CN104746127B - Double-cell device for preparing porous silicon by electrochemical method and method for preparing porous silicon - Google Patents
Double-cell device for preparing porous silicon by electrochemical method and method for preparing porous silicon Download PDFInfo
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- CN104746127B CN104746127B CN201510099634.1A CN201510099634A CN104746127B CN 104746127 B CN104746127 B CN 104746127B CN 201510099634 A CN201510099634 A CN 201510099634A CN 104746127 B CN104746127 B CN 104746127B
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Abstract
Aiming at the defects of porous silicon on SOI (Silicon on Insulator) wafers, the invention provides a double-cell device for preparing porous silicon by an electrochemical method and a method for preparing porous silicon. The double-cell device comprises an outer cell body, an inner cell body, a lower-layer gasket, an upper-layer gasket, cell body bolts, nuts and gasket bolts. The method comprises four steps, namely wafer preparation, wafer arrangement, device mounting and electrochemical corrosion. The device and the method provided by the invention have the beneficial effects as follows: the device and the method can be used exclusively for preparing porous silicon on SOI wafers and can also be used for preparing porous silicon on common wafers; and the shape of porous silicon prepared by the device and the method is controllable.
Description
Technical field
The invention belongs to a kind of technical field of semiconductor preparation, and in particular to for the double flute of porous silicon preparing electrochemical process
Device and the method for preparing porous silicon.
Background technology
SOI（Silicon on Insulator, the silicon in dielectric substrate）Technology is drawn between top layer silicon and backing bottom
One layer of buries oxide layer is entered.Manufacture its technique of soi structure device is different with tradition bulk silicon technological, and it is that in silicon substrate and actually have
It is embedded into one layer of SiO between effect silicon layer2Insulating barrier, manufacture using this insulating barrier as substrate transistor and using medium of oxides every
All of components and parts on off-chip piece, the technology can realize the bipolar, CMOS of compatibility and high pressure DMOS devices on a chips.Therefore
SOI materials are provided with the incomparable advantage of body silicon：The medium isolation of components and parts in integrated circuit can be realized, is thoroughly eliminated
Parasitic latch-up in Bulk CMOS circuit；Using integrated circuit made by this material also have parasitic capacitance it is little, collection
Into density it is high, speed is fast, process is simple, short-channel effect is little and is particularly well-suited to the advantages such as low voltage and low power circuits, therefore can
To say that SOI would be possible to become the low pressure of deep-submicron, the mainstream technology of low power consumption integrated circuit.
With developing rapidly for SOI technology, also obtained rapidly based on the related device of SOI substrate, interleaving techniques field
Development.Nano-structure porous silicon technical field for example in combination with SOI technology：Because nano-structure porous silicon is superior bio material, such as
Nanoporous silicon optical waveguide or photonic crystal can be prepared on SOI materials, then can prepare highly sensitive photo bio sensing
Device, becomes one of approach of Future Development biosensor array chip.While microelectromechanical systems（Micro Electro
Mechanical System, MEMS) technology progressively becomes interdisciplinary research in new high-tech field, defines including various micro- electricity
The micro-system of son, micromechanics, micro-optic and various data processing units, wherein the silicon substrate based on integrated circuit processing technology
Micro-processing technology quickly grows.And on the basis of microelectronics manufacture, the MEMS processing technique of silicon microstructure absorbs and merges it
His processing technique realizes various micro mechanical structures, using sensor on the SOI of MEMS technology development of new, performance is more excellent,
Stability is more preferable, reliability is higher.Porous silicon becomes the brand-new material in MEMS with its premium properties, in MEMS functional structures
The unrivaled advantage of other materials is embodied in the making of layer and sacrifice layer, good gas-sensitive property is possible with for MEMS
The fine vacuum encapsulation of the milli/microtorr magnitude such as pressure transducer, MEMS inertial sensor and MEMS oscillator.
At present the preparation method of porous silicon mainly has electrochemical erosion method, chemical corrosion method, spark erosion method, hydro-thermal corrosion
Method.Electrochemical erosion method therein is also referred to as anodic attack method, is to prepare a kind of the most frequently used method of porous silicon at present.Electrochemistry
Etch prepares the ultimate principle of porous silicon：In HF acid solutions, the silicon dangling bond on surface can be passivated by H, formed Si -- H bond or
Si-H2Key, in anode oxidation process, the positive potential of applying provides a large amount of holes for Si matrixes, and the F- in electrolyte is in silicon
Si -- H bond is bombarded with the help of matrix hole, Si -- H bond fracture F displaces a H, while discharging an electronics.Lose a H
Afterwards, another H on silicon is unstable, replaces and discharge an electronics by F then, and two for being displaced H constitutes a H2
Lose the silicon after H to be dissolved by HF, produce SiF4, then generate H with HF reactions2SiF6.Electrochemical erosion method according to electrolysis bath knot
Structure is divided into：Single cavity electrochemical erosion method, double-cell electrochemical etching, it is specific as follows：
Single cavity electrochemical corrosion is to do anode, platinized platinum using silicon chip（Pt) or graphite be negative electrode, HF acid with organic solvent
Or the mixed electrolytic solution Anodic Oxidation of inorganic solvent forms porous silicon.Prepare in porous silicon in single cavity electrochemical erosion method, be
Silicon chip is set to form good Ohmic contact with metal clip, traditional way is to be deposited with one layer of gold in the non-burnishing surface of silicon chip in advance
Category layer（Al the part Electroless Plating Ni for) or in silicon chip contacting with metal clip, which increases the cost and difficulty of experiment, also can be right
Silicon chip is polluted with damaging, and easily causes the modified of silicon chip, and repeatability is low.Meanwhile, thickness of metal film uniformity is not easily-controllable
System, is easily caused porous silicon aperture size, porosity and porous silicon layer thickness uneven.
