CN113484446A - Method for testing micro-pollution on surface of packaging bag for clean room - Google Patents
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- 238000004806 packaging method and process Methods 0.000 title claims abstract description 58
- 238000012360 testing method Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 34
- 150000002500 ions Chemical class 0.000 claims abstract description 24
- 150000001450 anions Chemical class 0.000 claims abstract description 10
- 150000001768 cations Chemical class 0.000 claims abstract description 10
- 239000000919 ceramic Substances 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 5
- 239000012498 ultrapure water Substances 0.000 claims abstract description 5
- 238000004364 calculation method Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 31
- 239000002184 metal Substances 0.000 claims description 18
- 238000011109 contamination Methods 0.000 claims description 16
- 238000004255 ion exchange chromatography Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000009616 inductively coupled plasma Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229920001774 Perfluoroether Polymers 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 229920001903 high density polyethylene Polymers 0.000 claims description 4
- 239000004700 high-density polyethylene Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- -1 polypropylene Polymers 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 229910052755 nonmetal Inorganic materials 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052714 tellurium Inorganic materials 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 9
- 238000001514 detection method Methods 0.000 description 7
- 239000000356 contaminant Substances 0.000 description 6
- 238000012856 packing Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
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- 229910001410 inorganic ion Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
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- 230000035945 sensitivity Effects 0.000 description 2
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- 239000004677 Nylon Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 229920003023 plastic Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N2001/028—Sampling from a surface, swabbing, vaporising
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- Physics & Mathematics (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to the technical field of semiconductors. A method for testing micro-pollution on the surface of a packaging bag for a clean room comprises the following steps: firstly, cutting a packaging bag film in a sampling area of a clean room by using clean ceramic scissors; step two, using a sealer to seal the film into a bag with three closed sides and one open side; step three, adding an extracting solution into the bag, adjusting the extracting solution according to the surface area of the bag, sealing the bag, and standing for 24 hours; then transferring the extracting solution into a clean empty bottle, testing the content of anions and cations in the extracting solution, and testing the content of metal elements in the extracting solution; step four, filling ultrapure water into another clean sample bottle and standing for 24 hours; testing the content of anions and cations in the extracting solution, and testing the content of metal elements in the extracting solution; step five: and taking the difference value of the two test results, and finally obtaining the content of the trace ions on the surface of the packaging bag to be tested and the content of the metal elements on the surface of the packaging bag through formula calculation.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method for testing surface pollution of a packaging bag.
Background
The packaging is an important link in the production process, and means that the operations such as wrapping and packaging are carried out on the product, so that the product is prevented from being polluted, collided, damaged and the like in the transportation and transmission process. Particularly, in the production process of semiconductor products, along with the continuous improvement of process requirements, the requirements on packaging are higher and higher. As for the selection of the packaging material, a plastic packaging bag is generally used for packaging the product, so that a better packaging effect is obtained.
Since the packing bag is in close contact with the packing material, the contaminants remaining on the surface of the packing bag are easily transferred to the packing material. For semiconductor devices and precision parts, trace contamination can cause product defects directly or indirectly to cause quality problems, so that surface contaminants of the packaging bag must be strictly controlled, thereby avoiding the pollution of the packaging bag to the packaging materials. Inorganic ion contamination and metal element contamination are two surface contaminants of concern in packaging bags. The monitoring of the micro-pollutants on the surface of the packaging bag plays an important role in reducing pollution and improving product yield. However, the packages tend to be of different sizes and do not have a fixed shape, making extraction and detection of contaminants within the package difficult.
For the detection of inorganic ionic contaminants and metal contaminants, commonly used detection techniques are Ion Chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS). IC is one of the most effective instruments for measuring the content of trace ions at present, has the advantages of low detection limit at ppb level, high sensitivity, simultaneous measurement of various ion contents and the like, and has been widely used for the research of ion contamination. An inductively coupled plasma mass spectrometer (hereinafter referred to as ICP-MS) is one of the most effective instruments for measuring trace elements at present, and is a trace element analysis technology which develops the fastest at present. ICP-MS has the advantages of low detection limit of ppt level, high sensitivity, wide linear dynamic range, simultaneous determination of contents of various elements and the like, so that the ICP-MS is widely and generally applied to the fields of environment, geology, semiconductors, biomedicine and nuclear application.
