CN108212912A - The cleaning method of glow discharge mass spectrometry equipment potsherd - Google Patents
The cleaning method of glow discharge mass spectrometry equipment potsherd Download PDFInfo
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- CN108212912A CN108212912A CN201611161131.3A CN201611161131A CN108212912A CN 108212912 A CN108212912 A CN 108212912A CN 201611161131 A CN201611161131 A CN 201611161131A CN 108212912 A CN108212912 A CN 108212912A
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- potsherd
- cleaning
- glow discharge
- mass spectrometry
- ultrasonic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
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- Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention provides a kind of cleaning method of glow discharge mass spectrometry equipment potsherd, including：Glow discharge mass spectrometry equipment potsherd is provided；First cleaning is carried out to potsherd；The second cleaning is carried out after first cleaning to potsherd, the second cleaning includes ultrasonic cleaning process；Technique is dried to potsherd under preset temperature after second cleaning.First cleaning is mainly used for removing the metal impurities on potsherd surface, since potsherd has more micropore in itself, easy adsorbing contaminant (such as dissolving metal object after the first cleaning) in micropore, therefore pass through ultrasonic cleaning process, the residual impurity in micropore after the first cleaning can be effectively removed, and when technique is dried under preset temperature, it can also make the residual impurity evaporation of remaining low melting point in micropore, so as to improve the impurity removal effect to potsherd, it is remaining to reduce potsherd impurity, and then improve the detection accuracy and detection efficiency of glow discharge mass spectrometry.
Description
Technical field
The present invention relates to elemental analysis field more particularly to a kind of cleaning sides of glow discharge mass spectrometry equipment potsherd
Method.
Background technology
Glow discharge mass spectrometry (Glow Discharge Mass Spectrometry, GDMS) is that current high purity solid is conductive
Material purity is analyzed and impurity component analyzes most efficient method.Glow discharge mass spectrometry is by the use of glow discharge source as ion source
Couple a kind of analysis method for carrying out mass spectral analysis with mass spectrometer, with high sensitivity, detection limit is low, can analyze 70 kinds simultaneously
The advantages that more than impurity element.Since glow discharge mass spectrometry can increasingly be widely used in height with Direct solid sampling
The analysis of the materials such as simple metal, alloy.
Glow discharge mass spectrometry is made of glow discharge ion source (GD sources) and mass spectrometer two parts.Glow discharge ion
The ion that source ionizes generation using inert gas (usually argon gas, pressure about 10Pa to 100Pa) under upper kilovolt voltage is hit
Sample surfaces to be hit to be allowed to sputter, the sample atoms for sputtering generation are diffused in plasma and are further ionized, and then by
Mass spectrometer collects detection.
But the detection accuracy and detection efficiency of prior art glow discharge mass spectrometry are relatively low.
Invention content
The present invention solves the problems, such as to be to provide a kind of cleaning method of glow discharge mass spectrometry equipment potsherd, raising aura
Discharge mass spectrographic detection accuracy and detection efficiency.
To solve the above problems, the present invention provides a kind of cleaning method of glow discharge mass spectrometry equipment potsherd, including：
Glow discharge mass spectrometry equipment potsherd is provided；First cleaning is carried out to the potsherd；After first cleaning, to institute
It states potsherd and carries out the second cleaning, second cleaning includes ultrasonic cleaning process；After second cleaning,
Technique is dried to the potsherd under preset temperature.
Optionally, first cleaning is acid cleaning process.
Optionally, in the step of carrying out the first cleaning to the potsherd, the pickling solution used is hydrofluoric acid, nitre
The mixed solution of acid and water.
Optionally, the process time of the acid cleaning process is 1 minute to 3 minutes.
Optionally, the step of carrying out the second cleaning to the potsherd includes：Using distilled water to the potsherd
Carry out pre-cleaning processes；After pre-cleaning processes, ultrasonic cleaning process is carried out to the potsherd in distilled water.
