CN105127883A - Space orientation regulating and controlling method and device for preparing single crystals with specific crystal surfaces on surfaces - Google Patents
Space orientation regulating and controlling method and device for preparing single crystals with specific crystal surfaces on surfaces Download PDFInfo
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- CN105127883A CN105127883A CN201510364164.7A CN201510364164A CN105127883A CN 105127883 A CN105127883 A CN 105127883A CN 201510364164 A CN201510364164 A CN 201510364164A CN 105127883 A CN105127883 A CN 105127883A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B41/00—Component parts such as frames, beds, carriages, headstocks
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B19/00—Single-purpose machines or devices for particular grinding operations not covered by any other main group
- B24B19/22—Single-purpose machines or devices for particular grinding operations not covered by any other main group characterised by a special design with respect to properties of the material of non-metallic articles to be ground
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Abstract
The invention relates to a device for determining and regulating and controlling space orientation of single crystals and a method for preparing single-crystal materials with specific crystal face orientation on the surfaces. The device comprises the single crystals, a connecting body of the single crystals, a base, a laser device, a pellicle mirror, a plane mirror and a reflection receiving screen. Laser irradiation is utilized for observing reflection signals of the single crystal materials from multiple directions so as to determine actual space orientation of the single crystals, and through regulation and the plasticity of the single crystals, the connecting body adjusts and changes the space orientation of the single crystals and the precise determining of the specific crystal faces, relative to the certain basic crystal face orientation, of the single crystals is achieved. Finally, through directional grinding polishing, the single-crystal materials with the target signal crystal faces can be obtained. The method is low in cost, easy to operate, high in precision and suitable for preparing the single-crystal materials with various crystal structures and shapes, and various basic crystal faces and ladder crystal faces of the materials. The method can be widely used for single-crystal material preparation of basic research, aerospace, chemical engineering, electron and other industries.
Description
Technical field
The invention belongs to monocrystal new high-tech material preparation field, relate to particularly a kind of can the method for spatial orientation of accuracy controlling monocrystal and a kind of device realizing the method by laser orientation, and utilize this regulate and control method to prepare the method on monocrystal particular crystal plane surface, especially prepare the method that surface is the monocrystal of high miller index surface.These apparatus and method can be widely used in the material preparation of basic research and electronics and chemical field.
Background technology
Surface has determines that the monocrystal material of high preferred orientation is the new high-tech material that a class is widely used in electronics, Aero-Space and chemical field, is also the cast material of the basic scientific researches such as material, physics, chemistry and catalysis.Controllably preparing the various monocrystal material with crystal face preferred orientation surface, the especially various material with specific high miller index surface surface, is the relevant high-quality device of preparation or the prerequisite of carrying out related basic research on model monocrystalline.
Under the prerequisite that the crossing crystal face of any two its indices of crystallographic plane known of the monocrystal of known crystal formation has been determined at the actual orientation in space, binding crystal is gained knowledge and to be calculated spatial relationship, is easy to the real space orientation of any particular crystal plane learning this monocrystal.In principle, as long as carry out cutting, grinding and polishing along determined actual orientation, just can obtain the monocrystal material that surface has particular crystal plane orientation.For the consideration of equipment, cost and operation ease, usually can carry out orientation to monocrystalline to be processed at Space Rotating special angle, to facilitate follow-up cutting, grinding and polishing.That at present carries out crystal plane orientation to this kind of material mainly utilizes X-ray diffraction, can realize the determination of the multiple high preferred orientation of the crystalline material of various structure in conjunction with angular displacement the method.But X-ray diffractometer apparatus expensive, complicated operation and need special protection in using, simultaneously due to the restriction of commercial angular displacement rotational angle, limits the preparation that some have the high miller index surface that important practical is worth.Another kind method utilizes laser reflection Directional Method, utilizes laser to irradiate the existing different crystal face of monocrystalline surface, and determine high preferred orientation by the angle rotating the skew of monocrystalline regulation and control reverberation, the method is easy, and cost is low.For the monocrystal material preparing some basic crystal face that monocrystalline surface has existed, the method is very easy.But to some crystal faces of the already present single facet of departure surface, especially some high miller index surfaces, early stage method often needs first to adjust crystal orientation, then cut, adjust the steps such as crystal orientation, again cutting more repeatedly repeats, and last acquisition could have the monocrystal of particular crystal plane.On the one hand, the method is very loaded down with trivial details in prepared by high miller index surface material, and on the other hand owing to relating to multi-step process, the error of a wherein small step all may cause the comparatively big error of final material orientation.The cutting process of multistep, multi-angle, causes on the one hand the loss of material all comparatively large, its use in precious metal material is limited to very much, also causes last prepared monocrystal much smaller than initial monocrystal on the other hand.There is the monocrystal of particular crystal plane orientation to preparation table mask, then require that the size of initial monocrystal can not be too little.And the preparation of the perfect monocrystal of bulk also has larger challenge at present.
