CN100526497C - Deposition film making system of pulse laser with controllable magnetic field - Google Patents
Deposition film making system of pulse laser with controllable magnetic field Download PDFInfo
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- CN100526497C CN100526497C CNB2006100018087A CN200610001808A CN100526497C CN 100526497 C CN100526497 C CN 100526497C CN B2006100018087 A CNB2006100018087 A CN B2006100018087A CN 200610001808 A CN200610001808 A CN 200610001808A CN 100526497 C CN100526497 C CN 100526497C
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Abstract
This invention relates to a pulse laser deposition (PLD) system with controllable magnetic field. The system adds an extra magnetic field device to traditional PLD apparatus. The system comprises: a vacuum room with a convex chamber set on the side wall, and a target assembly and a substrate heater are set in the convex chamber; a quartz glass window set above the convex chamber; a set of electromagnet assembly. The coil of the electromagnet assembly is set at the outer wall of the convex chamber. Two iron-core magnetic poles are connected to both ends of the substrate heater via sealed flange rings. The electromagnet assembly is connected to a computer via controlling power supply. The substrate heater and the target assembly do not contact the iron cores of the electromagnet assembly. The system has such advantages as simple structure and easy operation. The system can easily apply intensity-controllable magnetic field during growth or annealing process of the thin film, thus can grow thin films that cannot be grown by traditional PLD apparatus. This invention provides an effective experimental device for preparing novel thin film samples with special structures.
Description
Technical field
The present invention relates to a kind ofly prepare the device of film, particularly a kind of deposition film making system of pulse laser with controllable magnetic field with pulsed laser deposition.
Background technology
Pulsed laser deposition (hereinafter to be referred as PLD) is the most frequently used now one of the method for film for preparing.A typical PLD equipment is mainly by vacuum chamber, well heater, target assembly, compositions such as chip bench and inflation system.PLD equipment is simple, easy handling, and sedimentation rate is fast, is widely used in perovskite oxide film, multilayer film and the laminated film etc. of growth components complexity.
Thin film study field now, nano compound film be owing to have the superiority of conventional composite materials and modern nano material, caused the extensive concern of researcher and obtained deep day by day research to form and be important advanced subject.And in the nano compound film research, a very important aspect is exactly about distribution and the shape problem of nano particle in conventional composite materials matrix.As document 1:Optical nonlinearity enhancement viageometric anisotropy, theoretical analysis shows among the Phys.Rev.E56 (1997) 1322, when the metal nanoparticle in the metal nano laminated film had anisotropic structure, the non-linear optical effect of material strengthened greatly.The distribution of nano particle and shape can also change the absorption peak position of matrix material, improve the figure of merit ratio of its third-order non-linear effect.Report among the document 2:Chains composed of nanosize metal particles and identifying thefactors driving theirformation.Applied.Physics.Letter 70 (1997) 2469, prepare in the sample process with chemical process, because the introducing of foreign field, make Fe, Co, Ni nano particle form difform chain-like structure, produced anisotropic shape, remarkable change has taken place in character.And the present film sample that also can't realize preparing with PLD this special construction.Because conventional P LD equipment does not have the externally-applied magnetic field function, in the laminated film of being grown the distribution of nano particle in substrate material be at random, unordered, in amorphous or polycrystalline film, be approximately spherical.Though the ellipsoid nano particle that general orientation is arranged can occur in the film preferably in crystallinity, this moment, the concentration of nano particle can not be too high.Because the too high crystallinity that can destroy matrix membrane of concentration is arranged still for unordered, spherical nano particle.But concrete reference 3:Pulsed laserdeposition of thinfilms D.B.Chrisey, G.K.Hubler John Wiley﹠amp; Sons, Inc.1994.And among the document 4:Evidenceof ferromagnetic behavior of smallliquid droplets produced from amorphous alloys bylaser ablation.Applied.Physics.Letter 72 (1998) 3455, add the experiment in magnetic field though reported use PLD film-forming process.But used magnet is permanent magnet, and added magnetic field has only 1T and fixing.Because magnet is placed near the substrate, so substrate temperature can not be too high (＜3500C), otherwise magnet will lose magnetism fully, so its use is very restricted.And the introducing of film-forming process high-intensity magnetic field also can cause the track of moving charged particle in the plumage brightness that big deflection takes place, and does not grow the fine film thereby have to think of a way.