Optionally, the pre-cleaning processes include at least 3 times leaching operations；The step of leaching operation, includes：By institute
Potsherd is stated to immerse in distilled water；The potsherd is taken out from the distilled water.
Optionally, the pre-cleaning processes include the leaching operation of 3 times to 5 times.
Optionally, the step of carrying out ultrasonic cleaning process to the potsherd in distilled water includes at least 3 times distillations
Water is cleaned by ultrasonic；The step of distilled water is cleaned by ultrasonic includes：It is clear that the distilled water ultrasound is carried out using ultrasonic oscillator
It washes, the power of the ultrasonic oscillator is 150W to 500W, and output frequency is 20KHz to 40KHz, and scavenging period is 1 minute
To 3 minutes.
Optionally, the step of carrying out ultrasonic cleaning process to the potsherd in distilled water includes the steaming of 3 times to 5 times
Distilled water is cleaned by ultrasonic.
Optionally, it is to the step of potsherd the second cleaning of progress：In distilled water to the potsherd into
Row ultrasonic cleaning process.
Optionally, the step of carrying out ultrasonic cleaning process to the potsherd in distilled water includes at least 5 times distillations
Water is cleaned by ultrasonic；The step of distilled water is cleaned by ultrasonic includes：It is clear that the distilled water ultrasound is carried out using ultrasonic oscillator
It washes, the power of the ultrasonic oscillator is 150W to 500W, and output frequency is 20KHz to 40KHz, and scavenging period is 1 minute
To 3 minutes.
Optionally, the step of carrying out ultrasonic cleaning process to the potsherd in distilled water is including 5 times to 10 times
Distilled water is cleaned by ultrasonic.
Optionally, the step of technique being dried to the potsherd under preset temperature includes：Under normal pressure to described
Potsherd is dried, and preset temperature is 150 degrees Celsius to 250 degrees Celsius, and drying time is 30 minutes to 90 minutes.
Optionally, the step of technique being dried to the potsherd under preset temperature includes：To the potsherd into
Row vacuum drying, preset temperature are 150 degrees Celsius to 250 degrees Celsius, and drying time is 30 minutes to 90 minutes.
Compared with prior art, technical scheme of the present invention has the following advantages：
After the present invention carries out the first cleaning to glow discharge mass spectrometry equipment with potsherd, the is carried out to the potsherd
Two cleanings, second cleaning include ultrasonic cleaning process, and after second cleaning, in default temperature
Technique is dried to the potsherd under degree；First cleaning is mainly used for removing the metal on the potsherd surface
Impurity, since the potsherd has more micropore in itself, in the micropore easily adsorbing contaminant (such as：First cleaning
Dissolving metal object after technique), therefore by ultrasonic cleaning process of the present invention, first cleaning can be effectively removed
After technique in the micropore residual impurity (such as：Dissolving metal object after first cleaning), and in preset temperature
Under when technique is dried to the potsherd, the residual impurity evaporation of remaining low melting point in the micropore can also be made；Therefore
By scheme of the present invention, the removal effect to impurity on the potsherd can be improved, is reduced in the potsherd micropore
Impurity it is remaining, it might even be possible to thoroughly remove the impurity, so as to the influence that impurity is avoided to detect glow discharge mass spectrometry,
And then improve the detection accuracy and detection efficiency of glow discharge mass spectrometry.
In alternative, the step of potsherd the second cleaning of progress, is included：Using distilled water to the pottery
Tile carries out pre-cleaning processes；After pre-cleaning processes, ultrasonic cleaning process is carried out to the potsherd in distilled water.Pass through
The pre-cleaning processes first can largely remove the first cleaning on the potsherd surface before ultrasonic cleaning process is carried out
The residual cleaning solution of technique, also can remove the potsherd surface residual impurity (such as：After first cleaning
Dissolving metal object), convenient for subsequently carrying out ultrasonic cleaning process, be conducive to improve cleaning efficiency.
