CN111321454A - Method for preparing luminous porous silicon in parallel arrangement - Google Patents
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- CN111321454A CN111321454A CN202010145601.7A CN202010145601A CN111321454A CN 111321454 A CN111321454 A CN 111321454A CN 202010145601 A CN202010145601 A CN 202010145601A CN 111321454 A CN111321454 A CN 111321454A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25F3/02—Etching
- C25F3/12—Etching of semiconducting materials
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- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
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Abstract
The invention provides a method for preparing luminescent porous silicon in parallel arrangement, which comprises the following steps: 1) ultrasonically cleaning a silicon wafer; 2) preparing corrosive liquid 2; 3) taking a plurality of platinum electrodes 7, wherein each platinum electrode 7 consists of a platinum sheet 9 and a platinum wire 6, placing a P-type monocrystalline silicon wafer 8 between every two platinum electrodes 7, fixing the silicon wafer 4) by using a clamping plate 5-1, a clamping plate 5-2, a bolt 3 and a nut 4), putting the fixed silicon wafer into a container 1, and adding a corrosive liquid 2; 5) according to the sequence from left to right, the odd platinum wires 6 are connected to the anode of a power supply, the even platinum wires 6 are connected to the cathode of the power supply, and a sinusoidal current-X-YmA is introduced, wherein the values of X and Y are 10-400, and the period of the sinusoidal current is 5-30 s; 6) and cleaning the reacted silicon wafer to obtain the double-sided porous silicon wafer. The invention solves the problem that only one porous silicon wafer can be prepared in one electrochemical anodic corrosion experiment, and realizes the preparation of a plurality of double-sided porous silicon wafers by one corrosion.
Description
Technical Field
The invention relates to a preparation method of porous silicon, in particular to a method for preparing luminescent porous silicon in parallel arrangement.
Background
The porous silicon is a porous material with nanometer silicon atom clusters as a framework. Because of its good electroluminescent property, photoluminescence property, unique dielectric property and large specific surface area and hole controllability, it has wide application in the fields of biological and chemical sensors, photoelectric devices, integrated circuits, biological imaging, drug delivery, solar cells and photoelectric communication.
At present, the preparation method of porous silicon mainly comprises an electrochemical anodic corrosion method, a hydrothermal corrosion method, a spark corrosion method, a light radiation assisted chemical corrosion method and the like, wherein the electrochemical anodic corrosion method is the most commonly used method. According to the characteristics of the electrochemical etching method, the electrochemical etching device is designed into a single groove and a double groove. The single-groove etching method is characterized in that one surface of a silicon wafer is directly connected with a copper sheet or aluminum sheet electrode, the copper sheet or aluminum sheet is connected with the anode of a power supply, the other surface of the silicon wafer is contacted with hydrofluoric acid etching liquid, a platinum wire electrode in the etching liquid is connected with the cathode of the power supply, and the silicon wafer is etched by hydrofluoric acid to generate a porous silicon layer under the power-on condition. The double-groove etching method is similar to the method of sticking the bottoms of two single grooves together and placing a silicon wafer in the middle. That is, in the double-bath etching method, both sides of a silicon wafer are filled with an etching solution, the silicon wafer is fixed in the middle, the silicon wafer divides the electrolytic bath into two independent electrolytic baths, and two platinum sheets are respectively used as a cathode and an anode. At present, the porous silicon is prepared by an electrochemical anodic corrosion method, only one piece of porous silicon can be prepared in one experiment, the whole silicon wafer is not corroded into the porous silicon, only a part of the part which is contacted with a corrosive liquid is changed into the porous silicon, and the preparation needs to be repeated when enough porous silicon is required to be obtained. Particularly in the fields of drug delivery, batteries and the like, the amount of porous silicon powder required for one drug delivery or battery experiment needs to be repeatedly prepared many times.
Disclosure of Invention
The invention aims to provide a method for preparing light-emitting porous silicon in parallel arrangement, which solves the problem that only one porous silicon wafer can be prepared in one electrochemical anodic corrosion experiment and realizes the preparation of a plurality of porous silicon wafers in one corrosion.
