CN111974752A - Supercritical fluid cleaning method and device - Google Patents

Supercritical fluid cleaning method and device Download PDF

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Publication number
CN111974752A
CN111974752A CN202010691159.8A CN202010691159A CN111974752A CN 111974752 A CN111974752 A CN 111974752A CN 202010691159 A CN202010691159 A CN 202010691159A CN 111974752 A CN111974752 A CN 111974752A
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China
Prior art keywords
cleaning
supercritical fluid
fluid
workpiece
chamber
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CN202010691159.8A
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Chinese (zh)
Inventor
杨景峰
李卫平
杨凡
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Shanghai fuludi Fluid Technology Co.,Ltd.
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Luoyang Maitoufeng Technology Development Co ltd
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Priority to CN202010691159.8A priority Critical patent/CN111974752A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0021Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B13/00Accessories or details of general applicability for machines or apparatus for cleaning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0064Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
    • B08B7/0071Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating

Abstract

The invention discloses a supercritical fluid cleaning method and a device thereof, wherein the cleaning method comprises the following steps: continuously introducing supercritical fluid into the cleaning chamber; alternately changing the pressure in the cleaning chamber or the temperature of the workpiece to cause contaminants to detach from the surface of the workpiece; and discharging the pollutants separated from the workpiece along with the supercritical fluid to finish the cleaning of the workpiece. The cleaning device comprises: a fluid storage tank for providing a fluid source, wherein the fluid source is converted into supercritical fluid; and the cleaning chamber is connected with the fluid storage tank, can be filled with or discharged with supercritical fluid, and is formed by at least two cleaning cavities with different cross sectional areas. The supercritical fluid cleaning method and the device thereof repeatedly form cavities or bubbles in the pollutants by alternately changing the pressure of the cleaning chamber or the temperature of the workpiece and continuously and repeatedly circulate, so that the pollutants are separated from the surface of the workpiece to achieve the purpose of cleaning, and the high diffusion coefficient of the supercritical fluid is favorable for mass transfer between the pollutants and the fluid, thereby greatly improving the cleaning rate.

Description

Supercritical fluid cleaning method and device
Technical Field
The invention relates to the technical field of precision part cleaning, in particular to a supercritical fluid cleaning method and a supercritical fluid cleaning device.
Background
In precision manufacturing, there is a cleaning process of workpieces, such as oil stains and impurities in complex grooves, blind holes, threaded holes, deep holes of parts such as precision electronic components, metal workpieces and the like. The traditional cleaning method uses organic solvents such as Freon, trichloroethane, trifluoromethylbenzene and the like, and has two main problems: firstly, the cleaning effect is poor, the requirements cannot be met, for example, the cleaning is not good before nitriding and nitrocarburizing parts, and the uniformity and the appearance quality of a carburized layer are influenced; the environmental pollution is serious, the harm to the human health of operators is great, the potential safety hazard of directly discharging the solvent is great, the environmental pollution is serious, and the use is forbidden or limited at home.
The supercritical fluid has higher dissolving capacity, low surface tension close to zero, low viscosity, strong diffusion capacity and dissolving capacity, can effectively clean and supercritically dry the fine structure on parts such as precise electronic elements, metal workpieces and the like, is green, tasteless and nontoxic, does not support combustion, and is environment-friendly, so the supercritical fluid is an ideal cleaning agent.
Published patent US09662686B2 discloses an apparatus and method for treating a surface of a semiconductor wafer that provides a treatment fluid in the form of dispersed bubbles in the treatment fluid that are generated at an acoustic pressure that is less than the acoustic pressure required to induce cavitation in the treatment fluid. The cleaning method comprises the following steps: positioning an object to be processed in a processing apparatus in a predetermined direction; supplying ultrasonic or megasonic energy to vibrate a fluid medium adjacent the article; and supplying a treatment fluid containing dispersed gas bubbles in a treatment liquid adjacent to the surface of the article, the gas bubbles being generated at an acoustic pressure of less than 1 bar.
Published patent CN106733945A discloses a supercritical state cleaning system, including purge chamber (4), gas supercharging device (11), first heating device (5) and carbon dioxide feeding mechanism, purge chamber (4) be connected with first heating device (5) and carbon dioxide feeding mechanism respectively, purge chamber (4) even have vacuum pump package (1), it takes in the air that comes into when getting into the purge chamber clean with the work piece, prevents the mixture of CO2 and air, improves the cleaning performance.
The published patent CN101190438A discloses a supercritical fluid cleaning method and system, wherein a supercritical fluid is used to clean the surface of a material having a surface microstructure, and then the supercritical fluid is used to perform the steps of soaking, cleaning and drying a component, wherein the surface of the component may include nano-holes or high aspect ratio microstructures, so that the supercritical fluid cleaning method can remove impurities or moisture on the surface of the component. The supercritical fluid cleaning system comprises a supercritical fluid source, a modifier supply source, a circulation loop and a processing tank. The treatment tank can be filled with and discharged with supercritical fluid; a supercritical fluid source connected to the processing tank to provide a supercritical fluid to the processing tank; the modifier supply source is connected with the processing tank to provide modifier to the processing tank; the circulating loop is provided with an outlet and an inlet, the inlet and the outlet are respectively connected with the processing tank, the supercritical fluid leaves the processing tank through the outlet of the circulating loop and then enters the processing tank through the inlet of the circulating loop, and the circulating loop can enable the supercritical fluid in the processing tank to circularly flow.
