CN106744672B - A kind of preparation facilities and preparation system of three-D nano-porous silicon - Google Patents
A kind of preparation facilities and preparation system of three-D nano-porous silicon Download PDFInfo
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- CN106744672B CN106744672B CN201611159904.4A CN201611159904A CN106744672B CN 106744672 B CN106744672 B CN 106744672B CN 201611159904 A CN201611159904 A CN 201611159904A CN 106744672 B CN106744672 B CN 106744672B
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- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 238000003486 chemical etching Methods 0.000 claims abstract description 69
- 230000035939 shock Effects 0.000 claims abstract description 63
- 238000006243 chemical reaction Methods 0.000 claims abstract description 57
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 18
- 230000003028 elevating effect Effects 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 6
- 239000002086 nanomaterial Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 239000002210 silicon-based material Substances 0.000 abstract description 2
- 239000011856 silicon-based particle Substances 0.000 description 34
- 238000000034 method Methods 0.000 description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 14
- 238000005530 etching Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 9
- 230000007797 corrosion Effects 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0004—Apparatus specially adapted for the manufacture or treatment of nanostructural devices or systems or methods for manufacturing the same
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
- B82B3/0038—Manufacturing processes for forming specific nanostructures not provided for in groups B82B3/0014 - B82B3/0033
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Weting (AREA)
Abstract
The present invention relates to the preparation fields of nanoporous silicon materials, provide a kind of preparation facilities of three-D nano-porous silicon, including pedestal, shock wave generator, shock wave power supply, work tank, chemical etching reaction vessel and thermometer, shock wave generator is set to the top of pedestal, work tank is set to the top of shock wave generator, chemical etching reaction vessel is set in work tank by clamping device, thermometer is set in chemical etching reaction vessel, heating element is provided in work tank, shock wave power supply is set to the side wall of pedestal, shock wave generator and heating element are connect with shock wave power circuit.The device is easy to operate, and three-D nano-porous silicon yield made from it, high hole are evenly distributed, aperture size is uniform.The present invention also provides a kind of preparation systems of three-D nano-porous silicon comprising the preparation facilities of above-mentioned three-D nano-porous silicon, three-D nano-porous silicon yield high-quality made from the system are good.
Description
Technical field
The present invention relates to the preparation fields of nanoporous silicon materials, in particular to a kind of three-D nano-porous silicon
Preparation facilities and preparation system.
Background technique
3-D nano, structure has unique dielectric property, photoelectric characteristic, microelectronics compatibility and big specific surface area,
Answer it extensively in sensing element, sensor, illuminating material, photoelectric device, integrated circuit, solar battery and field of lithium
With.In recent years, the excellent performance due to 3-D nano, structure material on lithium cell cathode material, lot of domestic and international well-known expert
Start to carry out the R&D work of the 3-D nano, structure based on silicon particle with research institution, research achievement shows basis material silicon
Grain mostlys come from metal metallurgy smelting silicon, crystalline silicon, silico-aluminum and natural material, and silicon particle is prepared as basis material
The method of nano-structure porous silicon mainly uses various forms of chemical attacks.Experimental result shows, three wieners of each method preparation
Rice structure has excellent performance on lithium battery, it is shown that the good architectural characteristic of three-dimensional nanometer material.
But there is also certain problems for the 3-D nano, structure prepared at present.Firstly, the electric conductivity of silicon particle is bad.
When as lithium cell cathode material, the later period be improve electric conductivity, to three-D nano-porous silicon also need to be doped or packet carbon at
Reason, increases technology difficulty and cost；Secondly, the structure of three-D nano-porous silicon is uneven.With the reduction of silicon particle size,
Intergranular corrosion is uneven in chemical corrosion process, and especially hole depth corrosion is limited, has very big shadow for the performance of material
It rings；Again, the preparation method low output of current three-D nano-porous silicon, it is at high cost.
Summary of the invention
The present invention provides a kind of preparation facilities of three-D nano-porous silicon, it is intended to improve existing three-D nano-porous silicon
Preparation facilities is complicated for operation, low yield, three-D nano-porous silicon face hole obtained is unevenly distributed, aperture size difference
Larger problem.
