CN221485289U

CN221485289U - Detection system for additive content in copper etching liquid

Info

Publication number: CN221485289U
Application number: CN202323255588.9U
Authority: CN
Inventors: 李欣; 曹壮; 曹顺有; 陶传安
Original assignee: Jiangsu Fulate Automation Equipment Co ltd
Current assignee: Jiangsu Fulate Automation Equipment Co ltd
Priority date: 2023-11-30
Filing date: 2023-11-30
Publication date: 2024-08-06
Anticipated expiration: 2033-11-30

Abstract

The utility model discloses a detection system for the content of an additive in copper etching liquid, wherein a liquid inlet, an air inlet and a liquid outlet are arranged on a measuring dish; the CDA pipeline is connected with an air inlet of the measuring vessel; the flushing branch is connected with a liquid inlet of the measuring vessel; the sample circulation pipeline comprises a sample input pipeline, a sample output pipeline, a sample buffer pipeline and a three-way electromagnetic valve, the sample output pipeline is communicated with the CDA pipeline, the sample input pipeline and the sample output pipeline are respectively provided with a three-way electromagnetic valve, and the sample buffer pipeline is connected between the two three-way electromagnetic valves; the flushing branch, the sample input pipeline and the liquid inlet of the measuring vessel are communicated with the rotary switching valve; the liquid medicine pipeline is communicated with a liquid inlet of the measuring vessel. The utility model combines the characteristics of production equipment, can accurately measure the content of the additive in the etching liquid used in production, and combines an instant replenishment system to quantitatively replenish.

Description

Detection system for additive content in copper etching liquid

Technical Field

The utility model relates to a system for detecting the content of an additive in copper etching liquid.

Background

In the TFT industry, a wet etching section mostly uses copper etching liquid to process a large-size substrate; in the past, a copper etching solution in a dosage form is used, the concentration of copper ions in the solution rises rapidly, and frequent liquid exchange is needed to prevent safety accidents. With the increasing maturity of the production process, the research of each reagent manufacturer on the copper acid liquid medicine is more and more intensive, and the research and development of the additive for complexing copper ions in the production process are performed to inhibit the decomposition of hydrogen peroxide, prolong the service life of the liquid medicine and improve the production safety, which is called as the two-dosage copper etching liquid.

The two-agent copper etching solution needs to be supplied with the additive in the production process, so that the content of the additive in the etching solution used in the current production needs to be known, and the additive is quantitatively supplied by combining an optimal process supply curve; the near infrared analyzer is commonly used as a measuring instrument in the industry to detect the content of the additive, the modeling of the near infrared analysis method is difficult, the content of copper ions gradually rises in the production process to influence the measurement, and the content of the additive cannot be accurately measured.

Disclosure of Invention

The utility model aims to solve the problems in the prior art and provides a system for detecting the content of an additive in copper etching liquid.

The utility model adopts the technical scheme that:

A system for detecting the content of an additive in a copper etching solution comprises

The measuring vessel is provided with a liquid inlet, an air inlet and a liquid outlet;

A CDA pipeline; the CDA pipeline is connected with an air inlet of the measuring vessel;

The flushing branch is connected with the liquid inlet of the measuring vessel;

The sample circulating pipeline comprises a sample input pipeline, a sample output pipeline, a sample buffer pipeline and a three-way electromagnetic valve, wherein the sample output pipeline is communicated with the CDA pipeline, the sample input pipeline and the sample output pipeline are respectively provided with the three-way electromagnetic valve, and the sample buffer pipeline is connected between the two three-way electromagnetic valves;

The flushing branch, the sample input pipeline and the liquid inlet of the measuring vessel are communicated with the rotary switching valve;

and the liquid medicine pipeline is communicated with the liquid inlet of the measuring vessel.

Further, the CDA pipeline and the flushing branch pipeline are respectively provided with a pneumatic valve and a pressure regulating valve.

Further, an overflow pipe is arranged on the side wall of the measuring vessel, and the overflow pipe is communicated with a liquid outlet of the measuring vessel.

Further, a titration pump is arranged on the liquid medicine pipeline.

Further, a stirrer and a PH composite electrode are arranged on the measuring vessel.

The utility model has the following beneficial effects:

The utility model combines the characteristics of production equipment, can accurately measure the content of the additive in the etching liquid used in production, and combines an instant replenishment system to quantitatively replenish. The utility model improves the automation degree of the detection process and realizes the accuracy of data in the processes of automatic sampling, quantitative analysis and continuous measurement; the problems of low detection precision, long detection time, high labor cost and the like in the traditional detection process are solved.