Published patent CN101740337A discloses a semiconductor carbon dioxide supercritical purging and cleaning machine, wherein a magnetic rotating device is arranged in a cleaning cavity, and a carbon dioxide supercritical fluid has zero surface tension, low viscosity, strong diffusion capacity and dissolving capacity, and can effectively clean and supercritically dry a fine structure on a silicon wafer. The semiconductor carbon dioxide supercritical purging and cleaning machine has the main structure that a cleaning cavity is arranged, and an ideal cleaning effect can be achieved by adding a magnetic rotating structure and matching with a nozzle in the design.
Although the above-mentioned published patents US09662686B2, CN106733945A, CN101190438A and CN101740337A all disclose the technical solution of cleaning precision workpieces, electronic components or semiconductors by using supercritical fluid as cleaning agent, they have the defects of poor cleaning effect, low cleaning efficiency and high cleaning cost.
Disclosure of Invention
The invention aims to solve the problems that: aiming at the defects in the prior art, a supercritical fluid cleaning method and a supercritical fluid cleaning device for the precision parts are provided.
The main technical scheme of the invention is that supercritical fluid is used as cleaning agent, the characteristic that the density of the supercritical fluid is violent in change with temperature and pressure near a critical point is utilized, and cavities or bubbles are repeatedly formed in pollutants by alternately changing the temperature and the fluid pressure of a workpiece, so that the pollutants are separated from the surface of the workpiece, and the aim of cleaning the workpiece is further achieved.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided a supercritical fluid cleaning method for removing contaminants from the surface of a precision part, comprising the steps of:
continuously introducing supercritical fluid into the cleaning chamber;
alternately changing the pressure in the cleaning chamber or the temperature of the workpiece to cause the supercritical fluid to repeatedly form cavities or bubbles in contaminants on the surface of the workpiece, the contaminants being released from the surface of the workpiece;
and discharging the pollutants separated from the workpiece along with the supercritical fluid to finish workpiece cleaning.
Further, in the supercritical fluid cleaning method, the supercritical fluid is carbon dioxide, nitrogen, water, air or inert gas.
Further, in the supercritical fluid cleaning method, the process of alternately changing the pressure in the cleaning chamber is: and pulse-type introducing the supercritical fluid, or introducing the supercritical fluid into the cleaning chambers with different cross-sectional areas.
Further, in the supercritical fluid cleaning method, the process of alternately changing the temperature of the workpiece is: and changing the surface temperature of the workpiece by adopting a heating mode.
Further, in the supercritical fluid cleaning method, the discharged supercritical fluid containing the pollutants is subjected to decompression separation, pressurization and temperature reduction, and then is converted into the supercritical fluid again for recycling.
Further, in the supercritical fluid cleaning method, the method further comprises:
and before the supercritical fluid is introduced into the cleaning chamber, one or more of methanol, ethanol and acetone are added into the supercritical fluid in advance for mixing.
In a second aspect the invention provides a supercritical fluid cleaning apparatus according to the method of any one of claims 1 to 6, comprising:
a fluid storage tank for providing a fluid source, wherein the fluid source is converted into supercritical fluid after pressurization and heat exchange;
and the cleaning chamber is connected with the fluid storage tank, can be filled with or discharged with the supercritical fluid, and is composed of at least two cleaning cavities with different cross sectional areas.
Further, the supercritical fluid cleaning apparatus further comprises:
and the heater is arranged on the workpiece rack in the cleaning chamber to heat the workpiece.
Further, the supercritical fluid cleaning apparatus further comprises:
a booster pump connected to the fluid storage tank; and
the inlet of the heat exchanger is connected with the booster pump, and the outlet of the heat exchanger is connected with the cleaning chamber;
and the fluid source in the fluid storage tank is converted into supercritical fluid to be introduced into the cleaning chamber after being subjected to pressurization treatment by the booster pump and heat exchange treatment by the heat exchanger in sequence.
Further, the supercritical fluid cleaning apparatus further comprises:
the induced draft fan is connected with the cleaning chamber; and
the inlet of the separation tank is connected with the induced draft fan, and the outlet of the separation tank is respectively connected with the fluid storage tank and the heat exchanger;
and the supercritical fluid containing the pollutants discharged from the cleaning chamber is sent into the separation tank through the induced draft fan to be subjected to pressure reduction and separation treatment, and the separated fluid is stored in the fluid storage tank or is converted into supercritical fluid to be introduced into the cleaning chamber in a circulating manner after being subjected to heat exchange through the heat exchanger.
Further, on the supercritical fluid cleaning apparatus, the cleaning chamber comprises a first cleaning cavity and a second cleaning cavity which are adjacently arranged and smoothly transited, wherein:
an air inlet on the first cleaning cavity is connected with the heat exchanger;
an air outlet on the second cleaning cavity is connected with the induced draft fan;
and the cross-sectional area of the first cleaning cavity is larger than that of the second cleaning cavity.