The present invention also provides a kind of preparation systems of three-D nano-porous silicon, prepare the yield of three-D nano-porous silicon
Height, performance are good.
The present invention is implemented as follows:
A kind of preparation facilities of three-D nano-porous silicon, including pedestal, shock wave generator, shock wave power supply, work tank, change
It learns etching reaction container and thermometer, shock wave generator is set to the top of pedestal, work tank is set to shock wave generator
Top, chemical etching reaction vessel is set in work tank by clamping device, and thermometer is set to chemical etching reaction
In container, be provided with heating element in work tank, shock wave power supply is set to the side wall of pedestal, the circuit of shock wave generator and plus
Circuit connection of the circuit of thermal element with shock wave power supply.
Further, in preferred embodiments of the present invention, clamping device includes upright bar interconnected and folder, upright bar
It is fixedly connected on pedestal, folder is located in the outer wall of chemical etching reaction vessel.
Further, in preferred embodiments of the present invention, clamping device further includes elevating lever, elevator, and upright bar is hollow
And side wall offers a shaped opening along its length, elevating lever is set in upright bar, and elevator is set in pedestal, elevating lever
Bottom end is connect with elevator, and folder passes through a shaped opening far from one end of chemical etching reaction vessel and connect with elevating lever.
Further, in preferred embodiments of the present invention, clamping device further includes cross bar, and it is separate that cross bar is connected to upright bar
One end of pedestal, thermometer are connect far from one end of chemical etching reaction vessel with cross bar.
It further, further include suction pump in preferred embodiments of the present invention, the bottom of chemical etching reaction vessel is set
It is equipped with filter, one is formed between filter and the bottom wall of chemical etching reaction vessel and goes out sap cavity, chemical etching reactor pair
The side wall that sap cavity should be gone out offers fluid hole, and fluid hole is connected to suction pump.
Further, in preferred embodiments of the present invention, filter includes filter membrane and filter body, filter membrane
Edge is detachably connected with filter body, and the inner wall of filter body and chemical etching reaction vessel is detachably connected.
Further, in preferred embodiments of the present invention, the inner wall of chemical etching reaction vessel is provided with for placing
The annular protrusion of filter body, and the first gasket is provided between filter body and annular protrusion.
Further, in preferred embodiments of the present invention, filter body includes the supporting network and fastening of mutual snapping
Part, filter membrane are located between supporting network and fastener.
Further, in preferred embodiments of the present invention, supporting network is provided with the second sealing close to the side of fastener
Pad, fastener are provided with third gasket close to the side of supporting network.
A kind of preparation system of three-D nano-porous silicon, the preparation facilities including above-mentioned three-D nano-porous silicon.
The beneficial effects of the present invention are: the preparation facilities for the three-D nano-porous silicon that the present invention obtains by above-mentioned design,
The preparation facilities of three-D nano-porous silicon provided by the invention, can be in three-D nano-porous silicon because it is with shock wave generator
Shock wave auxiliary one side guarantee silicon particle fine dispersion is carried out to silicon particle in preparation process and induces clipped wire in etching solution
Sub- uniform deposition realizes that silicon particle surface hole defect is uniformly distributed in corrosion process；Another aspect shock wave promotes corrosion product energy
It is excluded in time from hole, fresh corrosive liquid can be supplemented rapidly, and efficient, the high-precision for being able to achieve hole etch, so that finally
The aperture size of three-D nano-porous silicon obtained is uniform, and the device simple structure is easy to operate.Three-dimensional provided by the invention
The preparation system of nano-structure porous silicon, because it includes the preparation facilities of above-mentioned three-D nano-porous silicon, so that using this system system
The three-D nano-porous silicon yield obtained is high, and the hole of three-D nano-porous silicon particle is evenly distributed, and aperture size is uniform.