How can on the basis of easy laser reflection Directional Method, high miller index surface can be adjusted to the method for desired position by development easily, and then development is for the preparation of various easy, economic, the easy-operating method with the single-crystal surface of high miller index surface, it is the focus that the scientific research personnel in new high-tech material Scientific Industries circle technology and basic research field pays close attention to always.
Summary of the invention
The present invention is directed to now methodical limitation, propose a kind of easy laser assisted carries out spatial orientation adjustment method to monocrystal, construct and a kind ofly can accurately determine the device with the high preferred orientation of regulating monocrystal body in very wide range, and developed the method for the monocrystal material that preparation surface is particular crystal plane on this basis.
The invention provides following technical scheme:
[1] regulate a method for the spatial orientation of monocrystal, the method for the spatial orientation of described adjustment monocrystal comprises the following steps:
(1) monocrystal with the surf zone that wherein there are at least two known crystal faces is prepared;
(2) being fixed on by described monocrystal via deformable connector can on the pedestal of Three dimensional rotation;
(3) make laser incide described surf zone, receiving screen records the position of the pip produced by the reflection of described known crystal face;
(4) turn to the spatial rotational amount needed for object space orientation by monocrystal described in the position calculation of described known crystal face, and described pedestal is rotated the spatial rotational amount with described required spatial rotational amount complementation;
(5) by making described connector be out of shape the position regulating described monocrystal, make laser again incide described surf zone, and the corresponding pip that described known crystal face is produced is in the position of record in step (2);
(6) original position is got back in described pedestal rotation.
[2] method Gen Ju [1], wherein, described at least two known crystal faces are basic crystal faces and around the symmetrical low index crystal plane of described basic crystal face.
[3] method Gen Ju [1], wherein, described monocrystal is face-centered cubic packing crystal, described at least two known crystal faces are (100) crystal faces and around symmetrical four (111) crystal faces of described (100) crystal face, and (100) crystal face described in described laser vertical incidence.
[4] according to the method according to any one of [1]-[3], wherein, in step (1), described monocrystal is formed by heating and melting recrystallization method.
[5] preparation method on the particular crystal plane surface of monocrystal, described preparation method comprises:
Adopt the method for the spatial orientation of the adjustment monocrystal Gen Ju [1], the particular crystal plane of monocrystal is adjusted in processing plane;
With non deformable medium, described monocrystal is fixed on described pedestal; And
In processing plane, carry out machined, obtain the particular crystal plane surface of monocrystal.
[6] preparation method Gen Ju [5], wherein said monocrystal is face-centered cubic packing crystal, and described particular crystal plane is selected from the group be made up of the following: the ladder crystal face [n (111) × (111)] with (111) platform (111) step; There is the ladder crystal face [n (100) × (111)] of (100) platform (111) step; There is the ladder crystal face of (100) platform and (110) step; There is the ladder crystal face of (111) platform and (111) and (100) step; And there is the crystal face of (100) platform and (111) and (100) ladder,
Wherein, in the method for the spatial orientation of described adjustment monocrystal according to claim 1, described at least two known crystal faces are (100) crystal faces and around symmetrical four (111) crystal faces of described (100) crystal face, described laser vertical is incident in described (100) crystal face, and in step (4), the spatial rotational of described pedestal is the rotation in the normal of (100) crystal face and the determined plane of normal of (111) crystal face, or around the incident axle rotation of laser and the combination at the determined Plane Rotation of described normal.
[7] regulate a device for the spatial orientation of monocrystal, described device comprises:
Can the pedestal of Three dimensional rotation;
Deformable connector, described deformable connector one end is fixed on described pedestal, and one end is connected with described monocrystal;
The lasing light emitter of Emission Lasers;
Light path regulator control system, the input path that the regulation and control of described light path regulator control system irradiate described monocrystal from the laser of described lasing light emitter and the reflected light path of laser reflected from described monocrystal at least partially;
Reflection receivable shields, and described reflection receivable screen receives the laser of reflection.
[8] device Gen Ju [7], wherein
Described deformable connector be can the wire of manual deformation, rubber bar or their combination.
[9] device Gen Ju [7], wherein
Described pedestal can rotate around trunnion axis and vertical axes respectively;
Described light path regulator control system comprises spectroscope and level crossing, described spectroscope by a part from the laser reflection of the horizontal direction of laser instrument to vertical direction, and make in the laser of vertically reflection at least partially through, described level crossing reflects through the reflects laser on described spectroscopical vertical direction to horizontal direction, and pip is formed on wall
Laser to tiltedly lower reflection forms pip in operating table surface.
