CN109369171A - A kind of mass spectrum ionization source electrode material and preparation method thereof - Google Patents

A kind of mass spectrum ionization source electrode material and preparation method thereof Download PDF

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Publication number
CN109369171A
CN109369171A CN201811156226.5A CN201811156226A CN109369171A CN 109369171 A CN109369171 A CN 109369171A CN 201811156226 A CN201811156226 A CN 201811156226A CN 109369171 A CN109369171 A CN 109369171A
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source electrode
mass spectrum
ionization source
electrode material
preparation
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王姜
蒋红
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Zhenjiang Huai Ruian Material Science & Technology Co Ltd
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Zhenjiang Huai Ruian Material Science & Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/45—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides
    • C04B35/4504—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides containing rare earth oxides
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3289—Noble metal oxides
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/442—Carbonates
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/447—Phosphates or phosphites, e.g. orthophosphate, hypophosphite
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
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Abstract

The invention discloses a kind of mass spectrum ionization source electrode materials and preparation method thereof, and the electrode material is made of the raw material of following parts by weight: 0.5~0.8 part of lanthanum carbonate, 0.3~0.6 part of yttrium phosphate, 0.4~0.7 part of praseodymium iodide, 3~5 parts of platinum dioxides, 88~94 parts of copper oxide.The mass spectrum ionization source electrode material effectively increases the detection sensitivity of the efficiency of transmission of ion and mass spectrometer on ion transmission electrode in conjunction with noble metal platinum using rare earth element.Preparation method is simple and easy, heavy metal free pollution.