The currently common test means for the ion pollution and the metal pollution on the solid surface is a throwing immersion sampling method, namely, an extraction solution with a proper volume is selected to soak the surface of a sample, the sample is recovered after a certain time, and the inorganic ion content and the metal pollutant content on the surface of a component can be obtained through IC and ICP-MS tests. However, for the packaging bag, the density is often lower than that of water, and the packaging bag cannot be completely immersed in the water under the action of buoyancy, so that the micro-pollution content on the surface of the packaging bag cannot be accurately measured by adopting a throwing immersion method.
Therefore, it is important to develop a method for testing the micro-contamination on the surface of the clean room packaging bag.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for testing the surface micro-pollution of a packaging bag for a clean room, which aims to solve at least one technical problem.
In order to achieve the above object, the present invention provides a method for testing micro-contamination on a surface of a clean room packaging bag, comprising the steps of:
firstly, cutting a packaging bag film by using clean ceramic scissors in a sampling area of a clean room of 100 or above grade;
step two, using a sealer to seal the film into a bag with three closed sides and one open side;
step three, adding an extracting solution into the bag, adjusting the extracting solution according to the surface area of the bag, sealing the bag, and standing for 24 hours;
then transferring the extracting solution into a clean empty bottle, testing the content of anions and cations in the extracting solution by using ion chromatography, and testing the content of metal elements in the extracting solution by using an inductively coupled plasma mass spectrometer;
step four, filling ultrapure water into another clean sample bottle, and standing for 24 hours to serve as a blank;
testing the content of anions and cations in the extracting solution by using ion chromatography, and testing the content of metal elements in the extracting solution by using an inductively coupled plasma mass spectrometer;
step five: and taking the difference value of the two test results, and finally obtaining the content of the trace ions on the surface of the packaging bag to be tested and the content of the metal elements on the surface of the packaging bag through formula calculation.
Further preferably, between the first step and the second step, the film is purged with nitrogen to remove surface particles.
Further preferably, in the third step, after sealing, the mixture is left standing for 24 hours, a corner of the mixture is cut off by using ceramic scissors, and the extracting solution is transferred out.
Further preferably, the detectable trace ions on the surface of the packaging bag to be detected comprise F-、Cl-、NO2 -、Br-、NO3 -、PO4 3-、SO4 2-、Li+、Na+、NH4 +、K+、Mg2+And Ca2+。
Further preferably, the detectable elements include metal elements of the second period to the sixth period and 5 kinds of non-metal elements of B, Si, As, Se, and Te.
Further preferably, in the third step, the injection amount of the extract solution is 2000ml per square meter.
Further preferably, the clean sample bottle is made of High Density Polyethylene (HDPE), polypropylene (PP) or Perfluoroalkoxy (PFA).
The sample liquid contained in the HDPE or PP sample bottle is used for testing the ion content, and the sample liquid contained in the PFA sample bottle is used for testing the metal element content.
Further preferably, the clean sample bottle is washed with pure water for at least six times before use and dried for standby.
It is further preferred that, in step five,
the unit of the content of the trace ions on the surface of the packaging bag to be detected is E11molecules/cm2；
Wherein: cpThe content of the surface trace ions measured in the third step is in the unit of mu g/L;
CBthe content of the surface trace ions measured in the step four is in the unit of mu g/L;
v is the volume of the extracting solution, and the unit is mL;
NAavogalois constants: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
It is further preferred that, in step five,
the unit of the metal element content of the surface of the packaging bag is E10atoms/cm2；
Wherein: cpThe concentration of the metal element measured in the third step is ng/L;
CBmeasuring the concentration of the metal element in ng/L in the fourth step;
v is the volume of the extracting solution, and the unit is mL;
NAavogalois constants: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
Has the advantages that:
the invention adopts the water-containing extraction method which is simple and convenient to operate, and on one hand, the contact with air is avoided, so that the inside of the packaging bag is ensured not to be polluted; on the other hand, the efficiency of extracting the micro-pollution on the surface of the packaging bag can be effectively improved.
Drawings
FIG. 1 is a flow chart of the process of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
In specific example 1, a surface micro-contamination analysis of a polyethylene packaging bag. The method comprises the following steps:
step one, in a sampling area of a clean room of class 100 or above, a clean ceramic scissors is used to cut off a film of a lower packing bag, as shown in fig. 1 (a). Clean ceramic scissors are carefully used to penetrate the packaging film to avoid sawing and chopping actions and to prevent particle generation.
