CN114163135A - Low-pressure corrosion device and method for quartz microporous plate - Google Patents

Low-pressure corrosion device and method for quartz microporous plate Download PDF

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Publication number
CN114163135A
CN114163135A CN202111500933.3A CN202111500933A CN114163135A CN 114163135 A CN114163135 A CN 114163135A CN 202111500933 A CN202111500933 A CN 202111500933A CN 114163135 A CN114163135 A CN 114163135A
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China
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cup
solution
corrosion
microporous plate
quartz
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CN202111500933.3A
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CN114163135B (en
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孙伟民
严云翔
刘世杰
陈旭东
耿涛
闫奇
王佳斌
金夕人
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Harbin Engineering University
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Harbin Engineering University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00Surface treatment of glass, not in the form of fibres or filaments, by etching
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a low-pressure corrosion method for a quartz microporous plate, and belongs to the field of processing technologies. When the size of the micropores in the quartz microporous plate is smaller than the required size, a corrosion reaming method is provided. The method achieves the purpose of enlarging the pore diameter of the micropores by corroding the quartz plate through the corrosive solution, and because bubbles in the corrosive solution can cause uneven corrosion. The device for manufacturing the low pressure consists of a vacuum air pump, a first solution cup, a second solution cup, an etching solution, a plurality of air valves and a connecting conduit.