Summary of the invention
The objective of the invention is to overcome the function that conventional P LD equipment does not have externally-applied magnetic field, in the laminated film of being grown the distribution of nano particle in substrate material be at random, unordered and intimate for the spheric defective; Thereby provide a kind of deposition film making system of pulse laser that adds controlled high-intensity magnetic field, can utilize this system, in film growth or annealing process, interaction acquisition nano particle by high-intensity magnetic field and magnetic nanoparticle, paramagnetic particles or motion charged ion is drawn as elliposoidal, and the film that major axis aligns along field direction, realize conventional P LD the sample that can't grow.
The object of the present invention is achieved like this:
Deposition film making system of pulse laser with controllable magnetic field provided by the invention comprises: vacuum chamber and the vacuum unit of being made up of mechanical pump, molecular pump and pipeline; Gas cylinder is placed on outside the vacuum chamber, by the inflation system of needle-valve on the vacuum-chamber wall and vacuum chamber composition; Target assembly and substrate heater are installed in the vacuum chamber; Connect to form heating temperature control part by the first control power supply and substrate heater; Excimer pulse laser is placed on outside the vacuum chamber, and after the pulse laser of its generation focused on through condenser lens, through the beam flying specular reflectance, the silica glass window by vacuum chamber shone on the target; It is characterized in that: described vacuum chamber is arranged to sidewall has one to protrude the chamber, in this protrudes the chamber described target assembly and described substrate heater is installed; Described silica glass window is arranged on and protrudes the top, chamber; Also comprise a cover electromagnet assembly, the magnet coil of this assembly is placed on vacuum chamber and protrudes the outside, chamber, iron core two magnetic poles pass through the both sides that the tongued and grooved flanges articulating arrives substrate heater in the chamber, and the electro-magnet in the described electromagnet assembly links to each other with computer by the second control power supply; The iron core noncontact of substrate heater and target assembly and electro-magnet.
In above-mentioned technical scheme, the roundel that described target assembly is made by 4 stainless steels is installed on the big disk to be formed; Fixing target on the roundel; Big disk rotates by the gear driven bearing, rotates the exchange that realizes between different targets thereby drive roundel; Simultaneously, roundel is realized rotation under also can driving at the motor of self bearing, and its rotating speed can accurately be controlled by computer, thereby makes laser beat different positions at target.A whole set of target assembly also can be realized moving forward and backward by corresponding transmission mechanism.
In above-mentioned technical scheme, described electromagnet assembly is for producing the DC electromagnet of 0～2T controlling magnetic field, its magnetic core adopts the pure iron that magnetic permeability is big and remanent magnetism is little, its diameter is at 10～300mm, two magnetic pole air gaps, 0～100mm scope is adjustable, electro-magnet can be realized any magneticstrength between 0～2T by control power supply and computer control.And can be by the repeatable operation that adds magnetic field and demagnetizing field in the computer control certain hour interval.
The invention has the advantages that, apparatus of the present invention are simple, easy to operate, can very easily realize applying than high-intensity magnetic field in film preparation or the annealing process, realize conventional P LD equipment the film that can not grow, the film of being grown obtains nano particle and is drawn as elliposoidal, and the film that aligns along field direction of major axis, significantly changes the structure and the performance of conventional film.