The invention provides a method for preparing luminescent porous silicon in parallel arrangement, which is characterized by sequentially comprising the following steps of:
1) sequentially putting a P-type monocrystalline silicon wafer 8 with the thickness of 400-1000 mu m into acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-15 min, removing surface dirt, and naturally airing in the air for later use;
2) mixing absolute ethyl alcohol and 40% hydrofluoric acid solution according to the volume ratio of 1: 6-2: 1 to prepare corrosive liquid 2;
3) taking a plurality of platinum electrodes 7, wherein each platinum electrode 7 consists of a platinum sheet 9 and a platinum wire 6, a P-type monocrystalline silicon wafer 8 is placed between every two platinum electrodes 7, the platinum wires 6 are vertically upward, then the platinum electrodes are clamped from two ends by using a clamping plate 5-1 and a clamping plate 5-2, four bolts 3 respectively penetrate through round holes 11 corresponding to the clamping plate 5-1 and the clamping plate 5-2, and then the clamping plate 5-1 and the clamping plate 5-2 are fixed by using nuts 4;
4) placing the device fixed in the step 3) at the bottom of a container 1, pouring the corrosive liquid 2 in the step 2) into the container 1, and enabling the liquid level of the corrosive liquid to be higher than the height of the P-type monocrystalline silicon wafer 8 in the step 3);
5) connecting all the odd-numbered platinum wires 6 to the anode of the same power supply, connecting all the even-numbered platinum wires 6 to the cathode of the same power supply, and introducing sinusoidal current-X-YmA, wherein the values of X and Y are between 10 and 400, the period of the sinusoidal current is 5 to 30s, and the total time length is 60 to 240 min;
6) and taking out the reacted P-type monocrystalline silicon wafer 8, cleaning the P-type monocrystalline silicon wafer with absolute ethyl alcohol, drying the P-type monocrystalline silicon wafer at room temperature to obtain a double-sided porous silicon sample, and emitting visible light from the porous silicon under the irradiation of ultraviolet light.
The P-type monocrystalline silicon wafer 8 in the step 1) is a rectangular silicon wafer, and the length and width of the silicon wafer are equal to those of the platinum sheet 9.
Two parallel platinum wires 10 are respectively welded on two surfaces of the platinum sheet 9 in the step 3), the distance between the two platinum wires 10 on each surface is smaller than the width of the silicon wafer, and the platinum wires 10 are parallel to the platinum wires 6.
The container 1, the bolt 3, the nut 4, the plate 5-1 and the clamping plate 5-2 are made of polytetrafluoroethylene.
The method is different from the common electrochemical corrosion method for preparing the porous silicon. A common electrochemical corrosion method can only prepare a piece of porous silicon once, and a single-groove corrosion method can only corrode one part of one surface of a silicon wafer once. In the invention, a plurality of platinum wires 6, a plurality of platinum electrodes 7 and a plurality of P-type monocrystalline silicon wafers 8 are all fixed by utilizing a clamping plate 5-1 and a clamping plate 5-2, and then are electrified and corroded in a corrosive liquid 2; in the reaction process, due to the existence of the platinum wire 10, a sufficient gap is formed between each platinum sheet 9 and the adjacent P-type monocrystalline silicon piece 8 to allow the corrosive liquid 2 to flow, so that two surfaces of each P-type monocrystalline silicon piece 8 are in direct contact with the corrosive liquid 2; because the platinum wires 6 are in the order from left to right, all the odd platinum wires 6 are connected with the anode of the same power supply, and all the even platinum wires 6 are connected with the cathode of the same power supply, the two surfaces of each P-type monocrystalline silicon piece 8 have the same potential difference; and because the introduced sinusoidal current is-X-YmA, and the values of X and Y are between 10 and 400, the current has positive and negative exchange, so that both sides of each P-type monocrystalline silicon piece 8 can be corroded. Therefore, the method can prepare a plurality of double-sided etched porous silicon wafers at one time.
The method has the advantages that a plurality of pieces of porous silicon with double-sided corrosion can be prepared by one experiment, and the method is simple and convenient to operate, low in cost and more suitable for industrial application.
Drawings
Fig. 1 is a schematic structural diagram of the overall device of the present invention.
Fig. 2 is a schematic front view of the platinum electrode 7.
Fig. 3 is a schematic side view of the platinum electrode 7.
