CN109336563A - A kind of working electrode material of mass ion source and preparation method thereof - Google Patents
A kind of working electrode material of mass ion source and preparation method thereof Download PDFInfo
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- CN109336563A CN109336563A CN201811157252.XA CN201811157252A CN109336563A CN 109336563 A CN109336563 A CN 109336563A CN 201811157252 A CN201811157252 A CN 201811157252A CN 109336563 A CN109336563 A CN 109336563A
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- 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
- C04B35/10—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 aluminium oxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
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- H—ELECTRICITY
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- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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- 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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Abstract
The invention discloses working electrode material of a kind of mass ion source and preparation method thereof, the material is made of following raw material by weight: 29~41 parts of graphenes, 15~20 parts of lithium nitrates, 15~20 parts of manganese acetates, 44~50 parts of aluminium oxide, 0.8~1.2 part of holmium fluoride, 1.5~3.5 parts of coupling agents.The working electrode material effectively increases the electric conductivity of the working electrode of mass ion source, realizes the compound of inorganic conductive material and organic matter, after forming chemical bond, will promote electron-transport, to improve the ion transmission efficiency of working electrode.It prepares low raw-material cost, is suitable for promoting.
Description
Technical field
The invention belongs to mass ions source domains, and in particular to a kind of working electrode material and its preparation of mass ion source
Method.
Background technique
Mass spectrography is one of analysis method that is known most sensitive and having wide range of applications, and the instrument that this method uses is known as
Mass spectrograph.Mass spectrograph is using ion source, mass analyzer and ion detector as core.Ion source is to make sample molecule in high vacuum
Under the conditions of the device that ionizes.Molecule after ionization can further be fragmented into a variety of of smaller quality because receiving excessive energy
Fragment ion and neutral particle.They obtain the mean kinetic energy with identical energy under accelerating field effect and enter quality point
Parser.Mass analyzer is the ion by while into different quality therein, by the device of mass-to-charge ratio m/e size separation.Point
Ion from after sequentially enters ion detector, and acquisition amplification ion signal handles through computer, is depicted as mass spectrogram.Ion
Source, mass analyzer and ion detector are all each, and there are many types.Mass spectrograph is divided into isotope mass spectrometer, inorganic by application range
Mass spectrograph and organic mass spectrometer；It is divided into high-resolution, middle resolution and Low Resolution Mass Spectra instrument by resolving power；It is divided by working principle quiet
State instrument and dynamic instrument.Mass ion source in the prior art, the higher cost of working electrode, and electrode material at low cost
Expect that its electric conductivity causes anxiety.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides working electrode material and its preparation side of a kind of mass ion source
Method, the material effectively increase the electric conductivity of working electrode, realize compound, the formationization of inorganic conductive material and organic matter
After learning key, electron-transport will be promoted, to improve the ion transmission efficiency of working electrode.And low raw-material cost, suitable for pushing away
Extensively.
The present invention is achieved by the following technical solutions:
A kind of working electrode material of mass ion source, is made of following raw material by weight: 29~41 parts of graphenes, 15
~20 parts of lithium nitrates, 15~20 parts of manganese acetates, 44~50 parts of aluminium oxide, 0.8~1.2 part of holmium fluoride, 1.5~3.5 parts of coupling agents.
Preferably, the coupling agent is titanate coupling agent TMC-101 or TMC-102.
A kind of preparation method of the working electrode material of mass ion source, comprising the following steps:
Step 1) weighs graphene, lithium nitrate, manganese acetate, aluminium oxide, holmium fluoride as raw material by weight；
Raw material is placed in high-speed mixer by step 2), and the pure and mild coupling agent of benzene of 10 times of raw material weight meters, high-speed stirring is added
It mixes uniformly mixed；
Mixed liquor after stirring is placed in reaction kettle by step 3), heating stirring, is discharged, and precipitating is washed, is placed in by filtering
Drying and processing is carried out in dryer；
Precipitating after drying is placed in high-temperature calcination machine and calcines by step 4)；
It is cooled to room temperature and is taken out to get the working electrode material of the mass ion source is arrived after step 5) calcining.
Further, the speed of the step 2) high-speed stirred is 2000~2500r/min, and the time is 5~8h.
Further, the temperature of the step 3) heating stirring is 70~100 DEG C, and the time is 15~30min.