The anode and negative electrode of double-cell electrochemical etching is all platinized platinum（Pt）Or graphite electrode, silicon chip is fixed on electrolysis bath
Centre, electrolysis bath is separated into not connected independent half grooves of two solution, silicon wafer polishing facing to negative electrode, non-burnishing surface pair
Anode, is switched on power, electric current flows to another half groove from one and half grooves through silicon chip, against the burnishing surface anodic solution of negative electrode
Form porous silicon.Prepare in porous silicon in double flute electrochemical corrosion, because silicon chip need not form Ohmic contact without the need in silicon
The non-burnishing surface evaporating Al electrode of piece, so reducing experimental cost and operation difficulty.Simultaneously double-cell electrochemical etching is relative
Evenly, hole is more dense for the porous silicon surface pattern prepared in single cavity electrochemical erosion method, with better performance, therefore
Become the method for currently preparing porous silicon most main flow.
But the dual bath apparatus of traditional porous silicon preparing electrochemical process are fixed on silicon wafer clamping between double flute, right respectively
Two electrolysis baths switch on power, and electric current forms loop so as to carry out electrochemical corrosion perpendicular through silicon chip, and soi wafer is special
Insulating oxide in structure can block electric current, so the dual bath apparatus of traditional porous silicon preparing electrochemical process cannot be in SOI
Porous silicon is prepared on silicon chip, prepared by the porous silicon for being merely capable of meeting on common silicon chip.If added to traditional electrochemical corrosion
Work technique and device are improved, and can just expand the preparation method of porous silicon, moreover it is possible to control the various structures of porous silicon well
Parameter.Such as, Chinese patent 201310332854.5 describes a kind of method that selectivity prepares porous silicon on new SOI silicon,
The method is corroded the bottom silicon on soi wafer for the first time using the preparation that porous silicon is carried out after corroding twice on soi wafer
A groove is etched, the insulating barrier exposed in groove is corroded for the second time, then using electrochemical etching method in groove correspondence
Upper layer of silicon on prepare porous silicon.But such preparation method process is loaded down with trivial details, need first to carry out a dry etching and one
Secondary wet etching carries out again electrochemical corrosion and prepares porous silicon, during easily structure is caused to damage and destroyed, technology difficulty
It is larger.
In sum, a kind of dual bath apparatus of new porous silicon preparing electrochemical process are designed so as to both can realize general
The controllable standby of porous silicon on logical silicon chip, can more meet the needs of technology development, complete on SOI silicon the controllable of porous silicon
Getting everything ready has very great value.
The content of the invention
For above-mentioned deficiency of the existing electrochemical erosion method on soi wafer is prepared on porous silicon, the present invention provides a kind of
Dual bath apparatus for porous silicon preparing electrochemical process and the method for preparing porous silicon.The device can both be exclusively used in soi wafer
The preparation of upper porous silicon, it is also possible to realize the preparation of porous silicon on common silicon chip, and controlled shape prepared by porous silicon.This
The technical process that bright realization prepares porous silicon is simple, and obtained porous silicon aperture size, porosity and porous silicon thickness are uniform.This
Invention is adopted the technical scheme that：
For the dual bath apparatus of porous silicon preparing electrochemical process, including outer cell body 1, interior cell body 2, lower floor's packing ring, upper strata pad
Circle 4, cell body bolt 5, nut 6 and packing ring bolt 7.
The outer cell body 1 is open-topped hollow container.The groove of more than 4 is provided with the cavity bottom surface of outer cell body 1
Body bolt 5.The cell body bolt 5 is vertically connected with the cavity bottom surface of outer cell body 1, and equal at the middle part of each cell body bolt 5
It is provided with the limited block of annular.
Lower floor's packing ring has 2 for discoideus, wherein 1 lower floor's packing ring is provided with lower floor's packing ring corrosion window, claims
To there is packing ring corrosion window lower floor of lower floor packing ring 31, lower floor's packing ring corrosion window is not provided with another 1 lower floor's packing ring, referred to as without under
Layer packing ring corrosion window lower floor packing ring 32.
In each of the lower the edge of layer packing ring is provided with the lower floor packing ring side channel body bolt positioning hole corresponding with cell body bolt 5.
In each of the lower the edge of the top surface of layer packing ring is provided with the packing ring bolt 7 of more than 4.The packing ring bolt 7 with lower floor packing ring
Top surface vertically connects.In each of the lower the edge of layer packing ring is provided with the mounting hole of more than 1.
The upper strata packing ring 4 is in discoideus.The upper strata packing ring corrosion window of more than 1 is provided with the middle part of upper strata packing ring 4.
On upper strata, the edge of packing ring 4 is provided with the upper strata packing ring side channel body bolt positioning hole corresponding with cell body bolt 5, the packing ring 4 on upper strata
Edge be additionally provided with the upper strata packing ring side packing ring bolt positioning hole corresponding with packing ring bolt 7.On upper strata, the edge of packing ring 4 sets
There is the mounting hole of more than 1.
The interior cell body 2 is the cylindrical body of upper and lower opening.The base for horizontally outward extending is provided with the bottom of interior cell body 2.
The base is identical with the quantity of cell body bolt 5, and one is provided with each base of interior cell body 2 with the phase of cell body bolt 5
Corresponding inside groove side cell body bolt positioning hole.
When making the upper porous silicon layer of soi wafer with this dual bath apparatus, upper strata packing ring 4 is enclosed within and corrodes window without underlay ring layer
On the packing ring bolt 7 of lower floor's packing ring 32 of mouth, by the nut 6 for screwing the top of packing ring bolt 7, by upper strata packing ring 4 and without lower floor
Packing ring corrosion window lower floor packing ring 32 links together.To link together without the He of packing ring corrosion window lower floor of lower floor packing ring 32
Upper strata packing ring 4 is enclosed within the annular stop block of cell body bolt 5.Interior cell body 2 is enclosed within cell body bolt 5 again, and screws cell body spiral shell
The nut 6 at the top of bolt 5, so as to by interior cell body 2, upper strata packing ring 4, without packing ring corrosion window lower floor of lower floor packing ring 32 and outer cell body 1
Link together.
