CN109097756A - A kind of heating device that the high temperature film for thin metal deposits - Google Patents
A kind of heating device that the high temperature film for thin metal deposits Download PDFInfo
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- CN109097756A CN109097756A CN201810995176.3A CN201810995176A CN109097756A CN 109097756 A CN109097756 A CN 109097756A CN 201810995176 A CN201810995176 A CN 201810995176A CN 109097756 A CN109097756 A CN 109097756A
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- base band
- conductive metal
- film
- metal
- stick
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical 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
- C23C16/46—Chemical 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 characterised by the method used for heating the substrate
Abstract
The invention belongs to technical field of film preparation, the heating device of specially a kind of high temperature film deposition for thin metal.The present invention has redesigned electrode group unit；Conductive metal stick of the metal base band Jing Guo N number of special setting is supported by it and well contacts with it, and conductive metal stick is not rolled with the movement of metal base band.Conductive metal stick with metal base band is linear contacts conduction, and play a supportive role to metal base band and make it deformation occurs, avoid generating spark phenomenon, ensure that the later period application of film.The present invention is suitable for the heating of the one-sided metallic base band of different in width thickness；And heating rate is high, uniformity of temperature profile, and efficiency is high, while can realize the continuous preparation of plural layers.These advantages are particularly important for the preparation of industrialization of film, the quality for preparing film can be improved, and reduce cost.
Description
Technical field
The invention belongs to technical field of film preparation, the heating that specially a kind of high temperature film for thin metal deposits is filled
It sets.
Background technique
In field of film preparation, in order to realize the control growth of film, and then reach control thin film physics chemical property
Purpose, it usually needs the silicon for giving film growth accompanying.
In film growth preparation, superior reaction chamber is needed, is designed for complex reaction room, just to the temperature of reaction environment
It is required that it is higher, and then heater must also make corresponding change.Because gas reaction has strict requirements for temperature in cavity,
Require to develop temperature uniformly, lifting temperature rapidly, stablize, favorable repeatability the features such as high performance thin film deposition hot
System.That is: there is the growth temperature being rapidly heated to each layer film is grown；It can control heater and realize different set temperatures,
Meet the needs of growth plane SH wave film；Have good repeatability, makes the material to grow out every time property having the same
Matter.
At present common heating method there are several types of: (1) thermal conductivity heats, and generallys use Resistant heating, even if
With the higher resistance wire of resistance, high current is passed to, is that resistance wire generates a large amount of Joule heat in a short time, so that resistance wire
Temperature rises to 1500~2000 DEG C, then makes on heat conduction pattern to substrate.And this deficiency is, what it was heated
Object cannot be too big, to avoid poor contact between substrate and heater strip, so as to cause the phenomenon that substrate uneven heating is even.And
This heating method is unfavorable for the growth preparation of continuous band film.(2) radiant type heats, i.e., substrate is placed in a high temperature
In the irradiation range of heater, infrared ray radiated by heater etc. gives silicon.This heating method is to heater
Quantity, spatial distribution etc. there are strict requirements, to guarantee that substrate obtains temperature that is sufficiently high and being evenly distributed.But in reality
In, it is larger that this heater designs more difficult and required space.(3) induction type heats, i.e., conductor is placed in the electricity of high frequency
In magnetic field, make the electric current that passband rate is induced in conductor, generation heat is heating up under the function of current, this heating side
The heating rate of formula is fast, the temperature of substrate surface can be made to reach 800~1000 DEG C within several seconds.And this heating method deficiency exists
In to silicon, must be requested that substrate is that have certain thickness electric conductor, and regular shape, resistivity are evenly distributed.This
Outside, this heating method also has very high requirement, and the electromagnetic shielding that claimed apparatus equipment has had to induction power supply, to prevent
Only the electronic equipment of surrounding and human body are damaged.
Above-mentioned heating method respectively has superiority and inferiority point, and energy needed for they have in common that substrate heating is that have external transfer
Or convert, but in transfer or conversion process, really the energy required for substrate heating is seldom, most
Energy is wasted by resistance wire or power supply itself.It is that discomfort shares when preparing film on wide, long strip metal substrate
The heating method of (1) is stated, especially for mobile metal substrate.And (2) although heating can be used for it is such wide, long
The heating of strip metal substrate, but design well must be carried out to heating source just can guarantee temperature along metal substrate length and width
Degree direction is uniformly distributed, but such heating source is usually more complicated.Heating Metal Substrate is carried out using the heating method of (3)
When band, then require the very high skin depth limit value that just can guarantee alternating electric field of electric field frequency in material internal to improve efficiency.?
