CN107089664B - Preparation method of nano porous silicon material - Google Patents
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Abstract
The invention provides a preparation method of a nano porous silicon material, which comprises the following steps of firstly, smelting an alloy into a uniform melt by an electromagnetic induction smelting technology; then, preparing a precursor Al-Cu-Si alloy thin strip by adopting a single-roller rotary quenching method; secondly, performing dealloying treatment on the alloy thin strip by using a nitric acid solution or a mixed solution of nitric acid and hydrochloric acid; and finally, cleaning and drying the obtained product to prepare the nano porous silicon material. The method has the advantages of low cost, simple process, low requirement on equipment, short production period, high yield, good repeatability and high material recycling rate, and the obtained nano-porous silicon has the characteristics of large specific surface area, small pore diameter, large pore volume and uniform pore diameter distribution, is suitable for large-scale production and has high economic value and market application value.
Description
Technical Field
The invention belongs to the technical field of porous material preparation, and particularly relates to a preparation method of a nano porous silicon material.
Background
As a high-porosity semiconductor material, the nano porous silicon has the advantages of high specific surface area, good permeability, low thermal conductivity, high chemical activity, high lithium storage capacity, good biological activity, moderate band gap, strong adsorption capacity to chemical and biological molecules, low toxicity, symbiosis and compatibility to biological tissues, easy integration, miniaturization and the like, and can be widely applied to energetic materials, luminescent materials, solar cells, fuel cells, supercapacitors, sensors, medical materials, biological imaging and the like. At present, the preparation of porous silicon mainly comprises a corrosion method, a template method and a magnesiothermic reduction reaction method, and the following methods are commonly used: (1) the electrochemical anodic corrosion method is to use direct current or pulse current to carry out anodic oxidation on a monocrystalline silicon piece in electrolyte containing hydrofluoric acid to generate a porous silicon film. The method has the advantages of simple and convenient operation and the disadvantages of uneven pore distribution, low yield and poor repeatability of the prepared porous silicon. (2) Hydrothermal corrosion method, which utilizes the high temperature and high pressure of hydrothermal reaction and controls corrosionThe concentration, the corrosion temperature and the corrosion time of the solution realize the regulation and control of the porous silicon pore structure. (3) The magnesiothermic reduction reaction method adopts Mg to react SiO2Reducing the mixture into a mixture of Si and MgO in a medium temperature zone (650-900 ℃), and then removing MgO in the product by hydrochloric acid. The method has the advantages of low cost, high yield, high specific surface area and the defects of uneven pore size distribution, poor repeatability and poor corresponding performance stability. (4) The template method is to grow Si in the gap position of the crystal by taking the ordered photonic crystal as a template, and finally remove the template. The method has the advantages that the ordered porous silicon material can be prepared, and the defect that the prepared nano porous silicon is limited to low-dimensional materials. (5) The dealloying method is a method for selectively removing one or more components in the alloy through physical dissolution or chemical corrosion, and has the characteristics of simple operation and good repeatability. The regulation and control of the porous silicon pore structure can be realized by controlling the preparation process and the structure of the precursor.
The domestic patent CN103979487A introduces a preparation method of doped porous silicon spheres. Si balls with certain doping concentration are selected as raw materials, and porous silicon balls are prepared by an ultrasonic-assisted acid etching method.
The domestic patent CN103337612A introduces a nano porous silicon-carbon composite material and a preparation method thereof. The nano porous silicon-carbon composite material is prepared by performing dealloying treatment on the Al-Si/C alloy thin strip.
The domestic patent CN105399100A introduces a preparation method of nano-porous silicon. Alloying Si powder and Mg powder to prepare precursor Mg2And then carrying out dealloying treatment on the Si/Mg composite material, and finally carrying out acid washing, centrifugation and drying on the obtained product to prepare the nano porous silicon.
