CN114163135B - Low-pressure corrosion device and method for quartz micro-pore plate - Google Patents

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

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Publication number
CN114163135B
CN114163135B CN202111500933.3A CN202111500933A CN114163135B CN 114163135 B CN114163135 B CN 114163135B CN 202111500933 A CN202111500933 A CN 202111500933A CN 114163135 B CN114163135 B CN 114163135B
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cup
solution
corrosion
etching
solution cup
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CN114163135A (en
Inventor
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 micro-pore plate, and belongs to the field of processing technology. When the micropore size in the quartz micropore plate is smaller than the required size, a corrosion reaming method is provided. The method can reduce the number of bubbles in the solution and lead the corrosion rate of the quartz micropore plate to be more balanced. The device for manufacturing low pressure consists of a vacuum air pump, a first solution cup, a second solution cup, a corrosion solution, a plurality of air valves and a connecting conduit, wherein the corrosion cup can be pumped into near vacuum through specific operation steps, so that bubbles are separated out, and the uniform corrosion of the solution to the micro-pore plate is facilitated.

Description

Low-pressure corrosion device and method for quartz micro-pore plate
Technical Field
The invention relates to the field of processing technology, in particular to a quartz micro-pore plate low-pressure corrosion device and method.
Background
In some particular applications, it is desirable to use quartz microplates with a large number of microporations. When the actual quartz micropore plate is processed, the micropore diameter on the actual plate is slightly smaller than the required diameter possibly due to factors such as overlarge manufacturing error or unreasonable design. In which case the reworking takes a considerable amount of cost and time. And reaming of a large number of quartz micropores can be performed by adopting a solution corrosion method. In the corrosion process of the micro-pore plate, micro-bubbles are separated out from the corrosion solution due to heating, stirring and other reasons and are easy to attach on the micro-pores, so that quartz at the micro-pores cannot be contacted with the corrosion solution, different corrosion rates of all the micro-pores can be caused, and single micro-pores are uneven.
Disclosure of Invention
The purpose of the invention is that: in order to expand micropores on a quartz micropore plate and enable the micropore plate to meet actual requirements, a micropore plate reaming method is provided and a set of device is designed. The method utilizes a low-pressure environment to extract bubbles in the solution, and avoids uneven corrosion caused by blocking 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 etching device for a quartz micro-pore plate comprises a vacuum air pump, a first solution cup, a second solution cup, an etching 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 pipes connected with the second solution cup and the vacuum air pump are inserted into the first solution cup shallowly, and the guide pipes connected with the corrosion cup are 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 pipes connected with the corrosion cup and the vacuum air pump are inserted into the second solution cup shallowly, and the guide pipes connected with the first solution cup are inserted deeply; the corrosion cup is connected with the first solution cup and the second solution cup through two guide pipes and corresponding air valves respectively, the guide pipe connected with the first solution cup is inserted shallow into the corrosion cup, the guide pipe connected with the second solution cup is inserted deep, and the corrosion cup is used for placing a micropore plate to be corroded; the etching solution is placed in the first solution cup, the vacuum air pump is started to pump air from the second solution cup and the etching cup, the solution in the first solution cup flows into the etching cup and the second solution cup by utilizing the air pressure difference, the first solution cup is pumped, the solution in the second solution cup returns to the first solution cup, and then the repeated circulation operation is carried out, so that the air pressure in the etching cup can be further reduced, the etching solution reacts with the micropore plate, and the micropore aperture is enlarged.
Further, 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 micro-pore plate comprises the following steps:
preparing an etching solution;
connecting the low pressure etching apparatus according to claim 1 or 2;
manufacturing a near-vacuum low-pressure environment to separate out micro bubbles in the corrosive solution;
the corrosion solution is placed in an environment of appropriate temperature along with the microplate to initiate corrosion.
Compared with the prior art, the invention has the beneficial effects that:
under the condition that the size of micropores in the processed quartz microporous plate is smaller than the required size, the method can be used for corroding and reaming to meet the requirements without reprocessing, and unnecessary production cost and time cost are reduced.
Compared with other reaming methods, the method has the advantages of simple operation, low cost, controllable reaming size and capability of obtaining micropores with any size by controlling the corrosion time.
According to the principle that bubbles in the solution can influence the uniformity of corrosion, the number of the bubbles in the solution is reduced by the device, the method is particularly important for micropores which are easy to be blocked by gas in a liquid environment, the blocked bubbles in the micropores are extracted to enable the corrosion solution to be fully contacted with the micropores, so that the corrosion rate is more uniform, and the corrosion effect is more obvious.
Drawings
FIG. 1 is a schematic diagram of a structure for preparing a microplate etching solution according to the present invention;
