阅读说明：本技术 一种饱和二氧化碳溶液制备设备 (Saturated carbon dioxide solution preparation equipment ) 是由 钱诚 童建 王禹涵 于 2021-06-25 设计创作，主要内容包括：本申请涉及一种饱和二氧化碳溶液制备设备,通过水加热以去除部分空气以降低水中溶解的气体含量,再将水和二氧化碳气体均降温到5-10℃,以使二氧化碳气体在水中的溶解度较常温下提高,相当于气体处于过饱和状态,再将混合液升温到所需温度,从而保证了水中的二氧化碳处于饱和状态。(The application relates to saturated carbon dioxide solution preparation equipment, through the heating of water in order to get rid of partial air in order to reduce the gas content of aquatic dissolution, all cool down 5-10 ℃ with water and carbon dioxide gas again to make the solubility of carbon dioxide gas improve under the normal atmospheric temperature in aquatic, be equivalent to that gas is in the oversaturation state, heat up the mixed solution to required temperature again, thereby guaranteed that the carbon dioxide of aquatic is in the saturation state.)

1. A saturated carbon dioxide solution production apparatus characterized by comprising:

the water treatment module comprises a heater (11) for heating water to 60-70 ℃ and a refrigerator for cooling the heated water to 5-10 ℃;

the gas treatment module comprises a three-way valve (21) connected with the high-pressure gas storage tank and an evaporator (22) used for heating the carbon dioxide flowing out of the high-pressure gas storage tank;

the mixing module comprises a gas-liquid mixing tank (31) and a mixed liquid outlet which are respectively connected with the water treatment module and the gas treatment module; a manual valve (14) for controlling the on-off of the flow channel is arranged between the gas-liquid mixing tank (31) and the water treatment module, and a gas-liquid separation valve (33) is further arranged at the liquid outlet of the mixed liquid so as to discharge the gas overflowing from the mixed liquid due to temperature rise.

2. The saturated carbon dioxide solution preparing apparatus according to claim 1, wherein the refrigerator includes a first heat exchanger (12) and a second heat exchanger (13), the temperature of water is lowered to room temperature by exchanging heat with air through the first heat exchanger (12), and the temperature of water at room temperature is lowered to 5-10 ℃ by passing the water at room temperature through the second heat exchanger (13).

3. The saturated carbon dioxide solution preparation equipment according to claim 2, wherein one end of the second heat exchanger (13) is connected with an outlet of the high-pressure gas storage tank, the carbon dioxide gas flows out from the high-pressure gas storage tank to cool the water under the condition of controlling the flow rate, and the carbon dioxide gas flowing out from the second heat exchanger (13) and the carbon dioxide gas flowing out from the evaporator (22) are merged and then introduced into the gas-liquid mixing tank (31).

4. The saturated carbon dioxide solution preparation apparatus according to claim 1, wherein the refrigerator is a first heat exchanger (12), the first heat exchanger (12) exchanges heat with the carbon dioxide gas flowing out of the high-pressure gas storage tank to reduce the temperature to 5-10 ℃, and the carbon dioxide gas flowing out of the first heat exchanger (12) and the carbon dioxide gas flowing out of the evaporator are merged and then introduced into the gas-liquid mixing tank.

5. The apparatus for producing a saturated carbon dioxide solution according to any one of claims 1 to 4, wherein the conductivity of the mixed liquid flowing out of the gas-liquid mixing tank (31) is measured by a conductivity measuring instrument (32) to determine whether or not the mixed liquid is saturated with the carbon dioxide gas.

6. The saturated carbon dioxide solution preparation apparatus according to any one of claims 1 to 5, wherein the gas flowing out of the gas-liquid mixing tank (31) is collected by a discharge tank (34).

7. The saturated carbon dioxide solution production apparatus according to any one of claims 1 to 6, wherein the gas-liquid mixing tank is provided in plurality in parallel.

8. The saturated carbon dioxide solution preparation apparatus according to any one of claims 1 to 7, wherein the gas outlet end of the gas-liquid separation valve (33) is connected to a dehumidification tank (38) to remove moisture, and the gas from which moisture is removed is introduced to the front of the gas-liquid mixing tank (31) to be mixed with the gas entering the gas-liquid mixing tank (31).

9. The saturated carbon dioxide solution production apparatus according to any one of claims 1 to 8,

a gas discharge port of the gas-liquid mixing tank (31) is connected to a discharge tank (34) through a third valve (35) and a second flowmeter (36).