When making the upper porous silicon layer of non-soi wafer with this dual bath apparatus, upper strata packing ring 4 corrosion of underlay ring layer is enclosed within into
On the packing ring bolt 7 of lower floor's packing ring 31 of window, by the nut 6 for screwing the top of packing ring bolt 7, so as to by the He of upper strata packing ring 4
There is packing ring corrosion window lower floor of lower floor packing ring 31 to link together.There is packing ring corrosion window lower floor of lower floor pad by what is linked together
Circle 31 and upper strata packing ring 4 are enclosed within the annular stop block of cell body bolt 5.Interior cell body 2 is enclosed within cell body bolt 5 again, and is screwed
The nut 6 at the top of cell body bolt 5, so as to by interior cell body 2, upper strata packing ring 4, have packing ring corrosion window lower floor of lower floor packing ring 31 with
Outer cell body 1 links together.
The dual bath apparatus method that selectivity prepares porous silicon on SOI silicon provided using the present invention, is entered as follows
OK：
Step 1. is for piece：Soi wafer is chosen, and is cleaned by ultrasonic, subsequently under nitrogen protection dehydration is bakeed；
Step 2. silicon chip is disposed：Soi wafer is placed in it is central without packing ring corrosion window lower floor of lower floor packing ring 32, need to
The SOI silicon for preparing porous silicon faces up, and upper strata packing ring 4 is enclosed within into the packing ring of the lower floor's packing ring 32 without underlay ring layer corrosion window
On bolt 7, then linked together by upper strata packing ring 4 and without packing ring corrosion window lower floor of lower floor packing ring 32 by nut 6；
Step 3. device is installed：To link together without packing ring corrosion window lower floor of lower floor packing ring 32 and upper strata packing ring 4
It is enclosed within the annular stop block of cell body bolt 5 subsequently, by interior cell body 2, upper strata packing ring 4, without packing ring corrosion window lower floor of lower floor pad
Circle 32 links together with outer cell body 1；
Step 4. electrochemical corrosion：Inwardly injection mol ratio is 1 in cell body 2:2 HF/C2H5OH corrodes electrolyte,；Outwards
The injection mol ratio of cell body 1 is 1:2 HF/C2H5OH corrodes electrolyte or NaCl electrolyte；One graphite electrode is inserted into water jacket
In electrolyte in body 1, and connect power anode；Another graphite electrode is inserted in the electrolyte in interior cell body 2, and is connected
Power cathode, is 30mA/cm with after-applied electric current density2Unidirectional current, corrosion 30min to 40min；Finally take out after corrosion
Soi wafer, obtains finished product.
The dual bath apparatus method that selectivity prepares porous silicon on non-SOI silicon provided using the present invention, as follows
Carry out：
Step 1. is for piece：The silicon chip of one piece of 4 inches of twin polishing is chosen, scribing obtains the silicon chip after 4 pieces of cuttings, described to cut
The size of the silicon chip after cutting is the square of 1.5cm；Respectively the silicon chip after aforementioned cutting is entered with acetone soln and dehydrated alcohol
Row is cleaned by ultrasonic；Subsequently by the silicon chip after ultrasonic cleaning under nitrogen protection, on the hot plate of 150 DEG C of temperature dehydration bakee 1min；
Step 2. silicon chip is disposed：Obtained by step 14 pieces of silicon chips for cleaning and bakeing lower floor's pad has been placed in into respectively
On 4 corrosion windows of circle corrosion window lower floor packing ring 31, upper strata packing ring 4 is enclosed within into lower floor's pad of underlay ring layer corrosion window
On the packing ring bolt 7 of circle 31, upper strata packing ring 4 and there will be packing ring corrosion window lower floor of lower floor packing ring 31 to link together；
Step 3. device is installed：There are packing ring corrosion window lower floor of lower floor packing ring 31 and upper strata packing ring 4 by what is linked together
It is enclosed within the annular stop block of cell body bolt 5；Interior cell body 2 is enclosed within cell body bolt, by interior cell body 2, upper strata packing ring 4, under having
Layer packing ring corrosion window lower floor packing ring 31 links together with outer cell body 1.
Step 4. electrochemical corrosion：Inwardly injection mol ratio is 1 in cell body 2:2 HF/C2H5OH corrodes electrolyte；Outwards
The injection mol ratio of cell body 1 is 1:2 HF/C2H5OH corrodes electrolyte or NaCl electrolyte；One graphite electrode electrode is inserted
In the electrolyte of outer cell body 1, and connect power anode, another graphite electrode electrode inserted in the electrolyte in interior cell body 2,
And connect power cathode, it is 20mA/cm with after-applied electric current density2Unidirectional current, and etching time 20min to 30min, finally
Obtain finished product.
The solution have the advantages that：
The present invention has simple structure, easy to operate, the characteristics of safe.Ordinary silicon can both have been met using the present invention
The preparation of porous silicon on piece, it is also possible to meet the preparation of porous silicon on SOI, while by the selection to packing ring, can prepare not
The porous silicon of similar shape or while prepare the porous silicon of multiple shapes, such as rounded porous silicon, rectangular cellular silicon, rectangular cellular silicon
Array, full wafer porous silicon, realize that a groove is multiplex.Safe, good sealing effect of the invention, mounts and separates device very convenient
Simply.
Description of the drawings
Fig. 1 is the top view of the present invention.
Fig. 2 is the schematic perspective view of Fig. 1.
Fig. 3 is the schematic perspective view of Fig. 1 China and foreign countries cell body 1 and its upper groove body bolt 5.
The schematic perspective view of lower floor's packing ring 31 of Tu4Shi You lower floors packing ring corrosion window.
Fig. 5 is that the solid of the upper strata packing ring 4 that the lower floor's packing ring 31 for being shown with lower floor's packing ring corrosion window with Fig. 4 matches is shown
It is intended to.
Fig. 6 is the three-dimensional signal of the interior cell body 2 that the lower floor's packing ring 31 for being shown with lower floor's packing ring corrosion window with Fig. 4 matches
Figure.
Fig. 7 is the schematic perspective view of the lower floor's packing ring 32 without lower floor's packing ring corrosion window.