The dealloying method is used to prepare nano porous material, and solid solution, alloy compound, amorphous alloy, ultrafine crystal alloy, etc. are often selected as precursor. The choice of the precursor alloy has a significant influence on the pore size, pore size distribution and pore volume of the porous material. Wherein, after the alloy compound is dealloyed, mesoporous materials with uniform pore distribution and large pore volume can be obtained, and the pore structure is not obviously related to the size of the precursor. The choice of alloy compound and corrosion system directly determines the efficiency of preparing porous materials and the cost of production. Therefore, the choice of precursor and etching system has always been a key issue for the preparation of nanoporous materials.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a nano porous silicon material.
The invention is realized by the following technical scheme, and provides a preparation method of a nano porous silicon material, which comprises the following steps:
(1) placing Al, Cu and Si metal raw materials into a quartz tube, completely melting the raw materials into a melt by using an electromagnetic induction heating device, and then preserving the heat of the melt above the liquidus temperature of the melt to obtain a uniform melt;
(2) spraying the uniform melt onto the surfaces of copper rollers with different rotating linear speeds by using a single-roller rotary quenching device, and obtaining alloy thin strips with different thicknesses, namely precursor Al-Cu-Si alloy thin strips through a cooling solidification process;
(3) and putting the precursor Al-Cu-Si alloy thin strip into a nitric acid-containing aqueous solution for selective corrosion, taking out the precursor Al-Cu-Si alloy thin strip until no obvious bubbles emerge, and then cleaning and drying the precursor Al-Cu-Si alloy thin strip to obtain the nano porous silicon material.
The preparation method has the advantages of low cost of raw materials, simple process, low requirement on equipment, short production period, high yield, good repeatability and high repeated utilization rate of materials, and the obtained nano porous silicon has the advantages of high specific surface area, small pore diameter, large pore volume, suitability for large-scale production, high economic value and market application value.
Preferably, in the step (1), the metal raw material consists of the following atomic percentages: 40-85% of Al, 10-30% of Si and 5-30% of Cu.
Preferably, in the step (1), the metal raw material is selected from simple substances of Al, Cu and Si or a pre-smelted Al-Cu-Si ternary alloy.
Preferably, in the step (1), the heat preservation temperature of the melt is 800-1100 ℃, and the heat preservation time is at least 2 minutes. To ensure the homogeneity of the composition of the melt alloy.
Preferably, in the step (2), the rotation linear speed of the copper roller is 0.5-30m/s, and the thickness of the obtained precursor Al-Cu-Si alloy thin strip is 23-280 μm.
Preferably, in the step (2), the cooling speed in the cooling solidification process is 250-20000 ℃/s.
Preferably, in the step (3), the aqueous solution containing nitric acid is a nitric acid solution or a mixed solution of nitric acid and hydrochloric acid.
Preferably, in the step (3), the mass fraction of the nitric acid solution is 5-40%, the mass fraction of the nitric acid in the mixed solution of the nitric acid and the hydrochloric acid is 5-40%, and the mass fraction of the hydrochloric acid is 0-25%. Wherein the hydrochloric acid mainly plays a role in accelerating corrosion.
Preferably, in the step (3), the corrosion temperature is controlled to be 20-80 ℃.
Preferably, step (3) further comprises introducing bubbles generated in the corrosion process into the aqueous solution of saturated air for treatment. Bubbles generated in the corrosion process are introduced into a water solution of saturated air, so that the pollution of nitrogen oxides to the environment is eliminated.
The invention has the beneficial effects that:
the preparation method has the advantages of low raw material cost, simple process, low equipment requirement, short production period, high yield, good repeatability and high material recycling rate, and the obtained nano porous silicon has high specific surface area (21.2-42.1 m)2Per g), small pore diameter (19 nm-42 nm) and large pore volume (0.08-0.28 cm)3And/g), is suitable for large-scale production, and has higher economic value and market application value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 SEM scanning spectrum of nano-porous silicon corresponding to example 5 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The application of the principles of the present invention will now be described in further detail with reference to specific embodiments.