Technical Field

The application belongs to the technical field of wafer cleaning auxiliary equipment, and particularly relates to saturated carbon dioxide solution preparation equipment.

Background

When cleaning a wafer, a saturated carbon dioxide aqueous solution is used as a cleaning liquid. For example, as mentioned in "inhibition of recrystallization defect on pad surface optimized by wet cleaning process", when removing fluorine ions on the surface of a bonding pad prepared by a semiconductor chip, the last step needs to use deionized water for cleaning, carbon dioxide is introduced into the deionized water to effectively inhibit the influence of cleaning time on metal corrosion, and the difference of the defects on the surface of a wafer is very large if carbon dioxide is introduced in the step of cleaning the deionized water.

Therefore, a saturated carbon dioxide solution is required to be prepared as a cleaning solution, so that the stability of the concentration in the carbon dioxide solution can be ensured, and a stable cleaning process is guaranteed.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: in order to solve the defects in the prior art, the preparation equipment for the carbon dioxide solution is provided.

The technical scheme adopted by the invention for solving the technical problems is as follows:

a saturated carbon dioxide solution production apparatus comprising:

the water treatment module comprises a heater for heating water to 60-70 ℃ and a refrigerator for cooling the heated water to 5-10 ℃;

the gas treatment module comprises a three-way valve connected with the high-pressure gas storage tank and an evaporator used for heating the carbon dioxide flowing out of the high-pressure gas storage tank;

the mixing module comprises a gas-liquid mixing tank and a mixed liquid outlet which are respectively connected with the water treatment module and the gas treatment module; a manual valve for controlling the on-off of the flow channel is arranged between the gas-liquid mixing tank and the water treatment module, and a gas-liquid separation valve is further arranged at the liquid outlet of the mixed liquid so as to discharge the gas overflowing from the mixed liquid due to temperature rise.

Preferably, the saturated carbon dioxide solution preparing apparatus of the present invention, the refrigerator includes a first heat exchanger and a second heat exchanger, the temperature of the water is lowered to room temperature by exchanging heat with the air through the first heat exchanger, and the room temperature water is lowered to 5-10 ℃ through the second heat exchanger.

Preferably, in the saturated carbon dioxide solution preparation apparatus of the present invention, one end of the second heat exchanger is connected to an outlet of the high-pressure gas storage tank, the carbon dioxide gas flowing out of the high-pressure gas storage tank is used to cool water under the condition of controlling the flow rate, and the carbon dioxide gas flowing out of the second heat exchanger and the carbon dioxide gas flowing out of the evaporator are merged and then introduced into the gas-liquid mixing tank.

Preferably, in the saturated carbon dioxide solution preparation equipment, the refrigerator is a first heat exchanger, the first heat exchanger exchanges heat with the carbon dioxide gas flowing out of the high-pressure gas storage tank so as to reduce the temperature to 5-10 ℃, and the carbon dioxide gas flowing out of the first heat exchanger and the carbon dioxide gas flowing out of the evaporator are converged and then introduced into the gas-liquid mixing tank.

Preferably, in the saturated carbon dioxide solution preparation apparatus of the present invention, the conductivity of the mixed solution flowing out of the gas-liquid mixing tank is measured by a conductivity measuring device to determine whether the carbon dioxide gas in the mixed solution is saturated.

Preferably, in the saturated carbon dioxide solution production apparatus of the present invention, the gas flowing out of the gas-liquid mixing tank is collected by the discharge tank.

Preferably, in the saturated carbon dioxide solution production apparatus according to the present invention, the gas-liquid mixing tank is provided in plurality in parallel.

Preferably, in the saturated carbon dioxide solution preparation apparatus of the present invention, the gas outlet end of the gas-liquid separation valve is connected to a dehumidification tank to remove moisture, and the gas from which moisture is removed is introduced to the gas-liquid mixing tank to be mixed with the gas entering the gas-liquid mixing tank.

Preferably, the saturated carbon dioxide solution producing apparatus of the present invention,

and a gas discharge port of the gas-liquid mixing tank is connected with the discharge tank through a third valve and a second flowmeter.

The invention has the beneficial effects that:

according to the preparation equipment of the saturated carbon dioxide solution, part of air is removed through water heating to reduce the content of gas dissolved in water, then both the water and the carbon dioxide gas are cooled to 5-10 ℃, so that the solubility of the carbon dioxide gas in the water is improved at a normal temperature, namely the gas is in a supersaturated state, and then the temperature of the mixed solution is raised to a required temperature, so that the carbon dioxide in the water is ensured to be in the saturated state.