Fig. 4 is a schematic structural view of the splint 5-1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but the present invention is not limited thereto.
The invention provides a method for preparing luminescent porous silicon in parallel arrangement, which is characterized by sequentially comprising the following steps of:
1) sequentially putting a P-type monocrystalline silicon wafer 8 with the thickness of 400-1000 mu m into acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-15 min, removing surface dirt, and naturally airing in the air for later use;
2) mixing absolute ethyl alcohol and 40% hydrofluoric acid solution according to the volume ratio of 1: 6-2: 1 to prepare corrosive liquid 2;
3) taking a plurality of platinum electrodes 7, wherein each platinum electrode 7 consists of a platinum sheet 9 and a platinum wire 6, a P-type monocrystalline silicon wafer 8 is placed between every two platinum electrodes 7, the platinum wires 6 are vertically upward, then the platinum electrodes are clamped from two ends by using a clamping plate 5-1 and a clamping plate 5-2, four bolts 3 respectively penetrate through round holes 11 corresponding to the clamping plate 5-1 and the clamping plate 5-2, and then the clamping plate 5-1 and the clamping plate 5-2 are fixed by using nuts 4;
4) placing the device fixed in the step 3) at the bottom of a container 1, pouring the corrosive liquid 2 in the step 2) into the container 1, and enabling the liquid level of the corrosive liquid to be higher than the height of the P-type monocrystalline silicon wafer 8 in the step 3);
5) connecting all the odd-numbered platinum wires 6 to the anode of the same power supply, connecting all the even-numbered platinum wires 6 to the cathode of the same power supply, and introducing sinusoidal current-X-YmA, wherein the values of X and Y are between 10 and 400, the period of the sinusoidal current is 5 to 30s, and the total time length is 60 to 240 min;
6) and taking out the reacted P-type monocrystalline silicon wafer 8, cleaning the P-type monocrystalline silicon wafer with absolute ethyl alcohol, drying the P-type monocrystalline silicon wafer at room temperature to obtain a double-sided porous silicon sample, and emitting visible light from the porous silicon under the irradiation of ultraviolet light.
In the present invention, the sources of all raw materials are not particularly limited, and they may be commercially available.
Referring to fig. 1, in the method for preparing luminescent porous silicon in parallel arrangement, the device comprises a container 1, an etching solution 2, a bolt 3, a nut 4, a clamping plate 5-1 and a clamping plate 5-2, a platinum wire 6, a platinum electrode 7 and a P-type monocrystalline silicon piece 8, wherein the platinum electrode 7 and the P-type monocrystalline silicon piece 8 are alternately arranged.
Referring to fig. 2 and 3, the platinum electrode 7 is composed of a platinum wire 6 and a platinum sheet 9, and two platinum wires 10 parallel to the platinum wire 6 are welded to the upper surface and the lower surface of the platinum sheet 9, respectively.
Referring to fig. 4, the clamping plate 5-1 and the clamping plate 5-2 are respectively provided with four round holes, and all platinum electrodes 7 and P-type monocrystalline silicon wafers 8 in the middle are fixed by adjusting four bolts 3 and four nuts 4.
In the invention, all the odd platinum wires 6 are connected to the anode of the same power supply and all the even platinum wires 6 are connected to the cathode of the same power supply in sequence from left to right, so that each P-type monocrystalline silicon piece 8 is under the same potential difference, besides, the current is introduced in a sine current-X-YmA, the values of X and Y are 10-400, the period is 5-30 s, and the flowing direction of the current is periodically and alternately changed, so that both sides of each P-type monocrystalline silicon piece 8 can be corroded.
In the invention, the distance between two platinum wires 10 on each surface of the platinum sheet 9 is smaller than the width of the P-type monocrystalline silicon piece 8, so that the platinum wires 10 support a certain gap between the platinum sheet 9 and the P-type monocrystalline silicon piece 8, and the platinum wires 10 on the same platinum sheet 9 are vertically parallel, thus not only enabling the corrosive liquid to freely flow, but also enabling the gas generated by the reaction to be quickly discharged.
In order to further illustrate the present invention, the following will describe the method for preparing luminescent porous silicon in parallel alignment according to the present invention in detail with reference to the examples.