Principle of the present invention is, under the prerequisite that the crystal face (being referred to herein as known crystal face) of any two crossing its indices of crystallographic plane known on the single-crystal surface of known crystal formation has been determined at the actual orientation in space, can gain knowledge to calculate and learn the orientation of any crystal face of monocrystal material at real space by binding crystal.Laser is utilized to irradiate and the reflected signal of multi-faceted observation monocrystal material described known crystal face on the surface, and the accurate control combined the pedestal of fixing monocrystal material and the plastic joining body of monocrystal material and modulation, the fine adjustment to monocrystalline high preferred orientation can be realized.Finally by machined as orientation polishing of milling obtains having the monocrystal material in aimed single crystal face.
The present invention utilizes simple optical substrate and plastic joining body, achieve the accuracy controlling of locus to monocrystal and orientation in conjunction with laser reflection method, providing a kind of simple, convenient, economic preparation table mask has the method for the monocrystal material of particular crystal plane orientation.
Beneficial effect of the present invention comprises:
1. assist orientation to reconcile method relative to conventional X-ray diffraction, with low cost, the simple to operate and safety of method of the present invention, without the need to special protection.Tradition monocrystalline orientation method is multiplex to X-ray diffraction, need the instrument of Large expensive and supporting annex, and method therefor of the present invention mainly uses lower powered laser and simple light path to realize.
2. relative to existing laser assisted orientation control method, method of the present invention can simple and quick by any specific crystal face at crystals particularly high miller index surface be adjusted to be easy to process position.This method adjusts repeatedly without the need to multistep, and precision is high, and material unaccounted-for (MUF) is little, does not need the initial single crystal of large volume.
3. the method orientation accuracy is high.The method mainly adjusts the error of angle from the optical bench placing monocrystalline to the error of single facet orientation, and the repetitive positioning accuracy of business-like optical bench can meet the requirement of single facet accurate pointing below 0.01 °.
4. the method is applied widely, may be used for any monocrystal in principle.Particularly, when surface easily can be prepared, and there is monocrystalline ball or the single crystal grain of symmetrical basic crystal face, the advantage that the method carries out the orientation of monocrystalline crystal face is more obvious, the various high miller index surfaces large relative to the basic crystal face anglec of rotation can be prepared easily, and particular/special requirement is not had to the kind of monocrystal material itself and character.
5. the method use low cost simple instrument condition under, for operating personnel provide very easily and fast, high-precision position adjustments means.The wire as connector may used in its preferred embodiment, rubber bar, as the resin of mounting medium, and use metope and operating desk etc. as receiving screen, be suitable for use in very much in such as general laboratory operation, and without the need to increasing special equipment and input.
6. the inventive method cost is low, simple to operate, precision is high, be applicable to having the monocrystal material of various crystal structure and shape, can be used for the various basic crystal face of these materials and the preparation of ladder crystal face.The monocrystal material preparation of the industries such as basic research, Aero-Space, chemical industry and electronics can be widely used in.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from the following description of the accompanying drawings of embodiments, wherein:
Fig. 1 is for the crystal of face-centered cubic packing, the interplanar spatial relation of various high-index surface and basis;
Fig. 2 is the flow chart of the method for first aspect present invention.
Fig. 3 is the flow chart of the method for second aspect present invention.
Fig. 4 be mention in the present invention can in space the pedestal of Three dimensional rotation.
Fig. 5 is for the device of laser reflection determination monocrystalline high preferred orientation and light path schematic diagram in the present invention;
Fig. 6 is the schematic diagram of the monocrystalline ball of the metal of the face-centered cubic packing prepared through flame melt method mentioned in the present invention;
Fig. 7 is the cyclic voltammetry curve according to prepared Pt [n (111) × (111)] the serial crystal face of one of embodiment of the present invention;
Fig. 8 is the x-ray diffraction spectra according to prepared Pt (331) (i.e. Pt [3 (111) × (111)]) face of one of embodiment of the present invention;
Fig. 9 is the cyclic voltammetry curve according to prepared Pt [n (100) × (111)] the serial crystal face of one of embodiment of the present invention;
Detailed description of the invention
In a first aspect of the present invention, the invention provides a kind of method of spatial orientation of accuracy controlling monocrystal, as shown in Figure 2, comprise the following steps:
(1) monocrystal with the surf zone that wherein there are at least two known crystal faces is prepared;
(2) being fixed on by described monocrystal via deformable connector can on the pedestal of Three dimensional rotation;
(3) make laser incide described surf zone, receiving screen records the position of the pip produced by the reflection of described known crystal face;
(4) turn to the spatial rotational amount needed for object space orientation by monocrystal described in the position calculation of described known crystal face, and described pedestal is rotated the spatial rotational amount with described required spatial rotational amount complementation;
(5) by making described connector be out of shape the position regulating described monocrystal, make laser again incide described surf zone, and the corresponding pip that described known crystal face is produced is in the position of record in step (2);
(6) original position is got back in described pedestal rotation.