Further, the temperature of the step 3) drying and processing is 200~350 DEG C, and the time is 1~2h.
Further, the temperature of the step 4) calcining is 1100~1300 DEG C, and the time is 2~4h.
Beneficial effects of the present invention are as follows:
The working electrode material of mass ion source of the invention, it is low in cost using graphene as main conductive material,
A small amount of Rare-earth Element Holmium is added, the electric conductivity of working electrode is effectively increased, using titanate coupling agent, by lithium nitrate, vinegar
This kind of inorganic material of sour manganese, aluminium oxide and graphene are closely mixed, and compound, the formation of inorganic conductive material and organic matter is realized
After chemical bond, electron-transport will be promoted, to improve the ion transmission efficiency of working electrode.
Specific embodiment
Present invention is further elaborated in following combination specific embodiment.
Embodiment 1
A kind of working electrode material of mass ion source, is made of following raw material by weight: 29 parts of graphenes, 15 parts of nitre
Sour lithium, 15 parts of manganese acetates, 44 parts of aluminium oxide, 0.8 part of holmium fluoride, 1.5 parts of titanate coupling agent TMC-101.
Preparation method includes the following steps:
(1) 29 parts of graphenes, 15 parts of lithium nitrates, 15 parts of manganese acetates, 44 parts of aluminium oxide, 0.8 part of fluorination are weighed by weight
Holmium is as raw material.
(2) raw material is placed in high-speed mixer, the pure and mild 1.5 parts of titanate coupling agents of benzene of 10 times of raw material weight meters is added
TMC-101,2000r/min high-speed stirred 5h are uniformly mixed.
(3) mixed liquor after stirring is placed in reaction kettle, 70 DEG C of heating stirring 15min, is discharged, filtering will precipitate water
It washes, is placed in dryer and carries out drying and processing, drying temperature is 200 DEG C, time 1h.
(4) precipitating after drying is placed in high-temperature calcination machine, 1100 DEG C of calcining 2h.
(5) it is cooled to room temperature and is taken out to get the working electrode material of the mass ion source is arrived after calcining.
Embodiment 2
A kind of working electrode material of mass ion source, is made of following raw material by weight: 41 parts of graphenes, 20 parts of nitre
Sour lithium, 20 parts of manganese acetates, 50 parts of aluminium oxide, 1.2 parts of holmium fluorides, 3.5 parts of titanate coupling agent TMC-102.
Preparation method includes the following steps:
(1) 41 parts of graphenes, 20 parts of lithium nitrates, 20 parts of manganese acetates, 50 parts of aluminium oxide, 1.2 parts of fluorinations are weighed by weight
Holmium is as raw material.
(2) raw material is placed in high-speed mixer, the pure and mild 3.5 parts of titanate coupling agents of benzene of 10 times of raw material weight meters is added
TMC-102,2500r/min high-speed stirred 8h are uniformly mixed.
(3) mixed liquor after stirring is placed in reaction kettle, 100 DEG C of heating stirring 30min, is discharged, filtering will precipitate water
It washes, is placed in dryer and carries out drying and processing, drying temperature is 350 DEG C, time 2h.
(4) precipitating after drying is placed in high-temperature calcination machine, 1300 DEG C of calcining 4h.
(5) it is cooled to room temperature and is taken out to get the working electrode material of the mass ion source is arrived after calcining.
Embodiment 3
A kind of working electrode material of mass ion source, is made of following raw material by weight: 35 parts of graphenes, 18 parts of nitre
Sour lithium, 18 parts of manganese acetates, 46 parts of aluminium oxide, 1.0 parts of holmium fluorides, 2.5 parts of titanate coupling agent TMC-101.
Preparation method includes the following steps:
(1) 35 parts of graphenes, 18 parts of lithium nitrates, 18 parts of manganese acetates, 46 parts of aluminium oxide, 1.0 parts of fluorinations are weighed by weight
Holmium is as raw material.
(2) raw material is placed in high-speed mixer, the pure and mild 2.5 parts of titanate coupling agents of benzene of 10 times of raw material weight meters is added
TMC-101,2400r/min high-speed stirred 6h are uniformly mixed.
(3) mixed liquor after stirring is placed in reaction kettle, 80 DEG C of heating stirring 20min, is discharged, filtering will precipitate water
It washes, is placed in dryer and carries out drying and processing, drying temperature is 300 DEG C, time 1.5h.
