CN100526498C - Deposition film making system of pulse laser with added electric field - Google Patents
Deposition film making system of pulse laser with added electric field Download PDFInfo
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- CN100526498C CN100526498C CNB2006100018091A CN200610001809A CN100526498C CN 100526498 C CN100526498 C CN 100526498C CN B2006100018091 A CNB2006100018091 A CN B2006100018091A CN 200610001809 A CN200610001809 A CN 200610001809A CN 100526498 C CN100526498 C CN 100526498C
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- pulse laser
- fixed plate
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Abstract
This invention relates to a pulse laser deposition (PLD) system with extra electric field. The system adds an extra strong electric field device to the substrate heater of the traditional PLD apparatus. The electric field device comprises two metal plate electrodes, which are set in the notches of two concave ceramic blocks. The two ceramic blocks are vertically set and parallel to each other on a ceramic fixation plate. A through hole is drilled on one side of the notch of the ceramic block. Wire coated with ceramic pipe penetrates the through hole from the metal plate electrode, and is connected to a resistor and transformer power supply to form the whole circuit system. The system has simple structure. The system can obviously alter the microstructures of the grown thin films, and further alter the properties of the thin films. 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 with pulsed laser deposition, particularly a kind of pulsed laser deposition that adds under the highfield effect prepares membrane system.
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 mainly contains 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.E 56 (1997) 1322, and the non-linear optical effect of material strengthens greatly when aligning when the metal nanoparticle in the metal nano laminated film has.Document 2:Effective nonlinear optical properties of metal-dielectric composite media withshape distribution, analyze among the Phys.Rev.E64 (2001) 036615 and point out, the distribution of nano particle and shape can change the absorption peak position of matrix material, improve the figure of merit ratio of its third-order non-linear effect.Apply electric field and be and realize that nano particle aligns the effective means with alteration of form.And conventional P LD equipment does not have the function of added electric field, in the laminated film of being grown the distribution of nano particle in substrate material be at random, unordered, and in amorphous or polycrystalline film, all 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, the nano particle that makes is arranged still for unordered, spherical.And if directly add highfield by metal polar plate at the substrate two ends, owing to charged particle in the plumage brightness can conducting two electrodes cause and instantaneous sparking discharge will have a strong impact on the growth for Thin Film quality.But concrete reference 3:Pulsed laser deposition of thin films D.B.Chrisey, G.K.Hubler John Wiley ﹠amp; Sons, Inc.1994.
Summary of the invention
The objective of the invention is to: utilize in the preparation thin-film process and apply electric field, realize that nano particle aligns with particle shape in the film to change.Design adds the deposition film making system of pulse laser of highfield, and can effectively utilize this system, apply strong electric field in film growth or annealing process, the interaction by particle in highfield and the film obtains the film of special construction, 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 provided by the invention is on conventional P LD Equipment Foundations, adds that a cover adds the isolated plant of highfield.Specifically comprise vacuum chamber, its vacuum is realized by the vacuum unit that mechanical pump, molecular pump and pipeline are formed; Be placed on the outer gas cylinder of vacuum chamber, form inflation system by needle-valve on the vacuum-chamber wall and vacuum chamber, to realize different atmospheres; 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; Target assembly and substrate heater are installed in the vacuum chamber; Connect to form heating temperature control part by control power supply and substrate heater; It is characterized in that: described substrate heater rear is provided with an extra electric field device, and this extra electric field device is " recessed " shape and four inferior horns by two and is equipped with the ceramic block of screw, two metal sheet electrodes, a ceramic fixed plate and a metallic rod and forms; Wherein said two metal sheet electrodes, be positioned over respectively in the groove of described " recessed " shape ceramic block, two ceramic blocks are perpendicular to ceramic fixed plate, and parallel to each other being fixed on the ceramic fixed plate, and a metallic rod top that is installed on the vacuum chamber base is fixed on ceramic fixed plate bottom; Groove one side of ceramic block is made a call to a wire through-hole, and the lead that is with vitrified pipe passes from the wire through-hole on the metal sheet electrode, links to each other with transformer frequency response with a resistance.
In above-mentioned technical scheme, also comprise retaining clip, described retaining clip be rectangular in shape (
) metalwork, stick at two of square metalwork and to have screw; Have draw-in groove on the described ceramic fixed plate, this draw-in groove is provided with along the long limit of ceramic fixed plate, by retaining clip two ceramic blocks is fixed in the draw-in groove of ceramic fixed plate, makes that the spacing between two ceramic blocks is adjustable.