Be easy under high frequency, in vacuum cavity generate high-frequency electric field coupling and excited plasma so that induction heating and grade from
Daughter occurs simultaneously, this is unfavorable to the accurate control of growth temperature.
When being heated to strip metal substrate base band, compared with above-mentioned common heating method, by metal liner
Electric current is introduced in base band, using the resistance of metal base band itself come adstante febre, device is more simple and efficiency is higher.Currently,
Existing related patents (CN106521457A) by a similar method heats metal substrate.But it can be due in this patent
It is to be placed using electrode slice two rows, and metal substrate base band is mostly flexible strip, when depositing wide film due to metal substrate
Base band is wide and curves inwardly, and therefore electric discharge caused by metal substrate base band border and electrode loose contact can be caused existing
As, therefore it is unfavorable for the film growth preparation of wide metal substrate base band.
Summary of the invention
For above-mentioned there are problem or deficiency, when preparing film to solve energization self-heating metal base band, width it is larger and
The metal base band of thinner thickness can deformation occurs or distortion, strikes sparks so as to cause electrode and base band poor contact, thus nothing
The problem of method later period uses.The present invention provides a kind of heating devices that the high temperature film for thin metal deposits.
This for high temperature film deposition heating device include the positive and negative electrode group unit being mounted in vacuum cavity, it is thin
Film vitellarium, external impressed current source, two winders.Metal base band (back side conductive processing) is drawn from a winder to one
Electrode group unit in traction to another electrode group unit, is finally coiled in another winding after the plated film of film-growth zone
On disk, external power supply provides the heated current of electrode group unit.
The electrode group unit is made of two rotating wheels, conductive metal stick, conductive metal bar fixing device and support frame,
Metal base band is heated；The mechanism of its heating method is: from heated current is in contact with it by conductive metal stick from base band
It imported into inside metal base band, and is flowed on the metal base band being located in film crystallizing field, generated because of base band self-resistance
Temperature needed for Joule heat reaches film growth, while being flowed out by another mutually isostructural electrode group, form one completely
Current path.
The rotation wheel surface is smooth, does not have relative friction between metal base band, and axle center insulation is used to support Metal Substrate
Band, one constitutes the channel of metal base band with winder, another constitutes metal with conductive metal stick and film-growth zone respectively
The channel of base band；Position is adjustable on the support frame for it, to realize that the contact force between metal base band and conductive metal stick adjusts.
The conductive metal stick is connect with external power supply, supports robust metal base band, and metal is constituted between rotating wheel
The channel of base band；N number of conductive metal stick parallel equidistant is fixed on conductive metal bar fixing device, and conductive metal stick is same
Side end face is on same camber line on conductive metal bar fixing device, between conductive metal stick and conductive metal bar fixing device
Insulation, and N >=5.One resistance unit of each conductive metal stick and external connection constitutes an electrode unit, each electrode unit
It is formed and is electrically connected by current dividing circuit, current dividing circuit is series resistance.When work, metal base band and N number of conductive gold
The cambered surface for belonging to bar construction directly fits contact, and conductive metal stick is not rolled with the movement of metal base band.
Support frame for installing conductive metal bar fixing device and two rotating wheels, and with conductive metal bar fixing device and
It insulate between rotating wheel.
Further, the current dividing circuit realizes that evenly distributing for electric current is input to Metal Substrate through conductive metal stick
Band.
The present invention has redesigned electrode group unit；Conductive metal stick of the metal base band Jing Guo N number of special setting, is propped up by it
It supports and is well contacted with it.Conductive metal stick on the one hand with metal base band is linear contacts conduction, form relatively uniform heating
Mode；On the other hand make that metal base band will not deformation occurs to the supporting role of metal base band, to avoid bad because contacting
The phenomenon that side is burnt in sparking is generated, ensure that the later period application of its product.The channel that rotating wheel and conductive metal stick are formed, so that golden
Category base band is directly fitted with conductive metal stick to be contacted, and conductive metal stick is not rolled with the movement of metal base band, it is ensured that the two
Between contact it is excellent, and complete by two winders the process continuously wound.The present invention is suitable for various one-sided metallic substrates
Heating, and heating rate is high, and uniformity of temperature profile, efficiency is high, while can realize prepared by the continuous winding of Multilayer single film.
