WO2019192494A1 - 增强射频辉光放电质谱信号强度的装置及方法 - Google Patents
增强射频辉光放电质谱信号强度的装置及方法 Download PDFInfo
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- WO2019192494A1 WO2019192494A1 PCT/CN2019/081067 CN2019081067W WO2019192494A1 WO 2019192494 A1 WO2019192494 A1 WO 2019192494A1 CN 2019081067 W CN2019081067 W CN 2019081067W WO 2019192494 A1 WO2019192494 A1 WO 2019192494A1
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- sample
- signal intensity
- radio frequency
- glow discharge
- magnet
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
- H01J37/32018—Glow discharge
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- 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
- G01N27/68—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 electric discharge to ionise a gas
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/3266—Magnetic control means
- H01J37/32669—Particular magnets or magnet arrangements for controlling the discharge
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/105—Ion sources; Ion guns using high-frequency excitation, e.g. microwave excitation, Inductively Coupled Plasma [ICP]
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/4697—Generating plasma using glow discharges
Definitions
- the invention belongs to the technical field of inorganic mass spectrometry.
- the present invention relates to the field of analytical materials for radio frequency glow discharge mass spectrometry, and more particularly to apparatus and methods for enhancing the signal intensity of radio frequency glow discharge mass spectrometry using magnets.
- Glow Discharge Mass Spectrometry has the characteristics of high direct injection, high sensitivity, small matrix effect, and more than 70 elements in one time. It is widely used in the analysis of trace elements in high purity conductor materials.
- RF glow discharge mass spectrometry has attracted much attention due to its ability to directly analyze conductors, semiconductors, and non-conductor materials.
- the charged particles move back and forth between the electrodes under the action of the electric field force. Taking one cycle as an example, in the negative half cycle of the RF source, a large amount of positive ions move toward the surface of the sample, and the sample accumulates a large amount of positive charges.
- the Penning ionization in the cathodic sputtering and negative glow region of the cathode dark region is the two key factors affecting the signal intensity. Improving the sputtering and ionization efficiency is an important idea to improve the test results.
- some RF glow discharge instruments such as rf-GD-OES, rf-GD-AES, etc.
- the signal intensity of matrix elements and impurity elements in the sample is improved to some extent.
- the material, size, and magnetic induction intensity distribution of the magnet are fixed.
- the magnetic field cannot be adjusted in real time during the test, and the signal strength adjustment needs to be improved.
- the invention aims to provide a device and a method for enhancing the signal intensity of a radio frequency glow discharge mass spectrometer by using a magnet to enhance the signal intensity of the material when the material is low in the existing RF glow discharge mass spectrometry, and to enhance the signal of the inorganic material by the enhanced RF glow discharge mass spectrometer. strength.
- a first apparatus and method of the present invention provides, on the one hand, a device for enhancing the signal intensity of a radio frequency glow discharge mass spectrum using an array magnet,
- a sample introduction device having a sample injection rod and a sample fixed thereto;
- An array magnet reinforcement having a housing and an array of magnets
- the array magnet reinforcement is fixed between the injection rod and the sample in the sample introduction device and is in close contact with the sample.
- the array magnet enhancement improves the performance of the RF glow discharge mass spectrometer for material analysis.
- the structure of the invention is simple and reasonable, can effectively improve the signal strength and analytical sensitivity of the instrument, and is suitable for a glow discharge mass spectrometer or the like.
- the outer casing is made of a metal or an alloy.
- the outer casing is a cylinder, a rectangular parallelepiped or a cube.
- the outer diameter of the outer casing should be less than or equal to the inner diameter of the sample introduction device and the height is less than the height of the sample introduction device.
- the array-arranged magnets are composed of a plurality of permanent magnets having the same magnetic line direction.
- the array-arranged magnets are in close contact with the upper and lower surfaces of the outer casing.
- the array-arranged magnets are placed in a housing, and the magnetic induction direction of each magnet is parallel to the sample.
- the sample may comprise: a sample of a conductor, a semiconductor, a non-conductive material.
- a method for enhancing the intensity of a signal intensity of a radio frequency glow discharge mass spectrum using an array magnet comprising: a sample introduction device having a sample injection rod with a sample attached thereto, and an array magnet having a housing and an array of magnets arranged in an array
- the device of the reinforcement includes the following steps;
- the array magnet reinforcement is mounted and fixed between the sample rod and the sample in the sample introduction device, and is closely attached to the sample;
- the current is conducted to the sample through the injection rod and the casing, and the device forms a magnetic field on the side of the sample near the discharge battery;
- the sample to be tested is scanned and the signal intensity is recorded.
- the device is placed between the injection rod and the sample in the sample introduction device, after the RF power source is started, the current is conducted to the sample through the injection rod and the metal shell, and the array magnet enhancement device is on the side of the sample near the discharge battery.
- the formation of a magnetic field generates an oscillating magnetic field, thereby prolonging the electron motion path to increase the collision probability of electrons and neutral particles, and improving the ionization efficiency, thereby increasing the ion signal intensity.
- a second apparatus and method of the present invention provides, on the one hand, a device for enhancing the signal intensity of a radio frequency glow discharge mass spectrum using a ring magnet,
- a sample introduction device having a sample rod and having a ceramic gasket fixed thereto;
- a ring magnet reinforcement having a casing and a ring magnet
- the annular magnet is placed in the outer casing, and the annular magnet reinforcement is fixed between the injection rod and the ceramic spacer in the sample introduction device.
- the use of a ring magnet reinforcement improves the performance of the RF glow discharge mass spectrometer for material analysis.
- the device has a simple structure, and the inorganic material samples analyzed by the device of the invention include: conductors, semiconductors, non-conductor materials, etc., without the need of a conductor material, without complicated sample preparation work, avoiding pollution, and reducing analysis cost.
- the signal intensity is high during discharge, the discharge is stable, and the signal-to-noise ratio (S/N) is ideal, which shortens the analysis time and improves the analysis efficiency.
- the outer casing is made of metal or alloy.
- the outer casing may be a hollow cylinder, a hollow cube or a hollow cuboid.
- the outer diameter of the annular magnet is smaller than the outer diameter of the outer casing, and the inner diameter is larger than the inner diameter of the outer casing, and the height of the annular magnet is smaller than that of the outer casing. height.
- the sample to be tested is located in the inner bore of the annular magnet.
- the sample to be tested is surrounded to form a magnetic field reinforcing portion, and the sample is embedded in the ring magnet.
- the current is conducted to the sample through the injection rod and the outer casing.
- the sample to be tested may include: a conductor, a semiconductor, a non-conductor material.
- Another aspect provides a method for enhancing the signal intensity of a radio frequency glow discharge mass spectrometer using a ring magnet, using a sample introduction device having a sample rod and having a ceramic spacer fixed thereto, and a ring magnet reinforcement having a casing and a ring magnet
- the device includes the following steps:
- the sample to be tested is scanned and the signal intensity is recorded.
- the annular magnetic field enhancement portion has a circular magnetic induction line distribution. Under the action of electric field force and Lorentz force, the electrons make a spiral motion around the magnetic induction line, and the electron trajectory is prolonged, which greatly increases the collision probability of electrons and atoms. The ionization efficiency is improved compared to the case where no magnetic field is applied. In addition, more ionized argon ions bombard the surface of the sample under the action of an electric field, and the sputtering rate is also increased.
- a third apparatus and method of the present invention provides, on the one hand, a device for enhancing the signal intensity of a radio frequency glow discharge mass spectrometer using an adjustable magnetic field,
- a sample introduction device having a sample injection rod and a sample fixed thereto;
- An adjustable magnetic field enhancement having an outer casing and an electromagnet consisting of a powered solenoid and an iron core,
- the electromagnet is placed in the outer casing,
- the adjustable magnetic field enhancement portion is fixed between the injection rod and the sample in the sample introduction device.
- the use of this device to analyze metal, semiconductor, and non-conductor materials eliminates the need for conductive materials, eliminates the need for complex sample preparation, avoids contamination, and reduces analysis costs.
- the signal intensity is high during discharge, and the discharge is stable.
- the magnetic induction intensity can be adjusted by changing the current of the energizing solenoid, thereby adjusting the signal intensity to obtain an ideal signal-to-noise ratio. (S/N), shorten analysis time and improve analysis efficiency.