Description of drawings
Fig. 1: the present invention adds the impulse laser deposition system synoptic diagram of high-intensity magnetic field
Fig. 2: electro-magnet synoptic diagram used in the present invention
Drawing is described as follows:
(1) excimer laser; (2) condenser lens; (3) beam flying mirror;
(4) electro-magnet; (5) quartz window; (6) sight glass window;
(7) substrate heater; (8) control power supply; (9) substrate;
(10) vacuum unit; (11) gas cylinder; (12) glass window;
(13) target assembly; (14) vacuum chamber; (15) protrude the chamber;
(16) iron core; (17) coil; (18) control power supply;
(19) computer; (20) tongued and grooved flanges ring
Embodiment
Embodiment 1: be described in detail below in conjunction with drawings and Examples
Press accompanying drawing 1, impulse laser deposition system that adds high-intensity magnetic field of making shown in Figure 2.
Present embodiment is on conventional P LD Equipment Foundations, adds a cover and adds that the high-intensity magnetic field device realizes, promptly on the basis of conventional P LD equipment vacuum chamber 14, chamber 15 is protruded in design one.In this protrudes chamber 15, target assembly 13 and substrate heater 7 are installed; Target assembly 13 adopts the assembly of conventional P LD equipment, and the roundel that this target assembly 13 is made by 4 stainless steels is installed on the big disk to be formed; Fixing target on the roundel; Big disk can rotate by the bearing of gear driven, rotates to realize the exchange between different targets thereby drive roundel; Simultaneously, roundel is realized rotation under also can driving at the motor of self bearing, and its rotating speed can accurately be controlled by computer, thereby makes laser beat different positions at target, and a whole set of target assembly also can be realized moving forward and backward by corresponding transmission mechanism.The joule heating heating that substrate heater 7 produces when adopting the monocrystalline silicon piece galvanization links to each other with the first control power supply 8 of EUROTHEM818 model.Substrate 9 is placed on the substrate heater 7.When target and substrate are installed, can be respectively target assembly 13 and substrate heater 7 be moved on to the glass window 12 places operation of vacuum chamber 14.One of present embodiment overlaps the repeatable operation that adds magnetic field and demagnetizing field in the computer control certain hour interval, the DC electromagnet that can produce 0～2T controlling magnetic field, its magnetic core adopts the pure iron that magnetic permeability is big and remanent magnetism is little, its diameter is between 10～300mm, and two magnetic pole air gaps, 0～100mm scope is adjustable.This high-intensity magnetic field device protrudes the coil 17 that electro-magnet 4 is placed in 15 outsides, chamber at vacuum chamber 14, and two magnetic pole N, the S of iron core 16 receive in the chamber by tongued and grooved flanges ring 20.Electro-magnet 4 is by the second control power supply 18 and computer 19 controls.Substrate heater 7 all can not contact with the iron core 16 of electro-magnet 4 with target assembly 13.The vacuum tightness of vacuum chamber 14 realizes that by the vacuum unit 10 that mechanical pump, molecular pump and the pipeline of its below are formed vacuum tightness is read by ZDF-9 compound vacuum gauge.Gas cylinder 11 is communicated with vacuum chamber 14 by the needle-valve on the vacuum-chamber wall, forms inflation system, to realize different atmospheres.Excimer laser 1 is placed on outside the vacuum chamber 14, and after the pulse laser of its generation focused on through condenser lens 2, through 3 reflections of beam flying mirror, the silica glass window 5 that protrudes 15 tops, chamber by vacuum chamber 14 shone on the target.Can be by observing in 6 pairs of vacuum chambers of glass window.
This apparatus structure is simple, easily installs, and is easy to operate.Use this device can be easy to be implemented in and apply controlled high-intensity magnetic field in film growth or the annealing process,, can realize the remarkable change of membrane structure and performance by the interaction of magnetic field and material.For the film of the novel special construction of preparation research provides effective means.
Embodiment 2:
The device of Application Example 1 externally-applied magnetic field, preparation Fe/BaTiO
3Laminated film.
