserted into, is connected in the shank of sample stage 17.
Sample support rod 16 is installed on downstream closure disk 15 although in the above embodiments, describing, should
Understand, it can also be installed on upstream closure disk 25, or in certain embodiments, support rod 16 can be omitted, and be substituted
Ground, sample stage 17 can be arranged on a support, and the support can be placed to quartz ampoule 10 neutralizes and taken from quartz ampoule 10
Go out.
Some embodiments of the present utility model are described above.It should be understood that the utility model is not limited to these embodiments,
But various modifications, change can be carried out and substituted.For example, interface described above can be using various suitable in the prior art
Interface, as long as meet sealing or ventilation requirement.Scope of the present utility model is by appended claims and its equivalent
Definition.
Claims (11)
1. a kind of Multifunctional inductor coupled plasma strengthens chemical gas-phase deposition system, it is characterised in that the system includes:
Body for accommodating deposition substrate, the upstream end of the body is provided with least one gas access, and downstream is set
Vacuumize interface;
Constant temperature oven, around the part for accommodating the deposition substrate of the body;And
Inductive coupling plasma generator, around the part positioned at the constant temperature oven upstream of the body, so that on edge
It is spaced a distance on the direction of the axis of the body with the deposition substrate.
2. the system as claimed in claim 1, it is characterised in that scope of the distance in 10cm to 1.5m.
3. system as claimed in claim 2, it is characterised in that scope of the distance in 20cm to 1.2m.
4. system as claimed in claim 3, it is characterised in that scope of the distance in 30cm to 1m.
5. the system as claimed in claim 1, it is characterised in that the inductively coupled plasma generating means has 10 to 300
Watt operating power and about 13.56MHz working frequency.
6. the system as claimed in claim 1, it is characterised in that the upstream end of the body has upstream flange, itself and upstream
Closure disk is sealingly engaged to seal the body, and the gas access is formed on upstream closure disk, and
The downstream of the body has downstream flange, and it is sealingly engaged to seal the body with downstream closure disk, described to take out
Vacuum interface formation is on downstream closure disk.
7. system as claimed in claim 6, it is characterised in that the downstream closure disk also has the specimen holder being formed thereon
Interface is for installing sample support rod, and the end extended in the body of the sample support rod is provided with for branch
The sample stage of the deposition substrate is held, sample stage level height is in cavity cross-section center.
8. the system as claimed in claim 1, it is characterised in that the inductive coupling plasma generator includes:
Around the coil of the body;And
Coil brace for fixing each coil turn in the coil.
9. the system as claimed in claim 1, it is characterised in that the constant temperature oven includes upper and lower part, and the top is with
There is depression to accommodate the body on the apparent surface in portion, the upper and lower part is connected through the hinge so as to the top energy
Around hinge axle is rotated is provided with refractory fibre and air cooling equipment to surround or expose in the body, constant temperature oven.
10. system as claimed in claim 9, it is characterised in that the constant temperature oven includes one or more warm areas, each warm area
With the heating element heater being arranged in the depression and the temperature control equipment associated with the heating element heater.
11. the system as claimed in claim 1, it is characterised in that the body is quartzy body.
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CN108151529A (en) * | 2017-12-22 | 2018-06-12 | 合肥费舍罗热工装备有限公司 | A kind of dual temperature area open-type sliding rail stove |
CN109336096A (en) * | 2018-10-19 | 2019-02-15 | 钟国仿 | A kind of equipment and preparation method of open continuous growth carbon nanomaterial |
CN109371384A (en) * | 2018-12-13 | 2019-02-22 | 深圳市捷佳伟创新能源装备股份有限公司 | The reaction chamber structure of plasma deposition furnace |
CN110629200A (en) * | 2019-09-20 | 2019-12-31 | 理想晶延半导体设备(上海)有限公司 | Semiconductor processing equipment |
CN113201726A (en) * | 2021-04-30 | 2021-08-03 | 浙江大学杭州国际科创中心 | Preparation method of two-dimensional material |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN108151529A (en) * | 2017-12-22 | 2018-06-12 | 合肥费舍罗热工装备有限公司 | A kind of dual temperature area open-type sliding rail stove |
CN109336096A (en) * | 2018-10-19 | 2019-02-15 | 钟国仿 | A kind of equipment and preparation method of open continuous growth carbon nanomaterial |
CN109336096B (en) * | 2018-10-19 | 2023-09-26 | 深圳市纳设智能装备有限公司 | Equipment for open type continuous growth of carbon nano material and preparation method |
CN109371384A (en) * | 2018-12-13 | 2019-02-22 | 深圳市捷佳伟创新能源装备股份有限公司 | The reaction chamber structure of plasma deposition furnace |
CN110629200A (en) * | 2019-09-20 | 2019-12-31 | 理想晶延半导体设备(上海)有限公司 | Semiconductor processing equipment |
CN113201726A (en) * | 2021-04-30 | 2021-08-03 | 浙江大学杭州国际科创中心 | Preparation method of two-dimensional material |
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