The film was purged with nitrogen to remove surface particles.
And step two, sealing the film into a bag with three closed sides and one open side by using a sealing machine. See (b) in fig. 1.
Step three, according to the surface area of 0.126m2: the extract was added to the bag in a volume of 0.252L, see (c) in FIG. 1. And then capped, see (d) in fig. 1. And standing for 24 hours.
The extract was then transferred to a clean empty bottle, see (e) in fig. 1. And testing the content of anions and cations in the extracting solution by using ion chromatography, and recording the content as a later value.
Testing the content of metal elements in the extracting solution by using an inductively coupled plasma mass spectrometer; is recorded as the latter value.
Step four, filling ultrapure water into another clean sample bottle, and standing for 24 hours to serve as a blank;
the content of anions and cations in the extract was measured by Ion Chromatography (IC) and recorded as the previous value.
And (4) testing the content of the metal elements in the extracting solution by using an inductively coupled plasma mass spectrometer (ICP-MS), and recording the content as a previous value.
Step five: and taking the difference value of the two test results, and calculating by the following formula to obtain a result, namely the trace ion pollution content on the surface of the packaging bag to be tested.
The unit of the content of the trace ions on the surface of the packaging bag to be detected is E11molecules/cm2；
Wherein: cpThe content of the surface trace ions measured in the third step is expressed as a unit of mug/L and is recorded as a 'rear value';
CBthe content of the surface trace ions measured in the fourth step is expressed as a unit of mug/L and is recorded as a front value;
v is the volume of the extracting solution, and the unit is mL;
NA is the Avogastron constant: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
The results are calculated and shown in Table 1.
TABLE 1
And taking the difference value of the two test results, and calculating by the following formula to obtain a result, namely the content of the metal element on the surface of the packaging bag to be tested.
The unit of the metal element content of the surface of the packaging bag is E10atoms/cm2；
Wherein: cpThe concentration of the metal element measured in the third step is ng/L;
CBmeasuring the concentration of the metal element in ng/L in the fourth step;
v is the volume of the extracting solution, and the unit is mL;
NAavogalois constants: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
The results are calculated and shown in Table 2.
TABLE 2
Specific example 2
A method for analyzing micro-pollution on the surface of a nylon packaging bag. The method comprises the following steps:
step one, cutting off the packaging bag film by using clean ceramic scissors in a sampling area of a clean room with the grade of 100 or above. Clean ceramic scissors are carefully used to penetrate the packaging film to avoid sawing and chopping actions and to prevent particle generation.
The film was purged with nitrogen to remove surface particles.
Step two, using a sealer to seal the film into a bag with three closed sides and one open side;
step three, according to the surface area of 0.126m2: the bag was filled with the extract in an amount of 0.252L, followed by sealing and leaving the chamber clean for 24 hours.
The extract was then transferred to a clean sample vial.
The content of anions and cations in the extract was measured by Ion Chromatography (IC) and recorded as the latter value.
The content of metal elements in the extract was measured by ICP-MS and recorded as the latter value.
Step four, filling ultrapure water into another clean sample bottle, and standing for 24 hours to serve as a blank.
The content of anions and cations in the extract was measured by Ion Chromatography (IC) and recorded as the previous value.
Measuring the content of metal elements in the extracting solution by ICP-MS, and recording as a previous value;
step five: and taking the difference value of the two test results, and calculating by the following formula to obtain a result, namely the trace ion pollution content on the surface of the packaging bag to be tested.
The unit of the content of the trace ions on the surface of the packaging bag to be detected is E11molecules/cm2；
Wherein: cpThe content of the surface trace ions measured in the third step is expressed as a unit of mug/L and is recorded as a 'rear value';
CBthe content of the surface trace ions measured in the fourth step is expressed as a unit of mug/L and is recorded as a front value;
v is the volume of the extracting solution, and the unit is mL;
NAavogalois constants: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
The results were calculated as shown in the following table.
Where "/" in the above table means below the detection limit.
And taking the difference value of the two test results, and calculating by the following formula to obtain a result, namely the content of the metal element on the surface of the packaging bag to be tested.
The unit of the metal element content of the surface of the packaging bag is E10atoms/cm2；
Wherein: cpThe concentration of the metal element measured in the third step is ng/L;
CBmeasuring the concentration of the metal element in ng/L in the fourth step;
v is the volume of the extracting solution, and the unit is mL;
NAavogalois constants: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
The results were calculated as shown in the following table.