Description

Low-pressure corrosion device and method for quartz microporous plate
Technical Field
The invention relates to the field of processing technologies, in particular to a low-pressure corrosion device and method for a quartz microporous plate.
Background
In some special applications, a quartz microplate with a large number of micropores is required. When an actual quartz micropore plate is processed, the diameter of micropores on an actual plate is slightly smaller than that required due to factors such as overlarge manufacturing error or unreasonable design. In this case, rework is costly and time consuming. And the reaming of the large number of quartz micropores can be carried out by adopting a solution etching method. In the corrosion process of the microporous plate, microbubbles are separated out from the corrosion solution due to heating, stirring and the like and are easily attached to the micropores, so that the quartz at the position cannot contact the corrosion solution, the corrosion rate of each micropore is different, and the single micropore is uneven.
Disclosure of Invention
The purpose of the invention is as follows: in order to enlarge micropores on a quartz micropore plate and enable the micropore plate to meet the actual requirement, a micropore plate reaming method is provided, and a set of device is designed. The method utilizes a low-pressure environment to pump out the bubbles in the solution, and avoids uneven corrosion caused by blocking of the micropores by the bubbles. The method can uniformly and controllably enlarge the size of the micropores, and saves the cost of secondary processing.
A low-pressure corrosion device for a quartz microporous plate comprises a vacuum air pump, a first solution cup, a second solution cup, a corrosion solution, an air valve and a connecting conduit; the first solution cup is respectively connected with the second solution cup, the vacuum air pump and the corrosion cup through three guide pipes and corresponding air valves, the guide pipe connected with the second solution cup and the vacuum air pump is inserted shallowly in the first solution cup, and the guide pipe connected with the corrosion cup is inserted deeply; the second solution cup is respectively connected with the first solution cup, the vacuum air pump and the corrosion cup through three guide pipes and corresponding air valves, the guide pipe connected with the corrosion cup and the vacuum air pump is inserted shallowly in the second solution cup, and the guide pipe connected with the first solution cup is inserted deeply; the corrosion cup is respectively connected with the first solution cup and the second solution cup through two guide pipes and corresponding air valves, the guide pipe connected with the first solution cup is inserted shallowly in the corrosion cup, the guide pipe connected with the second solution cup is inserted deeply, and the corrosion cup is used for placing a microporous plate to be corroded; the method comprises the steps of putting a corrosion solution in a first solution cup, opening a vacuum air pump to pump air from a second solution cup and the corrosion cup, enabling the solution in the first solution cup to flow into the corrosion cup and the second solution cup by utilizing air pressure difference, pumping air from the first solution cup, enabling the solution in the second solution cup to return to the first solution cup, and then performing multiple circulation operations to further reduce the air pressure in the corrosion cup, wherein the corrosion solution reacts with a microporous plate, so that the aperture of the micropore is enlarged.
Furthermore, sealing cup covers are arranged on the corrosion cup, the first solution cup and the second solution cup.
A low-pressure corrosion method for a quartz microporous plate comprises the following steps:
preparing an etching solution;
connecting a low pressure corrosion device according to claim 1 or 2;
manufacturing a near-vacuum low-pressure environment to separate out micro bubbles in the corrosive solution;
and placing the etching solution and the microporous plate into a proper temperature environment to start etching.
Compared with the prior art, the invention has the beneficial effects that:
under the condition that the size of the micropores in the processed quartz microporous plate is smaller than the required size, the method does not need to be processed again, the method is used for corroding and reaming to meet the requirement, and unnecessary production cost and time cost are reduced.
Compared with other hole enlarging methods, the method has the advantages of simple operation and low cost, micropores with any size can be obtained by controlling the corrosion time, and the hole enlarging size is controllable.
The method reduces the quantity of the bubbles in the solution through the device according to the principle that the bubbles in the solution can influence the uniformity of corrosion, which is particularly important for micropores which are easily blocked by gas in a liquid environment, and the bubbles blocked in the micropores are extracted to ensure that the corrosive solution can be fully contacted with the micropores, so that the corrosion rate is more uniform, and the corrosion effect is more remarkable.
Drawings
FIG. 1 is a schematic structural diagram of the preparation of an etching solution for a microplate according to the present invention;
wherein, each reference number in the figure means: 1 is a sealing cup cover, 2 is a first solution cup 2, 3 is a corrosion cup 3, 4 is a microporous plate, 5 is a solution cup 5, 6 is an air pump, and 7-11 is an air valve switch.
Detailed Description
The invention provides a low-pressure corrosion method of a quartz microporous plate, which comprises the following steps:
1) and preparing a solution required by corrosion.
2) The air pump 6, the first solution cup 2, the second solution cup 5, the etching cup 3, the conduit and the air valve are connected together as shown in the figure.
3) The corrosive solution is put into the first solution cup 2, the microporous plate 6 is put into the corrosive cup 3, and all joints are sealed to ensure no air leakage.
4) The solution replacement was performed according to a procedure, which was repeated several times so that the etching solution was present in the etching cup 3 and the gas pressure was as low as possible.
5) The etching cup 3 is opened and is etched for a certain time at a specified temperature together with the etching solution and the microplate 6 therein.
The technical solution of the present invention will be described in detail with reference to specific examples, but the following examples are only preferred embodiments of the present invention, and not all embodiments. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
The microporous plate material to be reamed in this example is quartz, and the microporous plate is used for fixing the optical fiber at the array end of the integrating field unit. Due to the machining precision, the micro-holes are slightly small in size and cannot pass through the optical fibers. The specific operation comprises the following steps:
1) a56.1 g/mol KOH solution was prepared. The KOH reagent used had a KOH content of 85%. According to the volume of the etching cup 3, 400ml of the solution is prepared. 211g of KOH reagent was measured out and put into an etching cup 3, and deionized water was slowly added to 400ml while stirring with a glass rod.
2) And opening a heating switch of the constant-temperature ultrasonic cleaning instrument, setting the heating temperature to be 80 ℃, preheating for 30 minutes (oscillating for 5 minutes), and enabling the cleaning instrument to enter constant-temperature circulation.
3) And putting the microporous plate and the clamp into a small ultrasonic cleaner for oscillation cleaning for 3 minutes.
4) The microplate with the holder is placed in the etching cup 3, the vacuum apparatus is connected as shown in fig. 1, and the sealing at the interface is ensured.
5) Manufacturing a microporous plate in a low-pressure corrosion environment:
a) vacuum pumping
Firstly ensuring that 5 air valves are closed, firstly opening the air pump 6, then opening the air valves 10 and 8 in sequence, and waiting for a period of time to enable the corrosion cup 3 and the second solution cup 5 to enter a near vacuum state. The air valves 8 and 10 are then closed and the air pump is turned off.
b) Feeding the solution
Ensure 5 valves are closed, slowly open air valve 7, and control air valve 8 to allow the solution in solution cup 2 to slowly flow into corrosion cup 3 while excess solution enters second solution cup 5. And closing the air valves 8 and 7 in sequence when the corrosive solution passes through the microporous plate.
c) Replacement solution
After ensuring that the 5 air valves are all in a closed state, the air pump is opened, the air valves 9 and 11 are opened in sequence, and when almost all the solution in the second solution cup 5 enters the first solution cup 2, the solution replacement from the second solution cup 5 to the first solution cup 2 is completed. The air valves 11 and 9 are closed and the air pump 6 is then turned off.
d) Circulating air extraction
After the solution replacement is completed, the steps a) and b) are carried out. The circulation is carried out for 2-3 times. And finishing the solution filling in the micropores.
6) The vacuum circulating conduit is pulled out, the corrosion cup is placed in an ultrasonic cleaning instrument, and the PVC plate is pressed to prevent side turning.
7) And measuring the temperature of the corrosive solution by using a temperature measuring probe, and starting timing when the temperature of the solution is 80 ℃. The etching time is set according to the actual size of the micropores, and the microplate holders can be slightly shaken in the solution during the etching process (the step is to eliminate bubbles generated by ultrasonic oscillation and attached to the vicinity of the micropores).
8) And (4) taking out the microporous plate after the corrosion time is over, putting the microporous plate into a small ultrasonic cleaning instrument for vibration cleaning for 5 minutes, and drying the microporous plate by using compressed air after the microporous plate is taken out.
After the experiment after corroding for a certain time, the optical fiber can pass through the micropores, and the sizes of the micropores are more uniform after measurement. The method is proved to be effective.
The object of the invention has been achieved completely effectively by the embodiments described above. It will be appreciated by persons skilled in the art that the present invention includes, but is not limited to, the description of the embodiments above. Any modifications that do not depart from the invention are intended to be included within the scope of the appended claims.
The invention discloses a low-pressure corrosion method for a quartz microporous plate, and belongs to the field of processing technologies. When the size of the micropores in the quartz microporous plate is smaller than the required size, a corrosion reaming method is provided. The method uses the etching solution to etch the quartz plate to achieve the purpose of enlarging the aperture of the micropore. The invention provides a low-pressure corrosion method which can reduce the number of bubbles in a solution and enable the corrosion rate of a quartz microporous plate to be more balanced, because the bubbles in a corrosion solution can cause uneven corrosion. The device for manufacturing the low pressure consists of a vacuum air pump 6, a first solution cup 2, a second solution cup 5, an etching cup 3, an etching solution, a plurality of air valves and a connecting conduit. The etching cup can be pumped to be close to vacuum through a specific operation step, so that bubbles are separated out. Is beneficial to the uniform corrosion of the solution to the microporous plate.