Drawings

Fig. 1 is a structural diagram of the present utility model.

Fig. 2 is a schematic diagram of a rotary switching valve.

Detailed Description

The utility model is further described below with reference to the accompanying drawings.

Referring to fig. 1 and 2, a system for detecting the content of an additive In a copper etching solution according to the present utility model includes a measuring dish 10, a CDA line, a flushing branch (i.e., "Water In" In fig. 1), a rotary switching valve 6, a sample circulation line, and a chemical liquid line 14.

The measuring vessel 10 is provided with a liquid inlet, a gas inlet and a liquid outlet, and a CDA pipeline is connected with the gas inlet of the measuring vessel 10; the flushing branch is connected with the liquid inlet of the measuring vessel 10, and the liquid medicine pipeline is communicated with the liquid inlet of the measuring vessel 10.

The Sample circulation pipeline comprises a Sample input pipeline (i.e. Sample In fig. 1), a Sample output pipeline (i.e. Sample Return In fig. 1), a Sample buffer pipeline 13, a first three-way electromagnetic valve 3 and a second three-way electromagnetic valve 4.

The three valve ports of the second three-way electromagnetic valve 4 are respectively communicated with a sample output pipeline, a sample buffer pipeline 13 and a CDA pipeline. The three valve ports of the first three-way electromagnetic valve 3 are respectively communicated with the sample input pipeline, the sample buffer pipeline 13 and the rotary switching valve 6.

Six ports are arranged on the rotary switching valve 6, and are correspondingly a first port 61, a second port 62, a third port 63, a fourth port 64, a fifth port 65 and a sixth port 66, wherein the first port 61 is communicated with the fourth port 64, a sample input pipeline is communicated with the fifth port 65, the sixth port 66 is a liquid outlet, and the rotary switching valve is always communicated with the original position in pairs (namely, the original position 61 port is the same as the original position 62 port, and the switching position 61 port is communicated with the 66 port). The flushing branch communicates with the second valve port 62 and the third valve port 63 communicates with the measuring dish 10.

The sample circulation pipeline in the utility model enables the sample to always process the flowing state, when the sample needs to be added into the measuring vessel 10, the opening and the closing of the first three-way electromagnetic valve 3 and the second three-way electromagnetic valve 4 are controlled, so that the sample input pipeline and the sample buffer pipeline 13 and the sample output pipeline and the sample buffer pipeline 13 are not conducted, and at the moment, the sample buffer pipeline 13 stores the sample temporarily. Then the opening and closing of the second three-way electromagnetic valve 4 are controlled, so that the CDA pipeline is communicated with the sample buffer pipeline 13,

At this time, the rotary switching valve is switched to a switching position, and a sample is pressed into the rotary switching valve 6 through air pressure, namely the sample is pressed into the fifth valve port 65, at this time, the fifth valve port 65 is communicated with the fourth valve port 64, the fourth valve port 64 is directly communicated with the first valve port 61 through a pipeline, the first valve port 61 of the switching position is communicated with the sixth valve port 66 again, and the sample is circularly replaced through 65-64-61-66. After the obtained sample is replaced for a certain time, the switching action of the rotary switching valve is ensured, at the moment, the rotary switching valve returns to the original position, the first valve port 61 is communicated with the second valve port 62, the third valve port 63 is communicated with the fourth valve port 64, the Water In is opened through the pneumatic valve 1, and the sample is replaced and flows into the measuring dish 10 through the 62-61-64-63.

The CDA line is provided with a pressure regulating valve 9 and a second pneumatic valve 2, and the flushing branch is provided with a pressure regulating valve 9 and a first pneumatic valve 1.

The additive in the copper etching liquid is organic mixed acid composed of twenty or more components, 0.5mol/L sodium hydroxide is used as a titration reagent, namely, a liquid medicine pipeline 14 is communicated with NaOH, the additive can be reacted into organic acid salt through a neutralization reaction, the neutralization reaction is finished (through PH potential detection), the consumption of the sodium hydroxide is recorded, and the concentration of the additive is calculated through a chemical reaction proportionality coefficient. The specific process is as follows:

1) The pressure regulating valve 9 is designed on the flushing branch to regulate the pressure of the DIW and monitor the pressure through the pressure gauge, so that the DIW quantity supplied in a certain time is ensured to be a fixed value; the first pneumatic valve 1 is opened to inject pure water to wash the measuring dish 10 through the water pipe, the pneumatic drain valve 11 is opened to drain water, the measuring dish is thoroughly cleaned by repeating the above process for three times, and the residual influence is eliminated.