- the magnetic field generated by the energized solenoid is mainly used to improve the analysis performance of the material by the RF glow discharge mass spectrometer, and the magnetic field strength is adjusted by adjusting the coil current to realize the real-time regulation of the signal intensity.
- the outer casing is made of metal or alloy.
- the outer casing is a cylinder, a cube or a rectangular parallelepiped.
- the outer diameter of the outer casing is less than or equal to the inner diameter of the sampling device, and the height is less than the height of the sampling device.
- the length of the electromagnet is smaller than the inner diameter of the outer casing, the diameter of the electromagnet is smaller than the height of the outer casing, and the number of turns of the coil is n ⁇ 5.
- the electromagnet is fixed in the outer casing using an insulating material
- Lead wires of the energizing solenoid are passed out from the two small holes on the side of the outer casing and connected to a power source.
- the power source can be a direct current power source or an alternating current power source.
- the sample can include a sample of a conductor, a semiconductor, a non-conductive material.
- Another aspect provides a method for enhancing the signal intensity of an RF glow discharge mass spectrometer using an adjustable magnetic field, comprising using a sample introduction device having a sample injection rod and having a sample attached thereto, and having a housing and an energized solenoid and a core
- the device for adjusting the magnetic field reinforcing portion of the electromagnet comprises the following steps;
- the sample to be tested is scanned and the signal intensity is recorded.
- the adjustable magnetic field enhancement section generates magnetism under the energization condition of the solenoid.
- Under the action of the electric field force and the Lorentz force the electrons are spirally moved around the magnetic induction line, and the movement path of the electron is prolonged. , greatly increasing the collision probability of electrons and atoms.
- the ionization efficiency is improved.
- more ionized argon ions bombard the surface of the sample under the action of an electric field, and the sputtering rate is also increased.
- Signal enhancement The signal strength is related to the energized solenoid current.
- RF light-emitting discharge mass spectrometry has important technical problems such as low ion signal intensity and low sensitivity when analyzing materials or deep analysis of non-conductor materials (crystal, ceramic, powder, etc.), which restricts rf-GD- The use of MS in the field of new materials.
- the invention discloses a device and a method for enhancing the signal intensity of a radio frequency glow discharge mass spectrometer, which can regulate the motion behavior of the discharge gas particles and electrons (the dominant role in the ionization process) in the process of the photoionization. Under the action of no magnetic field, the trajectory of electrons is relatively simple, and the ionization efficiency is low.
- the device and method of the invention will effectively solve the key technical problems of low sensitivity of rf-GD-MS analysis, and at the same time promote the development and application of rf-GD-MS.
- Figure 1 is a cross-sectional view showing a sample introduction device in an array magnet enhanced radio frequency glow discharge mass spectrometry signal intensity device according to an embodiment of the present invention.
- Fig. 2 is a plan view showing an array magnet reinforcing portion in an array magnet enhanced radio frequency glow discharge mass spectrometry signal intensity device according to an embodiment of the present invention.
- Figure 3 is a cross-sectional view showing a sample introduction device in a device for ring-shaped magnet enhanced radio frequency glow discharge mass spectrometry signal intensity according to an embodiment of the present invention.
- Fig. 4 is a plan view showing a ring magnet reinforcing portion in a device for ring-shaped magnet enhanced radio frequency glow discharge mass spectrometry signal intensity according to an embodiment of the present invention.
- Fig. 5 is a plan view showing a ring magnet reinforcing portion in the apparatus for ring-shaped magnet enhanced radio frequency glow discharge mass spectrometry signal intensity according to the second embodiment of the present invention.
- Figure 6 is a cross-sectional view showing a sample introduction device in an apparatus using an adjustable magnetic field enhanced radio frequency glow discharge mass spectrum signal according to an embodiment of the present invention.
- Fig. 7 is a plan view showing an adjustable magnetic field reinforcing portion in a device using an adjustable magnetic field enhanced radio frequency glow discharge mass spectrum signal according to an embodiment of the present invention.
- the invention provides a device for enhancing the signal intensity of a radio frequency glow discharge mass spectrometer by using a magnet, which is applied to a radio frequency glow discharge mass spectrometer and belongs to the technical field of inorganic mass spectrometry, and is mainly used for analyzing inorganic materials in a radio frequency power mode (including: conductor, semiconductor and non- Conductor material) to solve the problems of low signal intensity and low sensitivity existing in existing mass spectrometer devices.
- a radio frequency power mode including: conductor, semiconductor and non- Conductor material
- the first device provided by the present invention is an array magnet enhanced radio frequency glow discharge mass spectrometry signal intensity device.
- Figure 1 is a cross-sectional view showing a sample introduction device in an array magnet enhanced radio frequency glow discharge mass spectrometry signal intensity device according to an embodiment of the present invention.
- the array magnet enhanced radio frequency discharge mass spectrometry signal intensity device of this embodiment mainly comprises: a sample introduction device having a sample injection rod 10 and a sample 4 fixed thereto; and a magnet having a casing 5 and an array arrangement Array magnet reinforcement of (array magnet 6).
- the array magnet reinforcement is fixed between the injection rod 10 and the sample 4 in the sample introduction device, and is in close contact with the sample 4.
- the cymbal 1, the ceramic spacers 2, 3, and the sample 4 are sequentially laid flat above the outer casing 5.
- the surface of the cymbal 1, ceramic spacers 2, 3 is smooth and smooth.
- the ceramic spacers 2, 3 are insulated and used to maintain vacuum; the cymbal 1 is used for electrical conduction, which is movable between the ceramic spacers 2, 3 and the top of the sample introduction device for easy disassembly cleaning.
- Both the sample 4 and the upper and lower surfaces of the outer casing 5 are smooth surfaces.
- the array magnet 6 is placed inside the outer casing 5, and the upper and lower surfaces are in close contact with the outer casing 5.
- the sample cells 7, 7, and 9 are connected together, and the sample cell is viewed from the outside as a whole.
- Fig. 2 is a plan view showing an array magnet reinforcing portion in an array magnet enhanced radio frequency glow discharge mass spectrometry signal intensity device according to an embodiment of the present invention.
- the outer casing 5 and the array magnet 6 for its interior constitute the array magnet reinforcement.
- the material of the outer casing 5 may be a metal (for example, copper) or an alloy (for example, brass), and the shape may be a cylinder, a rectangular parallelepiped, a square, or the like, and the upper surface and the lower surface are smooth and flat.
- the array magnets 6 are magnets arranged in an array.
- the array magnet 6 is preferably composed of a plurality of permanent magnets having the same magnetic line direction.
- the outer diameter (diameter) of the outer casing 5 is less than or equal to the inner diameter of the sample introduction device of Figure 1, and the height is less than the height of the sample introduction device.
- the magnetic induction direction of the array magnet 6 is parallel to the sample 4, and the upper and lower faces of the array magnet 6 abut against the outer casing 5.
- the sample that can be analyzed by radio frequency glow discharge mass spectrometry can be a sample of inorganic materials, including: conductors, semiconductors, non-conductor materials, and the like.
- the array magnet reinforcement portion is placed between the injection rod 10 and the sample 4 in the sample introduction device and fixedly clamped. After the RF power supply is started, the current is conducted to the sample 4 through the injection rod 10 and the outer casing 5.
- the array magnet reinforcement forms a magnetic field on the side of the sample 4 near the discharge battery, and the array magnet is enhanced compared with the use of the magnetic field or the use of the entire magnetic field.
- the part can generate an oscillating magnetic field, thereby prolonging the electron motion path, increasing the collision probability of electrons with neutral particles, increasing the ionization efficiency, and thereby increasing the ion signal intensity.
- the array magnet 6 in the present invention may be a permanent magnet block having the same or different sizes and a uniform magnetic line direction, and is magnetically self-bonded in an array as an array.
- the size of the array is m ⁇ n (m is a row, n is a column, m ⁇ 2, n ⁇ 2, and m and n may be equal or unequal).
- the array magnet 6, the magnet model can be selected according to the need of the magnetic field strength (for example, the model can be selected as N35, the coercive force is 876kA/m, the magnetic permeability is 1.05), the total height of the magnet is smaller than the height of the outer casing.
- the metal material is processed into a cylindrical outer casing at normal temperature and pressure (taking brass material and cylindrical shape as an example).