Fig. 8 is that the solid of the upper strata packing ring 4 matched with the lower floor's packing ring 32 without lower floor's packing ring corrosion window shown in Fig. 7 is shown
It is intended to.
Fig. 9 is the top view of the interior cell body 2 matched with the lower floor's packing ring 32 without lower floor's packing ring corrosion window shown in Fig. 7.
Figure 10 be lower floor's packing ring corrosion window and upper strata packing ring corrosion window be circle have lower floor's packing ring corrosion window
Lower floor's packing ring 31 and the upper strata packing ring 4 for matching schematic perspective view.
Figure 11 corrodes window for the lower floor's packing ring that has that lower floor's packing ring corrosion window and upper strata packing ring corrosion window are quasi-circular
Lower floor's packing ring 31 of mouth and the schematic perspective view of the upper strata packing ring 4 for matching.
Figure 12 is having for the rectangular array of reserved scribe line for lower floor's packing ring corrosion window and upper strata packing ring corrosion window
The schematic perspective view of lower floor's packing ring 31 of lower floor's packing ring corrosion window and the upper strata packing ring 4 for matching.
Figure 13 is the A-A sectional views of Fig. 1.
Specific embodiment
The present invention is described in detail below in conjunction with the accompanying drawings：
Referring to Fig. 1, for the dual bath apparatus of porous silicon preparing electrochemical process, including outer cell body 1, interior cell body 2, lower floor's pad
Circle, upper strata packing ring 4, cell body bolt 5, nut 6, packing ring bolt 7, as shown in Figure 2.
Referring to Fig. 3, the outer cell body 1 is open-topped hollow container.4 are provided with the cavity bottom surface of outer cell body 1
Cell body bolt 5 above.The cell body bolt 5 is vertically connected with the cavity bottom surface of outer cell body 1, and in each cell body bolt 5
Middle part be equipped with annular limited block.
Lower floor's packing ring has 2 for discoideus, wherein 1 lower floor's packing ring is provided with lower floor's packing ring corrosion window, claims
For the lower floor's packing ring 31 for having lower floor's packing ring corrosion window, as shown in Figure 4.Lower floor's packing ring corrosion is not provided with another 1 lower floor's packing ring
Window, referred to as without packing ring corrosion window lower floor of lower floor packing ring 32, as shown in Figure 7.
In each of the lower the edge of layer packing ring is provided with the lower floor packing ring side channel body bolt positioning hole corresponding with cell body bolt 5.
In each of the lower the edge of the top surface of layer packing ring is provided with the packing ring bolt 7 of more than 4.The packing ring bolt 7 with lower floor packing ring
Top surface vertically connects.In each of the lower the edge of layer packing ring is provided with the mounting hole of more than 1.
The upper strata packing ring 4 is in discoideus.The upper strata packing ring corrosion window of more than 1 is provided with the middle part of upper strata packing ring 4,
Referring to Fig. 5 or Fig. 8.On upper strata, the edge of packing ring 4 is provided with the upper strata packing ring side channel body bolt positioning corresponding with cell body bolt 5
Hole, on upper strata, the edge of packing ring 4 is additionally provided with the upper strata packing ring side packing ring bolt positioning hole corresponding with packing ring bolt 7.On upper strata
The edge of packing ring 4 is provided with the mounting hole of more than 1.
Referring to Fig. 6 or Fig. 9, the interior cell body 2 is the cylindrical body of upper and lower opening.The bottom of interior cell body 2 be provided with level to
The base of outer extension.The base is identical with the quantity of cell body bolt 5, and one is provided with each base with cell body bolt
5 corresponding inside groove side cell body bolt positioning holes.
When making the upper porous silicon layer of soi wafer with this dual bath apparatus, soi wafer is placed in without lower floor's packing ring corrosion window
The middle position of mouthful lower floor packing ring 32, and the silicon for needing the soi wafer for preparing porous silicon is faced up after placement, it is ensured that the SOI silicon
Piece can be completely covered the corrosion window of upper strata packing ring 4, will by upper strata packing ring side packing ring bolt positioning hole corresponding with packing ring bolt 7
Upper strata packing ring 4 is enclosed within the packing ring bolt 7 of the lower floor's packing ring 32 without underlay ring layer corrosion window, the top of the packing ring bolt 7
It is furnished with nut 6, so as to link together by upper strata packing ring 4 and without packing ring corrosion window lower floor of lower floor packing ring 32.By with cell body
The corresponding lower floor's packing ring side packing ring bolt positioning hole of bolt 5 upper strata packing ring bolt positioning hole corresponding with cell body bolt 5 will connect
Being enclosed within the annular stop block of cell body bolt 5 without packing ring corrosion window lower floor of lower floor packing ring 32 and upper strata packing ring 4 together.It is logical
Cross inside groove side cell body bolt positioning hole interior cell body 2 is enclosed within cell body bolt, the top of the cell body bolt 5 is furnished with nut 6
, so as to link together with outer cell body 1 by interior cell body 2, upper strata packing ring 4, without packing ring corrosion window lower floor of lower floor packing ring 32.
Referring to Figure 13, when making the upper porous silicon layer of non-soi wafer with this dual bath apparatus, silicon chip silicon chip is placed in down
On the corrosion window of layer packing ring corrosion window lower floor packing ring 31, and silicon chip is completely covered with lower floor's packing ring corrosion window
The corrosion window of layer packing ring 31, by upper strata packing ring side corresponding with packing ring bolt 7 packing ring bolt positioning hole by 4 sets of upper strata packing ring
On the packing ring bolt 7 of the lower floor's packing ring 31 for having underlay ring layer corrosion window, the top of the packing ring bolt 7 is furnished with nut 6, from
And by upper strata packing ring 4 and have packing ring corrosion window lower floor of lower floor packing ring 31 to link together.Under corresponding with cell body bolt 5
Under the having that packing ring bolt positioning hole upper strata packing ring bolt positioning hole corresponding with cell body bolt 5 in layer packing ring side will link together
Layer packing ring corrosion window lower floor packing ring 31 and upper strata packing ring 4 are enclosed within the annular stop block of cell body bolt 5.By inside groove side groove
Body bolt positioning hole is enclosed within interior cell body 2 on cell body bolt, and the top of the cell body bolt 5 is furnished with nut 6, so as to by inside groove
Body 2, upper strata packing ring 4, there is packing ring corrosion window lower floor of lower floor packing ring 31 to link together with outer cell body 1.