Drawings

The technical solution of the present application is further explained below with reference to the drawings and the embodiments.

Fig. 1 is a schematic structural view of a water treatment module and a gas treatment module in a saturated carbon dioxide solution production apparatus according to an embodiment of the present application;

FIG. 2 is a schematic structural diagram of one embodiment of a water mixing module in a saturated carbon dioxide solution preparation apparatus according to an embodiment of the present application;

FIG. 3 is a schematic structural view of another embodiment of a water mixing module in a saturated carbon dioxide solution production apparatus according to an embodiment of the present application;

FIG. 4 is a flow chart of a process for preparing a saturated carbon dioxide solution according to example 1 of the present application;

the reference numbers in the figures are:

11-a heater; 12-a first heat exchanger; 13-a second heat exchanger; 14-manual valves;

21-three-way valve; 22-an evaporator; 23-a first valve; 24-a first flow meter; 25-a filter; 26-a one-way valve; 27-a second valve;

31-gas-liquid mixing tank; 32-conductivity measurer; 33-a gas-liquid separation valve; 34-a discharge tank; 35-a third valve; 36-a second flow meter; 37-a fourth valve; 38-dehumidification tank.

Detailed Description

It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.

In the description of the present application, it is to be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for convenience in describing the present application and for simplicity in description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed in a particular orientation, and be operated in a particular manner, and are not to be considered limiting of the scope of the present application. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the invention, the meaning of "a plurality" is two or more unless otherwise specified.

In the description of the present application, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art through specific situations.

The technical solutions of the present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.

Example 1

The embodiment provides a preparation method of a saturated carbon dioxide solution, as shown in fig. 4, including the following steps:

s1: heating water to 60-70 deg.C and removing part of air by using negative pressure, and cooling water to 5-10 deg.C, such as 5 deg.C, 6 deg.C, 7 deg.C, 8 deg.C, 9 deg.C or 10 deg.C;

the reduction of the temperature of the water to 5-10 ℃ can be achieved by:

1, exchanging heat with air through a first heat exchanger to reduce the water temperature to room temperature, and reducing the water temperature to 5-10 ℃ through a refrigerator.

The refrigerator is a second heat exchanger, one end of the second heat exchanger is connected with an outlet of the high-pressure gas storage tank, and carbon dioxide gas flows out of the high-pressure gas storage tank to cool water under the condition of controlling flow. The temperature can be better controlled by heat exchange at two ends.

2, a first heat exchanger is arranged to exchange heat with the carbon dioxide gas flowing out of the high-pressure gas storage tank so as to reduce the temperature to 5-10 ℃, and the carbon dioxide gas flowing out of the first heat exchanger and the carbon dioxide gas flowing out of the evaporator are converged and then introduced into the gas-liquid mixing tank.

S2: heating the carbon dioxide to 5-10 ℃ by an evaporator;

s3: carrying out the treatment on water with the temperature of 5-10 ℃ and carbon dioxide gas with the temperature of 5-10 ℃ in a gas-liquid mixing tank;

s4: and introducing the mixed solution into a temperature rising device to rise the temperature to the required temperature, and enabling gas in the temperature rising process to be emitted through a gas-liquid separation valve.

In the preparation method of the saturated carbon dioxide solution of the embodiment, water is heated to 60-70 ℃, negative pressure is used for removing part of air to reduce the content of gas dissolved in the water, then both the water and the carbon dioxide gas are cooled to 5-10 ℃, so that the solubility of the carbon dioxide gas in the water is improved at a normal temperature, namely the gas is in a supersaturated state, and then the temperature of the mixed solution is raised to a required temperature, thereby ensuring that the carbon dioxide in the water is in a saturated state.

The other end of the first heat exchanger is air, and the temperature is reduced through normal-temperature air.

Further, second heat exchanger one end and high-pressure gas storage tank exit linkage, flow out carbon dioxide gas through the high-pressure gas storage tank under the condition of control flow and cool down water to the temperature that brings when fully doing benefit to the high-pressure gas storage tank output gas falls. The carbon dioxide flowing out of the high-pressure gas storage tank can rapidly cool the periphery, so that only part of the carbon dioxide flows into the second heat exchanger to participate in cooling water. Of course, part of the carbon dioxide flowing out of the high-pressure gas storage tank can be introduced into the heat preservation tank around the gas-liquid mixing tank, so that the gas-liquid mixing tank is kept at 5-10 ℃, and the carbon dioxide is easy to freeze when the temperature is too low. The gas-liquid mixing tank is positioned in the heat preservation tank, so that the gas-liquid mixing tank keeps a lower temperature.