Description of the drawings
Fig. 1 is after using a kind of cleaning method of glow discharge mass spectrometry equipment potsherd, measured by glow discharge mass spectrometry
The content of impurity element and the graph of relation of detection time；
Fig. 2 is the flow diagram of one embodiment of cleaning method of glow discharge mass spectrometry equipment potsherd of the present invention；
Fig. 3 is the structure diagram of potsherd corresponding to step S1 in embodiment described in Fig. 2；
Fig. 4 is the flow diagram corresponding to step S3 in embodiment described in Fig. 2；
Fig. 5 is the structure diagram corresponding to step S31 in embodiment described in Fig. 4；
After Fig. 6 is the cleaning method using glow discharge mass spectrometry equipment potsherd of the present invention, glow discharge mass spectrometry is surveyed
Obtain the content of impurity element and the graph of relation of detection time.
Specific embodiment
By background technology it is found that the detection accuracy of glow discharge mass spectrometry and detection efficiency are to be improved.Analyze its reason
It is：
Two panels potsherd discrete and being arranged in parallel is equipped in glow discharge mass spectrometry equipment, the potsherd, which is located at, treats test sample
Between product and glow discharge ion source (GD sources)；In glow discharge mass spectrometry equipment, sample to be tested side be cathode, glow discharge
Ion source side is anode, for playing insulating effect the anode and cathode is isolated, to prevent positive and negative anodes in the potsherd
It is in direct contact, so as to avoid the occurrence of short circuit phenomenon.
Wherein, the shape of the potsherd is circular ring shape, i.e., described potsherd center has through-hole, glow discharge mass spectrometry inspection
During survey, the ionic bombardment sample to be tested surface that inert gas ionizes generation under upper kilovolt voltage is allowed to sputter,
Sputtering generate sample atoms diffused in plasma by the through-hole, therefore the potsherd surface be susceptible to it is to be measured
Sample reverse sputtering depositional phenomenon, i.e. sample atoms easily occur deposition on the potsherd surface and form sample deposit.
In addition, ionized inert gas generate ionic bombardment sample to be tested surface when, the ion simultaneously also hit described in
Potsherd surface sputters the potsherd.Therefore when the potsherd surface has the sample deposit of other samples
When, the sample deposit having on the potsherd surface can become the impurity in detection process instantly, that is, cause to examine instantly
The problems such as measuring the phenomenon that existing impurity content is higher, increasing so as to cause detection inaccuracy or detection stabilization time.
Since the cost of potsherd is higher, in order to solve, the detection of impurity band is inaccurate or detection stability time increases
The problems such as, the method that mainly uses for：After each sample detection, replace and clean the potsherd, and after cleaning
It reuses.Specifically, the step of cleaning the potsherd includes：Acid cleaning process is carried out to the potsherd；After acid cleaning process,
The potsherd is cleaned using distilled water, to reach deacidification effect；After distilled water cleaning, using acetone to the ceramics
Piece is cleaned, and the partial moisture on the potsherd is removed using the effumability of acetone；After acetone cleaning, by the ceramics
Piece naturally dry.
But since the potsherd has more micropore in itself, easily adsorb in the micropore minute impurities (such as：
Dissolving metal object after acid cleaning process), and the impurity is difficult to clean by distilled water and remove, therefore it is micro- to remove the potsherd
The effect of impurity is not obvious in hole.
With reference to reference to figure 1, show after being cleaned to potsherd, the content of impurity element measured by glow discharge mass spectrometry
With the graph of relation of detection time, wherein abscissa represents detection time, and ordinate represents impurity content in detection.By
After the relation curve 15 is it is found that clean potsherd, still there is the phenomenon that impurity content is higher, potsherd in when detection
Interior residual impurity easily impacts the detection of high-purity material (4N-6N) result；And detection time to 75 minutes or so when
Impurity content just tends towards stability, therefore detection efficiency is still corresponding relatively low.