Example 1
1) Sequentially putting the P-type monocrystalline silicon wafer 8 with the thickness of 600 mu m into acetone, ethanol and deionized water, respectively ultrasonically cleaning for 10min to remove surface dirt, and naturally airing in the air for later use;
2) mixing absolute ethyl alcohol and 40% hydrofluoric acid solution according to the volume ratio of 1:1 to prepare corrosive liquid 2;
3) taking a plurality of platinum electrodes 7, wherein each platinum electrode 7 consists of a platinum sheet 9 and a platinum wire 6, a P-type monocrystalline silicon wafer 8 is placed between every two platinum electrodes 7, the platinum wires 6 are vertically upward, then the platinum electrodes are clamped from two ends by using a clamping plate 5-1 and a clamping plate 5-2, four bolts 3 respectively penetrate through round holes 11 corresponding to the clamping plate 5-1 and the clamping plate 5-2, and then the clamping plate 5-1 and the clamping plate 5-2 are fixed by using nuts 4;
4) placing the device fixed in the step 3) at the bottom of a container 1, pouring the corrosive liquid 2 in the step 2) into the container 1, and enabling the liquid level of the corrosive liquid to be higher than the height of the P-type monocrystalline silicon wafer 8 in the step 3);
5) connecting all the odd platinum wires 6 to the anode of the same power supply, connecting all the even platinum wires 6 to the cathode of the same power supply, and introducing a sinusoidal current of-200 mA, wherein the period of the sinusoidal current is 15s, and the total time duration is 120min according to the sequence from left to right of the platinum wires 6 in the step 3);
6) and taking out the reacted P-type monocrystalline silicon wafer 8, cleaning the P-type monocrystalline silicon wafer with absolute ethyl alcohol, drying the P-type monocrystalline silicon wafer at room temperature to obtain a double-sided porous silicon sample, and emitting visible light from the porous silicon under the irradiation of ultraviolet light.
Example 2
1) Sequentially putting the P-type monocrystalline silicon wafer 8 with the thickness of 400 mu m into acetone, ethanol and deionized water, respectively ultrasonically cleaning for 10min to remove surface dirt, and naturally airing in the air for later use;
2) mixing absolute ethyl alcohol and 40% hydrofluoric acid solution according to the volume ratio of 2:1 to prepare corrosive liquid 2;
3) taking a plurality of platinum electrodes 7, wherein each platinum electrode 7 consists of a platinum sheet 9 and a platinum wire 6, a P-type monocrystalline silicon wafer 8 is placed between every two platinum electrodes 7, the platinum wires 6 are vertically upward, then the platinum electrodes are clamped from two ends by using a clamping plate 5-1 and a clamping plate 5-2, four bolts 3 respectively penetrate through round holes 11 corresponding to the clamping plate 5-1 and the clamping plate 5-2, and then the clamping plate 5-1 and the clamping plate 5-2 are fixed by using nuts 4;
4) placing the device fixed in the step 3) at the bottom of a container 1, pouring the corrosive liquid 2 in the step 2) into the container 1, and enabling the liquid level of the corrosive liquid to be higher than the height of the P-type monocrystalline silicon wafer 8 in the step 3);
5) connecting all the odd platinum wires 6 to the anode of the same power supply, connecting all the even platinum wires 6 to the cathode of the same power supply, and introducing a sinusoidal current of-10 mA, wherein the period of the sinusoidal current is 30s, and the total time length is 240min according to the sequence from left to right of the platinum wires 6 in the step 3);
6) and taking out the reacted P-type monocrystalline silicon wafer 8, cleaning the P-type monocrystalline silicon wafer with absolute ethyl alcohol, drying the P-type monocrystalline silicon wafer at room temperature to obtain a double-sided porous silicon sample, and emitting visible light from the porous silicon under the irradiation of ultraviolet light.