In conclusion the present invention is suitable for the heating of the one-sided metallic base band of different in width thickness；And heating rate is high,
Uniformity of temperature profile, efficiency is high, while can realize the continuous winding preparation of plural layers.Industrialization of these advantages for film
It prepares particularly important, the quality of prepared film can be improved, while reducing the preparation cost of film.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of embodiment device；
Fig. 2 is the structural schematic diagram of embodiment electrode group unit；
Fig. 3 is the partial top view of embodiment electrode unit；
Fig. 4 is embodiment current dividing circuit schematic diagram；
Fig. 5 is that the x-ray diffraction 2Theta of the GdYBCO film of three different locations in embodiment plating filmed metals base band is swept
Tracing；
Fig. 6 is x-ray diffraction Omega scanning and the Phi of the GdYBCO film in embodiment plating filmed metals base band middle position
Scanning curve；
Appended drawing reference: 1- winder 1,2- rotating wheel, 3- support frame, 4- current sharing resistors, 5- conductive metal stick, 6- are thin
Film vitellarium, 7- external impressed current source, 8- conductive metal bar fixing device, 9- winder 2
Specific embodiment
The present invention is described further with reference to the accompanying drawings and examples.
Device shown in FIG. 1 is used for second-generation high-temperature superconductor Gd0.5Y0.5Ba2Cu3O7-x(GdYBCO) system of film
It is standby.Take one section of long 150mm, the short sample of width 12mm is placed in vitellarium, and the Hastelloy of its deposited good buffer layer thin film
Flexible base band (LaMnO3/homo-epi MgO/IBAD-MgO/SDP-Y2O3/ Hastelloy), by the back side of this section of sample through throwing
Then light processing is joined end to end it with leash (naked base band) by the way of welding, finally with realizing good electrical contact
The position of metal substrate flexibility base band Yu film-growth zone spray head is fixed and regulated according to the embodiment above, and will traction
In band connection to winder, and connect circuit.The quality for weighing metal organic source is respectively the Y of 128.5mg (TMHD)3、
The Gd (TMHD) of 143.0mg3, 676.9mg Ba (TMHD)3, 343.2mg Cu (TMHD)3With the Zr (TMHD) of 16.5mg3
(TMHD:2,2,6,6- tetramethyl -3,5- heptadione), are dissolved in the tetrahydrofuran solvent of 5ml, and be placed in sonic oscillation together
Enabled sufficiently dissolution, forms uniformly clear metal organic source solvent.Power supply is opened, is passed to metal substrate flexibility base band
The electric current (voltage about 39V) of 25.8A.Traction electric machine is opened, metal substrate flexibility base band sample is drawn to film-growth zone；To
After temperature is stablized, i.e., current and power supply is not fluctuating, by 310 DEG C of metal organic source feeding of vaporization chamber by the way of peristaltic pump
Middle flash distillation is further formed metal organic source steam；The metal organic source steam under the drive of Ar further with O2And N2O gas
Body mixing is finally ejected into the metal substrate flexibility base band by vitellarium through spray head and anti-by 320 DEG C of appendixs
GdYBCO film should be generated.
Conductive metal stick uses Ag-W alloy bar, because the electric current for giving metal substrate flexibility base band to heat during the experiment is big
I.e. required temperature is higher, the flexible base band temperature of metal substrate and gas pressure in vacuum are higher, this requires electrode and metal substrate flexible
There is good electrical connection between base band, otherwise will result in the electric discharge between base band and electrode and burn electrode and base band, and Ag-W
Alloy bar has both highly conductive and dystectic characteristic, and oxidation resistance is strong, and has the function of printing electric arc, therefore is very suitable to this
Kind working environment.
Heat electrode distribution current resistor figure as shown in figure 4, simultaneously in the present embodiment use 6 Ag-W alloy bars,
And assume that the resistance of Ag-W stick is ignored, in order to keep the electric current on every Ag-W stick equal, it is assumed that the electric current is I, then electric current
The total current of source output is 6I.It according to Kirchhoff's law, then distributes resistance Rn=R*n/ (6-n), the distribution electricity in embodiment
Resistance is using identical metal base band and according to made of above formula calculating structural tailoring.
It is put into the GdYBCO sample that will be prepared and is connected with O2Annealing furnace in, taken out after keeping the temperature 30 minutes at 500 DEG C,
And the film sample is characterized.
The structure of prepared GdYBCO film is as shown in Figure 5 and Figure 6.
It is shown in Fig. 5, the diffraction maximum in face (00l) of three different locations (two edges and centre) is all very sharp, diffraction maximum
Intensity it is also similar, and all without miscellaneous peak, show that the GdYBCO crystal grain of three positions is pure c-axis growth, also illustrate this
GdYBCO membrane crystallization quality in metal substrate flexibility base band is very uniform.
Value of a half width is respectively 1.68 ° and 2.96 ° in outside the face of two curves and face in Fig. 6, is shown in this position
Orientation very well, has the biaxial texture similar with GdYBCO film on monocrystalline outside GdYBCO pellicular front and in face.