- Copper shell internal dimensions 3 mm in diameter, Height 5 mm, copper shell thickness 0.5 mm.
- a magnet with a unit size of 5 mm ⁇ 5 mm ⁇ 5 mm (for example, a N35 neodymium iron boron magnet) is arranged in a magnetic structure (4 ⁇ 4 as an example), and the magnet combination is placed.
- an array magnetic field signal enhancement device array magnet enhancement portion is formed.
- the array array magnet enhancement portion is placed between the injection rod 10 and the sample 4 in the sample introduction device, and after the RF power source (not shown) is activated, the current is conducted to the sample 4 through the injection rod 10 and the outer casing 5, and the device is A magnetic field is formed on the side of the sample 4 near the discharge cell.
- the invention is further illustrated by another embodiment.
- the signal intensity of a typical element detected by an RF glow discharge mass spectrometer including an array magnet reinforcement and an array magnet enhancement is compared.
- RSS relative standard deviation
- raw yttrium oxide (Y 2 O 3 ), Bi 12 SiO 20 (BSO) and Ba 5.52 La 0.32 Ti 2 Nb 8 O 30 (BTN) materials are processed into wafers.
- the sample has a size of 20 mm in section diameter and 2 mm in thickness; it is washed with nitric acid (HNO 3 ), ultrapure water, ethanol, and dried. Subsequently, the sample was subjected to rf-GD-MS analysis under the conditions of RF source power: 30 W, discharge gas (Ar) flow rate: 1.1 cc/min.
- the second device provided by the present invention is a ring magnet enhanced radio frequency glow discharge mass spectrometry signal intensity device.
- Figure 3 is a cross-sectional view showing a sample introduction device in a device for ring-shaped magnet enhanced radio frequency glow discharge mass spectrometry signal intensity according to an embodiment of the present invention.
- the apparatus for enhancing the signal intensity of the radio frequency glow discharge mass spectrometer of the ring magnet of the embodiment mainly includes: a sample introduction device having a sample injection rod 29 and a ceramic spacer 23 fixed thereto;
- a ring magnet reinforcement portion 24 having a casing 24A and a ring magnet 24B;
- the annular magnet 24B is placed in the outer casing 24A, and the annular magnet reinforcement is fixed between the injection rod 29 and the ceramic spacer 23 in the sample introduction device.
- the crotch panel 21, the ceramic spacers 22, 23 are laid flat above the ring magnet reinforcement portion 24 in this order.
- the surface of the cymbal 21 and the ceramic spacers 22, 23 are smooth and smooth.
- the ceramic spacers 22, 23 are insulated and used to maintain vacuum; the cymbal 21 is for electrical conduction, and is movable between the ceramic spacers 22, 23 and the top of the sample introduction device for ease of disassembly cleaning.
- the sample 25 is embedded inside the annular magnet reinforcement 24.
- the sheet sample cells 27, 28, 29 are joined together, and the sample cell is viewed from the outside as a whole.
- FIG. 4 shows a plan view of a ring-shaped magnet reinforcement in the shape of a hollow cylinder.
- the outer casing 24A is made of metal (for example, copper) or an alloy (for example, brass).
- the outer diameter (diameter) is less than or equal to the inner diameter of the sample introduction device, and the inner hole diameter radius is larger than the diameter of the sample and smaller than the outer diameter (diameter) of the outer casing, and the height is smaller than the height of the sample introduction device.
- the magnet model can be selected according to the needs of the magnetic field strength (for example, a magnet of type N35, a coercive force of 876 kA/m, and a magnetic permeability of 1.05) can be selected.
- the outer diameter of the magnet is smaller than the outer diameter of the outer casing, the inner diameter is larger than the inner diameter of the outer casing, and the height of the magnet is smaller than the height of the outer casing.
- the magnetization direction is radial magnetization.
- the direction of magnetization is parallel to the surface of the sample.
- the outer casing 24A may be not only a hollow cylinder but also a hollow cube or a hollow rectangular parallelepiped.
- FIG. 5 shows a plan view of a ring-shaped magnet reinforcement in the shape of a hollow square.
- the sample 25 is embedded in the inner hole of the ring magnet 24B, the annular magnetic field enhancement portion is combined with the sample, and then placed in a sheet sample introduction device to be connected to the RF source. Adjust the appropriate discharge pressure and RF source power for discharge.
- the sample that can be analyzed by radio frequency glow discharge mass spectrometry can be a sample of inorganic materials, including: conductors, semiconductors, non-conductor materials, and the like.
- a hollow cylinder, a hollow cube or a hollow rectangular parallelepiped casing 24A Processing a hollow cylinder, a hollow cube or a hollow rectangular parallelepiped casing 24A, the casing 24A being made of metal or alloy.
- the ring magnet 24B is placed in the outer casing 24A to constitute a ring magnet reinforcement.
- a method for enhancing the signal intensity of a radio frequency glow discharge mass spectrum using the above apparatus comprises the following steps:
- the sample to be tested is scanned and the signal intensity is recorded.
- the metal material is processed into a hollow cylindrical shell 21 (taking brass material, hollow cylinder shape as an example), copper shell internal dimensions: outer diameter 30.5 Mm, metal shell with a bore radius of 20.5 mm, a height of 5 mm and a thickness of 0.5 mm.
- the ring magnet 24 is made of neodymium iron boron material, the magnet type is N35, the coercive force is 876 kA/m, the magnetic permeability is 1.05, the outer diameter of the magnet is 29 mm, the inner diameter is 19 mm, the height is 4.5 mm, and the magnetization direction is radial charge. Magnetic, forming a ring-shaped magnetic field enhancement unit.
- the annular magnetic field enhancement portion is combined with the sample and loaded into the chip sample introduction device.
- the current is conducted to the sample through the injection rod and the outer casing, and the device forms a magnetic field on the side of the sample near the discharge battery.
- the invention is further illustrated by another embodiment.
- the signal intensity of a typical element detected by a radio frequency glow discharge mass spectrometer containing a magnetic field enhancement portion and a magnetic field enhancement portion is compared.
- the greater the difference, the better the signal enhancement effect; Deviation (RSD %) indicates that the new device analyzes the discharge stability of the non-conductor sample. The smaller the value, the better the stability.
- the original yttrium oxide (Y 2 O 3 ), Bi 12 SiO 20 (BSO) and Ba 5.52 La 0.32 Ti 2 Nb 8 O 30 (BTN) materials were processed into a round piece sample having a size of 20 mm in section diameter and thickness. 2 mm; washed with nitric acid (HNO 3 ), ultrapure water, ethanol, and dried. Subsequently, the sample was subjected to rf-GD-MS analysis under the conditions of RF source power: 30 W, discharge gas (Ar) flow rate: 1.1 cc/min.
- the BSO Bi, BTN of Ba 2 O 3 was measured ion signal strength, respectively: 1.91 ⁇ 10 -11 A, 2.55 ⁇ 10 -11 A , 2.17 ⁇ 10 -11 A, relative standard deviation RSD (%) are: 9.8, 10.3, 10.7.
- Rf-GD-MS without ring magnet reinforcement was used to measure Ba in Y and BSO in Y 2 O 3 and Ba in BTN.
- the ion signal intensities were 9.54 ⁇ 10 -12 A and 1.65 ⁇ 10 -11 A, respectively.
- 1.03 ⁇ 10 -11 A, relative standard deviation RSD (%) are: 10.5, 11.5, 12.7.
- the comparison results show that the ion signal intensity and discharge stability obtained by rf-GD-MS analysis with the ring magnet reinforcement are obviously enhanced and improved.
- the third device provided by the present invention is an adjustable magnetic field enhanced radio frequency discharge mass spectrometry signal intensity device.
- Figure 6 is a cross-sectional view showing a sample introduction device in an apparatus using an adjustable magnetic field enhanced radio frequency glow discharge mass spectrum signal according to an embodiment of the present invention.
- the apparatus for adjusting the signal intensity of the magnetic field enhanced radio frequency glow discharge mass spectrum using the embodiment mainly includes: a sample introduction device having a sample injection rod 310 and having the sample 34 fixed; and an outer casing 35 and an electromagnet.
- the magnetic field enhancement section can be adjusted.
- the electromagnet consists of an energized solenoid and an iron core.