2) After the flushing is completed, the first pneumatic valve 1 is closed to stop DIW supply, the second pneumatic valve 2 is opened to be communicated with CDA to purge the container 10, residual water stains in the measuring dish 10 are purged completely, and the pneumatic drain valve 11 is closed.

3) The flushing branch ensures that the flow rate is a fixed value when DIW flows in through the pressure regulating valve 9 so as to control the inflow through time. The water inlet pipe inserted into the measuring dish 10 in the flushing branch is tightly attached to the inner wall of the measuring dish 10, so that no bubble is generated during DIW supply, the first pneumatic valve 1 is opened to inject pure water into the measuring dish 10, and the water inflow is controlled to be 60ml accurately according to time.

4) Sample In and Sample Return are responsible for continuous circulation of liquid medicine In the copper etching equipment process Tank, and the freshness of sampling of the measuring equipment is guaranteed. When sampling is needed, the third pneumatic valve 5 is opened, and the copper etching liquid sample is quantitatively obtained through the rotary switching valve 6 and injected into the measuring dish 10.

5) The stirrer 7 and the PH composite electrode 15 are arranged on the measuring vessel 10, and the copper etching liquid sample in the measuring vessel 10 and the pure water are stirred for 1min by opening the stirrer 7, so that the full mixing is ensured.

6) At this time, 0.5 mol/L NaOH is pumped by a titration pump 8, and is injected into a measuring dish 10 in an amount of 0.02ml each time, neutralization reaction occurs, stirring is needed for 30 seconds after each injection of NaOH, and the next injection is performed, so that the reaction of NaOH and additives is ensured to be complete.

7) By detecting the PH composite electrode 15 reading until the PH composite electrode 15 reading reaches 7.3PH (stoichiometric point), the operation of the titration pump 8 is stopped and the consumption of NaOH and PH reading are recorded.

8) And (3) bringing the consumption of NaOH of 0.5mol/L in the whole titration period into a model established in a laboratory, and calculating to obtain the concentration of the sample, namely the content of the copper etching liquid clock additive.

Note that: the copper etching liquid needs to be fresh in sampling, so that the calculated concentration is ensured to be the actual value of the additive content in the current process tank; the equipment cannot be impacted, inclined or vibrated in the measuring process, so that deviation of a measuring result is prevented; the measuring dish needs to be thoroughly cleaned after each measurement is completed, so that the measurement result is prevented from being influenced.

The utility model improves the automation degree of the detection process and realizes the accuracy of data in the processes of automatic sampling, quantitative analysis and continuous measurement; the problems of low detection precision, long detection time, high labor cost and the like in the traditional detection process are solved.

The foregoing is merely a preferred embodiment of the utility model, and it should be noted that modifications could be made by those skilled in the art without departing from the principles of the utility model, which modifications would also be considered to be within the scope of the utility model.

Claims

1. A detection system for the content of an additive in copper etching liquid is characterized in that: comprising

The measuring vessel (10) is provided with a liquid inlet, a gas inlet and a liquid outlet;

a CDA pipeline; the CDA pipeline is connected with an air inlet of the measuring vessel (10);

the flushing branch is connected with the liquid inlet of the measuring vessel (10);

The liquid inlet of the flushing branch, the sample input pipeline and the measuring dish (10) are communicated with the rotary switching valve (6);

The liquid medicine pipeline is communicated with a liquid inlet of the measuring vessel (10).

2. The system for detecting the content of the additive in the copper etching liquid according to claim 1, wherein: and the CDA pipeline and the flushing branch pipeline are respectively provided with a pneumatic valve and a pressure regulating valve.

3. The system for detecting the content of the additive in the copper etching liquid according to claim 1, wherein: an overflow pipe (12) is arranged on the side wall of the measuring vessel (10), and the overflow pipe (12) is communicated with a liquid outlet of the measuring vessel (10).

4. The system for detecting the content of the additive in the copper etching liquid according to claim 1, wherein: a titration pump (8) is arranged on the liquid medicine pipeline.

5. The system for detecting the content of the additive in the copper etching liquid according to claim 1, wherein: the measuring dish (10) is provided with a stirrer (7) and a PH composite electrode (15).