Therefore using the crystalline quality and favorable orientation of GdYBCO film prepared by heating device of the invention.
In conclusion the heating method that this base band is powered from the back side effectively overcomes the deficiency of original heating system, with
And the increase due to flexible metal substrate width, it is caused from base band border import electric current and there is a phenomenon where be curved to the inside；
Its principle, structure are simple, and rapidly, efficiency is high for heating, effectively avoid from electric current caused by an electric conductor importing electric current
Be unevenly distributed, so as to cause the excessively high phenomenon of local temperature, and be suitable for the metal substrate base band of different in width, the heating side
Formula has been able to achieve the continuous winding preparation of the GdYBCO film of the single side of wide, long metal substrate base band.
Claims (2)
1. a kind of heating device that the high temperature film for thin metal deposits, including the positive and negative electrode group being mounted in vacuum cavity
Unit, film-growth zone, external impressed current source and two winders, it is characterised in that:
Metal base band to be coated is drawn from a winder to an electrode group unit, after the plated film of film-growth zone,
It on traction to another electrode group unit, is finally coiled on another winder, external power supply provides adding for electrode group unit
Thermocurrent；
The electrode group unit is made of two rotating wheels, conductive metal stick, conductive metal bar fixing device and support frame, to gold
Belong to base band to be heated；The mechanism of its heating method is: heated current is imported by conductive metal stick from the base band place of being in contact with it
It is flowed to inside metal base band, and on the metal base band being located in film crystallizing field, the joule generated by base band self-resistance
Temperature needed for heat reaches film growth, while being flowed out by another mutually isostructural electrode group, form a complete electric current
Access；
The rotation wheel surface is smooth, does not have relative friction between metal base band, and axle center insulation is used to support metal base band,
One constitutes the channel of metal base band with winder, another constitutes metal base band with conductive metal stick and film-growth zone respectively
Channel；Position is adjustable on the support frame for it, to realize that the contact force between metal base band and conductive metal stick adjusts；
The conductive metal stick is connect with external power supply, supports robust metal base band, and metal base band is constituted between rotating wheel
Channel；N number of conductive metal stick parallel equidistant is fixed on conductive metal bar fixing device, and the same side of conductive metal stick
Face is on same camber line on conductive metal bar fixing device, between conductive metal stick and conductive metal bar fixing device absolutely
Edge, N >=5；One resistance unit of every conductive metal stick and external connection constitutes an electrode unit, and each electrode unit passes through electricity
It flows distributor circuit and forms electrical connection, current dividing circuit is series resistance；When work, metal base band and N number of conductive metal stick structure
At cambered surface directly fit contact, conductive metal stick is not rolled with the movement of metal base band；
Support frame as described above for installing conductive metal bar fixing device and two rotating wheels, and support frame and conductive metal stick and turn
Driving wheel insulate between each other.
2. the heating device deposited as described in claim 1 for the high temperature film of thin metal, it is characterised in that: the electric current point
Realize that evenly distributing for electric current is input to metal base band through conductive metal stick with circuit.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810995176.3A CN109097756B (en) | 2018-08-29 | 2018-08-29 | Heating device for high-temperature thin film deposition of thin metal |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810995176.3A CN109097756B (en) | 2018-08-29 | 2018-08-29 | Heating device for high-temperature thin film deposition of thin metal |
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| CN109097756B CN109097756B (en) | 2020-10-23 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377989A (en) * | 2001-03-30 | 2002-11-06 | 中国科学院物理研究所 | Heating method for preparing metal substrate film |
| TW201340770A (en) * | 2012-03-26 | 2013-10-01 | Chung-Nan Liu | High frequency electric heating rolling belt |
| CN104046963A (en) * | 2014-06-08 | 2014-09-17 | 电子科技大学 | Thin film sedimentation preparation device and method |
| CN106521457A (en) * | 2016-10-10 | 2017-03-22 | 电子科技大学 | Heating device for high-temperature thin film deposition |
-
2018
- 2018-08-29 CN CN201810995176.3A patent/CN109097756B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377989A (en) * | 2001-03-30 | 2002-11-06 | 中国科学院物理研究所 | Heating method for preparing metal substrate film |
| TW201340770A (en) * | 2012-03-26 | 2013-10-01 | Chung-Nan Liu | High frequency electric heating rolling belt |
| CN104046963A (en) * | 2014-06-08 | 2014-09-17 | 电子科技大学 | Thin film sedimentation preparation device and method |
| CN106521457A (en) * | 2016-10-10 | 2017-03-22 | 电子科技大学 | Heating device for high-temperature thin film deposition |
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| CN109097756B (en) | 2020-10-23 |
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