Furtherly, 4 cell body bolts 5 are evenly equipped with the cavity bottom surface of outer cell body 1, Fig. 3 is referred to.
Referring to Fig. 7, at the edge of the lower floor's packing ring 32 without lower floor's packing ring corrosion window the mounting hole of 2 is provided with.Under nothing
The top surface of lower floor's packing ring 32 of layer packing ring corrosion window is evenly equipped with 4 packing ring bolts 7.
Referring to Fig. 8,1 upper strata packing ring corrosion window is provided with packing ring 4 on upper strata, the upper strata packing ring corrosion window is in circle
Shape.1 square frame 41 is provided with the packing ring corrosion window of upper strata, by elongated upper strata packing ring linking arm 42 by square frame 41
A pair of outer walls link together with the inwall of adjacent upper strata packing ring corrosion window.On upper strata, the edge of packing ring 4 is provided with the waist of 2
Shape hole.
Referring to Fig. 9, the interior cell body 2 is hollow and upper and lower opening cuboid.In the bottom of 1 side wall of interior cell body 2
It is respectively equipped with 1 base for horizontally outward extending.1 interior cell body corresponding with cell body bolt 5 is provided with each base
Side channel body bolt positioning hole.
The material of lower floor's packing ring 32, upper strata packing ring 4 and interior cell body 2 without lower floor's packing ring corrosion window is polytetrafluoroethyl-ne
Alkene.Furtherly, 4 cell body bolts 5 are evenly equipped with the cavity bottom surface of outer cell body 1, Fig. 3 is referred to.
Referring to Fig. 4, at the edge of the lower floor's packing ring 31 for having lower floor's packing ring corrosion window the mounting hole of 2 is provided with.In the case where having
The top surface of lower floor's packing ring 31 of layer packing ring corrosion window is evenly equipped with 4 packing ring bolts 7.There is lower floor's pad of lower floor's packing ring corrosion window
Circle 31 is provided with lower floor's packing ring corrosion window of more than 1.
Referring to Fig. 5, the upper strata packing ring corrosion window corresponding with lower floor packing ring corrosion window is provided with packing ring 4 on upper strata.
On upper strata, the edge of packing ring 4 is provided with the mounting hole of 2.
Referring to Fig. 6, the interior cell body 2 is hollow and upper and lower opening pipe.It is uniform in the outside of the bottom port of interior cell body 2
There are 4 bases for horizontally outward extending.1 inside groove side cell body corresponding with cell body bolt 5 is provided with each base
Bolt positioning hole.
The material for having lower floor's packing ring 31, upper strata packing ring 4 and interior cell body 2 of lower floor's packing ring corrosion window is politef
Material.Referring to Fig. 4, furtherly, having on packing ring corrosion window lower floor of lower floor packing ring 31 4 lower floor's packing ring corrosion windows are provided with
Mouthful.Lower floor's packing ring corrosion window is square, and by 2 × 2 array arrangement.4 upper strata packing rings are provided with upper strata in packing ring 4
Corrosion window.The upper strata packing ring corrosion window is mutually corresponding with lower floor packing ring corrosion window.
Furtherly, 1 lower floor's packing ring corrosion window is provided with having on lower floor's packing ring 31 of lower floor's packing ring corrosion window.
Lower floor's packing ring corrosion window is rounded（As shown in Figure 10）, sub-circular（As shown in figure 11）, rectangle, reserved scribe line
Rectangular array（As shown in figure 12）, full wafer silicon chip shape, triangle, trapezoidal or interdigitated.1 upper strata is provided with upper strata in packing ring 4
Packing ring corrosion window.The upper strata packing ring corrosion window is mutually corresponding with lower floor packing ring corrosion window.
Furtherly, outer cell body 1, the material of interior cell body 2 are politef, wherein, the inside radius 12 of outer cell body 1
㎝, the ㎝ of outer radius 13 it is columnar structured, the thickness of groove bottom of outer cell body 1 is 0.8 ㎝, and the total height of outer cell body 1 is 6.8 ㎝.Groove
The radius of the annular stop block on body bolt 5 is 0.6 ㎝, is highly 0.4 ㎝, the bottom surface of the annular stop block and the chamber of outer cell body 1
Spacing between body bottom surface is 2 ㎝, and the spacing between the top surface of the annular stop block and the top surface of cell body bolt 5 is 2 ㎝.Cell body
The screw thread that the radius of bolt 5 is 0.4 ㎝, pitch is 0.1 ㎝, after installing successively for lower floor's packing ring, upper strata packing ring 4, interior cell body 2
Using the pinch seal of nut 6.A diameter of 9.6 ㎝ of lower floor's packing ring, the disk that thickness is 0.4 ㎝.
Embodiment 1
Dual bath apparatus based on above-mentioned porous silicon preparing electrochemical process selectivity on SOI silicon prepares porous silicon, from Fig. 3
Without inside groove shown in upper strata packing ring 4, Fig. 9 shown in packing ring corrosion window lower floor of lower floor packing ring 32, Fig. 8 shown in shown outer cell body 1, Fig. 7
Body 2, nut 6, prepare the square that porous silicon upper surface is shaped as the ㎝ of the length of side 6.5.Its concrete operation step is as follows：
Step 1. is for piece：From 4 inches of soi wafers.Silicon chip is cleaned by ultrasonic with 99.5% analytically pure acetone soln
5min, removes the grease contamination on surface, and deionized water is rinsed well.Then ultrasonic cleaning 5min is carried out with dehydrated alcohol,
The organic residue on surface is removed, deionized water is rinsed well.By silicon chip under nitrogen protection, on the hot plate of 150 DEG C of temperature
Dehydration bakees 1min.