Further, the supercritical fluid cleaning apparatus further comprises:
the first transfer chamber is arranged at the inlet of the first cleaning cavity; and
and the second transfer chamber is arranged at the outlet of the second cleaning cavity.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
(1) cavities or bubbles are repeatedly formed in the pollutants by alternately changing the pressure of the cleaning chamber or the temperature of the workpiece, and are continuously and repeatedly circulated, so that the pollutants are separated from the surface of the workpiece to achieve the purpose of cleaning, and the high diffusion coefficient of the supercritical fluid is favorable for mass transfer between the pollutants and the fluid, thereby greatly improving the cleaning rate;
(2) compared with the traditional cleaning technology, the supercritical fluid without environmental pollution is adopted as the cleaning agent, and the characteristics that the density of the supercritical fluid is changed along with the temperature and the pressure are utilized, so that the environment-friendly and clean production can be realized, and the cleaning agent has the characteristics of good economic benefit and remarkable environmental benefit;
(3) the cleaning device adopts a special cleaning chamber structure design, changes of supercritical fluid pressure are realized by utilizing different cross section sizes of adjacent cleaning cavities, the supercritical fluid is diffused into pollutants when the pressure is increased, bubbles are formed in the pollutants when the pressure is reduced, and the bubbles are continuously circulated repeatedly to separate the pollutants from a workpiece so as to achieve the purpose of cleaning;
(4) a heater is arranged on a workpiece rack in the cleaning chamber, the workpiece is repeatedly heated by the heater, so that the supercritical fluid repeatedly forms cavities or bubbles in the pollutants, and the cavities or bubbles are continuously and repeatedly circulated to separate the pollutants from the surface of the workpiece, thereby achieving the purpose of cleaning the workpiece;
(5) transfer chambers are respectively arranged at the inlet and the outlet at the two ends of the cleaning chamber, and workpieces enter the cleaning chamber through the transfer chambers, so that the influence on the supercritical state in the cleaning chamber is small, and the pressure balance in the cleaning chamber is ensured; after the cleaning is finished, the workpiece enters the transfer chamber from the cleaning chamber, and the pressure is reduced in the transfer chamber, so that the cleaning agent on the surface of the workpiece is further evaporated, the drying effect is achieved, and the cleaning efficiency is improved;
(6) the fluid discharged by the transfer chamber can be recycled or directly emptied, the supercritical fluid, the cleaning agent and the auxiliary agent are separated by the decompression separation tank, the auxiliary agent is recycled after being purified and dried, and the fluid is converted into the supercritical fluid after heat exchange and can be recycled.
Drawings
FIG. 1 is a schematic diagram of the structural principle of a supercritical fluid cleaning apparatus according to the present invention;
FIG. 2 is a schematic structural diagram of a cleaning chamber of a supercritical fluid cleaning apparatus according to the present invention;
FIG. 3 is a schematic diagram of the structure of a heater in a supercritical fluid cleaning apparatus according to the present invention;
wherein the reference symbols are:
the device comprises a fluid storage tank 1, a one-way valve 2, a booster pump 3, a heat exchanger 4, a flow regulating valve 5, a first transfer chamber 6, a workpiece inlet 7, a first quick-opening door 8, a first cleaning cavity 9, a second cleaning cavity 10, a second quick-opening door 11, a second transfer chamber 12, a workpiece outlet 13, an induced draft fan 14, a separation tank 15, a first stop valve 16, a second stop valve 17, a workpiece 18, a workpiece 19, a workpiece rack 20, a heater 21, a resistor 22, a power supply 23, a thyristor switch 23 and a temperature sensor 24.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
The embodiment provides a supercritical fluid cleaning method, which adopts a supercritical fluid as a cleaning agent, utilizes the characteristic that the density of the supercritical fluid has a relatively violent change in pressure near a critical point, and repeatedly forms cavities or bubbles in pollutants by alternately changing the fluid pressure so as to achieve the aim of separating the pollutants from the surface of a workpiece to clean. The higher dissolving capacity of the supercritical fluid is beneficial to dissolving the pollutants into the supercritical fluid, the near-zero surface tension of the supercritical fluid is beneficial to cleaning the pollutants in a narrow space, and the high diffusion coefficient of the supercritical fluid is beneficial to mass transfer between the pollutants and the fluid and improving the cleaning rate.
The supercritical fluid cleaning method provided in this embodiment is used to remove contaminants from the surface of precision components, including devices in IT manufacturing and MEMS manufacturing, and is characterized by small device size and narrow gaps. The supercritical fluid cleaning method comprises the following steps: step 1, continuously introducing supercritical fluid into a cleaning chamber, and keeping the supercritical fluid in the cleaning chamber; step 2, the characteristic that the density of the supercritical fluid is changed violently near the critical point is fully utilized, and the pressure in the cleaning chamber is changed alternately, so that the supercritical fluid repeatedly forms cavities or bubbles in the pollutants on the surface of the workpiece, and the pollutants are separated from the surface of the workpiece; and 3, discharging the pollutants separated from the workpiece along with the supercritical fluid, and decompressing and evaporating the supercritical fluid on the surface of the workpiece in the transfer chamber to finish cleaning the workpiece.
In the implementation, the supercritical fluid is carbon dioxide, nitrogen, water, air or inert gas, the higher dissolving capacity of the supercritical fluid is beneficial to dissolving the pollutants into the supercritical fluid, the near-zero surface tension of the supercritical fluid is beneficial to cleaning the pollutants in a narrow space, and the high diffusion coefficient of the supercritical fluid is beneficial to improving the cleaning rate by mass transfer between the pollutants and the fluid. Compared with the traditional cleaning technology, the supercritical fluid which does not pollute the environment is adopted as the cleaning agent, and the characteristics that the density of the supercritical fluid changes along with the temperature and the pressure are utilized, so that the environment-friendly and clean production can be realized, and the cleaning agent has the characteristics of good economic benefit and remarkable environmental benefit.