Example 1, prepared by the following steps:
(1) placing Al, Cu and Si in an atomic percentage of 85 to 5 to 10 percent in a quartz tube with an opening at the bottom end, completely melting the Al, Cu and Si into a melt by using an electromagnetic induction heating device, and then preserving the heat of the melt at 800 ℃ for 3min to obtain a uniform melt;
(2) spraying the uniform melt to the surface of a copper roller with the linear velocity of 0.5m/s by using a single-roller rotary quenching device, and obtaining an alloy thin strip with the thickness of 280 mu m, namely a precursor Al through the solidification process with the cooling rate of 250 ℃/s85Cu5Si10An alloy thin strip;
(3) preparing 400ml of 5 wt.% nitric acid solution in a 500ml beaker, putting the beaker into a constant-temperature water bath at 20 ℃, and weighing 10g of precursor Al in advance after the water temperature in the beaker is stabilized at 20 DEG C85Cu5Si10Slowly putting the alloy thin strip into a prepared nitric acid solution for selective corrosion, taking out the alloy thin strip until no obvious bubbles emerge, then washing the alloy thin strip by deionized water, and drying the alloy thin strip in a vacuum drying oven to obtain the nano porous silicon material.
The pore volume, the porosity, the specific surface area and the pore size of the nanoporous silicon prepared in the example are shown in table 1.
Example 2, prepared by the following steps:
(1) placing Al, Cu and Si into a quartz tube with an opening at the bottom end according to the atomic percentages of 76 percent to 10 percent to 14 percent, completely melting the Al, Cu and Si into a melt by using an electromagnetic induction heating device, and then preserving the heat of the melt at 850 ℃ for 5min to obtain a uniform melt;
(2) spraying the uniform melt to the surface of a copper roller with the linear velocity of 1.0m/s by using a single-roller rotary quenching device, and obtaining an alloy thin strip with the thickness of 162 mu m, namely a precursor Al through the solidification process with the cooling rate of 1500 ℃/s76Cu10Si14An alloy thin strip;
(3) preparing 400ml of 10 wt.% nitric acid solution in a 500ml beaker, putting the beaker into a constant-temperature water bath at 30 ℃, and weighing 10g of precursor Al in advance after the water temperature in the beaker is stabilized at 30 DEG C76Cu10Si14Slowly putting the alloy thin strip into a prepared nitric acid solution for selective corrosion, taking out the alloy thin strip until no obvious bubbles emerge, then washing the alloy thin strip by deionized water, and drying the alloy thin strip in a vacuum drying oven to obtain the nano porous silicon material.
The pore volume, the porosity, the specific surface area and the pore size of the nanoporous silicon prepared in the example are shown in table 1.
Example 3, prepared by the following steps:
(1) placing Al, Cu and Si into a quartz tube with an opening at the bottom end according to the atomic percentages of 67 percent to 15 percent to 18 percent, completely melting the Al, Cu and Si into a melt by using an electromagnetic induction heating device, and then preserving heat at 920 ℃ for 8min to obtain a uniform melt;
(2) spraying the uniform melt to the surface of a copper roller with the linear velocity of 2.0m/s by using a single-roller rotary quenching device, and obtaining an alloy thin strip with the thickness of 135 mu m, namely a precursor Al through the solidification process with the cooling rate of 3600 ℃/s67Cu15Si18An alloy thin strip;
(3) preparing 400ml of 15 wt.% nitric acid solution in a 500ml beaker, and putting the beaker into a constant-temperature water bath at 40 DEG CAfter the water temperature in the reaction vessel was stabilized at 40 ℃, 10g of the precursor Al was weighed in advance67Cu15Si18Slowly putting the alloy thin strip into a prepared nitric acid solution for selective corrosion, taking out the alloy thin strip until no obvious bubbles emerge, then washing the alloy thin strip by deionized water, and drying the alloy thin strip in a vacuum drying oven to obtain the nano porous silicon material.
The pore volume, the porosity, the specific surface area and the pore size of the nanoporous silicon prepared in the example are shown in table 1.