In step (1), first prepare one block of monocrystal, it has the surf zone that wherein there are at least two known crystal faces.Known crystal face alleged herein refers to the crystal face of its indices of crystallographic plane known be positioned on monocrystalline surface, and laser reflection face is served as in its effect, for determining the position of monocrystal, and is the basis of the spatial rotational amount needed for subsequent calculations.Known crystal face can be the arbitrary surfaces crystal face of monocrystal raw material.To the special requirement of the size of described at least two known crystal faces, as long as form laser reflection point under they can be in the irradiation of same beam of laser (laser beam) on screen simultaneously clearly.In order to operational convenience, at least two known crystal faces preferably can by people's discernable by eye, rapidly surf zone is aimed at laser.Easy in order on operating and calculating, preferably one of them known crystal face and laser vertical, and be low index crystal plane, most preferably be basic crystal face ((100) face as in face-centered cubic packing crystal).Easy in order on operating and calculating, other crystal faces are also preferably low index crystal plane ((111) face as in face-centered cubic packing crystal).When selected crystal face is low index, calculate relation between crystal face and previously described amount of spin more convenient.Although only need two known crystal faces just can complete the present invention, preferably, use multiple known crystal face, especially organize known crystal face around symmetrical another of known crystal face, easy and simple to handle to make, location fast.Symmetrical laser reflection point can help to judge the direction with the basic crystal face of laser vertical more easily, makes the location of monocrystal and resets more accurate and convenient.Such as, particularly preferably be using (100) crystal face with around its four symmetrical (111) crystal face as described known crystal face in the monocrystal of face-centered cubic packing, thus the laser reflection point of four (111) crystal faces will be symmetric (will be explained below).The vertical extent of (100) crystal face and incident laser can be judged from its symmetrical degree, and make between connector deformation phases easier to monocrystal carry out reset regulate.
In step (1), described surf zone can be formed by any way, but preferably, adopts heating and melting recrystallization method to be formed.Heating and melting recrystallization method is simple, quick, is easy to obtain the surf zone comprising the known crystal face met the demands.Heating and melting recrystallization method is particularly preferred for precious metal material.The size of surf zone and the thickness of laser beam match.
In step (2), deformable connector can be out of shape the spatial correlation between monocrystal and pedestal is changed, and can keep the described spatial correlation after changing.In some embodiments, deformable connector is out of shape the spatial correlation between monocrystal and pedestal is changed under external force, and after removing external force, keep the described spatial correlation after changing.Preferably, described deformable connector is plastic joining body, its position and angle that monocrystal can be made to be positioned at want.In laboratory conditions, preferred deformable connector is rubber bar or fine wire.Rubber bar or fine wire can pass through manpower subtle curvatures and torsion neatly, thus regulate position and the orientation of monocrystal easily.
In step (2), described pedestal be any can the pedestal of spatial rotational.Preferably, pedestal is optical table, and its schematic diagram as shown in Figure 4.Its part B can be rotated around normally vertical incident light axis, and part A can around horizontal axis.Certainly, pedestal also can translation, so that regulate the position of crystal.
In step (3), receiving screen can be one or more, as long as it is fixing and accurately can shows laser reflection point.In a preferred embodiment of the invention, known crystal face be face-centered cubic packing crystal (100) crystal face and around its (111) crystal face.In this case, when laser is incident straight down, the reverberation of (111) crystal face will be penetrated oliquely downward, therefore, receiving screen can utilize operating desk desktop reception with graph paper from the reverberation of (111) crystal face in the lab, convenient and cost-saving.Can by the laser that reflects straight up through level crossing refraction directive horizontal direction, in the case, can with the metope in laboratory as receiving screen, be also convenient and cost-saving.