Where "/" in the above table means below the detection limit.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.
Claims (10)
1. A method for testing micro-pollution on the surface of a packaging bag for a clean room is characterized by comprising the following steps:
firstly, cutting a packaging bag film by using clean ceramic scissors in a sampling area of a clean room of 100 or above grade;
step two, using a sealer to seal the film into a bag with three closed sides and one open side;
step three, adding an extracting solution into the bag, adjusting the extracting solution according to the surface area of the bag, sealing the bag, and standing for 24 hours;
then transferring the extracting solution into a clean empty bottle, testing the content of anions and cations in the extracting solution by using ion chromatography, and testing the content of metal elements in the extracting solution by using an inductively coupled plasma mass spectrometer;
step four, filling ultrapure water into another clean sample bottle, and standing for 24 hours to serve as a blank;
testing the content of anions and cations in the extracting solution by using ion chromatography, and testing the content of metal elements in the extracting solution by using an inductively coupled plasma mass spectrometer;
step five: and taking the difference value of the two test results, and finally obtaining the content of the trace ions on the surface of the packaging bag to be tested and the content of the metal elements on the surface of the packaging bag through formula calculation.
2. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: and between the first step and the second step, purging the film by using nitrogen to remove surface particles.
3. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: and step three, after sealing, standing for 24 hours, cutting off one corner by using ceramic scissors, and transferring the extracting solution.
4. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: detectable trace ions contained in the surface of the packaging bag to be detected comprise F-、Cl-、NO2 -、Br-、NO3 -、PO4 3-、SO4 2-、Li+、Na+、NH4 +、K+、Mg2+And Ca2+。
5. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: the detectable elements include metal elements of the second period to the sixth period and 5 kinds of non-metal elements of B, Si, As, Se, and Te.
6. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: in step three, the injection amount of the extracting solution is 2000ml per square meter.
7. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: the clean sample bottle is made of high-density polyethylene, polypropylene or perfluoroalkoxy resin.
8. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: the clean sample bottle is washed by pure water for more than six times before use and is dried for standby.
9. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: in the fifth step, the step of,
the unit of the content of the trace ions on the surface of the packaging bag to be detected is E11molecules/cm2；
Wherein: cpThe content of the surface trace ions measured in the third step is in the unit of mu g/L;
CBthe content of the surface trace ions measured in the step four is in the unit of mu g/L;
v is the volume of the extracting solution, and the unit is mL;
NAavogalois constants: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
10. The method for testing micro-contamination on a surface of a clean room packaging bag according to claim 1, wherein the method comprises the steps of: in the fifth step, the step of,
the unit of the content of the metal elements on the surface of the packaging bag is E10atoms/cm2；
Wherein: cpThe concentration of the metal element measured in the third step is ng/L;
CBmeasuring the concentration of the metal element in ng/L in the fourth step;
v is the volume of the extracting solution, and the unit is mL;
NAavogalois constants: 6.022 × 1023；
Aw is the relative atomic/molecular mass;
s is the internal surface area of the sealed bag and the unit is cm2。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115684328A (en) * | 2022-09-28 | 2023-02-03 | 上海富乐德智能科技发展有限公司 | Method for testing trace element pollution on surface of strong-hydrophobicity soft membrane |
| CN115792080A (en) * | 2022-12-05 | 2023-03-14 | 上海富乐德智能科技发展有限公司 | Method for testing trace ion pollution on surface of semiconductor manufacturing equipment component |
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| CN108020542A (en) * | 2017-12-21 | 2018-05-11 | 重庆超硅半导体有限公司 | The detection method of pollutant load in a kind of film magazine |
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2021
- 2021-08-04 CN CN202110890729.0A patent/CN113484446A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003177120A (en) * | 2001-08-30 | 2003-06-27 | Toppan Printing Co Ltd | Analyzing method of out-ion, measuring method of particle and elution, and clean film and its laminated material |
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| CN108020542A (en) * | 2017-12-21 | 2018-05-11 | 重庆超硅半导体有限公司 | The detection method of pollutant load in a kind of film magazine |
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| CN115684328A (en) * | 2022-09-28 | 2023-02-03 | 上海富乐德智能科技发展有限公司 | Method for testing trace element pollution on surface of strong-hydrophobicity soft membrane |
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