Detailed description of the invention
It, below will be to use required in embodiment in order to illustrate more clearly of the technical solution of embodiment of the present invention
Attached drawing be briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not to be seen as
It is the restriction to range, it for those of ordinary skill in the art, without creative efforts, can be with root
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the structural schematic diagram of the preparation facilities for the three-D nano-porous silicon that embodiment of the present invention provides；
Fig. 2 is the structural schematic diagram of chemical etching reaction vessel in Fig. 1；
Fig. 3 is the enlarged drawing in III region in Fig. 2；
Fig. 4 is the bottom view of filter in Fig. 2；
Fig. 5 is the top view of filter in Fig. 2；
Fig. 6 is the operational flowchart of the preparation method for the three-D nano-porous silicon that embodiment of the present invention provides.
Icon: the preparation facilities of the three-D nano-porous silicon of 100-；110- shock wave generator；120- shock wave power supply；When 121-
Between controller；130- work tank；131- heating element；140- chemical etching reaction vessel；141- goes out sap cavity；142- goes out liquid
Hole；143- annular protrusion；The first gasket of 145-；150- thermometer；160- clamping device；161- upright bar；162- folder；163-
Elevating lever；164- elevator；165- shaped opening；166- cross bar；170- filter；171- filter membrane；172- filter body；
173- supporting network；174- fastener；175- mesh；176- connecting column；177- connecting hole；The second gasket of 178-；179- third
Gasket；180- suction pump；181- suction tube；190- pedestal.
Specific embodiment
To keep the purposes, technical schemes and advantages of embodiment of the present invention clearer, implement below in conjunction with the present invention
The technical solution in embodiment of the present invention is clearly and completely described in attached drawing in mode, it is clear that described reality
The mode of applying is some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ability
Domain those of ordinary skill every other embodiment obtained without creative efforts, belongs to the present invention
The range of protection.Therefore, the detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit below and is wanted
The scope of the present invention of protection is sought, but is merely representative of selected embodiment of the invention.Based on the embodiment in the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts belongs to this
Invent the range of protection.
In the description of the present invention, it is to be understood that, term " on ", "lower", "vertical", "horizontal", "top", "bottom",
The orientation or positional relationship of the instructions such as "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of retouching
It states the present invention and simplifies description, rather than the equipment of indication or suggestion meaning or element must have a particular orientation, with specific
Orientation construction and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance
Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or
Implicitly include one or more of the features.In the description of the present invention, the meaning of " plurality " is two or more,
Unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc.
Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integral；It can be mechanical connect
It connects, is also possible to be electrically connected；It can be directly connected, can also can be in two elements indirectly connected through an intermediary
The interaction relationship of the connection in portion or two elements.It for the ordinary skill in the art, can be according to specific feelings
Condition understands the concrete meaning of above-mentioned term in the present invention.
In the present invention unless specifically defined or limited otherwise, fisrt feature second feature "upper" or "lower"
It may include that the first and second features directly contact, also may include that the first and second features are not direct contacts but pass through it
Between other characterisation contact.Moreover, fisrt feature includes the first spy above the second feature " above ", " above " and " above "
Sign is right above second feature and oblique upper, or is merely representative of first feature horizontal height higher than second feature.Fisrt feature exists
Second feature " under ", " lower section " and " following " include that fisrt feature is directly below and diagonally below the second feature, or is merely representative of
First feature horizontal height is less than second feature.
As shown in Figure 1, a kind of preparation facilities 100 of three-D nano-porous silicon provided by the invention includes pedestal 190, shock wave
Generator 110, shock wave power supply 120, work tank 130, chemical etching reaction vessel 140, clamping device 160 and thermometer
150.Shock wave generator 110 is set on pedestal 190, and work tank 130 is set on shock wave generator 110, and chemistry is carved
Erosion reaction vessel 140 is set in work tank 130 by clamping device 160, and thermometer 150 is set to etching reaction container
It is interior, heating element 131 is provided in work tank 130, shock wave power supply 120 is set to the side wall of pedestal 190, shock wave generator
110 and heating element 131 with 120 circuit connection of shock wave power supply.Shock wave generator 110 is for swashing chemical etching process
Wave auxiliary.