The potsherd surface will also be caused to be turned to be yellow in addition, cleaning for a long time is not thorough, so as to cause the potsherd
Service life declines.
To solve the above-mentioned problems, the present invention provides a kind of cleaning method of glow discharge mass spectrometry equipment potsherd, packet
It includes：Glow discharge mass spectrometry equipment potsherd is provided；First cleaning is carried out to the potsherd；After first cleaning,
The second cleaning is carried out to the potsherd, second cleaning includes ultrasonic cleaning process；Second cleaning
Afterwards, technique is dried to the potsherd under preset temperature.
After the present invention carries out the first cleaning to glow discharge mass spectrometry equipment with potsherd, the is carried out to the potsherd
Two cleanings, second cleaning include ultrasonic cleaning process, and after second cleaning, in default temperature
Technique is dried to the potsherd under degree；First cleaning is mainly used for removing the metal on the potsherd surface
Impurity, the potsherd have more micropore in itself, in the micropore easily adsorbing contaminant (such as：First cleaning
Dissolving metal object afterwards), by ultrasonic cleaning process of the present invention, institute after first cleaning can be effectively removed
State in micropore residual impurity (such as：Dissolving metal object after first cleaning), and to described under preset temperature
When technique is dried in potsherd, the residual impurity evaporation of remaining low melting point in the micropore can also be made；Therefore pass through this hair
The bright scheme, can improve the removal effect to impurity on the potsherd, and the impurity reduced in the potsherd micropore is residual
It is remaining, it might even be possible to thoroughly to remove the impurity, so as to the influence that impurity is avoided to detect glow discharge mass spectrometry, and then improve
Improve the detection accuracy and detection efficiency of glow discharge mass spectrometry.
It is understandable for the above objects, features and advantages of the present invention is enable to become apparent, below in conjunction with the accompanying drawings to the present invention
Specific embodiment be described in detail.
With reference to figure 2, the flow of one embodiment of cleaning method of glow discharge mass spectrometry equipment potsherd of the present invention is shown
Schematic diagram, the cleaning method of the present embodiment glow discharge mass spectrometry equipment potsherd include following basic step：
Step S1：Glow discharge mass spectrometry equipment potsherd is provided；
Step S2：First cleaning is carried out to the potsherd；
Step S3：After first cleaning, the second cleaning, the second cleaning packet are carried out to the potsherd
Include ultrasonic cleaning process；
Step S4：After second cleaning, technique is dried to the potsherd under preset temperature.
It, below will knot in order to which the cleaning method of glow discharge mass spectrometry equipment potsherd of the embodiment of the present invention is better described
It closes with reference to figure 3 to Fig. 6, specific embodiments of the present invention is further described.
With reference to referring to figs. 2 and 3, Fig. 3 is the structure diagram of potsherd corresponding to step S1 in embodiment described in Fig. 2.
Step S1 is performed, glow discharge mass spectrometry (Glow Discharge Mass Spectrometry, GDMS) equipment ceramics are provided
Piece 100 (as shown in Figure 3).
Glow discharge mass spectrometry is for analyzing high purity solid conductive material purity and impurity component, glow discharge mass spectrometry
It is made of glow discharge ion source and mass spectrometer two parts.In the present embodiment, the glow discharge mass spectrometry is used for High Purity Gold
The analysis of the materials such as category, alloy.
Specifically, two panels potsherd 100 discrete and being arranged in parallel, the potsherd are equipped in glow discharge mass spectrometry equipment
100 between sample to be tested and glow discharge ion source (GD sources), wherein a piece of potsherd 100 is located at the sample to be tested one
Side, another potsherd 100 are located at the glow discharge ion source side；In glow discharge mass spectrometry equipment, sample to be tested one
Side is cathode, and glow discharge ion source side is anode, the potsherd 100 for playing insulating effect, that is, be isolated it is described just
Pole and cathode, anode and cathode to be prevented to be in direct contact, so as to avoid the occurrence of short circuit phenomenon.