Description

A kind of mass spectrum ionization source electrode material and preparation method thereof
Technical field
The invention belongs to mass ions source domains, and in particular to a kind of mass spectrum ionization source electrode material and its preparation side Method.
Background technique
Mass spectrography (Mass Spectrometry, MS) i.e. with electric and magnetic fields by the ion of movement (electrically charged atom, Molecule or molecular fragment have molecular ion, isotope ion, fragment ion, rearrangement ion, multiple-charged ion, metastable ion, bear The ion that ion and heteroion interaction generate) by the method that is detected after their mass-to-charge ratio separation.Measure from Sub- exact mass is the compound composition that can determine ion.This is because the exact mass of nucleic is a multidigit decimal, it will never Quality there are two nucleic is the same, and the quality for never having a kind of nucleic is precisely the integer of another nucildic mass Times.Analyzing these ions can get the molecular weight of compound, chemical structure, cracks rule and be decomposed to form by unimolecule certain The information such as certain correlation existing for interionic.
Mass spectrometer be it is a kind of using stablize or variation electric/magnetic field by by ionization after gas phase sample to be tested from Son, the analysis instrument for being separated and being detected according to the difference of mass-to-charge ratio are believed by the mass-to-charge ratio and signal strength of sample to be tested Breath realizes qualitative and quantitative analysis.Mass spectrometer in the prior art, the ion transmission efficiency of ion transmission electrode is mostly not People's will to the greatest extent.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of mass spectrum ionization source electrode material and preparation method thereof, should Electrode material effectively increases the detection sensitivity of the efficiency of transmission of ion and mass spectrometer on ion transmission electrode.
The present invention is achieved by the following technical solutions:
A kind of mass spectrum ionization source electrode material, is made of the raw material of following parts by weight: 0.5~0.8 part of lanthanum carbonate, 0.3 ~0.6 part of yttrium phosphate, 0.4~0.7 part of praseodymium iodide, 3~5 parts of platinum dioxides, 88~94 parts of copper oxide.
A kind of preparation method of mass spectrum ionization source electrode material, comprising the following steps:
Step 1) weighs the pure lanthanum carbonate of chemistry, yttrium phosphate, praseodymium iodide, platinum dioxide, copper oxide as former by weight Material；
The raw material prepared be transferred in ball mill after tentatively mixing by step 2) carries out ball milling；
After step 3) ball milling, powder is taken out, is placed in dryer dry；
Alloy powder after drying is placed in high-temperature calcination machine and calcines by step 4)；
It is cooled to room temperature after step 5) calcining and takes out powder to get to the mass spectrum ionization source electrode material.
Further, the step 2) mechanical milling process is as follows: under nitrogen protection, raw material being first placed in horizontal ball mill In, it with the white ball ball milling of 12~15mm of diameter, is then transferred in ceramic ball mill, with the ceramics of 1.2~1.5mm of diameter Ball ball milling.
Further, the temperature of the step 3) drying is 300~400 DEG C, and the time is 30~40min.
Further, the step 4) calcination process is as follows: starvation, 1400~1500 DEG C of 2~4h of high-temperature calcination.
Beneficial effects of the present invention are as follows:
Mass spectrum ionization source electrode material of the invention effectively increases ion in conjunction with noble metal platinum using rare earth element The detection sensitivity of the efficiency of transmission of ion and mass spectrometer on transmission electrode.Preparation method is simple and easy, and heavy metal free is dirty Dye.
Specific embodiment
Present invention is further elaborated in following combination specific embodiment.
Embodiment 1
A kind of mass spectrum ionization source electrode material, is made of the raw material of following parts by weight: 0.5 part of lanthanum carbonate, 0.3 part of phosphoric acid Yttrium, 0.4 part of praseodymium iodide, 3 parts of platinum dioxides, 88 parts of copper oxide.
Preparation method includes the following steps:
(1) 0.5 part of pure lanthanum carbonate of chemistry, 0.3 part of yttrium phosphate, 0.4 part of praseodymium iodide, 3 parts of platinum dioxides, 88 parts of oxygen are weighed Change copper as raw material.
(2) raw material prepared is carried out after tentatively mixing, first raw material is placed in horizontal ball mill, under nitrogen protection, It with the white ball ball milling of 12~15mm of diameter, is then transferred in ceramic ball mill, continues under the protection of nitrogen, use diameter The Ceramic Balls ball milling of 1.2~1.5mm.
(3) after ball milling, powder is taken out, 300 DEG C of dry 30min in dryer are placed in.
(4) alloy powder after drying is placed in high-temperature calcination machine, starvation, 1400 DEG C of high-temperature calcination 2h.
(5) it is cooled to room temperature after calcining and takes out powder to get to the mass spectrum ionization source electrode material.
Embodiment 2
A kind of mass spectrum ionization source electrode material, is made of the raw material of following parts by weight: 0.8 part of lanthanum carbonate, 0.6 part of phosphoric acid Yttrium, 0.7 part of praseodymium iodide, 5 parts of platinum dioxides, 94 parts of copper oxide.
Preparation method includes the following steps:
(1) 0.8 part of pure lanthanum carbonate of chemistry, 0.6 part of yttrium phosphate, 0.7 part of praseodymium iodide, 5 parts of platinum dioxides, 94 parts of oxygen are weighed Change copper as raw material.
(2) raw material prepared is carried out after tentatively mixing, first raw material is placed in horizontal ball mill, under nitrogen protection, It with the white ball ball milling of 12~15mm of diameter, is then transferred in ceramic ball mill, continues under the protection of nitrogen, use diameter The Ceramic Balls ball milling of 1.2~1.5mm.
(3) after ball milling, powder is taken out, 400 DEG C of dry 40min in dryer are placed in.
(4) alloy powder after drying is placed in high-temperature calcination machine, starvation, 1500 DEG C of high-temperature calcination 4h.
(5) it is cooled to room temperature after calcining and takes out powder to get to the mass spectrum ionization source electrode material.
Embodiment 3
A kind of mass spectrum ionization source electrode material, is made of the raw material of following parts by weight: 0.6 part of lanthanum carbonate, 0.4 part of phosphoric acid Yttrium, 0.5 part of praseodymium iodide, 4 parts of platinum dioxides, 91 parts of copper oxide.
Preparation method includes the following steps:
(1) 0.6 part of pure lanthanum carbonate of chemistry, 0.4 part of yttrium phosphate, 0.5 part of praseodymium iodide, 4 parts of platinum dioxides, 91 parts of oxygen are weighed Change copper as raw material.
(2) raw material prepared is carried out after tentatively mixing, first raw material is placed in horizontal ball mill, under nitrogen protection, It with the white ball ball milling of 12~15mm of diameter, is then transferred in ceramic ball mill, continues under the protection of nitrogen, use diameter The Ceramic Balls ball milling of 1.2~1.5mm.
(3) after ball milling, powder is taken out, 350 DEG C of dry 35min in dryer are placed in.
(4) alloy powder after drying is placed in high-temperature calcination machine, starvation, 1450 DEG C of high-temperature calcination 3h.
(5) it is cooled to room temperature after calcining and takes out powder to get to the mass spectrum ionization source electrode material.
Test case 1
Conducting performance test is carried out to electrode material made from Examples 1 to 3, test result is as follows shown in table 1.
1 the performance test results of table
Test item Embodiment 1 Embodiment 2 Embodiment 3
Resistivity (Ω × cm) 1.6×10-5 1.4×10-5 1.5×10-5
Conductivity (S/cm) 0.08 0.07 0.06