(4) precipitating after drying is placed in high-temperature calcination machine, 1200 DEG C of calcining 3h.
(5) it is cooled to room temperature and is taken out to get the working electrode material of the mass ion source is arrived after calcining.
Test case 1
Conducting performance test, test result is as follows table 1 are carried out to working electrode material made from Examples 1 to 3.
1 the performance test results of table
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Resistivity (Ω × cm) | 0.8×10-5 | 0.6×10-5 | 0.7×10-5 |
| Conductivity (S/cm) | 1.4×10-2 | 1.8×10-2 | 1.6×10-2 |
Claims (7)
1. a kind of working electrode material of mass ion source, which is characterized in that be made of following raw material by weight: 29~41 parts
Graphene, 15~20 parts of lithium nitrates, 15~20 parts of manganese acetates, 44~50 parts of aluminium oxide, 0.8~1.2 part of holmium fluoride, 1.5~3.5
Part coupling agent.
2. a kind of working electrode material of mass ion source according to claim 1, which is characterized in that the coupling agent is
Titanate coupling agent TMC-101 or TMC-102.
3. a kind of preparation method of the working electrode material of mass ion source described in claim 1, which is characterized in that including with
Lower step:
Step 1) weighs graphene, lithium nitrate, manganese acetate, aluminium oxide, holmium fluoride as raw material by weight；
Raw material is placed in high-speed mixer by step 2), and the pure and mild coupling agent of benzene of 10 times of raw material weight meters is added, and high-speed stirred is mixed
It closes uniform；
Mixed liquor after stirring is placed in reaction kettle by step 3), heating stirring, is discharged, and precipitating is washed, is placed in drying by filtering
Drying and processing is carried out in machine；
Precipitating after drying is placed in high-temperature calcination machine and calcines by step 4)；
It is cooled to room temperature and is taken out to get the working electrode material of the mass ion source is arrived after step 5) calcining.
4. a kind of preparation method of the working electrode material of mass ion source according to claim 3, which is characterized in that step
The speed of rapid 2) the described high-speed stirred is 2000~2500r/min, and the time is 5~8h.
5. a kind of preparation method of the working electrode material of mass ion source according to claim 3, which is characterized in that step
The temperature of rapid 3) the described heating stirring is 70~100 DEG C, and the time is 15~30min.
6. a kind of preparation method of the working electrode material of mass ion source according to claim 3, which is characterized in that step
The temperature of rapid 3) the described drying and processing is 200~350 DEG C, and the time is 1~2h.
7. a kind of preparation method of the working electrode material of mass ion source according to claim 3, which is characterized in that step
The temperature of rapid 4) the described calcining is 1100~1300 DEG C, and the time is 2~4h.
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| CN201811157252.XA CN109336563A (en) | 2018-09-30 | 2018-09-30 | A kind of working electrode material of mass ion source and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112111145A (en) * | 2020-08-21 | 2020-12-22 | 东莞市雄林新材料科技股份有限公司 | Conductive TPU film and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101335345A (en) * | 2007-06-25 | 2008-12-31 | 索尼株式会社 | Cathode active material, method of producing the same and nonaqueous electrolyte secondary battery |
| CN106549146A (en) * | 2016-10-21 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of method that In-situ reaction prepares graphene-based lithium-rich manganic acid lithium electrode material |
| CN107834022A (en) * | 2017-11-29 | 2018-03-23 | 饶新元 | A kind of graphenic surface activation micro-porous electrode and preparation method thereof |
-
2018
- 2018-09-30 CN CN201811157252.XA patent/CN109336563A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101335345A (en) * | 2007-06-25 | 2008-12-31 | 索尼株式会社 | Cathode active material, method of producing the same and nonaqueous electrolyte secondary battery |
| CN106549146A (en) * | 2016-10-21 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of method that In-situ reaction prepares graphene-based lithium-rich manganic acid lithium electrode material |
| CN107834022A (en) * | 2017-11-29 | 2018-03-23 | 饶新元 | A kind of graphenic surface activation micro-porous electrode and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112111145A (en) * | 2020-08-21 | 2020-12-22 | 东莞市雄林新材料科技股份有限公司 | Conductive TPU film and preparation method thereof |
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