In this embodiment, the pressure in the cleaning chamber can be changed according to the process requirement, and the process of alternately changing the pressure in the cleaning chamber is as follows: the supercritical fluid is introduced in a pulse mode, so that the pressure in the cleaning chamber is adjusted, and the purpose of alternately changing the pressure in the cleaning chamber is achieved. As another preferred embodiment, the cleaning chamber structure design with different cross-sectional areas is adopted, the supercritical fluid is introduced into the cleaning chambers with different cross-sectional areas, the change of the pressure of the supercritical fluid is realized by utilizing different cross-sectional areas of adjacent cleaning cavities, the supercritical fluid is diffused into the pollutants when the pressure is increased, bubbles are formed in the pollutants when the pressure is reduced, and the repeated circulation is carried out continuously, so that the pollutants are separated from the workpiece to achieve the purpose of cleaning.
In the implementation, in order to promote the physicochemical chemical action between the workpiece surface pollutant and the supercritical fluid, some auxiliary agents such as methanol, ethanol, acetone and the like can be added before the supercritical fluid enters the cleaning chamber according to the requirements of the cleaning process, so as to improve the solubility of the pollutant in the supercritical fluid.
In the implementation, the discharged fluid containing the pollutants and the supercritical fluid can be recycled or directly emptied, after the fluid discharged by pressure reduction is subjected to pressure reduction separation, the supercritical fluid cleaning agent, the pollutants and the auxiliary agent are separated, and the auxiliary agent is purified and dried and then recycled; and the separated fluid is converted into supercritical fluid again after heat exchange and is used as a cleaning agent for recycling. Realizes the repeated utilization of resources, saves energy consumption and reduces production cost.
Example 2
The present embodiment provides a supercritical fluid cleaning method, which uses a supercritical fluid as a cleaning agent, and utilizes the characteristic that the density of the supercritical fluid changes sharply with the temperature near the critical point, and by changing the temperature of the workpiece alternately, cavities or bubbles are formed in the contaminants repeatedly, so as to separate the contaminants from the surface of the workpiece, thereby achieving the purpose of cleaning. The supercritical fluid has high dissolving capacity, which is beneficial to dissolving the pollutants into the supercritical fluid, the surface tension of the supercritical fluid close to zero is beneficial to cleaning the pollutants in narrow spaces, the defect that the traditional cleaning agent cannot enter the narrow spaces to effectively clean the pollutants under the action of the surface tension of the traditional cleaning agent is overcome, and the high diffusion coefficient of the supercritical fluid is beneficial to mass transfer between the pollutants and the fluid to improve the cleaning rate.
The supercritical fluid cleaning method provided in this embodiment is used to remove contaminants from the surface of precision components, including devices in IT manufacturing and MEMS manufacturing, and is characterized by small device size and narrow gaps. The supercritical fluid cleaning method comprises the following steps: step 1, continuously introducing supercritical fluid into a cleaning chamber, and keeping the supercritical fluid in the cleaning chamber; step 2, the characteristic that the density of the supercritical fluid is changed violently with the temperature near a critical point is fully utilized, and the temperature of the workpiece in the cleaning chamber is changed alternately, so that the supercritical fluid repeatedly forms cavities or bubbles in pollutants on the surface of the workpiece, and the pollutants are separated from the surface of the workpiece; and 3, discharging the pollutants separated from the workpiece along with the supercritical fluid, and decompressing and evaporating the supercritical fluid on the surface of the workpiece in the transfer chamber to finish cleaning the workpiece.
In the implementation, the supercritical fluid is carbon dioxide, nitrogen, water, air or inert gas, the higher dissolving capacity of the supercritical fluid is beneficial to dissolving the pollutants into the supercritical fluid, the near-zero surface tension of the supercritical fluid is beneficial to cleaning the pollutants in a narrow space, and the high diffusion coefficient of the supercritical fluid is beneficial to improving the cleaning rate by mass transfer between the pollutants and the fluid. Compared with the traditional cleaning technology, the supercritical fluid which does not pollute the environment is adopted as the cleaning agent, and the characteristics that the density of the supercritical fluid changes along with the temperature and the pressure are utilized, so that the environment-friendly and clean production can be realized, and the cleaning agent has the characteristics of good economic benefit and remarkable environmental benefit.
In this embodiment, the process of changing the temperature of the workpiece in a certain range alternately comprises: the surface temperature of the workpiece is changed by adopting a heating mode, the heating mode can adopt an electromagnetic induction heating mode or an electric heating wire heating mode, the workpiece is arranged on a workpiece rack in a cleaning chamber, an electromagnetic induction coil or an electric heating wire is arranged on the workpiece rack to repeatedly heat the workpiece, the temperature of the workpiece is changed alternately, the supercritical fluid repeatedly forms cavities or bubbles in pollutants to continuously and repeatedly circulate, and the pollutants are separated from the workpiece to achieve the aim of cleaning.
In the implementation, in order to promote the physicochemical chemical action between the workpiece surface pollutant and the supercritical fluid, some auxiliary agents such as methanol, ethanol, acetone and the like can be added before the supercritical fluid enters the cleaning chamber according to the requirements of the cleaning process, so as to improve the solubility of the pollutant in the supercritical fluid.