In above-mentioned technical scheme, described metal sheet electrode is for being difficult for materials such as oxidized red copper or stainless steel.Square in the middle of being shaped as, the runway shape of edge circular arc.Be mainly and prevent point discharge.The size of two plates generally is about 20～30mm, wide about 5～10mm by the size decision of substrate.
In above-mentioned technical scheme, described ceramic block is answered anti-high temperature more than 1000 ℃, and bigger specific inductivity is arranged, and less gas efficiency can satisfy application requiring in the vacuum chamber, and easily processing.As the microcrystalline mica pottery, the cured stone of liquid etc.
In above-mentioned technical scheme, described ceramic fixed plate is identical with ceramic block material performance requriements, and thickness is about 1～3mm, above draw-in groove that parallel quarter, two width were 2～3mm, the length of groove and spacing are looked the size decision of ceramic block.
In above-mentioned technical scheme, the resistance of described resistance is 10
4～10
8Ω is adjustable.Mainly be in film-forming process, prevent that circuit turn-on from causing danger.
In above-mentioned technical scheme, described transformer frequency response, its voltage is adjustable at 0～50000 volt.
Advantage of the present invention:
The deposition film making system of pulse laser that adds highfield provided by the invention is simple, easily installs, and is easy to operate.Utilize this system can be implemented in easily in system film or the annealing process and apply highfield, by adding the interaction of particle in highfield and the film, can grow conventional P LD equipment the membrane structure that can not grow, effectively realize aligning and alteration of form of nano particle in the nano compound film, and further significantly changed the performance of film.
Description of drawings
Fig. 1 adds the PLD system film system schematic of highfield for the present invention
Fig. 2 a is the assembly synoptic diagram of extra electric field device of the present invention
Fig. 2 b is the metal sheet electrode synoptic diagram in the extra electric field device of the present invention
Fig. 3 a conventional P LD does not have the Ag/BaTiO of extra electric field preparation
3Thin film transmission electron microscope figure
Fig. 3 b utilizes apparatus of the present invention to add the electric field of 1000V/cm in film-forming process, under all identical situation of other conditions with preparation Fig. 3 a sample, and the Ag/BaTiO of preparation
3Thin film transmission electron microscope figure (promptly utilizing device of the present invention and the thin film transmission electron microscope comparison diagram that utilizes the preparation of conventional P LD device)
Drawing is described as follows:
(1) excimer laser; (2) condenser lens; (3) beam flying mirror;
(4) silica glass window; (5) vacuum unit; (6) transformer frequency response;
(7) controllable electric power; (8) adjustable resistance; (9) gas cylinder;
(10) substrate heater; (11) extra electric field device; (12) substrate;
(13) target assembly; (14) vacuum chamber; (15) ceramic block;
(16) ceramic fixed plate; (17) metal sheet electrode; (18) retaining clip;
(19) lead; (20) metallic rod
Embodiment
Embodiment 1:
Press Fig. 1, make a PLD system film system that adds highfield shown in 2.
Utilize a PLD system film system, the substrate heater rear in the vacuum chamber 14 of this PLD system film system is provided with an extra electric field device.Traditional vacuum chamber 14, its vacuum tightness realizes that by the vacuum unit 5 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 9 is by needle-valve and vacuum chamber on pipeline and vacuum chamber 14 walls, so that different atmospheres to be provided.Target assembly 13 and substrate heater 10 are installed in vacuum chamber 14, the PLD system film system that the target assembly use is traditional, promptly the roundel of being made by 4 stainless steels is installed on the big disk and forms; 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 also can be under motor drives be realized rotation around self bearing, and its rotating speed can accurately be controlled by computer, thereby makes laser beat different positions at target.Also can realize moving forward and backward of target assembly 13 by corresponding transmission mechanism.The joule heating heating that substrate heater 10 produces when adopting silicon chip or resistance wire galvanization links to each other with the control power supply 8 of EUROTHEM818 model, and substrate 12 is placed on the substrate heater 10.