Example 3
1) Sequentially putting a P-type monocrystalline silicon wafer 8 with the thickness of 1000 mu m into acetone, ethanol and deionized water, respectively ultrasonically cleaning for 10min, removing surface dirt, and naturally airing in the air for later use;
2) mixing absolute ethyl alcohol and 40% hydrofluoric acid solution according to the volume ratio of 1:6 to prepare corrosive liquid 2;
3) taking a plurality of platinum electrodes 7, wherein each platinum electrode 7 consists of a platinum sheet 9 and a platinum wire 6, a P-type monocrystalline silicon wafer 8 is placed between every two platinum electrodes 7, the platinum wires 6 are vertically upward, then the platinum electrodes are clamped from two ends by using a clamping plate 5-1 and a clamping plate 5-2, four bolts 3 respectively penetrate through round holes 11 corresponding to the clamping plate 5-1 and the clamping plate 5-2, and then the clamping plate 5-1 and the clamping plate 5-2 are fixed by using nuts 4;
4) placing the device fixed in the step 3) at the bottom of a container 1, pouring the corrosive liquid 2 in the step 2) into the container 1, and enabling the liquid level of the corrosive liquid to be higher than the height of the P-type monocrystalline silicon wafer 8 in the step 3);
5) connecting all the odd platinum wires 6 to the anode of the same power supply, connecting all the even platinum wires 6 to the cathode of the same power supply, and introducing a sinusoidal current of-400 mA, wherein the period of the sinusoidal current is 5s, and the total time duration is 60min according to the sequence from left to right of the platinum wires 6 in the step 3);
6) and taking out the reacted P-type monocrystalline silicon wafer 8, cleaning the P-type monocrystalline silicon wafer with absolute ethyl alcohol, drying the P-type monocrystalline silicon wafer at room temperature to obtain a double-sided porous silicon sample, and emitting visible light from the porous silicon under the irradiation of ultraviolet light.
Claims (4)
1. A method for preparing luminescent porous silicon in parallel arrangement is characterized by sequentially comprising the following steps:
1) sequentially putting a P-type monocrystalline silicon wafer 8 with the thickness of 400-1000 mu m into acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-15 min, removing surface dirt, and naturally airing in the air for later use;
2) mixing absolute ethyl alcohol and 40% hydrofluoric acid solution according to the volume ratio of 1: 6-2: 1 to prepare corrosive liquid 2;
3) taking a plurality of platinum electrodes 7, wherein each platinum electrode 7 consists of a platinum sheet 9 and a platinum wire 6, a P-type monocrystalline silicon wafer 8 is placed between every two platinum electrodes 7, the platinum wires 6 are vertically upward, then the platinum electrodes are clamped from two ends by using a clamping plate 5-1 and a clamping plate 5-2, four bolts 3 respectively penetrate through round holes 11 corresponding to the clamping plate 5-1 and the clamping plate 5-2, and then the clamping plate 5-1 and the clamping plate 5-2 are fixed by using nuts 4;
4) placing the device fixed in the step 3) at the bottom of a container 1, pouring the corrosive liquid 2 in the step 2) into the container 1, and enabling the liquid level of the corrosive liquid to be higher than the height of the P-type monocrystalline silicon wafer 8 in the step 3);
5) connecting all the odd-numbered platinum wires 6 to the anode of the same power supply, connecting all the even-numbered platinum wires 6 to the cathode of the same power supply, and introducing sinusoidal current-X-YmA, wherein the values of X and Y are between 10 and 400, the period of the sinusoidal current is 5 to 30s, and the total time length is 60 to 240 min;
6) and taking out the reacted P-type monocrystalline silicon wafer 8, cleaning the P-type monocrystalline silicon wafer with absolute ethyl alcohol, drying the P-type monocrystalline silicon wafer at room temperature to obtain a double-sided porous silicon sample, and emitting visible light from the porous silicon under the irradiation of ultraviolet light.
2. The method for preparing light-emitting porous silicon in parallel arrangement according to claim 1, wherein the P-type monocrystalline silicon wafer 8 in step 1) is a rectangular silicon wafer, and the length and width of the silicon wafer are equal to those of the platinum sheet 9.
3. The method for preparing light-emitting porous silicon in parallel arrangement according to claim 1, wherein two parallel platinum wires 10 are welded on two surfaces of the platinum sheet 9 in the step 3), the distance between the two platinum wires 10 on each surface is smaller than the width of the silicon wafer, and the platinum wires 10 are parallel to the platinum wires 6.
4. The method for preparing luminescent porous silicon in parallel arrangement according to claim 1, wherein the material of the container 1, the bolt 3, the nut 4, the plate 5-1 and the clamping plate 5-2 is polytetrafluoroethylene.
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