In the implementation, the discharged fluid containing the pollutants and the supercritical fluid can be recycled or directly emptied, after the fluid discharged by pressure reduction is subjected to pressure reduction separation, the supercritical fluid cleaning agent, the pollutants and the auxiliary agent are separated, and the auxiliary agent is purified and dried and then recycled; and the separated fluid is converted into supercritical fluid again after heat exchange and is used as a cleaning agent for recycling. Realizes the repeated utilization of resources, saves energy consumption and reduces production cost.
Example 3
Referring to fig. 1, the present embodiment provides a supercritical fluid cleaning apparatus for cleaning precision components, including devices in IT manufacturing and MEMS manufacturing, which features small device size, narrow gap, and difficult cleaning of contaminants in the gap. The characteristic that the density of the supercritical fluid is violent in pressure change near a critical point is utilized, a special cleaning chamber structural design is adopted, the supercritical fluid is diffused into pollutants when the pressure is increased, bubbles are formed in the pollutants when the pressure is reduced, and the pollutants are continuously circulated repeatedly, so that the purpose of cleaning is achieved by separating the pollutants from the workpiece. The supercritical fluid has high dissolving capacity, which is beneficial to dissolving the pollutants into the supercritical fluid, the surface tension of the supercritical fluid close to zero is beneficial to cleaning the pollutants in narrow spaces, the defect that the traditional cleaning agent cannot enter the narrow spaces to effectively clean the pollutants under the action of the surface tension of the traditional cleaning agent is overcome, and the high diffusion coefficient of the supercritical fluid is beneficial to mass transfer between the pollutants and the fluid to improve the cleaning rate.
Referring to fig. 1, an embodiment of the invention provides a supercritical fluid cleaning apparatus for cleaning a precision component, including: a fluid storage tank 1 for providing a fluid source; the booster pump 3 is connected with the fluid storage tank 1, and a one-way valve 2 is arranged on a pipeline between the fluid storage tank 1 and the booster pump 3; the inlet of the heat exchanger 4 is connected with the booster pump 3, and the outlet of the heat exchanger is connected with the first cleaning cavity 9 through the flow regulating valve 5; a fluid source in the fluid storage tank 1 is converted into supercritical fluid after being subjected to pressurization treatment by a booster pump 3 and heat exchange treatment by a heat exchanger 4 in sequence; and the cleaning chamber is composed of a first cleaning cavity 9 and a second cleaning cavity 10 with different cross sections, the first cleaning cavity 9 is connected with the fluid storage tank 1, and supercritical fluid can be introduced or discharged.
In this embodiment, the supercritical fluid cleaning apparatus further includes: the induced draft fan 14 is connected with the second washing cavity 10; the inlet of the separation tank 15 is connected with the induced draft fan 14, the outlet of the separation tank is connected with the first stop valve 16 and the heat exchanger 4 through a pipeline, and the outlet of the separation tank is connected with the fluid storage tank 1 through a second stop valve 17 through a pipeline; the supercritical fluid containing the pollutants discharged from the cleaning chamber is sent into a separation tank through a draught fan to be subjected to pressure reduction and separation treatment, and the separated fluid is stored in a fluid storage tank or is converted into supercritical fluid to be circularly introduced into the cleaning chamber after being subjected to heat exchange through a heat exchanger so as to recycle the discharged supercritical fluid containing the pollutants.
After the cleaning is finished, the pollutants and the supercritical fluid which are discharged through the second cleaning cavity 10 in a decompression mode are sent into the separation tank 15 through the draught fan 14, the supercritical fluid cleaning agent, the pollutants and the auxiliary agent are separated in the separation tank 15, the auxiliary agent is purified and dried and then recovered, and the fluid is converted into the supercritical fluid again after heat exchange and is used as the cleaning agent for recycling, so that the recycling of resources is realized, the energy consumption is saved, and the production cost is reduced.
Example 4
Referring to fig. 1, the present embodiment provides a supercritical fluid cleaning apparatus for cleaning precision components, including devices in IT manufacturing and MEMS manufacturing, which features small device size, narrow gap, and difficult cleaning of contaminants in the gap. The characteristic that the density of the supercritical fluid is violent in the change of pressure and temperature near a critical point is utilized, the change of the pressure of the supercritical fluid and the temperature of a workpiece is realized by adopting a specially designed cleaning chamber structure and a heater structure and utilizing different cross sections of adjacent cleaning cavities, the supercritical fluid is diffused into pollutants when the pressure and the temperature are increased, bubbles are formed in the pollutants when the pressure and the temperature are reduced, and the repeated circulation is carried out continuously, so that the pollutants are separated from the workpiece to achieve the purpose of cleaning. The higher dissolving capacity of the supercritical fluid is beneficial to dissolving the pollutants into the supercritical fluid, the near-zero surface tension of the supercritical fluid is beneficial to cleaning the pollutants in a narrow space, and the high diffusion coefficient of the supercritical fluid is beneficial to mass transfer between the pollutants and the fluid and improving the cleaning rate.
Referring to fig. 1, a supercritical fluid cleaning apparatus for cleaning a precision component according to an embodiment includes: a fluid storage tank 1 for providing a fluid source; the booster pump 3 is connected with the fluid storage tank 1, and a one-way valve 2 is arranged on a pipeline between the fluid storage tank 1 and the booster pump 3; the inlet of the heat exchanger 4 is connected with the booster pump 3, and the outlet of the heat exchanger is connected with the first cleaning cavity 9 through the flow regulating valve 5; a fluid source in the fluid storage tank 1 is converted into supercritical fluid after being subjected to pressurization treatment by a booster pump 3 and heat exchange treatment by a heat exchanger 4 in sequence; a cleaning chamber, which is composed of a first cleaning cavity 9 and a second cleaning cavity 10 with different cross-sectional areas, wherein the first cleaning cavity 9 is connected with the fluid storage tank 1 and can be filled with or discharged with supercritical fluid; and the heater is arranged on the workpiece rack in the cleaning chamber to heat the workpiece.