wherein, each reference sign in the figure has the meaning as follows: 1 is a sealing cup cover, 2 is a first solution cup 2,3 is a corrosion cup 3,4 is a micro-pore 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 for a quartz micro-pore plate, which comprises the following steps:
1) And preparing a solution required for 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.
3) The etching solution is put into the first solution cup 2, the micro-pore plate 6 is put into the etching cup 3, and all the joints are sealed, so that no air leakage is ensured.
4) The solution replacement is carried out according to a certain procedure, repeated several times, so that the etching solution is present in the etching cup 3 and the air pressure is as low as possible.
5) The etching cup 3 is opened, and is etched for a certain time together with the etching solution therein and the microplate 6 under the condition of a specified temperature.
The technical scheme of the present invention will be described in detail with reference to specific examples, but the following examples are only preferred examples of the present invention, and not all the examples are included. Based on the examples in the embodiments, those skilled in the art can obtain other examples without making any inventive effort, which fall within the scope of the invention.
The microplate material to be reamed in this example is quartz, and the microplate is used to integrate the field-of-view cell array ends to secure the optical fibers. Due to the processing precision problem, the micropore size is slightly small and cannot pass through the optical fiber. The specific operation comprises the following steps:
1) A KOH solution of 56.1g/mol was prepared. The KOH reagent used had a KOH content of 85%. Depending on the volume of the etching cup 3, 400ml of solution needs to be prepared. 211g of KOH reagent was weighed into a etching cup 3, and deionized water was slowly added to 400ml while stirring with a glass rod.
2) The heating switch of the constant-temperature ultrasonic cleaning instrument is turned on, the heating temperature is set to 80 ℃, and the ultrasonic cleaning instrument is preheated for 30 minutes (5 minutes of oscillation) so that the cleaning instrument enters constant-temperature circulation.
3) The microplate was placed in a small ultrasonic cleaner together with a jig and cleaned by shaking for 3 minutes.
4) The microplate was placed in the etching cup 3 with the fixture, a vacuum device was attached as shown in fig. 1, and the interface was secured.
5) Manufacturing a microplate in a low-pressure corrosion environment:
a) Vacuumizing
Firstly, 5 air valves are closed, the air pump 6 is opened, then the air valves 10 and 8 are sequentially opened, and a period of time is waited for, so that the etching cup 3 and the second solution cup 5 enter a near vacuum state. The air valves 8 and 10 are then closed and the air pump is then turned off.
b) Feed solution
Ensure that the 5 valves are closed, the air valve 7 is slowly opened, the air valve 8 is controlled, the solution in the solution cup 2 slowly flows into the corrosion cup 3, and the redundant solution enters the second solution cup 5. When the corrosion solution passes through the micro-pore plate, the air valves 8 and 7 are closed in sequence.
c) Replacement solution
After the air valves are all closed, the air pump is opened, the air valves 9 and 11 are sequentially opened, and the solution in the second solution cup 5 almost enters the first solution cup 2 to finish the replacement of the solution from the second solution cup 5 to the first solution cup 2. The air valves 11 and 9 are closed and the air pump 6 is again closed.
d) Circulation air extraction
After the solution replacement is completed, steps a) and b) are performed. This is cycled 2-3 times. And (5) finishing filling the solution in the micropores.
6) And (3) removing the vacuum circulation conduit, putting the corrosion cup into an ultrasonic cleaner, and pressing the PVC plate to prevent rollover.
7) The temperature of the corrosion solution is measured by a temperature measuring probe, and timing is started when the temperature of the solution is 80 degrees. The etching time is set according to the actual size of the micro-holes, and the micro-hole plate seat can be gently 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 micro-holes).
8) And taking out the micro-pore plate after the corrosion time is over, putting the micro-pore plate into a small ultrasonic cleaner for vibration cleaning for 5 minutes, taking out, and drying by compressed air.
After corrosion for a certain time, through experiments, the optical fiber can pass through micropores, and the size of the micropores is uniform through measurement. This method proved to be effective.
The objects of the present invention have been fully achieved by the above embodiments. It will be apparent to those skilled in the art that the present invention includes, but is not limited to, those described in the above specific embodiments. Any modification which does not depart from the invention is intended to be included within the scope of the claims.
The invention discloses a low-pressure corrosion method for a quartz micro-pore plate, and belongs to the field of processing technology. When the micropore size in the quartz micropore plate is smaller than the required size, a corrosion reaming method is provided. The method can achieve the purpose of enlarging the aperture of the micropore by corroding the quartz plate by the corrosive solution. The invention provides a low-pressure corrosion method, which can reduce the number of bubbles in the solution and lead the corrosion rate of a quartz micro-pore plate to be more uniform because bubbles in the corrosion solution can lead the corrosion to be uneven. The device for manufacturing the low pressure consists of a vacuum air pump 6, a first solution cup 2, a second solution cup 5, a corrosion cup 3, a corrosion solution, a plurality of air valves and connecting pipes. The etching cup can be pumped to be close to vacuum through a specific operation step, so that bubbles are separated out. Is favorable for the uniform corrosion of the solution to the micro-pore plate.