Step 2. silicon chip is disposed：4 inches of soi wafers of placement are in without the central position of packing ring corrosion window lower floor of lower floor packing ring 32
Put, need the silicon for preparing porous silicon to face up, and enable silicon chip that the corrosion window of upper strata packing ring 4 is completely covered, by with packing ring
Upper strata packing ring 4 is enclosed within the lower floor's pad without underlay ring layer corrosion window by the corresponding upper strata packing ring side packing ring bolt positioning hole of bolt 7
On the packing ring bolt 7 of circle 32, the top of the packing ring bolt 7 is furnished with nut 6, so as to by upper strata packing ring 4 and without lower floor's packing ring corruption
Fenetre mouth lower floor packing ring 32 links together.
Step 3. device is installed：By lower floor's packing ring side corresponding with cell body bolt 5 packing ring bolt positioning hole and cell body spiral shell
The corresponding upper strata packing ring bolt positioning hole of bolt 5 will link together without packing ring corrosion window lower floor of lower floor packing ring 32 and upper strata pad
Circle 4 is enclosed within the annular stop block of cell body bolt 5.Interior cell body 2 is enclosed within by cell body spiral shell by inside groove side cell body bolt positioning hole
On bolt, the top of the cell body bolt 5 is furnished with nut 6, so as to by interior cell body 2, upper strata packing ring 4, without lower floor's packing ring corrosion window
Lower floor's packing ring 32 links together with outer cell body 1.
Step 4. electrochemical corrosion：Injection corrosion electrolyte in interior cell body 2, conventional corrosion electrolyte system has HF/
C2H5OH、HF/C2H5OH/HNO3、HF/H2O2Deng while producing many of different parameters specification from different corrosion system solution proportions
Hole silicon, the example use ratio is 1:2 HF/C2H5OH corrodes electrolyte system.The injection corrosion electrolyte or general of outer cell body 1
Logical electrolyte, described corrosion electrolyte system has HF/C2H5OH, HF/C2H5OH/HNO3, HF/H2O2 etc., while from not
The porous silicon of different parameters specification is produced with corrosion system solution proportion, the conventional NaCl solution of described electrolyte, the example makes
It is 1 with ratio:2 HF/C2H5OH corrodes electrolyte system.Two electrodes are inserted into the electrolyte in outer cell body 1 and interior cell body 2
In, generally from platinum Pt electrodes or graphite electrode, the example uses graphite electrode, the stone in insertion in the electrolyte inside of cell body 2
Electrode ink connects power cathode, inserts the graphite electrode connection power anode in the outer electrolyte inside of cell body 1.Herein power supply is used
DH1722 types DC current regulator power supply provides current stabilization, and electric current density is 30mA/cm when prepared by the example2.Etching time
30min。
Embodiment 2
Dual bath apparatus based on above-mentioned porous silicon preparing electrochemical process selectivity on non-SOI silicon prepares porous silicon, selects
Outer cell body 1, Fig. 4 shown in Fig. 3 is shown with interior shown in upper strata packing ring 4, Fig. 6 shown in packing ring corrosion window lower floor of lower floor packing ring 31, Fig. 5
Cell body 2, nut 6, while preparing 4 pieces of porous silicons, upper surface is shaped as the square of length of side 1.4cm.Its concrete operation step
It is as follows：
Step 1. is for piece：From the common silicon chip of 4 inches of twin polishings, scribing obtains 4 pieces of silicon chips, and size is 1.5cm's
Square.Ultrasonic cleaning 5min is carried out to silicon chip with 99.5% analytically pure acetone soln, the grease contamination on surface is removed, is used
Deionized water rinsing is clean.Then ultrasonic cleaning 5min is carried out with dehydrated alcohol, the organic residue on surface is removed, deionization is used
Water is rinsed well.By silicon chip under nitrogen protection, on the hot plate of 150 DEG C of temperature dehydration bakee 1min.
Step 2. silicon chip is disposed：4 pieces of silicon chips of placement are in 4 corrosion windows for having packing ring corrosion window lower floor of lower floor packing ring 31
On, and enable silicon chip to be completely covered with 4 corrosion windows of packing ring corrosion window lower floor of lower floor packing ring 31, by with packing ring spiral shell
Upper strata packing ring 4 is enclosed within the corresponding upper strata packing ring side packing ring bolt positioning hole of bolt 7 lower floor's packing ring of underlay ring layer corrosion window
On 31 packing ring bolt 7, the top of the packing ring bolt 7 is furnished with nut 6, so as to by upper strata packing ring 4 and have the corrosion of lower floor packing ring
Window lower floor packing ring 31 links together.
Step 3. device is installed：By lower floor's packing ring side corresponding with cell body bolt 5 packing ring bolt positioning hole and cell body spiral shell
The corresponding upper strata packing ring bolt positioning hole of bolt 5 has packing ring corrosion window lower floor of lower floor packing ring 31 and upper strata pad by what is linked together
Circle 4 is enclosed within the annular stop block of cell body bolt 5.Interior cell body 2 is enclosed within by cell body spiral shell by inside groove side cell body bolt positioning hole
On bolt, the top of the cell body bolt 5 is furnished with nut 6, so as to by interior cell body 2, upper strata packing ring 4, have lower floor's packing ring corrosion window
Lower floor's packing ring 31 links together with outer cell body 1.