The shape of the potsherd 100 is circular ring shape, i.e., described 100 center of potsherd has through-hole 110 (such as Fig. 3 institutes
Show), in glow discharge mass spectrometry detection process, inert gas ionizes the ionic bombardment sample to be tested of generation under upper kilovolt voltage
Surface is allowed to sputter, and the sample atoms for sputtering generation are diffused to by the through-hole 110 in plasma.
Potsherd 100 is same as the prior art described in the present embodiment, to the detailed description of the potsherd 100 herein no longer
It repeats.
Continuing with step S2 referring to figs. 2 and 3, is performed, progress first (as shown in Figure 3) to the potsherd 100 is clear
Wash technique.
When glow discharge mass spectrometry is detected detected sample, inert gas ionizes what is generated under upper kilovolt voltage
Ionic bombardment sample to be tested surface is allowed to sputter, and the sample atoms for sputtering generation pass through the through-hole 110 of the potsherd 100
(as shown in Figure 3) is diffused in plasma, therefore 100 surface of the potsherd is susceptible to sample to be tested reverse sputtering deposition now
As that is, sample atoms easily occur deposition on 100 surface of potsherd and form sample deposit, the sample deposit meeting
Impurity during as next sample detection.
The glow discharge mass spectrometry is used for the analysis of the materials such as high pure metal, alloy, therefore the detected sample is gold
Belong to material, correspondingly, the material of the sample deposit is metal.Therefore, in the present embodiment, first cleaning is acid
Technique is washed, the acid cleaning process is used to dissolve the metal sample deposit on 100 surface of potsherd, so as to reduce the ceramics
The impurity content of piece 100.In other embodiments, first cleaning can also use alkaline solution, and described first is clear
Solution is depending on the material of the metal sample deposit used by washing technique.
In the present embodiment, pickling solution is the mixed solution of hydrofluoric acid, nitric acid and water used by the acid cleaning process.Tool
Body, the potsherd 100 is immersed, acid cleaning process is carried out in pickling solution, hydrofluoric acid, nitric acid and water in the pickling solution
The ratio between volume percent content be 1:1:6；After completing the acid cleaning process, by the potsherd 100 from the pickling solution
Middle taking-up.
While in order to ensure to dissolve the effect of metal sample deposit, the waste of process time and cost is avoided, and if
The potsherd 100 is crossed to be in pickling solution for a long time, is also easy to increase process risk.Therefore, in the present embodiment, the acid
The process time for washing technique is 1 minute to 3 minutes.
Flow signal in the embodiment with reference to described in showing Fig. 2 with reference to figure 2, Fig. 4 and Fig. 5, Fig. 4 corresponding to step S3
Figure, Fig. 5 show the structure diagram corresponding to step S31 in embodiment described in Fig. 4.Step S3 is performed, it is right after the first cleaning
The potsherd 100 is (as shown in Figure 3) to carry out the second cleaning, and second cleaning includes ultrasonic cleaning process.
In the present embodiment, second cleaning includes the pre-cleaning processes and ultrasonic cleaning process that successively carry out.
Below in conjunction with attached drawing, the step of second cleaning, is described in detail.
As shown in figure 5, performing step S31, pre-cleaning processes are carried out to the potsherd 100 using distilled water 210.
By the pre-cleaning processes, pickling solution is largely remained to remove 100 surface of potsherd, also can remove
The potsherd surface residual impurity (such as：Dissolving metal object after first cleaning), convenient for subsequently being surpassed
Sound wave cleaning is conducive to improve cleaning efficiency.