In step (4), described " complementary spatial rotational amount " is defined as follows: for two-dimensional rotary, if object makes monocrystal turn clockwise θ angle along trunnion axis, then first by pedestal counterclockwise along horizontal rotational shaft θ angle; Utilize the location of laser reflection point subsequently, monocrystal is accurately regulated back initial position, now monocrystal to have turned clockwise θ angle relative to base coordinate system; Finally make pedestal get back to original position, be then equivalent to monocrystal and turned clockwise θ angle relative to absolute coordinate space system.The situation of three dimensions change in orientation can be extended to from above example.Preferably, the change of three dimensions orientation can be decomposed into along two the suitable company's of being coupling twice two-dimensional rotaries.Required monocrystal spatial orientation variable quantity can be determined according to actual needs.Such as, Fig. 1, for the crystal of face-centered cubic packing, shows the interplanar spatial relation of various high-index surface and basis.Such as, in high miller index surface preparation method described later, namely required spatial orientation variable quantity is the variable quantity that this high miller index surface moves to needed for processing plane.Preferably, the spatial rotational of pedestal is the rotation in the plane that the normal of described known crystal face is determined, or rotates and the combination of rotation in the plane that the normal of described known crystal face is determined around the incident axle of laser.Pedestal amount of spin needed for those skilled in the art can calculate according to the initial orientation of crystal and target orientation.Preferably, it can be decomposed into around the incident axle rotation of laser and the rotation in the plane that the normal of described different crystal face is determined, thus has been rotated by two steps of pedestal.Particularly, when one of them crystal face is perpendicular to laser incident direction, the plane that the normal of it and another crystal face is determined is perpendicular (rotation namely in its plane is around horizontal axis), thus two such steps are rotated and can be completed by two rotating shaft optical tables of an energy around the incident axle of laser and horizontal axis.This is very convenient, fast and cost-saving.Preferably, the decomposition computation of described variable quantity is undertaken by computer simulation.
In step (5), make monocrystal get back to initial position, i.e. " reset ", the distortion by artificial regulatory connector has come.Preferably, under the environment in laboratory, can be come as the rubber bar of connector or fine wire by bending and distortion by operating personnel.By constantly regulating to aim at for the purpose of laser reflection point, monocrystal is finally made to reset.The precision resetted is guaranteed by the reset of laser spots.The spot diameter of laser reflection point is about 2-3 millimeter, and when the light path of light path is more than 2 meters, and during laser spots substantial registration (hot spot error is less than 10%), the error of monocrystal orientation is no more than 0.01 °.Therefore, the present invention with the equipment of unusual low cost and shirtsleeve operation, can realize high-precision orientation.
After step (6), monocrystal just reaches the spatial orientation of target.
The monocrystal be suitable in said method can be face-centered cubic packing crystal, and the metal or alloy material of preferred face-centered cubic packing, as Au, Ag, Au, Pt, Ir, Rh and Pd etc.In this case, more preferably, initial monocrystal has (100) face and four monocrystalline balls around described (100) face symmetrical (111) surface, face.Such monocrystalline ball can be obtained by multiple method, such as heating and melting recrystallization method.Heating and melting recrystallization method is: make it form drop in wire one end by the wire of inductance or flame melting target material, then the slow molten drop by melting takes out flame, now drop condensation from wire one end, carry out the growth of crystal with drop and wire contact place for nucleus, globule shape monocrystal in the process of drop cooling curing, will be formed.
According to a preferred embodiment of the invention, adopt the light path shown in Fig. 5, under above-mentioned monocrystalline ball is placed in vertical laser, adjustment (100) orientation vertically upward, now can obtain the point of (100) surface reflection laser on vertical metope, horizontal plane can obtain the point of 4 (111) surface reflection lasers simultaneously.Record the position of (100) and (111) face pip respectively.According to the result of calculation of Target space position, the angle that the rotation with in surface determined with the normal in (111) face in (100) by the base of fixing monocrystalline ball is certain, then rotates a certain angle in the horizontal direction.Then by making connector be out of shape, adjustment monocrystalline ball, makes the reflective spot of (111) on the reflective spot in (100) face on metope and horizontal plane get back to original position.Finally make the base of fixing monocrystalline ball recover the angle before rotating, now direction is vertically upward Target space position.Be in the method for the monocrystal of particular crystal plane on aftermentioned preparation surface, process along this steering wheel, such as grinding and polishing, corresponding single facet can be obtained.
Monocrystal also can be hexagonal closs packing monocrystal, is preferably the metal or alloy material of six side Mi Dui, as Ru etc.; Can be body centred cubic packing monocrystal, be preferably the metal or alloy material of body centred cubic packing, as Fe etc.; Also can be diamond closs packing monocrystal, be preferably the material of diamond Mi Dui, as diamond and SiC etc.Monocrystal also can be nonmetallic materials, as sapphire, magnesia, crystal, rutile and diamond etc.As long as the monocrystal with the surf zone of the known crystal face of two or more of these materials obtained, can use the method for laser auxiliary control monocrystal spatial orientation of the present invention in advance.Preferably, at least two known crystal faces are basic crystal faces and around the symmetrical low index crystal plane of described basic crystal face.The present invention is particularly suitable for the position of basic crystal face according to known and low index crystal plane, and the high miller index surface of monocrystal is adjusted to desirable position.Between a certain target high miller index surface and each basic crystal face, there is the angular relationship determined, utilize geometrical relationship from a certain base surface rotation monocrystal, direction of rotation can be decomposed in two special faces: the such as determined vertical plane of the normal vector of horizontal plane and two base surfaces.After twice rotation, the crystal orientation of target crystal face can be rotated on the crystal orientation of original a certain base surface.