- the electromagnet is placed in the outer casing 35 to form an adjustable magnetic field enhancement portion that is placed between the sample 34 and the injection rod 310 in combination.
- the crotch panel 31, the ceramic spacers 32, 33, and the sample 34 are sequentially laid flat above the outer casing 35.
- the surface of the cymbal 31 and the ceramic spacers 32, 33 are smooth and smooth.
- the ceramic spacers 32, 33 are insulated and used to maintain vacuum; the cymbal 31 is used for electrical conduction, and is movable between the ceramic spacers 32, 33 and the top of the sample introduction device for ease of disassembly cleaning.
- Both the sample 34 and the upper and lower surfaces of the outer casing 35 are smooth surfaces.
- the solenoid 36 is placed inside the outer casing 35 with the upper and lower surfaces abutting against the outer casing 35.
- the sheet sample cells 37, 38, 39 are joined together, and the sample cell is viewed from the outside as a whole.
- the injection rod 310 is coupled to the outer casing 35 for fixing the cymbal 31, the ceramic spacers 32, 33, the sample 34, the outer casing 35 and the solenoid 36.
- a spring, not shown, is placed between the injection rod 310 and the outer casing 35 to clamp it.
- a metal core (iron core) 311 is placed in the middle of the solenoid 36 and is a core component of the solenoid magnet device.
- the lead 312 is pierced from a small hole reserved outside the sample cell for energization.
- the adjustable magnetic field enhancement portion is placed between the sample and the injection rod and fixed, and the lead wire is taken out from the small hole of the sample introduction device and energized (AC or DC), and the current can be adjusted to form a current as needed.
- Magnetic field enhancement device In the radio frequency mode, the radio frequency current is conducted to the sample 34 through the injection rod 310 and the outer casing 35, and the magnetic field of the magnetic field enhancement device is regulated by the external power source.
- the electromagnetic field enhancement device can generate an oscillating magnetic field, thereby prolonging the electron movement path to increase electrons and neutrality. The collision probability of the particles increases the ionization efficiency, thereby increasing the ion signal intensity.
- the invention has simple and reasonable structure, effectively improves the signal intensity and analytical sensitivity of the instrument, is suitable for elemental analysis of inorganic materials, and is convenient to use.
- the electromagnet is preferably made of a material such as soft iron or silicon steel, and an electromagnetic induction coil (the number of turns n ⁇ 5) is wound around the iron core, and the electromagnet is placed in the outer casing 35 so as to be in close contact with the outer casing. 35.
- the lead wire of the solenoid is passed out from the two small holes on the side of the outer casing 35 to form an adjustable magnetic field reinforcing portion.
- the size of the electromagnet is: the length of the electromagnet is smaller than the inner diameter of the outer casing 35, the diameter is smaller than the height of the outer casing 35, and the number of turns of the coil: n ⁇ 5.
- the electromagnet is placed in the outer casing 35, and the electromagnet is fixed using an insulating material, and the lead 312 of the solenoid 36 is passed out through the two small holes on the side of the outer casing 35.
- Samples 34 that can be analyzed by radio frequency glow discharge mass spectrometry include: conductors, semiconductors, non-conducting materials, and the like.
- the outer casing 35 is made of a metal such as copper or an alloy such as brass.
- the outer casing 35 can be a cylinder, a cube or a rectangular parallelepiped.
- the processing size is: the outer diameter (diameter) of the outer casing 35 is less than or equal to the inner diameter of the sample introduction device, and the height is smaller than the height of the sample introduction device.
- the upper surface and the lower surface of the outer casing 35 are smooth and flat.
- the invention provides a method for using an adjustable magnetic field enhanced radio frequency glow discharge mass spectrometer signal intensity, comprising a sample introduction device comprising a sample injection rod 310 and having a sample 34 fixed thereon, and having a housing 35 and consisting of an energized solenoid and an iron core
- the device for adjusting the magnetic field reinforcing portion of the electromagnet may include the following steps;
- the sample to be tested is scanned and the signal intensity is recorded.
- the fabrication of the adjustable magnetic field enhancement portion of the present invention may include the following steps:
- a cylindrical body, a cube or a rectangular outer casing 35 is processed, and the outer casing 35 is made of a metal or an alloy.
- the metal core 311 is selected, and the enameled wire is wound around the metal core 311 to make an electromagnet.
- the metal material is processed into a cylindrical outer casing (taking brass material and cylindrical shape as an example).
- the dimensions of the copper shell are: bottom surface diameter 50 mm, height 5 mm, copper shell thickness 0.5 Mm, solenoid size: metal core diameter 4 mm, length 49 mm, wire diameter 1 mm, number of turns: 45, place the solenoid in the copper shell, and use the insulating material to fix the solenoid, the solenoid
- the leads pass through the two small holes on the side of the case.
- the signal enhancement device is placed between the sample and the injection rod, and the lead wire is passed out from the small hole of the sheet discharge battery and connected to a power source (taking a DC power source as an example) to form an adjustable magnetic field enhancement portion.
- the electromagnet device is combined with the sample and loaded into the chip sample introduction device. After the RF power source is started, the current is conducted to the sample through the injection rod and the outer casing, and the device forms a magnetic field on the side of the sample near the discharge battery.
- the invention is further illustrated by another embodiment.
- the signal intensity of a typical element detected by an RF glow discharge mass spectrometer containing an adjustable magnetic field enhancement and an adjustable magnetic field enhancement is compared.
- relative standard deviation (RSD) %) indicates that the new device analyzes the discharge stability of the non-conductor sample. The smaller the value, the better the stability.
- the original yttria (Y 2 O 3 ), Bi 12 SiO 20 (BSO) and Ba 5.52 La 0.32 Ti 2 Nb 8 O 30 (BTN) materials are processed into a circle by using an adjustable magnetic field reinforcement to analyze non-conducting materials.
- the sheet sample has a size of 20 mm in cross section and a thickness of 2 mm; it is washed with nitric acid (HNO 3 ), ultrapure water, ethanol, and dried. Subsequently, the sample was analyzed under the conditions of RF source power: 30 W, discharge gas (Ar) flow rate: 1.1 cc/min.
- the Ba in the Y and BSO of Y 2 O 3 and the Ba in the BTN were measured.
- the ion signal intensities were: 1.85 ⁇ 10 -11 A, 2.56 ⁇ 10 - 11 A, 2.12 ⁇ 10 -11 A, relative standard deviation RSD (%) are: 8.5, 9.3, 9.7.
- the rf-GD-MS without using the solenoid magnet reinforcement was used to measure Ba in Y and BSO in Y 2 O 3 , and the ion signal intensity was 9.54 ⁇ 10 -12 A, 1.65 ⁇ 10 -11 A, 1.03 ⁇ 10 -11 A , the relative standard deviation RSD (%), respectively: 10.5,11.5,12.7.
- the comparison results show that the ion signal intensity and discharge stability obtained by rf-GD-MS analysis with this solenoid magnet enhancement are significantly enhanced and improved.
- the invention provides three structural designes of enhanced RF glow discharge mass spectrometry (rf-GD-MS) signal intensity device with simple structure, low cost and stable performance, and improves the RF glow discharge mass spectrometry (rf-GD-MS) pair.
- the ion signal intensity of the material test has the advantages of simple structure, low price, stable performance, etc., and can be widely applied, and is suitable for a radio frequency glow discharge mass spectrometer or the like.