Present embodiment add highfield device 11, shown in Fig. 2 a: be by 8
The square metalwork is as retaining clip 18, stick at two of square metalwork and to have screw, retaining clip 18, ceramic block 15 are installed in the draw-in groove place of ceramic fixed plate 16, utilize nut that the draw-in groove of the screw of ceramic block 15 belows and ceramic fixed plate 16 is fixedly connected and are in the same place.Two metal sheet electrodes 17 are positioned in the cutting of ceramic block 15, and metal sheet electrode 17 is red copper or stainless steel plate, and it is square in the middle of being shaped as, and four corner edge are the shape of circular arc, as Fig. 2 b.Two plain conductors 19 that are with vitrified pipe pass the through hole of ceramic block 15 tops and link on adjustable resistance 8 and the transformer frequency response 6 by the terminal stud on the metal sheet electrode.Complete assembly is fixed on vacuum chamber 14 inner bottom parts by the metallic rod 20 that is connected by ceramic fixed plate 16 intermediary apertures, is placed on the rear of substrate heater 10, and substrate heater 10 is between the ceramic block 15.Excimer laser 1 is placed on outside the vacuum chamber 14, and the pulse laser of its generation through 3 reflections of beam flying mirror, shines on the target by the silica glass window 4 on vacuum chamber 14 walls after focusing on through condenser lens 2.
Embodiment 2:
Utilize the device of embodiment 1 to prepare Ag/BaTiO
3Laminated film, concrete technology is as follows:
With Ag/BaTiO
3Target be fixed on and change on the target.With 5 * 10 * 0.5mm
3Two throwing MgO substrates are placed on the wide silicon well heater of 10mm, add parallel electric field device and whole external circuit, and the spacing of two ceramic blocks is adjusted to 11mm, and two metal polar plate spacings are 20mm.The distance of target and substrate is about 4cm.Take out base vacuum to 5 * 10
-4Pa, the inflated with nitrogen environment is to 10Pa.Substrate temperature keeps room temperature.Pulse laser uses the excimer laser of German LambdaPhysik company growth to produce, and working gas is XeCl, output wavelength 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.Adjusting changes target position, makes the plumage brightness contact substrate preferably.In deposition simultaneously, voltage is added to 2000V, respective electric field is about 1000V/cm.Realize adding in real time in the thin film growth process operation of highfield.The Ag/BaTiO that does not have the extra electric field preparation with reference to figure 3a for conventional P LD
3Thin film transmission electron microscope figure, Fig. 3 b utilizes the device of embodiment 1, adds the electric field of about 1000V/cm in film-forming process, under all identical situation of other conditions with preparation Fig. 3 a condition, the Ag/BaTiO of preparation
3Thin film transmission electron microscope figure (promptly utilize device of the present invention and the thin film transmission electron microscope comparison diagram that utilizes the preparation of conventional P LD device, see Fig. 3 b)., can see that the Ag nano particle has significantly to align by transmission electron microscope observing to the film sample of preparation, and shape is close to and becomes elliposoidal.The Ag nano particle that does not have a PLD systems produce of electric field with tradition is that the film of sphere and stochastic distribution has had very big change.Further experiment finds that its third-order nonlinear optical effect significantly strengthens.
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 and structure are made amendment or be 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 (7)
1. but the deposition film making system of pulse laser of an added electric field comprises vacuum chamber (14), the vacuum unit of being made up of mechanical pump, molecular pump and pipeline (5); Be placed on the outer gas cylinder (9) of vacuum chamber (14), be communicated with vacuum chamber (14) by the needle-valve on the vacuum-chamber wall and form inflation system; Mounted substrate well heater (10) and target assembly (13) in the vacuum chamber (14); Connect to form heating temperature control part by control power supply and substrate heater (10); It is characterized in that: described substrate heater (10) rear is provided with one and adds highfield device (11), and this adds highfield device (11) and is made up of ceramic block (15), two metal sheet electrodes (17), a ceramic fixed plate (16) and a metallic rod (20) that two " recessed " shapes and four inferior horns are equipped with screw; Wherein said two metal sheet electrodes (17), be positioned over respectively in the groove separately of ceramic block (15) of described two " recessed " shapes, described two ceramic blocks (15) are perpendicular to ceramic fixed plate (16), and parallel to each other being fixed on the ceramic fixed plate (16); Groove one side of described ceramic block (15) is made a call to a wire through-hole, and the lead (19) that is with vitrified pipe passes wire through-hole from metal sheet electrode (17), links to each other with transformer frequency response with a resistance; These the whole series add highfield device (11) and are fixed on vacuum chamber (14) inner bottom part by the described metallic rod (20) that is connected by ceramic fixed plate (16) intermediary aperture, be placed on the rear of substrate heater (10), and substrate heater (10) is between described two ceramic blocks (15); Excimer pulse laser (1) is placed on outside the vacuum chamber (14), and after the pulse laser of its generation focused on through condenser lens, through beam flying mirror (3) reflection, the silica glass window (4) by vacuum chamber (14) shone on the target.