In this embodiment, the supercritical fluid cleaning apparatus further includes: the induced draft fan 14 is connected with the second washing cavity 10; the inlet of the separation tank 15 is connected with the induced draft fan 14, the outlet of the separation tank is connected with the first stop valve 16 and the heat exchanger 4 through a pipeline, and the outlet of the separation tank is connected with the fluid storage tank 1 through a second stop valve 17 through a pipeline; the supercritical fluid containing the pollutants discharged from the cleaning chamber is sent into a separation tank through a draught fan to be subjected to pressure reduction and separation treatment, and the separated fluid is stored in a fluid storage tank or is converted into supercritical fluid to be circularly introduced into the cleaning chamber after being subjected to heat exchange through a heat exchanger so as to recycle the discharged supercritical fluid containing the pollutants.
After the cleaning is finished, the discharged supercritical fluid carries pollutants into a separation kettle, the pollutants dissolved in the supercritical fluid are separated out due to the reduction of the environmental pressure, and the fluid enters a cleaning chamber for recycling after pressurization and heating. Specifically, the pollutant-containing and supercritical fluid discharged by the second washing chamber 10 under reduced pressure is sent to the separation tank 15 through the induced draft fan 14, the supercritical fluid cleaning agent, the pollutant and the auxiliary agent are separated in the separation tank 15, the auxiliary agent is recovered after being purified and dried, and the fluid is converted into the supercritical fluid again after heat exchange and is recycled as the cleaning agent. Realizes the repeated utilization of resources, saves energy consumption and reduces production cost.
Example 5
Referring to FIG. 2, this embodiment provides a pressure-regulated clean room for use in embodiments 1-4 above. The cleaning chamber is used as a part of the superfluid flow channel and is divided into a first cleaning cavity 9 and a second cleaning cavity 10, the geometric shape and the size of the cleaning chamber can be determined according to the size of a workpiece, the first cleaning cavity 9 and the second cleaning cavity 10 are arranged adjacently, the cross section area of the first cleaning cavity 9 perpendicular to the flow direction is A1, the cross section area of the second cleaning cavity 10 part perpendicular to the flow direction is A2, and A1 is larger than A2. According to the continuous equation, the flow rate V1 of first cleaning chamber 9 will be greater than the flow rate V2 of second cleaning chamber 10, and the pressure P1 of the portion of second cleaning chamber 10 will be greater than the pressure P2 of the portion of first cleaning chamber 9 according to Bernoulli's equation, and the magnitudes of P1 and P2 can be varied by varying the magnitude of A1> A2.
In the pressure-adjustable cleaning chamber provided by this embodiment, an air inlet on a first cleaning cavity 9 is connected to a heat exchanger 4, and receives a supercritical fluid obtained by heat exchange and conversion of the heat exchanger 4; an exhaust port on the second cleaning cavity 10 is connected with an induced draft fan 14, and the supercritical fluid containing the pollutants after the workpiece is cleaned is discharged out of the second cleaning cavity 10 through the induced draft fan 14.
Example 6
Referring to fig. 3, the present embodiment provides a heating mechanism for heating a workpiece 18 in embodiments 2 and 4, including a workpiece holder 19, a heater 20, a resistor 21, a power supply 22, a thyristor switch 23, a temperature sensor 24, and a thyristor switch 25. The power supply 22 is supplied with 220V.
The workpiece 18 is held in a heater 22 mounted on the workpiece holder 19, the heater 22 has the function of rapidly raising and lowering the temperature of the workpiece 18, the temperature of the workpiece 18 is measured by a temperature sensor 26, then the temperature value of the workpiece 18 is transmitted to a silicon controlled switch 25, the silicon controlled switch 25 controls the on and off of a circuit according to the cleaning process parameters, and then the heater 22 is controlled to heat the workpiece 18.
Example 7
With continued reference to fig. 1 and 2, the present embodiment provides a transfer chamber mechanism for moving a workpiece into and out of a cleaning chamber, wherein a supercritical cleaning process is performed at a high pressure, and wherein the transfer chamber mechanism comprises: a first transfer chamber 6 disposed at an inlet of the first cleaning chamber 9; and a second transfer chamber 12 disposed at an outlet of the second cleaning chamber 10.
In the whole process of cleaning the workpiece, the first cleaning cavity 9 and the second cleaning cavity 10 work in a critical state, and the working temperature and the working pressure are higher. When the workpiece 18 is transferred to the first transfer chamber 6 from the outside or the previous process, the pressure and temperature in the first transfer chamber 6 should be normal temperature and normal pressure from the practical production point of view, two isolated sealed spaces are formed between the first transfer chamber 6 and the first cleaning chamber 9, and the first transfer chamber 6 is much smaller than the first cleaning chamber 9. After the workpiece to be cleaned enters the first transfer chamber 6, closing the first transfer chamber 6, and injecting high-pressure gas into the first transfer chamber 6 to balance the pressure of the first transfer chamber 6 with the pressure of the first cleaning cavity 9; then, the first quick-open door 8 between the first transfer chamber 6 and the first cleaning chamber 9 is opened, and the workpiece 18 is transferred from the first transfer chamber 6 to the first cleaning chamber 9; after the workpiece 18 is completely transferred from the transfer chamber 6 to the first cleaning chamber 9, the first quick-opening door 8 is closed, and the workpiece feeding operation is completed.