In a second aspect of the present invention, provide a kind of preparation method of particular crystal plane surface of monocrystal, as shown in Figure 3, described method comprises:
Use the method that monocrystal spatial orientation is changed according to a first aspect of the present invention, make the described particular crystal plane of monocrystal be adjusted in processing plane,
With non deformable medium, described monocrystal is fixed on described pedestal,
In processing plane, carry out machined, obtain the particular crystal plane surface of monocrystal.
Described machine-tooled method is conventional machine-tooled method, is preferably cutting, grinding, polishing etc.Preferred orientation is milled polishing.When applying machined to monocrystal, monocrystal is stressed generally can cause deformable connector to be out of shape.Therefore, need via non deformable medium, monocrystal to be fixed before machined, make it during machined, keep its spatial orientation.Preferred non deformable medium is resin.Preferably, will it be made to solidify in the space of resin filling between monocrystalline and pedestal, make target process crystal face and to fix with the relative position of pedestal and also can bear enough machined loads.
Preferably, in the described method making monocrystal spatial orientation change, one in described two known crystal faces is basic crystal face, and described basic crystal face is perpendicular to laser incident direction, and described machined surface is also perpendicular to described laser incident direction.Like this, in order to reach the object of last processing, only target crystal face need be made to change to the direction of initial basis crystal face.This can simplify calculating and operation greatly.Further, as mentioned above, preferably other crystal faces are around described basic crystal face Rotational Symmetry distribution, are conducive to by symmetrical pip rapidly by crystal location and reset.
Preparation method of the present invention preferably prepares the particular crystal plane surface of the monocrystal of face-centered cubic packing crystal, six sides close heap crystal, body centred cubic packing crystal or the close heap crystal of diamond.More preferably, described monocrystal is face-centered cubic packing crystal, and described particular crystal plane is the crystal face with the crystal face of the crystal face of (111) platform (111) ladder, the crystal face of (100) platform (111) ladder, the crystal face of (111) platform (100) ladder, the crystal face of (100) platform (110) ladder, (111) platform and (111) and (100) ladder, (100) platform and (111) and (100) ladder.These crystal faces are all the high-index surfaces that surface energy is higher, and it may be formed at monocrystalline surface hardly naturally or by simple process.But they are extremely important again in basic scientific research.The preparation of these single-crystal surfaces early stage all carries out orientation by X-ray diffraction.And this preparation method is especially easier than prior art, quick, low cost, and keep very high precision.Preferably, in the process of the above-mentioned particular crystal plane of preparation, (100) face of use face-centered cubic crystal and four (111) faces around the distribution of described (100) face Rotational Symmetry are as reflecting surface.Now, the spatial rotational of pedestal is the rotation in the normal of (100) crystal face and the determined plane of normal of (111) crystal face, or around the incident axle rotation of laser and the combination at the determined Plane Rotation of described normal.Such selection provide especially easy under the condition of low cost, fast operation and sufficiently high precision.
In a third aspect of the present invention, provide a kind of device of spatial orientation of regulating monocrystal body, described device comprises:
Can the pedestal of Three dimensional rotation;
Deformable connector, described deformable connector one end is fixed on pedestal, and one end is connected with monocrystal, and described connector makes monocrystal may be in all spatial orientations substantially;
The lasing light emitter of Emission Lasers;
Light path regulator control system, the input path that the regulation and control of described light path regulator control system irradiate the surf zone of the known crystal face of existence at least two of described monocrystal from the laser of described lasing light emitter and the reflected light path of laser reflected from the surf zone of described monocrystal at least partially;
Reflection receivable shields, and described reflection receivable screen receives the laser of reflection, and preferred two or more reflection receivable receiving screen, receives the reverberation from the known crystal face of difference respectively.
Device of the present invention is applicable to the method described in first aspect present invention and second aspect, about its each several part detailed description can see of the present invention first and second in.The inventive system comprises optical path adjusting system.A kind of particularly preferred simple light path regulating system can see Fig. 5: it comprises spectroscope and level crossing, described spectroscope is to described monocrystal incident to vertical direction from the laser reflection of the horizontal direction of laser instrument by a part, and make in the laser of vertically reflection at least partially through, described level crossing reflects through the reflects laser on described spectroscopical vertical direction to horizontal direction, and is forming pip as on the vertical wall of receiving screen.
Described device can also comprise the automatic or Semi-automatic control system controlling described pedestal and rotate.Can also make described control system of computerizeing control, described computer can calculate the data of Crystal Rotation.Described device can also comprise the miscellaneous part being beneficial to the method realizing the present invention first and second aspect or structure that any those skilled in the art easily expect.
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings.Being exemplary below by the embodiment be described with reference to the drawings, only for explaining the present invention, and can not limitation of the present invention being interpreted as.