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Abstract
针对现有射频辉光放电质谱分析材料时信号强度较低的问题,提供一种增强射频辉光放电质谱信号强度的装置及方法,以增强射频辉光放电质谱仪分析无机材料信号强度。包括:具有进样杆(10)且固定有样品(4)的进样装置;具有外壳(5)与阵列状排布的磁铁(6)的阵列磁铁增强部;阵列磁铁增强部固定于进样装置中的进样杆(10)与样品(4)之间,并且紧贴样品(4)。
Description
本发明属于无机质谱分析技术领域。具体而言本发明涉及射频辉光放电质谱仪分析材料领域,更具体而言,本发明涉及运用磁铁增强射频辉光放电质谱信号强度的装置及方法。
辉光放电质谱(GD-MS)法具有固体直接进样,灵敏度高,基体效应小,一次性分析70多种元素等特点,广泛应用于高纯导体材料的痕量元素分析。近年来,射频辉光放电质谱因能直接分析导体、半导体、非导体材料而备受关注。在射频模式下,带电粒子在电场力作用下在电极之间做往返运动,以一个周期为例,在射频源的负半周期中,大量正离子向样品表面移动,样品积累大量正电荷,而在射频源的正半周期,大量电子运动到样品表面并将正电荷中和,从而实现非导体材料的持续放电。由于电子运动能力远远高于正电离子,在样品表面形成的负偏压使得正电离子能够连续轰击样品。然而在使用射频辉光放电质谱分析半导体、非导体材料时,由于材料的导热性差,严重制约了射频源功率的大小,导致测试信号偏低,进而影响分析灵敏度。
在辉光放电中,发生在阴极暗区阴极溅射和负辉区的彭宁电离是影响信号强度的两个关键因素,提高溅射和离子化效率是改善测试效果的重要思路。对此,在一些射频辉光放电仪器中,比如rf-GD-OES、rf-GD-AES等,均有相关文献报道采用外加磁铁的方式来增强信号强度。外加磁铁后,电子在洛仑兹力的作用下,被磁场束缚在样品表面运动,提高了溅射效率,样品中元素的信号强度均得到较大程度的提高。外加磁场作用下,样品中基体元素和杂质元素的信号强度均得到一定程度的提高。然而磁铁的材料、大小、磁感应强度分布是固定的,在测试过程中不能对磁场进行实时调整,在信号强度的调控方面有待提高。
本发明旨在针对现有射频辉光放电质谱分析材料时信号强度较低的问题,提供运用磁铁增强射频辉光放电质谱信号强度的装置及方法,以增强射频辉光放电质谱仪分析无机材料信号强度。
本发明第一种装置及方法:一方面提供一种运用阵列磁铁增强射频辉光放电质谱信号强度的装置,
包括:
具有进样杆且固定有样品的进样装置;
具有外壳与阵列状排布的磁铁的阵列磁铁增强部;
阵列磁铁增强部固定于进样装置中的进样杆与样品之间,并且紧贴样品。
阵列磁铁增强部改善了射频辉光放电质谱仪对材料分析的性能。本发明的结构简单合理,能有效提高仪器信号强度与分析灵敏度,适用于辉光放电质谱仪或类似装置。
较佳为,所述外壳的材质为金属或合金。
优选地,所述外壳为圆柱体、长方体或正方体,
所述外壳的外径应小于或等于所述进样装置的内径,高度小于所述进样装置的高度。
优选地,所述阵列状排布的磁铁由多块磁感线方向一致的永久磁铁组合而成。
较佳为,所述阵列状排布的磁铁紧贴所述外壳的上下表面。
优选地,所述阵列状排布的磁铁置于外壳中,每块磁铁的磁感应方向与所述样品平行。
所述样品可包括:导体、半导体、非导体材料的样品。
另一方面,提供了一种运用阵列磁铁增强射频辉光放电质谱信号强度的方法,采用包括具有进样杆且固定有样品的进样装置、和具有外壳与阵列状排布的磁铁的阵列磁铁增强部的装置,包括以下步骤;
将阵列磁铁增强部安装固定于进样装置中的进样杆与样品之间,紧贴样品;
开启射频源,电流经过进样杆、外壳传导至样品,所述装置在样品靠近放电池的一侧形成磁场;
对样品待测元素进行扫描并记录信号强度。
该方法中,将装置放于进样装置中的进样杆和样品之间,射频电源启动后,电流经过进样杆、金属壳传导至样品,阵列磁铁增强装置在样品靠近放电池的一侧形成磁场,产生震荡磁场,进而延长电子运动路径增加电子与中性粒子的碰撞几率,提高离子化效率,从而提高离子信号强度。
本发明第二种装置及方法:一方面提供一种运用环形磁铁增强射频辉光放电质谱信号强度的装置,
包括:
具有进样杆且固定有陶瓷垫片的进样装置;
具有外壳与环状磁铁的环形磁铁增强部;
所述环状磁铁放置于所述外壳中,所述环形磁铁增强部固定于所述进样装置中的所述进样杆与所述陶瓷垫片之间。
采用环形磁铁增强部改善了射频辉光放电质谱仪对材料分析的性能。该装置构造简单,用本发明的这种装置分析的无机材料样品包括:导体、半导体、非导体材料等,无需借助导体材料,无需复杂的样品前处理工作,避免污染,降低分析成本。放电时信号强度高,放电稳定,信噪比(S/N)理想,缩短分析时间,提高分析效率。
优选地,
所述外壳材质为金属或合金。
所述外壳可以为空心圆柱体、空心正方体或空心长方体。
还可以是,所述外壳为空心圆柱体时,所述环状磁铁的外径小于所述外壳的外径,内径大于所述外壳的内孔径,所述环状磁铁的高度小于所述外壳的高度。
较佳为,待测样品位于所述环状磁铁的内孔中。
由此可将待测样品包围,形成一个磁场增强部,样品嵌入环状磁铁中,射频电源启动后,电流经过进样杆、外壳传导至样品。本发明结构简单合理,有效提高仪器信号强度与分析灵敏度,适用于无机材料的元素分析,且使用方便。
所述待测样品可以包括:导体、半导体、非导体材料。
另一方面提供一种运用环形磁铁增强射频辉光放电质谱信号强度的方法,采用包括具有进样杆且固定有陶瓷垫片的进样装置、和具有外壳与环状磁铁的环形磁铁增强部的装置,包括以下步骤:
将环形磁铁增强部安装固定于进样装置中的进样杆与陶瓷垫片之间;
将样品嵌入环状磁铁的内孔中;
连接射频源,调整合适的放电气压和射频源功率进行放电;
对样品待测元素进行扫描并记录信号强度。
环状磁场增强部具有环状磁感线分布,在电场力和洛伦兹力作用下,电子绕磁感线做螺旋运动,电子的运动轨迹延长,大大增加了电子与原子的碰撞几率,相比不加磁场的情况,离子化效率提高,此外,更多电离产生的氩离子在电场作用下轰击样品表面,溅射率也随之提高。
本发明第三种装置及方法:一方面提供一种运用可调节磁场增强射频辉光放电质谱信号强度的装置,
包括:
具有进样杆且固定有样品的进样装置;
具有外壳与由通电螺线管和铁芯组成的电磁铁的可调节磁场增强部,
所述电磁铁放置于外壳中,
所述可调节磁场增强部固定于所述进样装置中的所述进样杆与所述样品之间。
用这种装置分析金属、半导体、非导体材料时无需借助导体材料,无需复杂的样品前处理工作,避免污染,降低分析成本。放电时信号强度高,放电稳定,可通过改变通电螺线管电流大小调节磁感应强度,进而调节信号强度,获得理想的信噪比
(S/N),缩短分析时间,提高分析效率。主要采用通电螺线管产生的磁场来改善射频辉光放电质谱仪对材料的分析性能,通过调节线圈电流大小来调节磁场强度,进而实现信号强度的实时调控。
优选地,所述外壳材质为金属或合金。
优选地,所述外壳为圆柱体、正方体或长方体,
所述外壳的外径小于或等于所述进样装置的内径,高度小于所述进样装置高度。
优选地,所述电磁铁的长度小于所述外壳的内径,所述电磁铁的直径小于所述外壳的高度,线圈匝数n≥5。
较佳为,使用绝缘材料将所述电磁铁固定于所述外壳中,
将所述通电螺线管的引线从所述外壳侧面的两个小孔穿出并接入电源。
所述电源可为直流电源或交流电源。
所述样品可包括导体、半导体、非导体材料的样品。