Step 4. electrochemical corrosion：Injection corrosion electrolyte in interior cell body 2, described corrosion electrolyte system has HF/
C2H5OH、HF/C2H5OH/HNO3、HF/H2O2Deng while producing many of different parameters specification from different corrosion system solution proportions
Hole silicon, the example use ratio is 1:2 HF/C2H5OH corrodes electrolyte system.The injection corrosion electrolyte or general of outer cell body 1
Logical electrolyte, described corrosion electrolyte system has HF/C2H5OH, HF/C2H5OH/HNO3, HF/H2O2 etc., while from not
The porous silicon of different parameters specification is produced with corrosion system solution proportion, the conventional NaCl solution of described electrolyte, the example makes
It is 1 with ratio:2 HF/C2H5OH corrodes electrolyte system.Two electrodes are inserted into the electrolyte in outer cell body 1 and interior cell body 2
In, generally from platinum Pt electrodes or graphite electrode, the example uses graphite electrode, the stone in insertion in the electrolyte inside of cell body 2
Electrode ink connects power cathode, inserts the graphite electrode connection power anode in the outer electrolyte inside of cell body 1.Herein power supply is used
DH1722 types DC current regulator power supply provides current stabilization, and electric current density is 20mA/cm when prepared by the example2.Etching time
20min。
Claims (7)
1. the dual bath apparatus of porous silicon preparing electrochemical process are used for, it is characterised in that：Including outer cell body (1), interior cell body (2), under
Layer packing ring, upper strata packing ring (4), cell body bolt (5), nut (6) and packing ring bolt (7)；
The outer cell body (1) is open-topped hollow container；The groove of more than 4 is provided with the cavity bottom surface of outer cell body (1)
Body bolt (5)；The cell body bolt (5) is vertically connected with the cavity bottom surface of outer cell body (1), and in each cell body bolt (5)
Middle part be equipped with annular limited block；
Lower floor's packing ring has 2 for discoideus, wherein 1 lower floor's packing ring is provided with lower floor's packing ring corrosion window, is referred to as having
Packing ring corrosion window lower floor of lower floor packing ring (31), is not provided with lower floor's packing ring corrosion window, referred to as without lower floor on another 1 lower floor's packing ring
Packing ring corrosion window lower floor packing ring (32)；
In each of the lower the edge of layer packing ring is provided with the lower floor packing ring side channel body bolt positioning hole corresponding with cell body bolt (5)；
The edge of the top surface of each lower floor's packing ring is provided with the packing ring bolt (7) of more than 4；The packing ring bolt (7) with lower floor's packing ring
Top surface vertically connect；In each of the lower the edge of layer packing ring is provided with the mounting hole of more than 1；
The upper strata packing ring (4) is in discoideus；The upper strata packing ring corrosion window of more than 1 is provided with the middle part of upper strata packing ring (4)；
On upper strata, the edge of packing ring (4) is provided with the upper strata packing ring side channel body bolt positioning hole corresponding with cell body bolt (5), upper
The edge of layer packing ring (4) is additionally provided with the upper strata packing ring side packing ring bolt positioning hole corresponding with packing ring bolt (7)；In upper strata packing ring
(4) edge is provided with the mounting hole of more than 1；
The interior cell body (2) for upper and lower opening cylindrical body；The base for horizontally outward extending is provided with the bottom of interior cell body (2)；
The base is identical with the quantity of cell body bolt (5), and one is provided with each base of interior cell body (2) with cell body bolt
(5) corresponding inside groove side cell body bolt positioning hole；
When making the porous silicon layer on soi wafer with this dual bath apparatus, upper strata packing ring (4) is enclosed within without underlay ring layer corrosion window
Lower floor's packing ring (32) packing ring bolt (7) on, by screwing the nut (6) at the top of packing ring bolt (7), by upper strata packing ring (4)
With link together without packing ring corrosion window lower floor of lower floor packing ring (32)；To link together without under lower floor's packing ring corrosion window
Layer packing ring (32) and upper strata packing ring (4) are enclosed within the annular stop block of cell body bolt (5)；Again interior cell body (2) is enclosed within into cell body spiral shell
On bolt (5), and the nut (6) at the top of cell body bolt (5) is screwed, so as to by interior cell body (2), upper strata packing ring (4), without lower floor's packing ring
Corrosion window lower floor packing ring (32) links together with outer cell body (1)；
When making the porous silicon layer on non-soi wafer with this dual bath apparatus, upper strata packing ring (4) underlay ring layer corrosion window is enclosed within into
On the packing ring bolt (7) of lower floor's packing ring (31) of mouth, by screwing the nut (6) at the top of packing ring bolt (7), by upper strata packing ring
(4) and packing ring corrosion window lower floor of lower floor packing ring (31) links together；There is lower floor's packing ring corrosion window by what is linked together
Mouth lower floor's packing ring (31) and upper strata packing ring (4) are enclosed within the annular stop block of cell body bolt (5)；Again interior cell body (2) is enclosed within into groove
On body bolt (5), and the nut (6) at the top of cell body bolt (5) is screwed, so as to by interior cell body (2), upper strata packing ring (4), have lower floor
Packing ring corrosion window lower floor packing ring (31) links together with outer cell body (1).
2. dual bath apparatus for porous silicon preparing electrochemical process according to claim 1, it is characterised in that：
4 cell body bolts (5) are evenly equipped with the cavity bottom surface of outer cell body (1)；
2 mounting holes are provided with the edge of the lower floor's packing ring (32) without lower floor's packing ring corrosion window；Without lower floor's packing ring corrosion window
The top surface of lower floor's packing ring (32) of mouth is evenly equipped with 4 packing ring bolts (7)；
1 upper strata packing ring corrosion window is provided with packing ring (4) on upper strata, the upper strata packing ring corrosion window is rounded；On upper strata
1 square frame (41) is provided with packing ring corrosion window, by elongated upper strata packing ring linking arm (42) by the one of square frame (41)
Outer wall is linked together with the inwall of adjacent upper strata packing ring corrosion window；On upper strata, the edge of packing ring (4) is provided with 2 kidney-shapeds
Hole；
The interior cell body (2) is hollow and upper and lower opening cuboid；It is respectively equipped with the bottom of each side wall of interior cell body (2)
1 base for horizontally outward extending；1 inside groove side cell body corresponding with cell body bolt (5) is provided with each base
Bolt positioning hole；
The material of lower floor's packing ring (32), upper strata packing ring (4) and interior cell body (2) without lower floor's packing ring corrosion window is polytetrafluoroethyl-ne
Alkene.