Preferably, the preparation facilities 100 of three-D nano-porous silicon further includes time controller 121, and time controller page 121
It is set to the side wall of pedestal 190, the circuit of time controller 121 and the circuit connection of shock wave power supply 120.Time controller is set
121 purpose be can by time controller 121 setting time with control shock wave generator 110 circuit and shock wave power supply
The connection and disconnection of 120 circuit, so control shock wave generator 110 to the shock wave non-cutting time of chemical etching, can be effective
Save the time of operator.
Water is injected in work tank 130, water is heated by heating element 131, so that chemical etching reacts
Container 140 is heated, and chemical etching liquid is held in chemical etching reaction vessel 140, chemical etching reaction vessel 140 is by glass
Perhaps resistant material, which is made, is put into chemical etching reaction vessel 140 for silicon particle and etching liquid or cleaning solution, in water-bath plus
Three-D nano-porous silicon etching reaction is carried out under conditions of heat.
Time controller 121 can control the connection and disconnection of shock wave power supply 120 Yu 110 circuit of shock wave generator, pass through
The time of the connecting and disconnecting of the circuit of shock wave power supply 120 and shock wave generator 110 is set, on time controller 121 to control
The length of time that shock wave generator 110 processed emits shock wave is not required to artificial timing to reach intelligentized effect, effectively saving work
Make the working time of personnel.
Preferably, clamping device 160 includes upright bar 161 interconnected and folder 162, and one end of upright bar 161 is fixed to be connected
It is connected on pedestal 190, folder 162 is located in the outer wall of chemical etching reaction vessel 140.Folder 162 is reacted with chemical etching
The connection type of container 140 chemical etching reaction vessel 140 can be made to be readily disassembled so that be easily changed etching liquid in it or
Cleaning solution.
It should be pointed out that in other embodiments of the invention, clamping device 160 can be tool, and there are two sandwich parts
Clamping piece, two sandwich parts are located in the side wall of work tank 130 and the side wall of chemical etching reaction vessel 140 simultaneously respectively
On, chemical etching reaction vessel 140 is set in work tank 130.
Preferably, clamping device 160 further includes elevating lever 163, and upright bar 161 is hollow, and the side wall of upright bar 161 is provided with vertically
Shaped opening 165, side wall elevating lever 163 is set in upright bar 161, and elevator 164, elevating lever 163 are provided in pedestal 190
One end connect with elevator 164, folder 162 pass through a shaped opening 165 connect with elevating lever 163 far from one end of pedestal 190,
Folder 162 is located in the outer wall of chemical etching reaction vessel 140 far from one end of elevating lever 163, the circuit of elevator 164 and swashs
The circuit connection of wave power supply 120, elevator 164 control the lifting of elevating lever 163 and pass through folder in turn in the rotation of horizontal plane
162 drive the lifting of chemical etching reaction vessel 140 and rotation in the horizontal plane.
Preferably, clamping device 160 further includes 166 upright bar 161 of cross bar, and one end and cross bar 166 far from pedestal 190 rotate
Connection, end of the cross bar 166 far from upright bar 161 is detachably connected with thermometer 150.When the preparation facilities of three-D nano-porous silicon
After 100 work, when needing to take out chemical etching reaction vessel 140, firstly, thermometer 150 is removed, by 166 turns of cross bar
It moves to the surface for leaving chemical etching reaction vessel 140, increase elevating lever 163, drive on chemical etching reaction vessel 140
It rises, then chemical etching reaction vessel 140 is directly removed from folder 162.
It should be pointed out that in other embodiments of the invention, thermometer 150 can be through the direct sandwiched of clamping piece
In the side wall of chemical etching reaction vessel 140.