Example 4, prepared by the following steps:
(1) placing Al, Cu and Si in an atomic ratio of 58 to 20 to 22 in a quartz tube with an opening at the bottom end, completely melting the Al, Cu and Si into a melt by using an electromagnetic induction heating device, and then preserving the heat at 960 ℃ for 10min to obtain a uniform melt;
(2) spraying the uniform melt to the surface of a copper roller with the linear velocity of 5.0m/s by using a single-roller rotary quenching device, and obtaining an alloy thin strip with the thickness of 96 mu m, namely a precursor Al through the solidification process with the cooling rate of 7200 ℃/s58Cu20Si22An alloy thin strip;
(3) preparing 400ml of 25 wt.% nitric acid solution in a 500ml beaker, putting the beaker into a constant-temperature water bath at 50 ℃, and weighing 10g of precursor Al in advance after the water temperature in the beaker is stabilized at 50 DEG C58Cu20Si22Slowly putting the alloy thin strip into a prepared nitric acid solution for selective corrosion, taking out the alloy thin strip until no obvious bubbles emerge, then washing the alloy thin strip by deionized water, and drying the alloy thin strip in a vacuum drying oven to obtain the nano porous silicon material.
The pore volume, the porosity, the specific surface area and the pore size of the nanoporous silicon prepared in the example are shown in table 1.
Example 5, prepared by the following steps:
(1) placing Al, Cu and Si into a quartz tube with an opening at the bottom end according to atomic percentages of 49 percent, 25 percent and 26 percent, completely melting the Al, Cu and Si into a melt by using an electromagnetic induction heating device, and then preserving heat at 1000 ℃ for 10min to obtain a uniform melt;
(2) spraying the uniform melt to the surface of a copper roller with the linear velocity of 15.0m/s by using a single-roller rotary quenching device, and obtaining an alloy thin strip with the thickness of 47 mu m, namely a precursor Al through the solidification process with the cooling rate of 15200 ℃/s49Cu25Si26An alloy thin strip;
(3) preparing 400ml of a mixed solution of 30 wt.% nitric acid and 10% hydrochloric acid in a 500ml beaker, putting the beaker into a constant-temperature water bath at 60 ℃, and weighing 10g of precursor Al in advance after the water temperature in the beaker is stabilized at 60 DEG C49Cu25Si26Slowly putting the alloy thin strip into a prepared nitric acid solution for selective corrosion, taking out the alloy thin strip until no obvious bubbles emerge, then washing the alloy thin strip by deionized water, and drying the alloy thin strip in a vacuum drying oven to obtain the nano porous silicon material.
The pore volume, the porosity, the specific surface area and the pore size of the nanoporous silicon prepared in the example are shown in table 1.
Example 6, prepared by the following steps:
(1) placing Al, Cu and Si into a quartz tube with an opening at the bottom end according to the atomic percentages of 40: 30%, completely melting the Al, Cu and Si into a melt by using an electromagnetic induction heating device, and then preserving heat at 1100 ℃ for 6min to obtain a uniform melt;
(2) spraying the uniform melt onto the surface of a copper roller with the linear velocity of 30.0m/s by using a single-roller rotary quenching device, and obtaining an alloy thin strip with the thickness of 23 mu m, namely a precursor Al through the solidification process with the cooling rate of 20000 ℃/s40Cu30Si30An alloy thin strip;
(3) preparing 400ml of 40 wt.% nitric acid solution in a 500ml beaker, putting the beaker into a constant-temperature water bath at 80 ℃, and weighing 10g of precursor Al in advance after the water temperature in the beaker is stabilized at 80 DEG C40Cu30Si30Slowly putting the alloy thin strip into a prepared nitric acid solution for selective corrosion, taking out the alloy thin strip until no obvious bubbles emerge, then washing the alloy thin strip by deionized water, and drying the alloy thin strip in a vacuum drying oven to obtain the nano porous silicon material.
The pore volume, the porosity, the specific surface area and the pore size of the nanoporous silicon prepared in the example are shown in table 1.