Target assembly is moved on to vacuum chamber glass window place, is 99.99% Fe sheet and BaTiO with being cut into fan-shaped purity
3The composite target material of forming is fixed on to be changeed on the target.With 5 * 10 * 0.2mm
3Glass substrate be placed on the monocrystalline silicon substrate well heater platform.The monocrystalline silicon substrate well heater is moved on to the magnetic pole mid-way of electro-magnet.Adjust target assembly again, making target and substrate distance is about 40mm.Take out base vacuum to 5 * 10
-4Pa, inflated with nitrogen environment about 10
-3Pa.Substrate temperature rises to 700 ℃ and maintenance.Pulse laser uses the excimer laser of German Lambda Physik company growth to produce, and working gas is XeCl, output wave 308nm.Laser energy can reach 400mJ, adjustable repetitive frequency, pulsewidth 20ns, the about 1.5～3J/cm of target material surface energy density
2Regulate light path, laser is got on the target.For preventing that moving charged particle from changing track under the action of a magnetic field, apply magnetic field more immediately later at the plumage brightness, utilize the control computer of electro-magnet, setting the magnetic field maximum strength is 2T, and magnetic field is carried out from having to the circulation that almost disappears in the 10s interval.In this process, the time that 2T is kept in magnetic field is about 2s～3s.Be enough to significantly change film microstructure.The corresponding 0.1Hz or littler that is made as of laser repetition rate.
This device is easy and simple to handle, and the prepared film sample is done transmission electron microscope, can see when the atomic percent of Fe is higher, and nano particle is elongated by magnetic field and joins into chain, arranges along field direction.When Fe concentration was low, the Fe nano particle was drawn as elliposoidal, and major axis aligns along field direction.Further experiment finds that the third-order non-linear effect of film obviously strengthens.
Embodiment 3:
Prepare Fe/BaTiO when the device of Application Example 1, no magnetic field
3Film is annealed when adding high-intensity magnetic field outside.
Implementation process does not just add foreign field in the preparation process with example 2.The frequency of laser can be made as 2Hz more greatly than example 2 in the preparation process.To the film sample for preparing, be heated to 700 ℃, apply magnetic field 2T simultaneously.Kept 1 hour.
Change has taken place in distribution and shape that the result observes Fe nano particle in the film equally, though it is remarkable to be not so good as example 2, wide variation have taken place its character equally.
Embodiment 4:
The device of Application Example 1, externally-applied magnetic field prepare the Fe film.
Implementation process is with example 2, heated substrate to 800 ℃ in the preparation process.
To prepared film, can see that by atomic force microscope observation the Fe nanometer island of being grown is elongated and is connected to wire when no magnetic field under magnetic field.This structural modification the magnetic and the transport property of magnetic metal particle.Between the Fe nano wire, fill other metals, can study ferromagnetic/giant magnetoresistance effect that non-ferromagnetic interfacial effect causes very easily.
Embodiment 5:
The device of Application Example 1, the Fe film for preparing during to no magnetic field is annealed under magnetic field.
Implementation process does not add foreign field with example 4 in the preparation process.After preparation is finished, keep 800 ℃, annealing is 1 hour in 2T magnetic field.
Compare with no magnetic field situation, change has taken place in the appearance structure of Fe film equally.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: parts of the present invention are equal to replacement, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (2)
1. the deposition film making system of pulse laser with controllable magnetic field comprises vacuum chamber (14), the vacuum unit of being made up of mechanical pump, molecular pump and pipeline (10); Gas cylinder (11) is placed on outside the vacuum chamber (14), is communicated with vacuum chamber (14) by the needle-valve on the vacuum-chamber wall and forms inflation system; Target assembly (13) and substrate heater (7) are installed in the vacuum chamber, and the first control power supply (8) connects to form heating temperature control part with substrate heater (7); Excimer pulse laser (1) is placed on outside the vacuum chamber (14), and the pulse laser of its generation through the beam flying specular reflectance, shines on the target by silica glass window (5) after focusing on through condenser lens (2); It is characterized in that: described vacuum chamber (14) is arranged to sidewall has one to protrude chamber (15), in this protrudes chamber (15) described target assembly (13) and described substrate heater (7) is installed; Described silica glass window (5) is arranged on and protrudes top, chamber (15); Also comprise a cover electromagnet assembly, the magnet coil of this assembly (17) is placed on vacuum chamber and protrudes the outside, chamber (15), two magnetic poles of iron core (16) are by tongued and grooved flanges ring (20), receive the both sides of the substrate heater (7) in the vacuum chamber, the electro-magnet in the described electromagnet assembly (4) links to each other with computer by the second control power supply (18); Iron core (16) noncontact of substrate heater (7) and target assembly (13) and electro-magnet.