Claims (5)

1. a kind of mass spectrum ionization source electrode material, which is characterized in that be made of the raw material of following parts by weight: 0.5~0.8 part of carbon Sour lanthanum, 0.3~0.6 part of yttrium phosphate, 0.4~0.7 part of praseodymium iodide, 3~5 parts of platinum dioxides, 88~94 parts of copper oxide.
2. a kind of preparation method of mass spectrum ionization source electrode material described in claim 1, which is characterized in that including following step It is rapid:
Step 1) weighs the pure lanthanum carbonate of chemistry, yttrium phosphate, praseodymium iodide, platinum dioxide, copper oxide as raw material by weight；
The raw material prepared be transferred in ball mill after tentatively mixing by step 2) carries out ball milling；
After step 3) ball milling, powder is taken out, is placed in dryer dry；
Alloy powder after drying is placed in high-temperature calcination machine and calcines by step 4)；
It is cooled to room temperature after step 5) calcining and takes out powder to get to the mass spectrum ionization source electrode material.
3. a kind of preparation method of mass spectrum ionization source electrode material according to claim 2, which is characterized in that step 2) The mechanical milling process is as follows: under nitrogen protection, first raw material being placed in horizontal ball mill, with the white ball ball of 12~15mm of diameter Mill, is then transferred in ceramic ball mill, with the Ceramic Balls ball milling of 1.2~1.5mm of diameter.
4. a kind of preparation method of mass spectrum ionization source electrode material according to claim 2, which is characterized in that step 3) The temperature of the drying is 300~400 DEG C, and the time is 30~40min.
5. a kind of preparation method of mass spectrum ionization source electrode material according to claim 2, which is characterized in that step 4) The calcination process is as follows: starvation, 1400~1500 DEG C of 2~4h of high-temperature calcination.
CN201811156226.5A 2018-09-30 2018-09-30 A kind of mass spectrum ionization source electrode material and preparation method thereof Pending CN109369171A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2979515B2 (en) * 1990-01-22 1999-11-15 工業技術院長 Copper oxide conductive ceramics and method for producing the same
CN1730690A (en) * 2005-08-08 2006-02-08 河南科技大学 Rare earth copper alloy and its preparation method
CN105369051A (en) * 2015-11-09 2016-03-02 昆明贵金属研究所 Novel copper alloy and preparation method thereof
CN106587134A (en) * 2016-12-21 2017-04-26 上海第二工业大学 Preparation method of noble metal doped flower-like CuO nano material and method for preparing gas-sensitive element from same
CN106834791A (en) * 2017-01-16 2017-06-13 江西理工大学 A kind of rare earth oxide particles strengthen the preparation method of high-conductivity copper alloy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2979515B2 (en) * 1990-01-22 1999-11-15 工業技術院長 Copper oxide conductive ceramics and method for producing the same
CN1730690A (en) * 2005-08-08 2006-02-08 河南科技大学 Rare earth copper alloy and its preparation method
CN105369051A (en) * 2015-11-09 2016-03-02 昆明贵金属研究所 Novel copper alloy and preparation method thereof
CN106587134A (en) * 2016-12-21 2017-04-26 上海第二工业大学 Preparation method of noble metal doped flower-like CuO nano material and method for preparing gas-sensitive element from same
CN106834791A (en) * 2017-01-16 2017-06-13 江西理工大学 A kind of rare earth oxide particles strengthen the preparation method of high-conductivity copper alloy

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
李诚芳等，: "锂/氧化铜电池性能改善的研究：CuO的热处理对阴极性能的影响", 《应用科学学报》 *
黎文献主编: "《有色金属材料工程概论》", 30 June 2007, 冶金工业出版社 *

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