另一方面提供一种运用可调节磁场增强射频辉光放电质谱信号强度的方法,采用包括具有进样杆且固定有样品的进样装置、和具有外壳与由通电螺线管和铁芯组成的电磁铁的可调节磁场增强部的装置,包括以下步骤;
将所述可调节磁场增强部置于样品与进样杆之间,
将所述通电螺线管的引线从所述外壳侧面的小孔穿出并接入电源;
连接射频源,调整合适的放电气压和射频源功率进行放电;
对样品待测元素进行扫描并记录信号强度。
可调节磁场增强部在螺线管通电条件下,产生磁性,通电电流越大,磁性越强,在电场力和洛仑兹力作用下,电子绕磁感线做螺旋运动,电子的运动轨迹延长,大大增加了电子与原子的碰撞几率,相比不加磁场的情况,离子化效率提高,此外,更多电离产生的氩离子在电场作用下轰击样品表面,溅射率也随之提高,进而信号增强。信号强度大小与通电螺线管电流有关。
射频辉光放电质谱(rf-GD-MS)在分析非导体材料(晶体、陶瓷、粉末等)材料或者深度分析时,存在离子信号强度低、灵敏度低等关键技术问题,制约了rf-GD-MS在新材料领域的使用。发明增强射频辉光放电质谱信号强度的装置及方法,可以在辉光电离过程中调控放电气体粒子、电子(电离过程中起主导作用)的运动行为。无磁场作用下,电子的运动轨迹相对单一,离子化效率较低;而在电场力和洛伦兹力协同作用下,电子的运动路径会被有效弯曲和延长,从而增加了电子与等离子体中中性粒子的碰撞几率,提高离子化效率,进而提高rf-GD-MS分析的灵敏度。本发明的装置和方法将有效解决rf-GD-MS分析灵敏度低的关键技术问题,同时推动rf-GD-MS的发展与应用。
图1示出了本发明一实施形态的阵列磁铁增强射频辉光放电质谱信号强度装置中进样装置的剖面图。
图2示出了本发明一实施形态的阵列磁铁增强射频辉光放电质谱信号强度装置中阵列磁铁增强部的俯视图。
图3示出了本发明一实施形态的环形磁铁增强射频辉光放电质谱信号强度的装置中进样装置的剖面图。
图4示出了本发明一实施形态的环形磁铁增强射频辉光放电质谱信号强度的装置中环形磁铁增强部的俯视图。
图5示出了本发明第二实施形态的环形磁铁增强射频辉光放电质谱信号强度的装置中环形磁铁增强部的俯视图。
图6示出了本发明一实施形态的运用可调节磁场增强射频辉光放电质谱信号强度的装置中进样装置的剖面图。
图7示出了本发明一实施形态的运用可调节磁场增强射频辉光放电质谱信号强度的装置中可调节磁场增强部的俯视图。
以下结合附图和下述实施方式进一步说明本发明,应理解,附图及下述实施方式仅用于说明本发明,而非限制本发明。
本发明提供了运用磁铁增强射频辉光放电质谱信号强度装置,运用于射频辉光放电质谱仪,属于无机质谱分析技术领域,主要用于射频电源模式下分析无机材料(包括:导体、半导体及非导体材料),以解决现有质谱装置中存在的信号强度低、灵敏度低等问题。
本发明提供的第一种装置为阵列磁铁增强射频辉光放电质谱信号强度装置。
图1示出了本发明一实施形态的阵列磁铁增强射频辉光放电质谱信号强度装置中进样装置的剖面图。
如图1所示,该实施形态的阵列磁铁增强射频辉光放电质谱信号强度装置主要包括:具有进样杆10且固定有样品4的进样装置;和具有外壳5与阵列状排布的磁铁(阵列磁铁6)的阵列磁铁增强部。阵列磁铁增强部固定于进样装置中的进样杆10与样品4之间,并且紧贴样品4。
更具体而言,钽片1,陶瓷垫片2、3,样品4依次平放在外壳5的上方。钽片1,陶瓷垫片2、3的表面均平整光滑。陶瓷垫片2、3绝缘,且用于维持真空度;钽片1用于导电,其可活动地至于陶瓷垫片2、3与进样装置的顶部之间,从而易于拆卸清洗。样品4与外壳5上下表面均为光滑表面。阵列磁铁6置于外壳5内部,上下面紧贴外壳5。片状样品池7、8、9连接在一起,从外部观察样品池是一个整体。进样杆10与外壳5连接,以用于固定钽片1,陶瓷垫片2、3,样品4,外壳5。进样杆10与外壳5之间具有图未示的弹簧以将其夹紧。图2示出了本发明一实施形态的阵列磁铁增强射频辉光放电质谱信号强度装置中阵列磁铁增强部的俯视图。图2以圆柱形外壳、4×4=16阵列磁铁为例示出该阵列磁铁增强部。外壳5与至于其内部的阵列磁铁6组成了该阵列磁铁增强部。
外壳5的材料可为金属(例如铜)或合金(例如黄铜),形状可为圆柱体、长方体、正方体等,上表面与下表面光滑平整。阵列磁铁6为阵列状排布的磁铁。阵列磁铁6优选由多块磁感线方向一致的永久磁铁组合而成。
外壳5外径(直径)小于或等于图1中进样装置的内径,高度小于进样装置高度。
阵列磁铁6的磁感应方向与样品4平行,阵列磁铁6的上下面紧贴外壳5。
采用上述装置,射频辉光放电质谱可分析的样品可为无机材料样品,包括:导体、半导体、非导体材料等。
如图2所示,采用上述装置在射频辉光放电质谱分析无机材料时,将阵列磁铁增强部放于进样装置中进样杆10和样品4之间并固定夹紧。射频电源启动后,电流经过进样杆10、外壳5传导至样品4,阵列磁铁增强部在样品4靠近放电池的一侧形成磁场,与不使用磁场或使用整块磁场相比,阵列磁铁增强部可以产生震荡磁场,进而延长电子运动路径,增加电子与中性粒子的碰撞几率,提高离子化效率,从而提高离子信号强度。
本发明中的阵列磁铁6可以是由大小相同或不同、磁感线方向一致的永久磁铁块,按照磁铁磁性自行结合为阵列分布。阵列的大小为m×n(m为行,n为列,m≥2,n≥2,m和n可以相等也可以不相等)。阵列磁铁6,磁铁型号可以根据对磁场强度的需要选择不同型号(例如可以选用型号为N35,矫顽力为876kA/m,磁导率为1.05的磁铁),磁铁的总高度小于外壳的高度。
以下通过实施例1及实施例2具体说明本发明第一种装置及其有益效果。
实施例
1
在常温常压下,将金属材料加工成圆柱体外壳 (以黄铜材料、圆柱体形状为例)。铜壳内部尺寸:直径3 mm,
高度 5 mm, 铜壳厚度 0.5 mm。将16块单位尺寸5mm × 5 mm × 5 mm 的磁铁 (以N35钕铁硼磁铁为例) 按照自身磁性排列组成 (以4 × 4为例) 的点阵状磁铁结构,将该磁铁组合置于铜壳中,组成阵列状磁场信号增强装置(阵列磁铁增强部)。
使用时,将阵列阵列磁铁增强部放于进样装置中进样杆10和样品4之间,射频电源(图未示)启动后,电流经过进样杆10、外壳5传导至样品4,装置在样品4靠近放电池的一侧形成磁场。
使用完毕,取出阵列磁铁增强部,远离强电流、火源保存,同时避免敲击和剧烈振动,可重复使用。
实施例
2
下面通过另一实施例进一步说明本发明。在以下实施例,用含有阵列磁铁增强部和不含阵列磁铁增强部的射频辉光放电质谱仪检测到的典型元素的信号强度进行对比,二者差别越大,说明信号增强效果越好;用相对标准偏差 (RSD
%) 表示新装置分析非导体样品的放电稳定性,数值越小,说明稳定性越好。
以运用阵列磁铁增强部分析非导体材料为例,将原始氧化钇 (Y
2O
3)、Bi
12SiO
20 (BSO)及Ba
5.52La
0.32Ti
2Nb
8O
30
(BTN) 材料加工成圆片状试样,尺寸为:截面直径20 mm,厚度2 mm;用硝酸 (HNO
3)、超纯水、乙醇洗净,烘干。随后,在射频源功率:30W,放电气体 (Ar) 流速:1.1 cc/min的条件下对试样进行rf-GD-MS分析。利用装有本阵列磁铁增强部的rf-GD-MS对Y
2O
3中Y、BSO中Bi、BTN中Ba进行测定,离子信号强度分别为:2.28 × 10
-11
A,3.05 × 10
-11
A,2.59 × 10
-11
