CN109384457A - A kind of electrode material and preparation method thereof for mass spectrum ionization source - Google Patents
A kind of electrode material and preparation method thereof for mass spectrum ionization source Download PDFInfo
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- CN109384457A CN109384457A CN201811156384.0A CN201811156384A CN109384457A CN 109384457 A CN109384457 A CN 109384457A CN 201811156384 A CN201811156384 A CN 201811156384A CN 109384457 A CN109384457 A CN 109384457A
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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
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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
- H01J49/10—Ion sources; Ion guns
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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Abstract
The electrode material and preparation method thereof that the invention discloses a kind of for mass spectrum ionization source, the electrode material are made of the raw material of following parts by weight: 0.8~1.1 part of Dineodymium trisulfate, 0.4~0.6 part of samarium oxide, 0.3~0.7 part of gadolinium nitrate, 21~33 parts of silver oxides, 22~38 parts of cobaltous dichlorides, 56~69 parts of iron chloride.The electrode material effectively increases the ion transmission efficiency of working electrode, realizes the long-time stability of mass spectrum ionization source and mass spectrometer.Preparation method is simple and easy, is suitable for promoting.
Description
Technical field
The invention belongs to mass ions source domains, and in particular to a kind of electrode material and its preparation for mass spectrum ionization source
Method.
Background technique
Ion source (English name: Ion source) is to make neutral atom or molecular ionization, and therefrom draw ion beam current
Device.It is various types of ion accelerators, mass spectrograph, calutron, ion implantation apparatus, ion beam etching
The indispensable component of the equipment such as the neutral-beam injector in device, ion propeller and controlled fusion device.
According to different use condition and purposes, a plurality of types of ion sources are had been developed that at present.Had using wide
Arc-discharge ion source, PIG ion source and double-plasma ion source etc., these sources be all based on process gas discharge,
Often broadly it is known as arc source.Radio frequency ion source is then that ion is generated by the high-frequency discharge in gas, also there is extensive use
On the way.The appearance in novel heavy-ion source significantly improves the charge state of heavy ion, wherein more mature has electron cyclotron resonace ion
Source (ECR) and electron beam ion source (EBIS).Having for anion source better performances turns lotus type and two kinds of sputtering type.In certain condition
Under, the various ion sources based on process gas discharge can provide certain anion line.
Mass spectrum ionization source in the prior art, stability is poor, can not use for a long time, and its working electrode ion transmits
Efficiency need to be improved.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of electrode material for mass spectrum ionization source and its preparation side
Method, the electrode material effectively increase the ion transmission efficiency of working electrode, realize the length of mass spectrum ionization source and mass spectrometer
Phase stability, preparation method is simple and easy, is suitable for promoting.
The present invention is achieved by the following technical solutions:
A kind of electrode material for mass spectrum ionization source, is made of the raw material of following parts by weight: 0.8~1.1 part of Dineodymium trisulfate,
0.4~0.6 part of samarium oxide, 0.3~0.7 part of gadolinium nitrate, 21~33 parts of silver oxides, 22~38 parts of cobaltous dichlorides, 56~69 parts of chlorine
Change iron.
A kind of preparation method of the electrode material for mass spectrum ionization source, comprising the following steps:
Step 1) weighs Dineodymium trisulfate, samarium oxide, gadolinium nitrate, silver oxide, cobaltous dichloride, iron chloride as former by weight
Material；
The raw material prepared is placed in ball mill by step 2), and the protection of liquid feeding body carries out ball-milling treatment；
Step 3) takes out the powder after ball milling, is placed in dryer dry；
Powder after drying is transferred in high-temperature calcination stove by step 4), is carried out at high-temperature calcination under inert atmosphere protection
Reason；
After step 5) calcining, it is cooled to room temperature and takes out powder to get the electrode material for being used for mass spectrum ionization source described in.
Further, the step 2) ball-milling treatment is the white ball ball milling using 5~6mm of diameter, 20~40h of time.
Further, step 2) the protection liquid is ammonium hydroxide or acetone.