The experimental conditions, pore volume, porosity, specific surface area and pore size of the obtained nanoporous silicon of the examples listed in the present invention are shown in table 1. As can be seen from table 1, in all the examples, nanoporous silicon materials were obtained. With the increase of the rotation speed of the copper roller, the thickness of the precursor alloy is reduced, the pore volume, the porosity and the specific surface area of the obtained nano-porous silicon are increased, and the pore size is reduced. Therefore, the pore structure of the porous silicon can be effectively adjusted by controlling the composition of the alloy and the rotation speed of the copper roller. It can be found by comparing all the examples that the nanoporous silicon prepared under the conditions of example 5 has the optimal pore structure. By combining the above embodiments, it can be found that the higher the content of silicon in the precursor alloy is, the higher the concentration of the etching solution is required, and the higher the etching temperature is.
The nano porous silicon material prepared in example 5 is tested by a scanning electron microscope, and the test result is shown in the SEM scanning spectrum of fig. 1, and as can be seen from fig. 1, the prepared porous silicon is a continuous ligament pore structure, has a pore size of 20 to 50nm, belongs to a mesoporous material, and is a nano porous material with a high specific surface area.
Table 1 shows the pore volume, porosity, specific surface area, and pore diameter of the samples of the examples of the present invention
Of course, the above description is not limited to the above examples, and the undescribed technical features of the present invention can be implemented by or using the prior art, and will not be described herein again; the above embodiments and drawings are only for illustrating the technical solutions of the present invention and not for limiting the present invention, and the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that changes, modifications, additions or substitutions within the spirit and scope of the present invention may be made by those skilled in the art without departing from the spirit of the present invention, and shall also fall within the scope of the claims of the present invention.
Claims (4)
1. A preparation method of a nano porous silicon material comprises the following steps:
(1) placing Al, Cu and Si metal raw materials into a quartz tube, completely melting the raw materials into a melt by using an electromagnetic induction heating device, and then preserving the heat of the melt above the liquidus temperature of the melt to obtain a uniform melt; the metal raw material comprises the following atomic percentages: 40-85% of Al, 10-30% of Si and 5-30% of Cu;
(2) spraying the uniform melt to the surface of a copper roller with the rotation linear speed of 0.5-30m/s by using a single-roller rotary quenching device, and obtaining an alloy thin strip with the thickness of 23-280 mu m, namely a precursor Al-Cu-Si alloy thin strip, through a cooling solidification process at the cooling speed of 250-20000 ℃/s;
(3) putting the precursor Al-Cu-Si alloy thin strip into an aqueous solution containing nitric acid for selective corrosion, controlling the corrosion temperature at 20-80 ℃, taking out until no obvious bubbles emerge, then cleaning and drying to obtain the nano porous silicon material;
the aqueous solution containing nitric acid is a mixed solution of nitric acid and hydrochloric acid, the mass fraction of the nitric acid in the mixed solution of nitric acid and hydrochloric acid is 5-40%, and the mass fraction of the hydrochloric acid is 10-25%;
the obtained nano porous silicon material has a specific surface area of 21.2-42.1m2The pore diameter is 19nm-42nm, and the pore volume is 0.08-0.28cm3/g。
2. The method of claim 1, wherein the method comprises the following steps: in the step (1), the metal raw material is selected from simple substances of Al, Cu and Si or pre-smelted Al-Cu-Si ternary alloy.
3. The method of claim 1, wherein the method comprises the following steps: in the step (1), the heat preservation temperature of the melt is 800-1100 ℃, and the heat preservation time is at least 2 minutes.
4. The method of claim 1, wherein the method comprises the following steps: and (3) introducing bubbles generated in the corrosion process into a saturated air aqueous solution for treatment.
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| CN103118976A (en) * | 2010-09-17 | 2013-05-22 | 古河电气工业株式会社 | Porous silicon particle, porous silicon complex particle and methods for manufacturing thereof |
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