As depicted in figs. 1 and 2, it is preferable that the preparation facilities 100 of three-D nano-porous silicon further includes suction pump 180, chemistry
The bottom of etching reaction container 140 is provided with filter 170, between filter 170 and the bottom wall of chemical etching reaction vessel 140
It forms one and goes out sap cavity 141, the side wall of the corresponding chemical etching reaction vessel 140 of sap cavity 141 offers fluid hole 142 out, aspirates
Pump 180 is connected to by fluid hole 142 with sap cavity 141 out.By the suction force of suction pump 180 by chemical etching reaction vessel 140
Interior silicon particle is filtered, and silicon particle is left on filter 170, and discharge liquor then enters sap cavity from filter 170
141 are finally sucked 180 extraction of pump.
As shown in Figure 1-Figure 3, it is preferable that filter 170 includes filter membrane 171 and filter body 172, filter membrane 171
Edge be detachably set in filter body 172, and filter body 172 is detachably set to chemical etching reaction vessel
140 side wall, the aperture of filter membrane 171 is less than the partial size of silicon particle, to prevent filter membrane 171 easy to damage in aspiration procedure,
Multiple filtration film 171 can also be set on filter body 172.The side wall of chemical etching reaction vessel 140, which is provided with, to be used for
The annular protrusion 143 for placing filter 170, is provided with the first gasket 145 between filter body 172 and annular protrusion 143.
The purpose that the first gasket 145 is arranged is to guarantee the leakproofness of sap cavity 141 out.
As shown in Figure 3-Figure 5, further, filter body 172 includes supporting network 173 and fastener 174, filter membrane
171 are located between fastener 174 and supporting network 173, multiple mesh 175 are provided on supporting network 173, discharge liquor then penetrated
Filter membrane 171 is discharged by mesh 175.The purpose that supporting network 173 is arranged is that filter membrane 171 is prevented to be sucked in aspiration procedure
Power damage.It is provided with multiple connecting holes 177 on supporting network 173, is provided on fastener 174 corresponding with multiple connecting holes 177
Multiple connecting columns 176, a connecting column 176 penetrates filter membrane 171 and is inserted in a connecting hole 177 to realize fastener
174 are detachably connected with supporting network 173.Further, it is close close to the side of fastener 174 to be provided with second for supporting network 173
Packing 178 is provided with the through-hole cooperated with connecting column 176 on second gasket 178；Fastener 174 close to supporting network 173 one
Side is provided with third gasket 179, and the through-hole cooperated with connecting column 176, connecting column 176 are also equipped on third gasket 179
The through-hole on the second gasket 178 is initially passed through, then penetrates filter membrane 171, the through-hole then passed through on third gasket 179 is last
It is inserted in connecting hole 177.
The purpose that the second gasket 178 and setting third gasket 179 is arranged is in order to further ensure going out sap cavity 141
Leakproofness, so that suction pump 180 will not be silicon particle together with discharge liquor when aspirating to chemical etching reaction vessel 140
It aspirates and is lost.
It should be noted that the present invention is in the case where including suction pump 180 and filter 170, due to three-dimensional manometer
The preparation facilities 100 of porous silicon includes that shock wave generator 110 can equally reach the present invention by the way of shock wave auxiliary to silicon
Grain carries out the purpose of chemical etching.
Referring to Fig. 6, and referring also to Fig. 1-Fig. 5, below to the specific works of the preparation facilities 100 of three-D nano-porous silicon
Process is described in detail:
S1, it will be put into chemical etching liquid using the silicon particle after hydrofluoric acid clean and carry out chemical etching, and carved in chemistry
Apply shock wave auxiliary during erosion.
Specifically, firstly, weigh appropriate silicon particle, and silicon particle is put into container and is cleaned with using hydrofluoric acid,
The impurity on silicon particle surface is cleaned, can be stirred continuously silicon particle is enabled to be cleaned more in the process of cleaning
Sufficiently.Silicon particle after hydrofluoric acid clean is put into the chemical etching reaction vessel 140 for filling chemical etching liquid, and water is infused
Enter in work tank 130.Shock wave power supply 120 is opened, shock wave generator 110 generates shock wave and applies shock wave to chemical etching process
Auxiliary, while passing through the pulse width of the control shock wave generator 110 of shock wave power supply 120 and working time.Open shock wave power supply 120
While set on shock wave power supply 120 reaction needed for bath temperature, to guarantee the temperature change of chemical etching process not
More than 10 degrees Celsius.Shock wave non-cutting time and interval time are set on time controller 121.In other realities of the invention
It applies in example, if being not provided with time-controlling arrangement in the preparation facilities 100 of three-D nano-porous silicon, manual time-keeping also can be used
Mode controls shock wave non-cutting time.