2. but by the deposition film making system of pulse laser of the described added electric field of claim 1, it is characterized in that: also comprise retaining clip (18), described retaining clip (18) metalwork that is rectangular in shape is stuck at two of square metalwork and to be had screw; Have draw-in groove on the described ceramic fixed plate (16), this draw-in groove is provided with along the long limit of ceramic fixed plate (16), by retaining clip (18) two described ceramic blocks (15) is fixed in the described draw-in groove of described ceramic fixed plate (16).
3. but by the deposition film making system of pulse laser of the described added electric field of claim 1, it is characterized in that: described metal sheet electrode (17) is red copper or stainless steel plate, and it is square in the middle of being shaped as, and four corner edge are the shape of circular arc.
4. but by the deposition film making system of pulse laser of the described added electric field of claim 1, it is characterized in that: described ceramic block (15) is anti-pyritous microcrystalline mica pottery or the cured stone material of liquid more than 1000 ℃.
5. but by the deposition film making system of pulse laser of the described added electric field of claim 2, it is characterized in that: described ceramic fixed plate (16) is identical with the material performance requirement of described ceramic block (15), and thickness is 1～3mm; This pottery fixed plate (16) two described draw-in grooves at top parallel quarter, this draw-in groove width is 2～3mm, the size of the spacing of two described draw-in grooves and described ceramic block (15) is complementary.
6. but by the deposition film making system of pulse laser of the described added electric field of claim 1, it is characterized in that: the resistance of described resistance (8) is 10
4～10
8Ω is adjustable.
7. but by the deposition film making system of pulse laser of the described added electric field of claim 1, it is characterized in that: the voltage of described transformer frequency response (6) is adjustable at 0～50000 volt.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100018091A CN100526498C (en) | 2006-01-20 | 2006-01-20 | Deposition film making system of pulse laser with added electric field |
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| CNB2006100018091A CN100526498C (en) | 2006-01-20 | 2006-01-20 | Deposition film making system of pulse laser with added electric field |
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| CN100526498C true CN100526498C (en) | 2009-08-12 |
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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 |
| TWI485024B (en) * | 2013-01-15 | 2015-05-21 | Univ Nat Yunlin Sci & Tech | Laser processing device with auxiliary plate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1275777A (en) * | 1999-05-28 | 2000-12-06 | 中国科学院物理研究所 | Method for preparing oriented high-temp. superconducting film layer on non-texture basis |
| CN1379460A (en) * | 2001-06-27 | 2002-11-13 | 南京大学 | Method for orientation controlling growth of high-Tc ferroelectric film and prototype device of ferroelectric memory |
| JP2003197530A (en) * | 2001-12-25 | 2003-07-11 | Matsushita Electric Ind Co Ltd | Method for scavenging and depositing fine particle cluster |
| CN1622357A (en) * | 2004-12-16 | 2005-06-01 | 中国科学院物理研究所 | Method and device for preparing large area superconducting film adopting pulse laser deposition process |
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2006
- 2006-01-20 CN CNB2006100018091A patent/CN100526498C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1275777A (en) * | 1999-05-28 | 2000-12-06 | 中国科学院物理研究所 | Method for preparing oriented high-temp. superconducting film layer on non-texture basis |
| CN1379460A (en) * | 2001-06-27 | 2002-11-13 | 南京大学 | Method for orientation controlling growth of high-Tc ferroelectric film and prototype device of ferroelectric memory |
| JP2003197530A (en) * | 2001-12-25 | 2003-07-11 | Matsushita Electric Ind Co Ltd | Method for scavenging and depositing fine particle cluster |
| CN1622357A (en) * | 2004-12-16 | 2005-06-01 | 中国科学院物理研究所 | Method and device for preparing large area superconducting film adopting pulse laser deposition process |
Non-Patent Citations (1)
| Title |
|---|
| 电场对Au/SiO2及Au-Ag/SiO2表面结构与原子迁移特性的影响. 时方晓，曹立礼.真空科学与技术，第17卷第4期. 1997 * |
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