Claims (3)

1. The low-pressure etching device for the quartz micro-pore plate is characterized by comprising a vacuum air pump, a first solution cup, a second solution cup, an etching 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 pipes connected with the second solution cup and the vacuum air pump are inserted into the first solution cup shallowly, and the guide pipes connected with the corrosion cup are 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 pipes connected with the corrosion cup and the vacuum air pump are inserted into the second solution cup shallowly, and the guide pipes connected with the first solution cup are inserted deeply; the corrosion cup is connected with the first solution cup and the second solution cup through two guide pipes and corresponding air valves respectively, the guide pipe connected with the first solution cup is inserted shallow into the corrosion cup, the guide pipe connected with the second solution cup is inserted deep, and the corrosion cup is used for placing a micropore plate to be corroded; the etching solution is placed in the first solution cup, the vacuum air pump is started to pump air from the second solution cup and the etching cup, the solution in the first solution cup flows into the etching cup and the second solution cup by utilizing the air pressure difference, the first solution cup is pumped, the solution in the second solution cup returns to the first solution cup, and then the repeated circulation operation is carried out, so that the air pressure in the etching cup can be further reduced, the etching solution reacts with the micropore plate, and the micropore aperture is enlarged.
2. The low pressure etching apparatus for a quartz micro-well plate according to claim 1, wherein sealing cup covers are provided on the etching cup, the first solution cup and the second solution cup.
3. The low-pressure corrosion method for the quartz micro-pore plate is characterized by comprising the following steps of:
preparing an etching solution;
connecting the low pressure etching apparatus according to claim 1 or 2;
manufacturing a near-vacuum low-pressure environment to separate out micro bubbles in the corrosive solution;
the corrosion solution is placed in an environment of appropriate temperature along with the microplate to initiate corrosion.
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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