A,相对标准偏差RSD (%) 分别为:8.9,9.1,9.3。而未使用本阵列管磁铁增强部的rf-GD-MS对Y
2O
3中Y、BSO中Bi、BTN中Ba进行测定,离子信号强度分别为:9.54 × 10
-12
A,1.65 × 10
-11
A,1.03 × 10
-11
A,相对标准偏差RSD (%) 分别为:10.5,11.5,12.7。对比结果表明,利用装有本阵列磁铁增强部时rf-GD-MS分析获得的离子信号强度与放电稳定性有了明显的增强与提高。
本发明提供的第二种装置为环形磁铁增强射频辉光放电质谱信号强度装置。
图3示出了本发明一实施形态的环形磁铁增强射频辉光放电质谱信号强度的装置中进样装置的剖面图。
如图3所示,该实施形态的环形磁铁增强射频辉光放电质谱信号强度的装置主要包括:具有进样杆29且固定有陶瓷垫片23的进样装置;
具有外壳24A与环状磁铁24B的环形磁铁增强部24;
所述环状磁铁24B放置于所述外壳24A中,所述环形磁铁增强部固定于所述进样装置中的所述进样杆29与所述陶瓷垫片23之间。
更具体而言,钽片21,陶瓷垫片22、23依次平放在环形磁铁增强部24的上方。钽片21,陶瓷垫片22、23的表面均平整光滑。陶瓷垫片22、23绝缘,且用于维持真空度;钽片21用于导电,其可活动地至于陶瓷垫片22、23与进样装置的顶部之间,从而易于拆卸清洗。样品25嵌入环形磁铁增强部24内部。片状样品池27、28、29连接在一起,从外部观察样品池是一个整体。进样杆29与环形磁铁增强部24连接,以用于固定钽片21,陶瓷垫片22、23,环形磁铁增强部24,和样品25。图4示出了空心圆柱体形状的环形磁铁增强部的俯视图。外壳24A材质为金属(例如铜)或合金(例如黄铜)。外径(直径)小于或等于进样装置的内径,内孔直径半径大于样品的直径而小于外壳外径(直径),高度小于进样装置高度。
磁铁型号可以根据对磁场强度的需要选择不同型号(例如可以选用型号为N35,矫顽力为876kA/m,磁导率为1.05的磁铁)。磁铁的外径小于外壳的外径,内径大于外壳的内孔径,磁铁的高度小于外壳的高度。空心圆柱体情况下,充磁方向为径向充磁。空心正方体或空心长方体情况下,充磁方向与样品表面平行。
本发明中,外壳24A不仅可以为空心圆柱体,还可以为空心正方体或空心长方体。例如图5示出了空心正方体形状的环形磁铁增强部的俯视图。
使用环形磁铁增强部的辉光放电质谱仪分析材料时,将样品25嵌入环状磁铁24B的内孔中,将环状磁场增强部与样品组合后装入片状进样装置,连接射频源,调整合适的放电气压和射频源功率进行放电。
采用上述装置,射频辉光放电质谱可分析的样品可为无机材料样品,包括:导体、半导体、非导体材料等。
辉光放电质谱仪分析非导体材料信号增强装置的制作包括以下步骤:
加工环状磁铁24B,
加工空心圆柱体、空心正方体或空心长方体形状的外壳24A,外壳24A材质为金属或合金,
环状磁铁24B放置于外壳24A中,组成环形磁铁增强部。
采用上述装置增强射频辉光放电质谱信号强度的方法,包括以下步骤:
将环形磁铁增强部安装固定于进样装置中的进样杆29与陶瓷垫片之间;
将样品嵌入环状磁铁24B的内孔中;
连接射频源,调整合适的放电气压和射频源功率进行放电;
对样品待测元素进行扫描并记录信号强度。
以下通过实施例3及实施例4具体说明本发明第二种装置及其有益效果。
实施例
3
在常温常压下,将金属材料加工成空心圆柱体外壳21 (以黄铜材料、空心圆柱体形状为例),铜壳内部尺寸:外径30.5
mm,内孔半径20.5mm,高度5 mm ,厚度0.5mm的金属壳。
环状磁铁24选用钕铁硼材料,磁铁型号为N35,矫顽力为876kA/m,磁导率1.05,磁铁加工外径29 mm,内径19 mm,高度4.5 mm,充磁方向为径向充磁,组成环状磁场增强部。
使用时,将环状磁场增强部与样品组合后装入片状进样装置,射频电源启动后,电流经过进样杆、外壳传导至样品,装置在样品靠近放电池的一侧形成磁场。
使用完毕,取出磁铁增强装置,远离强电流、火源保存,同时避免敲击和剧烈振动,可重复使用。
实施例
4
下面通过另一实施例进一步说明本发明。在以下实施例,用含有磁场增强部和不含磁场增强部的射频辉光放电质谱仪检测到的典型元素的信号强度进行对比,二者差别越大,说明信号增强效果越好;用相对标准偏差 (RSD
%) 表示新装置分析非导体样品的放电稳定性,数值越小,说明稳定性越好。
将原始氧化钇 (Y
2O
3)、Bi
12SiO
20 (BSO)及Ba
5.52La
0.32Ti
2Nb
8O
30
(BTN) 材料加工成圆片状试样,尺寸为:截面直径20 mm,厚度2 mm;用硝酸 (HNO
3)、超纯水、乙醇洗净,烘干。随后,在射频源功率:30W,放电气体 (Ar) 流速:1.1 cc/min的条件下对试样进行rf-GD-MS分析。利用装有环形磁铁增强部的rf-GD-MS对Y
2O
3中Y、BSO中Bi、BTN中Ba进行测定,离子信号强度分别为:1.91 × 10
-11
A,2.55 × 10
-11
A,2.17 × 10
-11
A,相对标准偏差RSD (%) 分别为:9.8,10.3,10.7。而未使用环形磁铁增强部的rf-GD-MS对Y
2O
3中Y、BSO中Bi、BTN中Ba进行测定,离子信号强度分别为:9.54 × 10
-12
A,1.65 × 10
-11
A,1.03 × 10
-11
A,相对标准偏差RSD (%) 分别为:10.5,11.5,12.7。对比结果表明,利用装有环形磁铁增强部时rf-GD-MS分析获得的离子信号强度与放电稳定性有了明显的增强与提高。
本发明提供的第三种装置为可调节磁场增强射频辉光放电质谱信号强度装置。
图6示出了本发明一实施形态的运用可调节磁场增强射频辉光放电质谱信号强度的装置中进样装置的剖面图。
如图6所示,该实施形态的运用可调节磁场增强射频辉光放电质谱信号强度的装置主要包括:具有进样杆310且固定有样品34的进样装置;和具有外壳35与电磁铁的可调节磁场增强部。电磁铁由通电螺线管和铁芯组成。电磁铁放置于外壳35中,组成可调节磁场增强部,组合置于样品34与进样杆310之间。
更具体而言,钽片31,陶瓷垫片32、33,样品34依次平放在外壳35的上方。钽片31,陶瓷垫片32、33的表面均平整光滑。陶瓷垫片32、33绝缘,且用于维持真空度;钽片31用于导电,其可活动地至于陶瓷垫片32、33与进样装置的顶部之间,从而易于拆卸清洗。样品34与外壳35上下表面均为光滑表面。螺线管36置于外壳35内部,上下面紧贴外壳35。片状样品池37、38、39连接在一起,从外部观察样品池是一个整体。进样杆310与外壳35连接,以用于固定钽片31,陶瓷垫片32、33,样品34,外壳35和螺线管36。进样杆310与外壳35之间具有图未示的弹簧以将其夹紧。金属芯(铁芯)311置于螺线管36的中间,是螺线管磁铁装置的核心部件。引线312从样品池外外部预留的小孔穿出,用于通电。具体而言,将该可调节磁场增强部放于样品与进样杆之间并固定,将引线从进样装置的小孔穿出并通电(交流或直流),电流大小可以根据需要调节形成一个磁场增强装置。在射频模式下,射频电流经过进样杆310、外壳35传导至样品34,通过外置电源调控磁场增强装置的磁场大小,电磁场增强装置可以产生震荡磁场,进而延长电子运动路径增加电子与中性粒子的碰撞几率,提高离子化效率,从而提高离子信号强度。本发明结构简单合理,有效提高仪器信号强度与分析灵敏度,适用于无机材料的元素分析,且使用方便。