Embodiment 1
The orientation of Pt [n (111) × (111)] globule shape monocrystalline and preparation: Pt [n (111) × (111)] refer to the step surface of serving as reasons Pt surface (111) platform and (111) ladder forming, such as Pt (331) (i.e. Pt [3 (111) × (111)]) and Pt (332) (i.e. Pt [6 (111) × (111)]).By the Pt silk scorification crystallization of heating and melting recrystallization method by diameter 1mm, obtain the Pt monocrystalline bead that diameter is about about 2mm, first position relationship is as shown in Figure 6 found to be 4 (111) faces that square symmetry distributes on monocrystalline ball surface by visually observing, (100) face is had at the center in these 4 (111) faces, (100) face is due to very little, must examine and just can find.If do not find the basic crystal face of these self-assembling formations, can by monocrystalline ball again scorification and condensation-crystallization.
Be fixed on optical table by the other end of Pt silk, Pt silk serves as deformable connector (for saving Pt silk, a part for connector can utilize rubber bar) at this.Adopt light path as shown in Figure 5 and instrument, under monocrystalline ball is placed in laser (laser instrument uses the low-power laser of 5-15mW, and beam diameter is about 2mm).In order to make laser be radiated at above-mentioned surf zone, first a minute surface is placed on monocrystalline place, the position of reflective spot on record metope; Remove minute surface subsequently, then by manual adjustment as the Pt silk of connector or rubber bar, the position of adjustment monocrystal and direction, make to reflect back from the reverberation in (100) face along input path, reflective spot overlaps the position (hot spot error is no more than 10%) that metope records.Can use the position of the reflective spot in 4 (111) faces in this process as a reference, because when the position of (100) meets the demands, the reflective spot in 4 (111) faces should be just symmetrical.Then, on operating desk horizontal plane, find the reflective spot in four (111) faces respectively, mark their position as a reference.In order to obtain required step surface, by computer simulation, the spatial orientation variable quantity needed for calculated single crystal body.Result of calculation is as follows: regulate optical table to be rotated to an angle in horizontal plane by monocrystalline ball (be respectively 26.57 ° and 11.31 ° to the Pt (331) in the present embodiment and Pt (332)), the rotation with in surface certain angle then determined at (111) and (100) face normal (be respectively 46.51 ° and 50.24 ° to the Pt (331) in the present embodiment and Pt (332)).Now the position of each reflective spot changes.The position of manual adjustment monocrystal and direction make the position of each reflective spot get back to the position regulated before optical table again, reset to make monocrystalline ball.Along regulate before monocrystalline ball direction straight up carry out milling and polishing can obtain need single facet.
The step surface obtained is characterized.Fig. 7 is the electrochemistry cyclic voltammetry curve of Pt (331) (i.e. Pt [3 (111) × (111)]) in this serial crystal face and Pt (332) (i.e. Pt [6 (111) × (111)]), and its feature is consistent with the report in document.Fig. 8 is that the XRD of Pt (331) characterizes, and only from the signal of 331 crystal faces in collection of illustrative plates, illustrates that the single facet prepared according to this invention is accurately directed.
Embodiment 2
The orientation of Pt [n (100) × (111)] globule shape monocrystalline and preparation: Pt [n (100) × (111)] refer to the step surface of serving as reasons Pt surface (100) platform and (111) ladder forming.By the Pt silk scorification crystallization of heating and melting recrystallization method by diameter 1mm, obtain the Pt monocrystalline ball of about 2mm, by visually observing the surf zone that can find (100) face and four (111) faces symmetrical around this (100) face on monocrystalline ball surface.If do not find the basic crystal face of these self-assembling formations, can by monocrystalline ball again scorification and condensation-crystallization.
Be fixed on optical table by the other end of Pt silk, Pt silk serves as deformable connector (for saving Pt silk, a part for connector can utilize rubber bar) at this.Adopt light path as shown in Figure 5 and instrument, under monocrystalline ball is placed in laser (laser uses the low-power laser of 5-15mW, and beam diameter is about 2mm).In order to make laser be radiated at above-mentioned surf zone, first a minute surface is placed on monocrystalline place, the position of reflective spot on record metope; Remove minute surface subsequently, then by manual adjustment as the Pt silk of connector or rubber bar, the position of adjustment monocrystal and direction, make to reflect back from the reverberation in (100) face along input path, reflective spot overlaps the position (hot spot error is no more than 10%) that metope records.Can use the position of the reflective spot in 4 (111) faces in this process as a reference, because when the position of (100) meets the demands, the reflective spot in 4 (111) faces should be just symmetrical.Then, on operating desk horizontal plane, find the reflective spot in four (111) faces respectively, mark their position as a reference.In order to obtain required step surface, by computer simulation, the spatial orientation variable quantity needed for calculated single crystal body.Result of calculation is as follows: regulate rotation with in surface certain angle that monocrystalline ball is determined at (111) and (100) face normal by optical table (to Pt (100), Pt (19 in the present embodiment, 1,1), Pt (15,1,1), Pt (711) and Pt (511) is 0 ° respectively, 4.26 °, 5.41 °, 11.65 ° and 16.43 °).Now the position of each reflective spot changes.The position of manual adjustment monocrystal and direction make the position of each reflective spot get back to the position regulated before optical table again, reset to make monocrystalline ball.Along regulate before monocrystalline ball direction straight up carry out milling and polishing can obtain need single facet.