Further, the step 3) drying temperature is 300~450 DEG C, and the time is 30~50min.
Further, the step 4) inert atmosphere is argon gas or nitrogen.
Further, the temperature of the step 4) high-temperature calcination is 1500~1800 DEG C, and the time is 3~5h.
Beneficial effects of the present invention are as follows:
Electrode material for mass spectrum ionization source of the invention, select rear earth element nd, samarium, gadolinium, in conjunction with electric conductivity compared with
Strong silver effectively increases the ion transmission efficiency of working electrode, and the cobalt and iron of high stability is added, and realizes mass spectrum ionization
The long-time stability of source and mass spectrometer.Preparation method is simple and easy, is suitable for promoting.
Specific embodiment
Present invention is further elaborated in following combination specific embodiment.
Embodiment 1
A kind of electrode material for mass spectrum ionization source, is made of the raw material of following parts by weight: 0.8 part of Dineodymium trisulfate, 0.4 part
Samarium oxide, 0.3 part of gadolinium nitrate, 21 parts of silver oxides, 22 parts of cobaltous dichlorides, 56 parts of iron chloride.
Preparation method includes the following steps:
(1) 0.8 part of Dineodymium trisulfate, 0.4 part of samarium oxide, 0.3 part of gadolinium nitrate, 21 parts of silver oxides, 22 part two are weighed by weight
Cobalt chloride, 56 parts of iron chloride are as raw material.
(2) raw material prepared is placed in ball mill, ammonification water conservation carries out ball-milling treatment, using the white of 5~6mm of diameter
Ball ball milling, time 20h.
(3) powder after ball milling is taken out, 300 DEG C of dry 30min in dryer are placed in.
(4) powder after drying is transferred in high-temperature calcination stove, under argon atmosphere protection, at 1500 DEG C of high-temperature calcinations
Reason, time 3h.
(5) it after calcining, is cooled to room temperature and takes out powder to get the electrode material for being used for mass spectrum ionization source described in.
Embodiment 2
A kind of electrode material for mass spectrum ionization source, is made of the raw material of following parts by weight: 1.1 parts of Dineodymium trisulfates, 0.6 part
Samarium oxide, 0.7 part of gadolinium nitrate, 33 parts of silver oxides, 38 parts of cobaltous dichlorides, 69 parts of iron chloride.
Preparation method includes the following steps:
(1) 1.1 parts of Dineodymium trisulfates, 0.6 part of samarium oxide, 0.7 part of gadolinium nitrate, 33 parts of silver oxides, 38 part two are weighed by weight
Cobalt chloride, 69 parts of iron chloride are as raw material.
(2) raw material prepared is placed in ball mill, adds acetone protection to carry out ball-milling treatment, using the white of 5~6mm of diameter
Ball ball milling, time 40h.
(3) powder after ball milling is taken out, 450 DEG C of dry 50min in dryer are placed in.
(4) powder after drying is transferred in high-temperature calcination stove, under nitrogen atmosphere protection, at 1800 DEG C of high-temperature calcinations
Reason, time 5h.
(5) it after calcining, is cooled to room temperature and takes out powder to get the electrode material for being used for mass spectrum ionization source described in.
Embodiment 3
A kind of electrode material for mass spectrum ionization source, is made of the raw material of following parts by weight: 0.9 part of Dineodymium trisulfate, 0.5 part
Samarium oxide, 0.6 part of gadolinium nitrate, 28 parts of silver oxides, 34 parts of cobaltous dichlorides, 64 parts of iron chloride.
Preparation method includes the following steps:
(1) 0.9 part of Dineodymium trisulfate, 0.5 part of samarium oxide, 0.6 part of gadolinium nitrate, 28 parts of silver oxides, 34 part two are weighed by weight
Cobalt chloride, 64 parts of iron chloride are as raw material.
(2) raw material prepared is placed in ball mill, adds acetone protection to carry out ball-milling treatment, using the white of 5~6mm of diameter
Ball ball milling, time 30h.