The pre-cleaning processes include at least 3 times leachings and operate, to ensure to have good removal effect.Specifically, institute
It states distilled water 210 to be contained in container 200, described the step of leaching operation includes：The potsherd 100 is immersed into the distillation
In water 210 (direction is immersed as shown in arrow A1 in Fig. 5)；Then the potsherd 100 is taken out from the distilled water 210
(removing direction is as shown in arrow A2 in Fig. 5).3 are at least repeated that is, being operated by immersing and take out the leaching formed
It is secondary.
In the present embodiment, while in order to ensure good removal effect, the waste of process time and cost is avoided, it is described pre-
The number that cleaning carries out leaching operation is 3 times to 5 times.
Step S32 is performed, after completing pre-cleaning processes, ultrasonic cleaning is carried out to the potsherd 100 in distilled water
Technique
The potsherd 100 itself has more micropore (not shown), is easily adsorbed in the micropore of the potsherd 100 micro-
Small impurity (such as：Dissolving metal object after first cleaning), by the ultrasonic cleaning process, can effectively go
Except after first cleaning in the micropore residual impurity (such as：Dissolving metal after first cleaning
Object), so as to advantageously reduce the impurity of the potsherd 100 remnants.
Specifically, the step of carrying out ultrasonic cleaning process to the potsherd 100 in distilled water includes at least 3 times steamings
Distilled water is cleaned by ultrasonic, to ensure the effect with residual impurity in the good removal micropore.
Specifically, the step of distilled water is cleaned by ultrasonic includes：The distilled water is carried out using ultrasonic oscillator to surpass
Sound cleans, and the power of the ultrasonic oscillator is 150W to 500W, and output frequency is 20KHz to 40KHz.
It should be noted that the processing time that the distilled water is cleaned by ultrasonic is unsuitable too short, it is also unsuitable long.If processing
Time is too short, then is easy to cause that degree of cleaning is inadequate, removes the effect unobvious of residual impurity in the micropore；If during processing
Between it is long, completely removal residual impurity after, waste time instead, cause the increase of process costs, the decline of cleaning efficiency, and
It is also easy to increase process risk.For this purpose, in the present embodiment, the scavenging period that the distilled water is cleaned by ultrasonic is 1 minute to 3 points
Clock.
In the present embodiment, while in order to ensure residual impurity effect in the good removal micropore, when avoiding technique
Between and cost waste, the ultrasonic cleaning process carry out distilled water ultrasonic cleaning number be 3 times to 5 times.
It should also be noted that, in other embodiments, it is to the step of potsherd the second cleaning of progress：
Ultrasonic cleaning process is carried out to the potsherd in distilled water, i.e., only by ultrasonic cleaning process, to realize to the pottery
Second cleaning of tile.
At this point, the ultrasonic cleaning process be applied not only to remove in the micropore residual impurity (such as：Described first
Dissolving metal object after cleaning), it is additionally operable to remove the residual pickling solution on 100 surface of potsherd and the pottery
The residual impurity on 100 surface of tile.
Therefore, in order to only by the ultrasonic cleaning process to achieve the effect that cleaning, to institute in distilled water
It states the step of potsherd carries out ultrasonic cleaning process and includes at least 5 distilled water ultrasonic cleaning.Specifically, the distilled water surpasses
The step of sound cleans includes：The distilled water ultrasonic cleaning, the work(of the ultrasonic oscillator are carried out using ultrasonic oscillator
Rate is 150W to 500W, and output frequency is 20KHz to 40KHz, and scavenging period is 1 minute to 3 minutes.
Correspondingly, while in order to ensure good cleaning performance, the waste of process time and cost is avoided, only by super
When sound wave cleaning is to realize the second cleaning, the ultrasonic cleaning process carries out the number of distilled water ultrasonic cleaning
It is 5 times to 10 times.
With continued reference to Fig. 2, step S4 is performed, after the second cleaning, under preset temperature to the potsherd 100 (such as
Shown in Fig. 3) technique is dried.
The drying process is used to remove residual moisture in 100 surface of potsherd and micropore, in addition, by
The drying process is carried out under preset temperature, the impurity evaporation of remaining low melting point in the micropore can also be made.