Claims (3)

1. A low-pressure corrosion device for a quartz microporous plate is characterized by comprising a vacuum air pump, a first solution cup, a second solution cup, a corrosion solution, an air valve and a connecting conduit; the first solution cup is respectively connected with the second solution cup, the vacuum air pump and the corrosion cup through three guide pipes and corresponding air valves, the guide pipe connected with the second solution cup and the vacuum air pump is inserted shallowly in the first solution cup, and the guide pipe connected with the corrosion cup is inserted deeply; the second solution cup is respectively connected with the first solution cup, the vacuum air pump and the corrosion cup through three guide pipes and corresponding air valves, the guide pipe connected with the corrosion cup and the vacuum air pump is inserted shallowly in the second solution cup, and the guide pipe connected with the first solution cup is inserted deeply; the corrosion cup is respectively connected with the first solution cup and the second solution cup through two guide pipes and corresponding air valves, the guide pipe connected with the first solution cup is inserted shallowly in the corrosion cup, the guide pipe connected with the second solution cup is inserted deeply, and the corrosion cup is used for placing a microporous plate to be corroded; the method comprises the steps of putting a corrosion solution in a first solution cup, opening a vacuum air pump to pump air from a second solution cup and the corrosion cup, enabling the solution in the first solution cup to flow into the corrosion cup and the second solution cup by utilizing air pressure difference, pumping air from the first solution cup, enabling the solution in the second solution cup to return to the first solution cup, and then performing multiple circulation operations to further reduce the air pressure in the corrosion cup, wherein the corrosion solution reacts with a microporous plate, so that the aperture of the micropore is enlarged.
2. The low-pressure etching device for the quartz microporous plate of claim 1, wherein the etching cup, the first solution cup and the second solution cup are provided with sealing cup covers.
3. The low-pressure etching method of the quartz microporous plate is characterized by comprising the following steps of:
preparing an etching solution;
connecting a low pressure corrosion device according to claim 1 or 2;
manufacturing a near-vacuum low-pressure environment to separate out micro bubbles in the corrosive solution;
and placing the etching solution and the microporous plate into a proper temperature environment to start etching.
CN202111500933.3A 2021-12-09 2021-12-09 Low-pressure corrosion device and method for quartz micro-pore plate Active CN114163135B (en)

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