3. dual bath apparatus for porous silicon preparing electrochemical process according to claim 1, it is characterised in that：
4 cell body bolts (5) are evenly equipped with the cavity bottom surface of outer cell body (1)；
2 mounting holes are provided with the edge of the lower floor's packing ring (31) for having lower floor's packing ring corrosion window；There is lower floor's packing ring corrosion window
The top surface of lower floor's packing ring (31) of mouth is evenly equipped with 4 packing ring bolts (7)；Have on lower floor's packing ring (31) of lower floor's packing ring corrosion window
It is provided with lower floor's packing ring corrosion window of more than 1；
The upper strata packing ring corrosion window corresponding with lower floor packing ring corrosion window is provided with packing ring (4) on upper strata；In upper strata packing ring
(4) edge is provided with 2 mounting holes；
The interior cell body (2) is hollow and upper and lower opening pipe；4 water are evenly equipped with the outside of interior cell body (2) bottom port
The flat base for stretching out；It is provided with 1 inside groove side cell body bolt corresponding with cell body bolt (5) on each base to determine
Position hole；
The material for having lower floor's packing ring (31), upper strata packing ring (4) and interior cell body (2) of lower floor's packing ring corrosion window is polytetrafluoroethyl-ne
Alkene.
4. dual bath apparatus for porous silicon preparing electrochemical process according to claim 3, it is characterised in that：
4 lower floor's packing ring corrosion windows are provided with the lower floor's packing ring (31) for having lower floor's packing ring corrosion window；Lower floor's packing ring
Corrosion window is square, and by 2 × 2 array arrangement；4 upper strata packing ring corrosion windows are provided with upper strata in packing ring (4)；It is described
Upper strata packing ring corrosion window is mutually corresponding with lower floor packing ring corrosion window.
5. dual bath apparatus for porous silicon preparing electrochemical process according to claim 3, it is characterised in that：
1 lower floor's packing ring corrosion window is provided with the lower floor's packing ring (31) for having lower floor's packing ring corrosion window；Lower floor's packing ring
Corrosion window is rounded, sub-circular, rectangle, rectangular array, the full wafer silicon chip shape of reserved scribe line, triangle, trapezoidal or fork
Finger-type；1 upper strata packing ring corrosion window is provided with upper strata in packing ring (4)；The upper strata packing ring corrosion window and lower floor's packing ring corruption
Fenetre mouth is mutually corresponded to.
6. the arbitrary dual bath apparatus method that selectivity prepares porous silicon on SOI silicon according to claim 1 to 5, it is special
Levy and be：Carry out as follows：
Step one, standby piece：Soi wafer is chosen, and is cleaned by ultrasonic, subsequently under nitrogen protection dehydration is bakeed；
Step 2, silicon chip placement：Soi wafer is placed in without central authorities of packing ring corrosion window lower floor of lower floor packing ring (32), it would be desirable to
The SOI silicon for preparing porous silicon faces up, and upper strata packing ring (4) is enclosed within into the pad of the lower floor's packing ring (32) without underlay ring layer corrosion window
On circle bolt (7), then by nut (6) by upper strata packing ring (4) and without packing ring corrosion window lower floor of lower floor packing ring 32) it is connected to one
Rise；
Step 3, device are installed：To link together without packing ring corrosion window lower floor of lower floor packing ring (32) and upper strata packing ring (4)
It is enclosed within the annular stop block of cell body bolt (5), subsequently, by interior cell body (2), upper strata packing ring (4), without lower floor's packing ring corrosion window
Lower floor's packing ring (32) links together with outer cell body (1)；
Step 4, electrochemical corrosion：Inwardly injection mol ratio is 1 in cell body (2):2 HF/C2H5OH corrodes electrolyte, to water jacket
Body (1) injection mol ratio is 1:2 HF/C2H5OH corrodes electrolyte or NaCl electrolyte；One graphite electrode is inserted into water jacket
In electrolyte in body (1), and connect power anode；Another graphite electrode is inserted in the electrolyte in interior cell body (2), and
Connection power cathode, is 30mA/cm with after-applied electric current density2Unidirectional current, corrosion 30min to 40min；Finally take out corrosion
Soi wafer afterwards, obtains finished product.
7. the method that selectivity prepares porous silicon on non-SOI silicon of the arbitrary dual bath apparatus according to claim 1 to 5, its
It is characterised by：Carry out as follows：
Step one, standby piece：The silicon chip of one piece of 4 inches of twin polishing is chosen, scribing obtains the silicon chip after 4 pieces of cuttings, the cutting
The size of silicon chip afterwards is the square of 1.5cm；Respectively the silicon chip after aforementioned cutting is carried out with acetone soln and dehydrated alcohol
It is cleaned by ultrasonic；Subsequently by the silicon chip after ultrasonic cleaning under nitrogen protection, on the hot plate of 150 DEG C of temperature dehydration bakee 1min；
Step 2, silicon chip placement：Obtained by step one 4 pieces of silicon chips for cleaning and bakeing lower floor's packing ring has been placed in into respectively
On 4 corrosion windows of corrosion window lower floor packing ring (31), upper strata packing ring (4) is enclosed within into the lower floor of underlay ring layer corrosion window
On the packing ring bolt (7) of packing ring (31), by upper strata packing ring (4) and there is packing ring corrosion window lower floor of lower floor packing ring (31) to be connected to one
Rise；
Step 3, device are installed：There are packing ring corrosion window lower floor of lower floor packing ring (31) and upper strata packing ring (4) by what is linked together
It is enclosed within the annular stop block of cell body bolt (5)；Interior cell body (2) is enclosed within cell body bolt, by interior cell body (2), upper strata packing ring
(4) packing ring corrosion window lower floor of lower floor packing ring (31), links together with outer cell body (1)；
Step 4, electrochemical corrosion：Inwardly injection mol ratio is 1 in cell body (2):2 HF/C2H5OH corrodes electrolyte；To water jacket
Body (1) injection mol ratio is 1:2 HF/C2H5OH corrodes electrolyte or NaCl electrolyte；One graphite electrode is inserted into water jacket
In the electrolyte of body (1), and connect power anode, another graphite electrode is inserted in the electrolyte in interior cell body (2), and even
Power cathode is connect, is 20mA/cm with after-applied electric current density2Unidirectional current, and etching time 20min to 30min is final to obtain
Finished product.
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