In the present embodiment, the step of technique is dried to the potsherd 100 under preset temperature, includes：Under normal pressure
The potsherd 100 is dried.
It should be noted that in the drying process step, preset temperature is unsuitable too low, also unsuitable excessively high.It is if default
Temperature is too low, then the effect for removing residual moisture is poor or reach long the time required to drying effect；If preset temperature mistake
Height, easily generates harmful effect to the performance of the potsherd 100, and process risk is larger.For this purpose, in the present embodiment, temperature is preset
Spend is 150 degrees Celsius to 250 degrees Celsius.
The drying time of the drying process is set with preset temperature collocation, wherein, drying time is unsuitable too short,
It is unsuitable long.If drying time is too short, the effect for removing residual moisture is poor；If drying time is long, gone completely
After the residual moisture in 100 surface of potsherd and micropore, cross the potsherd 100 Celsius in 150 for a long time
Under degree to 250 degrees Celsius of temperature environment, harmful effect easily is generated to the performance of the potsherd 100 instead.For this purpose, this reality
It applies in example, drying time is 30 minutes to 90 minutes.
In other embodiments, the potsherd can also be dried in vacuo with described in realization under preset temperature
Drying process, for example, by using vacuum drying chamber.When being dried under vacuum conditions, be conducive in 100 micropore of potsherd
The precipitation of residual impurity, so as to be conducive to improve the removal effect of impurity on the potsherd 100.
Specifically, in the step of being dried in vacuo to the potsherd, preset temperature is Celsius for 150 degrees Celsius to 250
Degree, drying time are 30 minutes to 90 minutes.
In the present embodiment, the first cleaning is carried out with potsherd 100 (as shown in Figure 3) to glow discharge mass spectrometry equipment
Afterwards, the second cleaning is carried out to the potsherd 100, second cleaning includes ultrasonic cleaning process, and in institute
After stating the second cleaning, technique is dried to the potsherd 100 under preset temperature；First cleaning is main
For removing the metal impurities on 100 surface of potsherd, since the potsherd 100 itself has more micropore, (figure is not
Show), easily adsorb in the micropore minute impurities (such as：Dissolving metal object after first cleaning), therefore pass through
The ultrasonic cleaning process, can effectively remove after first cleaning in the micropore residual impurity (such as：Institute
State the dissolving metal object after the first cleaning), and when technique is dried to the potsherd 100 under preset temperature, also
It can make the impurity evaporation of remaining low melting point in the micropore, so as to improve the removal to impurity on the potsherd 100
Effect reduces the impurity content in 100 micropore of potsherd, it might even be possible to thoroughly remove the impurity, and then can be to avoid
The influence that impurity detects glow discharge mass spectrometry improves the detection accuracy and detection efficiency of glow discharge mass spectrometry.
With reference to reference to figure 6, after showing the cleaning method using glow discharge mass spectrometry equipment potsherd of the present invention, aura
Discharge the content of impurity element and the graph of relation of detection time measured by mass spectrum.Wherein abscissa represents detection time, indulges
Impurity content in coordinate representation detection.
By the relation curve 150 it is found that by the drying process under the ultrasonic cleaning process and preset temperature,
Impurity content is declined during detection, and can shorten detection stabilization time, such as can be foreshortened to 45 minutes by 75 minutes, from
And detection accuracy and detection efficiency can be improved.
In addition, by the present invention cleaning method, can also avoid the potsherd 100 occur cleaning for a long time it is halfway
Problem, therefore also help the service life for extending the potsherd 100.
Although oneself is disclosed in the preferred embodiments as above the present invention, present invention is not limited to this.Any art technology
Personnel without departing from the spirit and scope of the present invention, can make various changes or modifications, therefore protection scope of the present invention should
When being subject to claim limited range.