Further, after the step S3, the conductivity of the mixed liquid in the flow path of the gas-liquid mixing tank is measured by a conductivity measuring device to determine whether the mixed liquid is saturated with carbon dioxide gas.

Further, the gas flowing out of the gas-liquid mixing tank is collected by the discharge tank 34, and is discharged or reused after being treated uniformly.

Further, the gas-liquid mixing tank is provided in parallel. As shown in fig. 2, the inlets and outlets of the two gas-liquid mixing tanks are respectively communicated so that water, carbon dioxide gas, and discharged carbon dioxide gas can be introduced or discharged.

Further, the gas emitted from the gas-liquid separation valve is mixed with the carbon dioxide gas flowing out of the high-pressure gas storage tank through the dehumidification tank. The carbon dioxide gas is recycled, the temperature of the carbon dioxide gas flowing out of the high-pressure gas storage tank can be increased, and the temperature increasing speed is increased.

Example 2

The present embodiment provides a saturated carbon dioxide solution preparing apparatus, as shown in fig. 1 and 2, including:

the water treatment module comprises a heater 11 for heating water to 60-70 ℃ and a refrigerator for cooling the heated water to 5-10 ℃; the heater 11 may also be provided with a negative pressure device for accelerating the escape of gas from the water.

The gas treatment module comprises a three-way valve 21 connected with the high-pressure gas storage tank and an evaporator 22 used for heating the carbon dioxide flowing out of the high-pressure gas storage tank;

the mixing module comprises a gas-liquid mixing tank 31 and a mixed liquid outlet which are respectively connected with the water treatment module and the gas treatment module; a manual valve 14 for controlling the on-off of the flow passage is arranged between the gas-liquid mixing tank 31 and the water treatment module; a first valve 23, a first flowmeter 24 for measuring flow, a filter 25 for filtering impurities, a check valve 26 and a second valve 27 for preventing backflow are arranged between the gas-liquid mixing tank 31 and the gas processing module; the gas discharge port of the gas-liquid mixing tank 31 is connected to the discharge tank 34 through a third valve 35 and a second flow meter 36, and a fourth valve 37 may be provided in parallel to communicate the gas discharge port of the gas-liquid mixing tank 31 and the discharge tank 34 for safety. A plurality of the gas-liquid mixing tanks 31 may be provided in parallel as required.

Further, as shown in fig. 3, the mixed liquid outlet is further provided with a gas-liquid separation valve 33, an air outlet end of the gas-liquid separation valve 33 is connected with a dehumidification tank 38 to remove moisture, and the gas from which moisture is removed is introduced into the gas-liquid mixing tank 31 to be mixed with the gas entering the gas-liquid mixing tank 31, as shown in fig. 3.

The "water" in FIG. 2 is taken over the "water outflow" and "CO" in FIG. 1₂"take over" the carbon dioxide outflow.

The refrigerator has the following specific arrangement mode:

the refrigerator comprises a first heat exchanger 12 and a second heat exchanger 13, the temperature of water is reduced to room temperature by exchanging heat with air through the first heat exchanger 12, and then the temperature of room temperature water is reduced to 5-10 ℃ through the second heat exchanger 13.

One end of the second heat exchanger 13 is connected with an outlet of the high-pressure gas storage tank, the carbon dioxide gas flowing out of the high-pressure gas storage tank is used for cooling water under the condition of controlling the flow, and the carbon dioxide gas flowing out of the second heat exchanger 13 and the carbon dioxide gas flowing out of the evaporator 22 are converged and then introduced into the gas-liquid mixing tank 31.

2, the refrigerator is a first heat exchanger 12, the first heat exchanger 12 exchanges heat with the carbon dioxide gas flowing out of the high-pressure gas storage tank so as to reduce the temperature to 5-10 ℃, and the carbon dioxide gas flowing out of the first heat exchanger 12 and the carbon dioxide gas flowing out of the evaporator are converged and then introduced into the gas-liquid mixing tank.

An electrical conductivity measuring device 32 is disposed behind the gas-liquid mixing tank 31, and the electrical conductivity of the mixed liquid flowing out of the gas-liquid mixing tank 31 is measured by the electrical conductivity measuring device 32 to determine whether the mixed liquid is saturated with carbon dioxide gas.

In light of the foregoing description of the preferred embodiments according to the present application, it is to be understood that various changes and modifications may be made without departing from the spirit and scope of the invention. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.