2. by the described deposition film making system of pulse laser of claim 1 with controllable magnetic field, it is characterized in that: described electromagnet assembly is for producing the DC electromagnet of 0～2T controlling magnetic field, its magnetic core adopts the pure iron that magnetic permeability is big and remanent magnetism is little, its diameter is at 10～300mm, two magnetic pole air gaps, 0～100mm scope is adjustable, and electro-magnet is by second control power supply and the computer control.
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| CNB2006100018087A CN100526497C (en) | 2006-01-20 | 2006-01-20 | Deposition film making system of pulse laser with controllable magnetic field |
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| CNB2006100018087A CN100526497C (en) | 2006-01-20 | 2006-01-20 | Deposition film making system of pulse laser with controllable magnetic field |
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| CN100526497C true CN100526497C (en) | 2009-08-12 |
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Families Citing this family (7)
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| CN102877032B (en) * | 2012-09-04 | 2015-05-27 | 中国科学院合肥物质科学研究院 | Preparation system for pulse laser deposition film under intense magnetic field |
| CN103196773B (en) * | 2013-04-03 | 2015-01-07 | 大连理工大学 | Device for online measuring stoichiometric proportions and ingredient masses of PLD (Pulsed Laser deposition) film |
| CN103774097B (en) * | 2014-01-23 | 2015-07-01 | 中国科学院合肥物质科学研究院 | High-intensity magnetic field assisted pulsed laser deposition system |
| CN105925937B (en) * | 2016-06-26 | 2018-12-04 | 中国计量大学 | It is orientated the preparation method of thin magnetic film |
| CN106555166B (en) * | 2016-11-18 | 2018-09-21 | 北京航空航天大学 | A kind of ultra-thin film preparation, Characterization on Interface and regulation and control integrated system and application process |
| CN107884918A (en) * | 2017-11-13 | 2018-04-06 | 中国科学院合肥物质科学研究院 | High energy ultraviolet laser gatherer under a kind of high-intensity magnetic field |
| CN114959590A (en) * | 2022-04-16 | 2022-08-30 | 江西师范大学 | Tungsten disulfide composite nano-particles, preparation method thereof and application of tungsten disulfide composite nano-particles as hydrogen evolution reaction electrocatalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6024851A (en) * | 1997-12-02 | 2000-02-15 | The Aerospace Corporation | Apparatus for magnetic field pulsed laser deposition of thin films |
| CN1390977A (en) * | 2002-07-20 | 2003-01-15 | 复旦大学 | Process for preparing compound film at ordinary temp |
| US6805916B2 (en) * | 2001-01-17 | 2004-10-19 | Research Foundation Of The City University Of New York | Method for making films utilizing a pulsed laser for ion injection and deposition |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6024851A (en) * | 1997-12-02 | 2000-02-15 | The Aerospace Corporation | Apparatus for magnetic field pulsed laser deposition of thin films |
| US6805916B2 (en) * | 2001-01-17 | 2004-10-19 | Research Foundation Of The City University Of New York | Method for making films utilizing a pulsed laser for ion injection and deposition |
| CN1390977A (en) * | 2002-07-20 | 2003-01-15 | 复旦大学 | Process for preparing compound film at ordinary temp |
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