进一步,电磁铁采用软铁或硅钢等材料作为铁芯较佳,在铁芯外面卷绕电磁感应线圈(匝数n≥5),将电磁铁置于外壳35中,使其紧贴并充满外壳35,将螺线管的引线从外壳35侧面的两个小孔穿出,组成可调节磁场增强部。电磁铁的尺寸为:电磁铁长度小于外壳35的内径,直径小于外壳35的高度,线圈匝数:n≥5。电磁铁置于外壳35中,并使用绝缘材料将电磁铁固定,将螺线管36的引线312从外壳35侧面的两个小孔穿出。
射频辉光放电质谱可分析的样品34包括:导体、半导体、非导体材料等。外壳35材质为金属(例如铜)或合金(例如黄铜)。
参见图6及图7,外壳35可为圆柱体、正方体或长方体。加工尺寸为:外壳35外径(直径)小于或等于进样装置的内径,高度小于进样装置高度。外壳35上表面与下表面光滑平整较佳。
本发明提供的运用可调节磁场增强射频辉光放电质谱信号强度的方法,采用包括具有进样杆310且固定有样品34的进样装置、和具有外壳35与由通电螺线管和铁芯组成的电磁铁的可调节磁场增强部的装置,可包括以下步骤;
将所述可调节磁场增强部置于样品34与进样杆310之间,
将所述通电螺线管的引线312从所述外壳侧面的小孔穿出并接入电源;
连接射频源,调整合适的放电气压和射频源功率进行放电;
对样品待测元素进行扫描并记录信号强度。
另外,本发明可调节磁场增强部的制作可包括以下步骤:
1. 加工圆柱体、正方体或长方体的外壳35,外壳35材质为金属或合金。
2. 选取金属芯311,将漆包线卷绕在金属芯311上,制作电磁铁。
3. 将电磁铁置于外壳35中,并使用绝缘材料将其固定,将螺线管36的引线312从外壳35侧面的两个小孔穿出,小孔的孔径大小与引线312直径相适应。
4. 将该可调节磁场增强部置于样品34与进样杆310之间,使引线312从片状放电池外部预留)的小孔穿出并接入电源(直流或交流)。
以下通过实施例5及实施例6具体说明本发明第三种装置及其有益效果。
实施例
5
下面通过一实施例进一步说明本发明。在常温常压下,将金属材料加工成圆柱体外壳 (以黄铜材料、圆柱体形状为例),铜壳尺寸:底面直径50 mm,高度 5 mm, 铜壳厚度 0.5
mm,螺线管尺寸:金属芯直径4 mm,长度49 mm,导线直径1mm,匝数:45,将螺线管置于铜壳中,并使用绝缘材料将螺线管固定,将螺线管的引线从外壳侧面的两个小孔穿出。将该信号增强装置置于样品与进样杆之间,使引线从片状放电池的小孔穿出并接入电源(以采用直流电源为例),组成可调节磁场增强部。
使用时,将电磁铁装置与样品组合后装入片状进样装置,射频电源启动后,电流经过进样杆、外壳传导至样品,装置在样品靠近放电池的一侧形成磁场。
使用完毕,取出磁铁增强装置,远离强电流、火源保存,同时避免敲击和剧烈振动,可重复使用。
实施例
6
下面通过另一实施例进一步说明本发明。在以下实施例,用含有可调节磁场增强部和不含可调节磁场增强部的射频辉光放电质谱仪检测到的典型元素的信号强度进行对比,二者差别越大,说明信号增强效果越好;用相对标准偏差 (RSD
%) 表示新装置分析非导体样品的放电稳定性,数值越小,说明稳定性越好。
以运用可调节磁场增强部分析非导体材料为例,将原始氧化钇 (Y
2O
3)、Bi
12SiO
20 (BSO)及Ba
5.52La
0.32Ti
2Nb
8O
30
(BTN) 材料加工成圆片状试样,尺寸为:截面直径20 mm,厚度2
mm;用硝酸 (HNO
3)、超纯水、乙醇洗净,烘干。随后,在射频源功率:30W,放电气体 (Ar) 流速:1.1
cc/min的条件下对试样进行分析。利用装有本可调节磁场增强部的rf-GD-MS对Y
2O
3中Y、BSO中Bi、BTN中Ba进行测定,离子信号强度分别为:1.85 × 10
-11 A,2.56 × 10
-11
A,2.12 × 10
-11
A,相对标准偏差RSD (%) 分别为:8.5,9.3,9.7。而未使用本螺线管磁铁增强部的rf-GD-MS对Y
2O
3中Y、BSO中Bi、BTN中Ba进行测定,离子信号强度分别为:9.54 × 10
-12 A,1.65 × 10
-11
A,1.03 × 10
-11
A,相对标准偏差RSD (%) 分别为:10.5,11.5,12.7。对比结果表明,利用装有本螺线管磁铁增强部时rf-GD-MS分析获得的离子信号强度与放电稳定性有了明显的增强与提高。
本发明提供了三种结构简单、价格低廉、性能稳定的增强射频辉光放电质谱(rf-GD-MS) 信强度装置的结构设计,提高了射频辉光放电质谱 (rf-GD-MS) 对材料测试的离子信号强度,具有结构简单、价格低廉、性能稳定等优点,可广泛推广应用,适用于射频辉光放电质谱仪或类似装置。
Claims (9)
- 一种增强射频辉光放电质谱信号强度的装置,其特征在于,包括:具有进样杆且固定有样品的进样装置;具有外壳与阵列状排布的磁铁的阵列磁铁增强部;阵列磁铁增强部固定于进样装置中的进样杆与样品之间,并且紧贴样品。
- 根据权利要求1所述的增强射频辉光放电质谱信号强度的装置,其特征在于,所述阵列状排布的磁铁置于外壳中,每块磁铁的磁感应方向与所述样品平行。
- 一种增强射频辉光放电质谱信号强度的方法,采用包括具有进样杆且固定有样品的进样装置、和具有外壳与阵列状排布的磁铁的阵列磁铁增强部的装置,其特征在于,包括以下步骤;将阵列磁铁增强部安装固定于进样装置中的进样杆与样品之间,紧贴样品;开启射频源,电流经过进样杆、外壳传导至样品,所述装置在样品靠近放电池的一侧形成磁场;对样品待测元素进行扫描并记录信号强度。
- 一种增强射频辉光放电质谱信号强度的装置,其特征在于,包括:具有进样杆且固定有陶瓷垫片的进样装置;具有外壳与环状磁铁的环形磁铁增强部;所述环状磁铁放置于所述外壳中,所述环形磁铁增强部固定于所述进样装置中的所述进样杆与所述陶瓷垫片之间。
- 根据权利要求4所述的增强射频辉光放电质谱信号强度的装置,其特征在于,待测样品位于所述环状磁铁的内孔中。
- 一种增强射频辉光放电质谱信号强度的方法,采用包括具有进样杆且固定有陶瓷垫片的进样装置、和具有外壳与环状磁铁的环形磁铁增强部的装置,其特征在于,包括以下步骤:将环形磁铁增强部安装固定于进样装置中的进样杆与陶瓷垫片之间;将样品嵌入环状磁铁的内孔中;连接射频源,调整合适的放电气压和射频源功率进行放电;对样品待测元素进行扫描并记录信号强度。
- 一种增强射频辉光放电质谱信号强度的装置,其特征在于,包括:具有进样杆且固定有样品的进样装置;和具有外壳与由通电螺线管和铁芯组成的电磁铁的可调节磁场增强部,所述电磁铁放置于外壳中,所述可调节磁场增强部固定于所述进样装置中的所述进样杆与所述样品之间。
- 根据权利要求7所述的增强射频辉光放电质谱信号强度的装置,其特征在于,使用绝缘材料将所述电磁铁固定于所述外壳中,将所述通电螺线管的引线从所述外壳侧面的两个小孔穿出并接入电源。
- 一种增强射频辉光放电质谱信号强度的方法,采用包括具有进样杆且固定有样品的进样装置、和具有外壳与由通电螺线管和铁芯组成的电磁铁的可调节磁场增强部的装置,其特征在于,包括以下步骤;将所述可调节磁场增强部置于样品与进样杆之间,将所述通电螺线管的引线从所述样品池外部预留的小孔穿出并接入电源;连接射频源,调整合适的放电气压和射频源功率进行放电;对样品待测元素进行扫描并记录信号强度。
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