Similarly, when the workpiece 18 is transferred from the second cleaning chamber 10 to the second transfer chamber 12, the pressure and temperature in the second transfer chamber 12 should be normal temperature and normal pressure from the practical production point of view, two isolated sealed spaces are between the second cleaning chamber 10 and the second transfer chamber 12, and the second transfer chamber 12 is much smaller than the second cleaning chamber 10. After the workpiece 18 is cleaned in the first cleaning cavity 9 and the second cleaning cavity 10, injecting high-pressure gas into the second transfer chamber 12 to balance the pressure of the second transfer chamber 12 with the pressure of the second cleaning cavity 10; then, a second quick-opening door 11 between a second transfer chamber 12 and a second cleaning chamber 10 is opened, the workpiece 18 is transferred from the second cleaning chamber 10 into the second transfer chamber 12, the second quick-opening door 11 is closed after the transfer is finished, and the pressure in the second transfer chamber 12 is reduced to further evaporate the cleaning agent on the surface of the workpiece 18; then, the outlet of the second transfer chamber 12 is opened, and the cleaned workpiece is conveyed out to complete the workpiece discharging operation.
Example 8
Based on the cleaning methods and apparatuses of embodiments 1 to 7, this embodiment provides a supercritical fluid cleaning process for precision devices, including devices in IT manufacturing and MEMS manufacturing, which is characterized by small device size and narrow gap. The cleaning process flow is shown in figure 1, and a complete flow process is formed by three parts, including a supercritical fluid cleaning agent preparation and storage part, a supercritical fluid cleaning part and a recycling part.
In this embodiment, the supercritical fluid cleaning agent preparation and storage section includes preparation, pressurization and heating of the supercritical fluid source. The source of supercritical fluid can be commercially available as a liquid nitrogen tank or can be produced on-site as nitrogen gas from a nitrogen generator set. The supercritical fluid source flows out of the fluid storage tank 1 and sequentially passes through the one-way valve 2, the booster pump 3, the heat exchanger 4, the flow regulating valve 5, the first cleaning cavity 9, the first cleaning cavity 10, the induced draft fan 14, the separating tank 15, the first stop valve 16 and the heat exchanger 4 to form a complete supercritical fluid circulation.
In this embodiment, in order to realize the entrance and exit of the workpiece, the present embodiment provides a transfer chamber mechanism for the entrance and exit of the workpiece to and from the cleaning chamber, which includes a first transfer chamber 6 and a second transfer chamber 12, and a first cleaning chamber 9 and a second cleaning chamber 10 are respectively connected to the first transfer chamber 6 and the second transfer chamber 12.
In the cleaning process, the first cleaning chamber 9 and the second cleaning chamber 10 work in a critical state, and the working temperature and the pressure are relatively high. When the workpiece is transferred to the first transfer chamber 6 from the outside or the previous process, the pressure and temperature of the first transfer chamber 6 should be normal temperature and normal pressure from the practical production consideration, two isolated sealed spaces are arranged between the first transfer chamber 6 and the first cleaning cavity 9, and the first transfer chamber 6 is much smaller than the first cleaning cavity 9. After the workpiece enters the first transfer chamber 6, high-pressure gas is injected into the transfer chamber to equalize the pressure of the first transfer chamber 6 with the pressure of the first cleaning chamber 9. Then, the quick opening door between the first transfer chamber 6 and the first cleaning chamber 9 is opened, the workpiece is transferred from the first transfer chamber 6 to the first cleaning chamber 9, and the quick opening door is closed after the workpiece is transferred from the first transfer chamber 6 and the first cleaning chamber 9. After the cleaning of the work pieces in the first cleaning chamber 9 and the second cleaning chamber 10 is completed, the work pieces are conveyed out through the second transfer chamber 12.
In addition, in some occasions, some cleaning aids are required to be added in the cleaning requirement, the aids are used for promoting the physical and chemical action between the pollutants and the cleaning liquid, improving the solvent and diffusion of the pollutants in the cleaning liquid and the like, and the aids adopt one or more of methanol, ethanol and acetone.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.

Claims (12)

1. A supercritical fluid cleaning method, comprising the steps of:
continuously introducing supercritical fluid into the cleaning chamber;
alternately changing the pressure in the cleaning chamber or the temperature of the workpiece to cause the supercritical fluid to repeatedly form cavities or bubbles in contaminants on the surface of the workpiece, the contaminants being released from the surface of the workpiece;
and discharging the pollutants separated from the workpiece along with the supercritical fluid to finish workpiece cleaning.
2. The supercritical fluid cleaning method according to claim 1, wherein the supercritical fluid is carbon dioxide, nitrogen, water, air or inert gas.
3. The supercritical fluid cleaning method according to claim 1, wherein the process of alternating the pressure in the cleaning chamber is: and pulse-type introducing the supercritical fluid, or introducing the supercritical fluid into the cleaning chambers with different cross-sectional areas.
4. The supercritical fluid cleaning method according to claim 1, wherein the process of alternating the temperature of the workpiece is: and changing the surface temperature of the workpiece by adopting a heating mode.