The features such as design is small using shock wave pulse width, pressure peak is big, high energy, instantaneous and energy-controllable, on the one hand
Guarantee silicon particle fine dispersion and induce metallic uniform deposition in etching solution, realizes the silicon particle surface in corrosion process
Hole is uniformly distributed；Another aspect shock wave promotes corrosion product that can exclude in time from hole, and fresh corrosive liquid can be mended rapidly
It fills, efficient, the high-precision for being able to achieve hole etch.
In an embodiment of the present invention, chemical etching liquid can be the nitric acid including the 5-40mmol/L containing nitrate ion
The hydrogen peroxide of 1~5wt% of salt, the hydrofluoric acid of 2-8mol/L and specific gravity, nitrate include silver nitrate, ferric nitrate and copper nitrate
At least one of, due to react more stable using silver nitrate, preferred silver nitrate in the chemical etching liquid ingredient.The chemistry
The ingredient and proportion of etching liquid can more efficiently perform etching silicon particle.Preparing chemical etching liquid can be while by nitric acid
Salting liquid, hydrofluoric acid and hydrogen peroxide mix prepared simultaneously, are also possible to that nitrate and hydrofluoric acid are first carried out hybrid reaction,
Then hydrofluoric acid and hydrogen peroxide are subjected to hybrid reaction again, finally carry out mixed liquor obtained by two reactions to be mixed and made into chemical quarter
Lose liquid.
S2, the silicon particle after chemical etching is passed sequentially through into dust technology and deionized water is cleaned.
Specifically, after to chemical etching process, start suction pump 180, chemical etching liquid is pumped to out sap cavity 141
It is interior, it is extracted out by suction pump 180 by suction tube 181, when chemical etching liquid is taken out to the greatest extent, into chemical etching reaction vessel 140
Addition mass concentration is metal ion of the dust technology of 10%-20% to wash away silicon particle surface, logical after the completion of dust technology cleaning
It crosses suction pump 180 to aspirate chemical etching reaction vessel 140, dust technology is discharged.After dust technology is completely exhausted out, Xiang Hua
It learns in etching reaction container 140 and deionized water is added, silicon particle is cleaned again, to remove the dilute of silicon particle surface remaining
Nitric acid is extracted out deionized water using suction pump 180 after the completion of cleaning again, and deionized water wash number is 3-5 times.?
Replacement filter membrane 171 can be chosen whether after a certain cleaning process according to the toughness of filter membrane 171.
It should be pointed out that in the other embodiment of the present invention, according to the device for being not provided with filter and suction pump
The preparation of three-D nano-porous silicon is carried out, the discharge of chemical etching liquid, dust technology and deionized water can be being used for
The container for learning etching reaction takes out from reaction unit, then is extracted silicon particle using centrifuge.But this mode compared to
It is operated by the way of being provided with the preparation facilities 100 of three-D nano-porous silicon of suction pump 180 and filter 170 more complicated.
S3, the silicon particle after cleaning is subjected to centrifugation extraction.
Specifically, the silicon particle after cleaning is taken out, is placed in centrifuge, carry out centrifugation extraction, centrifugation, which is extracted, to be terminated
Silicon particle is taken out afterwards.
Scanning electron microscope will be placed in using three-D nano-porous silicon particle made from the preparation facilities 100 of three-D nano-porous silicon
Lower observation, hole are evenly distributed, and aperture size is uniform.