The step surface obtained is characterized.Fig. 9 is the electrochemistry cyclic voltammetry curve of this serial crystal face, and its feature is consistent with bibliographical information, can be widely used in the scientific research in the field such as catalysis, electro-catalysis.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (9)
1. regulate a method for the spatial orientation of monocrystal, the method for the spatial orientation of described adjustment monocrystal comprises the following steps:
(1) monocrystal with the surf zone that wherein there are at least two known crystal faces is prepared;
(2) being fixed on by described monocrystal via deformable connector can on the pedestal of Three dimensional rotation;
(3) make laser incide described surf zone, receiving screen records the position of the pip produced by the reflection of described known crystal face;
(4) turn to the spatial rotational amount needed for object space orientation by monocrystal described in the position calculation of described known crystal face, and described pedestal is rotated the spatial rotational amount with described required spatial rotational amount complementation;
(5) by making described connector be out of shape the position regulating described monocrystal, make laser again incide described surf zone, and the corresponding pip that described known crystal face is produced is in the position of record in step (2);
(6) original position is got back in described pedestal rotation.
2. method according to claim 1, wherein, described at least two known crystal faces are basic crystal faces and around the symmetrical low index crystal plane of described basic crystal face.
3. method according to claim 2, wherein, described monocrystal is face-centered cubic packing crystal, described at least two known crystal faces are (100) crystal faces and around symmetrical four (111) crystal faces of described (100) crystal face, and (100) crystal face described in described laser vertical incidence.
4. the method according to any one of claim 1-3, wherein, in step (1), described monocrystal is formed by heating and melting recrystallization method.
5. the preparation method on the particular crystal plane surface of monocrystal, described preparation method comprises:
Adopt the method for the spatial orientation of adjustment monocrystal according to claim 1, the particular crystal plane of monocrystal is adjusted in processing plane;
With non deformable medium, described monocrystal is fixed on described pedestal; And
In processing plane, carry out machined, obtain the particular crystal plane surface of monocrystal.
6. preparation method according to claim 5, wherein said monocrystal is face-centered cubic packing crystal, and described particular crystal plane is selected from the group be made up of the following: the ladder crystal face [n (111) × (111)] with (111) platform (111) step; There is the ladder crystal face [n (100) × (111)] of (100) platform (111) step; There is the ladder crystal face of (100) platform and (110) step; There is the ladder crystal face of (111) platform and (111) and (100) step; And there is the crystal face of (100) platform and (111) and (100) ladder,
Wherein, in the method for the spatial orientation of described adjustment monocrystal according to claim 1, described at least two known crystal faces are (100) crystal faces and around symmetrical four (111) crystal faces of described (100) crystal face, described laser vertical is incident in described (100) crystal face, and in step (4), the spatial rotational of described pedestal is the rotation in the normal of (100) crystal face and the determined plane of normal of (111) crystal face, or around the incident axle rotation of laser and the combination at the determined Plane Rotation of described normal.
7. regulate a device for the spatial orientation of monocrystal, described device comprises:
Can the pedestal of Three dimensional rotation;
Deformable connector, described deformable connector one end is fixed on described pedestal, and one end is connected with described monocrystal;
The lasing light emitter of Emission Lasers;
Light path regulator control system, the input path that the regulation and control of described light path regulator control system irradiate described monocrystal from the laser of described lasing light emitter and the reflected light path of laser reflected from described monocrystal at least partially;
Reflection receivable shields, and described reflection receivable screen receives the laser of reflection.
8. device according to claim 7, wherein
Described deformable connector be can the wire of manual deformation, rubber bar or their combination.
9. device according to claim 7, wherein
Described pedestal can rotate around trunnion axis and vertical axes respectively;
Described light path regulator control system comprises spectroscope and level crossing, described spectroscope by a part from the laser reflection of the horizontal direction of laser instrument to vertical direction, and make in the laser of vertically reflection at least partially through, described level crossing reflects through the reflects laser on described spectroscopical vertical direction to horizontal direction, and pip is formed on wall, the laser to tiltedly lower reflection forms pip in operating table surface.
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