5. The supercritical fluid cleaning method according to claim 1, wherein the discharged supercritical fluid containing the contaminants is subjected to decompression separation, pressurization and temperature reduction, and then is converted into the supercritical fluid again for recycling.
6. The supercritical fluid cleaning method according to claim 1, further comprising:
and before the supercritical fluid is introduced into the cleaning chamber, one or more of methanol, ethanol and acetone are added into the supercritical fluid in advance for mixing.
7. A supercritical fluid cleaning apparatus according to the method of any one of claims 1 to 6, comprising:
a fluid storage tank for providing a fluid source, wherein the fluid source is converted into supercritical fluid after pressurization and heat exchange;
and the cleaning chamber is connected with the fluid storage tank, can be filled with or discharged with the supercritical fluid, and is composed of at least two cleaning cavities with different cross sectional areas.
8. The supercritical fluid cleaning apparatus according to claim 7, further comprising:
and the heater is arranged on the workpiece rack in the cleaning chamber to heat the workpiece.
9. The supercritical fluid cleaning apparatus according to claim 7, further comprising:
a booster pump connected to the fluid storage tank; and
the inlet of the heat exchanger is connected with the booster pump, and the outlet of the heat exchanger is connected with the cleaning chamber;
and the fluid source in the fluid storage tank is converted into supercritical fluid to be introduced into the cleaning chamber after being subjected to pressurization treatment by the booster pump and heat exchange treatment by the heat exchanger in sequence.
10. The supercritical fluid cleaning apparatus according to claim 7, further comprising:
the induced draft fan is connected with the cleaning chamber; and
the inlet of the separation tank is connected with the induced draft fan, and the outlet of the separation tank is respectively connected with the fluid storage tank and the heat exchanger;
and the supercritical fluid containing the pollutants discharged from the cleaning chamber is sent into the separation tank through the induced draft fan to be subjected to pressure reduction and separation treatment, and the separated fluid is stored in the fluid storage tank or is converted into supercritical fluid to be introduced into the cleaning chamber in a circulating manner after being subjected to heat exchange through the heat exchanger.
11. The supercritical fluid cleaning apparatus according to claim 7, wherein the cleaning chamber comprises a first cleaning cavity and a second cleaning cavity arranged adjacently and smoothly transiting, wherein:
an air inlet on the first cleaning cavity is connected with the heat exchanger;
an air outlet on the second cleaning cavity is connected with the induced draft fan;
and the cross-sectional area of the first cleaning cavity is larger than that of the second cleaning cavity.
12. The supercritical fluid cleaning apparatus according to claim 11, further comprising:
the first transfer chamber is arranged at the inlet of the first cleaning cavity; and
and the second transfer chamber is arranged at the outlet of the second cleaning cavity.
CN202010691159.8A 2020-07-17 2020-07-17 Supercritical fluid cleaning method and device Pending CN111974752A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112974412A (en) * 2021-02-23 2021-06-18 中国核动力研究设计院 Chemical decontamination method and device for radioactive pollution by supercritical carbon dioxide
CN114018085A (en) * 2021-11-02 2022-02-08 珠海格力绿色再生资源有限公司 Device and method for cleaning air conditioner stamping oil by adopting supercritical technology
CN114798602A (en) * 2022-04-26 2022-07-29 四川博腾创达智能科技有限公司 Method for cleaning particle pollutants
CN114949924A (en) * 2022-06-09 2022-08-30 华南理工大学 Method for separating organic matters in mixed components by using reinforced supercritical fluid combined medium
CN115069685A (en) * 2022-07-22 2022-09-20 中国船舶重工集团公司第七0七研究所 Dry cleaning system and dry cleaning method for hemispherical harmonic oscillator for gyroscope
CN115540527A (en) * 2022-09-29 2022-12-30 浙江大学 Supercritical fluid drying system and drying method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112974412A (en) * 2021-02-23 2021-06-18 中国核动力研究设计院 Chemical decontamination method and device for radioactive pollution by supercritical carbon dioxide
CN114018085A (en) * 2021-11-02 2022-02-08 珠海格力绿色再生资源有限公司 Device and method for cleaning air conditioner stamping oil by adopting supercritical technology
CN114798602A (en) * 2022-04-26 2022-07-29 四川博腾创达智能科技有限公司 Method for cleaning particle pollutants
WO2023208255A1 (en) * 2022-04-26 2023-11-02 四川博腾创达智能科技有限公司 Cleaning method for particulate pollutants
CN114798602B (en) * 2022-04-26 2024-01-23 四川博腾创达智能科技有限公司 Method for cleaning particle pollutants
CN114949924A (en) * 2022-06-09 2022-08-30 华南理工大学 Method for separating organic matters in mixed components by using reinforced supercritical fluid combined medium
WO2023236388A1 (en) * 2022-06-09 2023-12-14 华南理工大学 Method for strengthening separation of organic matter in mixed component by means of supercritical fluid combined medium
CN115069685A (en) * 2022-07-22 2022-09-20 中国船舶重工集团公司第七0七研究所 Dry cleaning system and dry cleaning method for hemispherical harmonic oscillator for gyroscope
CN115540527A (en) * 2022-09-29 2022-12-30 浙江大学 Supercritical fluid drying system and drying method
CN115540527B (en) * 2022-09-29 2024-02-27 浙江大学 Supercritical fluid drying system and drying method

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