(3) powder after ball milling is taken out, 400 DEG C of dry 40min in dryer are placed in.
(4) powder after drying is transferred in high-temperature calcination stove, under argon atmosphere protection, at 1700 DEG C of high-temperature calcinations
Reason, time 4h.
(5) it after calcining, is cooled to room temperature and takes out powder to get the electrode material for being used for mass spectrum ionization source described in.
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.
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Resistivity (Ω × cm) | 4.3×10-4 | 4.5×10-4 | 5.1×10-4 |
| Conductivity (S/cm) | 2.3×10-2 | 2.7×10-2 | 2.5×10-2 |
Claims (7)
1. a kind of electrode material for mass spectrum ionization source, which is characterized in that be made of the raw material of following parts by weight: 0.8~1.1
Part Dineodymium trisulfate, 0.4~0.6 part of samarium oxide, 0.3~0.7 part of gadolinium nitrate, 21~33 parts of silver oxides, 22~38 parts of cobaltous dichlorides, 56
~69 parts of iron chloride.
2. a kind of preparation method of electrode material for mass spectrum ionization source described in claim 1, which is characterized in that including with
Lower step:
Step 1) weighs Dineodymium trisulfate, samarium oxide, gadolinium nitrate, silver oxide, cobaltous dichloride, iron chloride as raw material by weight；
The raw material prepared is placed in ball mill by step 2), and the protection of liquid feeding body carries out ball-milling treatment；
Step 3) takes out the powder after ball milling, is placed in dryer dry；
Powder after drying is transferred in high-temperature calcination stove by step 4), and high-temperature calcination processing is carried out under inert atmosphere protection；
After step 5) calcining, it is cooled to room temperature and takes out powder to get the electrode material for being used for mass spectrum ionization source described in.
3. a kind of preparation method of electrode material for mass spectrum ionization source according to claim 2, which is characterized in that step
Rapid 2) the described ball-milling treatment is the white ball ball milling using 5~6mm of diameter, 20~40h of time.
4. a kind of preparation method of electrode material for mass spectrum ionization source according to claim 2, which is characterized in that step
Rapid 2) the described protection liquid is ammonium hydroxide or acetone.
5. a kind of preparation method of electrode material for mass spectrum ionization source according to claim 2, which is characterized in that step
Rapid 3) the described drying temperature is 300~450 DEG C, and the time is 30~50min.
6. a kind of preparation method of electrode material for mass spectrum ionization source according to claim 2, which is characterized in that step
Rapid 4) the described inert atmosphere is argon gas or nitrogen.
7. a kind of preparation method of electrode material for mass spectrum ionization source according to claim 2, which is characterized in that step
The temperature of rapid 4) the described high-temperature calcination is 1500~1800 DEG C, and the time is 3~5h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102931388A (en) * | 2012-11-23 | 2013-02-13 | 惠州亿纬锂能股份有限公司 | Rare earth oxide clad lithium titanate anode material, preparation method thereof and lithium ion battery |
| CN103214038A (en) * | 2013-04-08 | 2013-07-24 | 严百坤 | Preparation method for carbon-coated ferroferric oxide-cobaltosic oxide composite negative electrode material |
| CN104821236A (en) * | 2015-04-03 | 2015-08-05 | 安徽江威精密制造有限公司 | Electrode material improving battery capacity of supercapacitor and preparation method thereof |
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- 2018-09-30 CN CN201811156384.0A patent/CN109384457A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102931388A (en) * | 2012-11-23 | 2013-02-13 | 惠州亿纬锂能股份有限公司 | Rare earth oxide clad lithium titanate anode material, preparation method thereof and lithium ion battery |
| CN103214038A (en) * | 2013-04-08 | 2013-07-24 | 严百坤 | Preparation method for carbon-coated ferroferric oxide-cobaltosic oxide composite negative electrode material |
| CN104821236A (en) * | 2015-04-03 | 2015-08-05 | 安徽江威精密制造有限公司 | Electrode material improving battery capacity of supercapacitor and preparation method thereof |
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