In conclusion the preparation facilities of three-D nano-porous silicon provided by the invention is because it is with shock wave generator, it can
Shock wave auxiliary is carried out to silicon particle in the preparation process of three-D nano-porous silicon, on the one hand guarantee silicon particle fine dispersion and is lured
Metallic uniform deposition in etching solution is led, realizes that silicon particle surface hole defect is uniformly distributed in corrosion process；On the other hand
Shock wave promotes corrosion product that can exclude in time from hole, and fresh corrosive liquid can be supplemented rapidly, is able to achieve the efficient, high of hole
Precision etching, so that the even aperture distribution of final three-D nano-porous silicon obtained, and the preparation dress of three-D nano-porous silicon
It is easy to operate to set simple structure.And filter and suction pump are set, enable to each cleaning step more convenient.
The preparation system of three-D nano-porous silicon provided by the invention is because of the system that it includes above-mentioned three-D nano-porous silicon
Standby device allows the system to efficiently and three-D nano-porous silicon is made in high texture.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation facilities of three-D nano-porous silicon, which is characterized in that including pedestal, shock wave generator, shock wave power supply, work
Make liquid bath, chemical etching reaction vessel and thermometer, the shock wave generator is set to the top of the pedestal, the work
Liquid bath is set to the top of the shock wave generator, and the chemical etching reaction vessel is set to the work by clamping device
In liquid bath, the thermometer is set in the chemical etching reaction vessel, and heating element, institute are provided in the work tank
State the side wall that shock wave power supply is set to the pedestal, the circuit of the circuit of the shock wave generator and the heating element is and institute
The circuit connection of shock wave power supply is stated, the preparation facilities of the three-D nano-porous silicon further includes suction pump, and the chemical etching is anti-
It answers the bottom of container to be provided with filter, forms one between the filter and the bottom wall of the chemical etching reaction vessel and go out
The side wall of sap cavity, the corresponding sap cavity out of the chemical etching reactor offers fluid hole, the fluid hole and the suction
Pump connection.
2. the preparation facilities of three-D nano-porous silicon according to claim 1, which is characterized in that the clamping device includes
Upright bar interconnected and folder, the upright bar are fixedly connected on the pedestal, and it is anti-that the folder is located in the chemical etching
Answer the outer wall of container.
3. the preparation facilities of three-D nano-porous silicon according to claim 2, which is characterized in that the clamping device also wraps
Elevating lever, elevator are included, the upright bar is hollow and side wall offers a shaped opening along its length, and the elevating lever is set to institute
It states in upright bar, the elevator is set in the pedestal, and the bottom end of the elevating lever is connect with the elevator, the folder
One end far from the chemical etching reaction vessel passes through described shaped opening and connect with the elevating lever.
4. the preparation facilities of three-D nano-porous silicon according to claim 3, which is characterized in that the clamping device also wraps
Cross bar is included, the cross bar is connected to the one end of the upright bar far from the pedestal, and the thermometer is anti-far from the chemical etching
One end of container is answered to connect with the cross bar.
5. the preparation facilities of three-D nano-porous silicon according to claim 1, which is characterized in that the filter included
Filter membrane and filter body, the edge of the filter membrane are detachably connected with the filter body, the filter body with
The inner wall of the chemical etching reaction vessel is detachably connected.
6. the preparation facilities of three-D nano-porous silicon according to claim 5, which is characterized in that the chemical etching reaction
The inner wall of container is provided with the annular protrusion for placing the filter body, and the filter body and the convex annular
The first gasket is provided between rising.
7. the preparation facilities of three-D nano-porous silicon according to claim 6, which is characterized in that the filter body packet
The supporting network and fastener of mutual snapping are included, the filter membrane is located between the supporting network and the fastener.
8. the preparation facilities of three-D nano-porous silicon according to claim 7, which is characterized in that the supporting network is close to institute
The side for stating fastener is provided with the second gasket, and the fastener is provided with third sealing close to the side of the supporting network
Pad.
9. a kind of preparation system of three-D nano-porous silicon, which is characterized in that including the described in any item three-dimensionals of claim 1-8
The preparation facilities of nano-structure porous silicon.
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