Claims (14)
1. a kind of cleaning method of glow discharge mass spectrometry equipment potsherd, which is characterized in that including：
Glow discharge mass spectrometry equipment potsherd is provided；
First cleaning is carried out to the potsherd；
After first cleaning, the second cleaning is carried out to the potsherd, it is clear that second cleaning includes ultrasonic wave
Wash technique；
After second cleaning, technique is dried to the potsherd under preset temperature.
2. the cleaning method of glow discharge mass spectrometry equipment potsherd as described in claim 1, which is characterized in that described first
Cleaning is acid cleaning process.
3. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 2, which is characterized in that the pottery
Tile was carried out in the step of the first cleaning, and the pickling solution used is the mixed solution of hydrofluoric acid, nitric acid and water.
4. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 2, which is characterized in that the pickling
The process time of technique is 1 minute to 3 minutes.
5. the cleaning method of glow discharge mass spectrometry equipment potsherd as described in claim 1, which is characterized in that the pottery
The step of tile the second cleaning of progress, includes：Pre-cleaning processes are carried out to the potsherd using distilled water；Prerinse work
After skill, ultrasonic cleaning process is carried out to the potsherd in distilled water.
6. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 5, which is characterized in that described pre- clear
It washes technique and includes at least 3 times leaching operations；
The step of leaching operation, includes：The potsherd is immersed in distilled water；By the potsherd from the distilled water
Middle taking-up.
7. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 6, which is characterized in that described pre- clear
Wash the leaching operation that technique includes 3 times to 5 times.
8. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 5, which is characterized in that in distilled water
In the step of ultrasonic cleaning process is carried out to the potsherd include at least 3 distilled water and be cleaned by ultrasonic；
The step of distilled water is cleaned by ultrasonic includes：The distilled water ultrasonic cleaning is carried out using ultrasonic oscillator, it is described
The power of ultrasonic oscillator is 150W to 500W, and output frequency is 20KHz to 40KHz, and scavenging period is 1 minute to 3 minutes.
9. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 8, which is characterized in that in distilled water
In to the potsherd carry out ultrasonic cleaning process the step of including the distilled water of 3 times to 5 times be cleaned by ultrasonic.
10. the cleaning method of glow discharge mass spectrometry equipment potsherd as described in claim 1, which is characterized in that described
Potsherd carry out the second cleaning the step of be：Ultrasonic cleaning process is carried out to the potsherd in distilled water.
11. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 10, which is characterized in that distilling
The step of carrying out ultrasonic cleaning process to the potsherd in water includes at least 5 distilled water and is cleaned by ultrasonic；
The step of distilled water is cleaned by ultrasonic includes：The distilled water ultrasonic cleaning is carried out using ultrasonic oscillator, it is described
The power of ultrasonic oscillator is 150W to 500W, and output frequency is 20KHz to 40KHz, and scavenging period is 1 minute to 3 minutes.
12. the cleaning method of glow discharge mass spectrometry equipment potsherd as claimed in claim 11, which is characterized in that distilling
The step of carrying out ultrasonic cleaning process to the potsherd in water is cleaned by ultrasonic including the distilled water of 5 times to 10 times.
13. the cleaning method of glow discharge mass spectrometry equipment potsherd as described in claim 1, which is characterized in that default
At a temperature of the step of technique is dried to the potsherd include：The potsherd is dried under normal pressure, presets temperature
It is 150 degrees Celsius to 250 degrees Celsius to spend, and drying time is 30 minutes to 90 minutes.
14. the cleaning method of glow discharge mass spectrometry equipment potsherd as described in claim 1, which is characterized in that default
At a temperature of the step of technique is dried to the potsherd include：The potsherd is dried in vacuo, preset temperature is
150 degrees Celsius to 250 degrees Celsius, drying time is 30 minutes to 90 minutes.
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| CN201611161131.3A CN108212912A (en) | 2016-12-15 | 2016-12-15 | The cleaning method of glow discharge mass spectrometry equipment potsherd |
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