CN103560060B - A kind of zirconium carbide hot cathode material and preparation method thereof - Google Patents
A kind of zirconium carbide hot cathode material and preparation method thereof Download PDFInfo
- Publication number
- CN103560060B CN103560060B CN201310528681.4A CN201310528681A CN103560060B CN 103560060 B CN103560060 B CN 103560060B CN 201310528681 A CN201310528681 A CN 201310528681A CN 103560060 B CN103560060 B CN 103560060B
- Authority
- CN
- China
- Prior art keywords
- zirconium carbide
- preparation
- negative electrode
- cathode material
- hot cathode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
- Solid Thermionic Cathode (AREA)
- Carbon And Carbon Compounds (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of zirconium carbide hot cathode material and preparation method thereof, belongs to Doped Refractory Metal Cathode Materials technical field.The emission properties feature of pure zirconium carbide negative electrode.Preparation method includes the following aspects, uses high energy ball mill to grind zirconium carbide powder, crosses 200 eye mesh screens.Powder body is put in grinding tool, adopt discharge plasma sintering technique to be sintered.Adopt line cutting, turnery processing, metallurgical polishing method obtain the pure zirconium carbide negative electrode of required size and surface-brightening.The feature of this hot cathode material is that preparation technology is simple, and emission properties is good, and uprising dew atmospheric performance is good.
Description
Technical field
The present invention relates to a kind of pure zirconium carbide hot cathode material and preparation method thereof, belong to Doped Refractory Metal Cathode Materials technical field.
Technical background
At present, in, in high power valve use remains the W-ThO with one-hundred-year history2Negative electrode, due to W-ThO2Serious fragility after the radioactive pollution of negative electrode and carbonization, it was shown that it is not desirable hot cathode material.
There are some researches show and process in rare earth oxide-tungsten, molybdenum cathode carbonization, the emitting performance of negative electrode can be greatly improved, but this kind of method needs, in carbonaceous gas such as benzene, natural gas atmosphere, rare earth oxide-tungsten, molybdenum negative electrode are carried out carbonization treatment, complex procedures.Lanthanum carbide is directly joined by the current method having worked out employing powder metallurgy prepares novel lanthanum carbide-tungsten cathode material (patent publication No. CN102184818A) in tungsten basal body, although the heat emission of this negative electrode is functional, but lanthanum carbide is unstable, easily react with the water in air, cause that the preparation condition of lanthanum carbide Doped Tungsten negative electrode is harsh, and this negative electrode easily lost efficacy.Due to zirconium carbide stable existence in an atmosphere, so the condition preparing zirconium carbide hot cathode material is simple, and preparing zirconium carbide negative electrode stable in properties, be unlikely to deteriorate inefficacy, find through emission properties test, the emission properties of zirconium carbide negative electrode is good.
Summary of the invention
Problem to be solved by this invention is to provide a kind of new hot cathode material and this material preparation method.First grind powder body, adopt discharge plasma sintering technique to prepare the hot cathode material of relatively high emission performance subsequently.
A kind of new hot cathode material of the present invention, by the zirconium carbide application as hot cathode material.
Zirconium carbide hot cathode material provided by the present invention is analytical pure zirconium carbide (zirconium carbide purity >=99.8%, containing the free carbon of≤0.2% mass), and the feature of its preparation method includes following step:
(1) zirconium carbide coarse granule raw material is put in high energy ball mill and grind, rotating speed 300～800r/min, grinds 4～10 hours, crosses 100～300 eye mesh screens；
(2) ground zirconium carbide fine powder is put in mould, adopt the method for discharge plasma sintering to be sintered molding, die mould pressure 30～60MPa, temperature range 1300～1500 DEG C, 2～4 DEG C/s of heating rate scope, be incubated 8～15min.
(3) adopt line cutting, turnery processing, metallurgical polishing method obtain the zirconium carbide negative electrode of required size and surface-brightening.
The technique that the employing present invention prepares zirconium carbide hot cathode material is simple, and preparation condition is easy, and the cathode construction prepared is fine and close, material stable existence, and well, uprising dew atmospheric performance is good for emission properties.
Accompanying drawing explanation
Fig. 1 is the pure zirconium carbide negative electrode of preparation zero field current density curve at different temperatures in embodiment 1；
Fig. 2 is the effective work function result of calculation of the pure zirconium carbide negative electrode of preparation in the embodiment 1 that Li Chasen straight-line method records.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following example.
Embodiment 1
The thick carbonization zirconium powder of 10g is put in high energy ball mill and grind, ratio of grinding media to material 5:1, using dehydrated alcohol as process inorganic agent, solid-to-liquid ratio 5:1, rotating speed 350r/min, keep 4 hours.Zirconium carbide powder after being ground by 7g is put in grinding tool, adopts discharge plasma sintering technique sintering, and heating rate is 4 DEG C/s, and 1350 DEG C of insulation 5min, pressure limit is 40MPa～55MPa, subsequently furnace cooling.To obtain, thickness is the zirconium carbide cylindrical piece of 12.047mm, and adopting metallographic pre-grinding, line cutting, locomotive machining, metallurgical polishing method to be processed into diameter is 8.892mm, and thickness is the cylinder of 1.525mm.In unactivated situation, test its emitting performance.Zero-field emission electric current density under each temperature conditions is as shown in table 1, and the effective work function value of this negative electrode is as shown in table 2.Zero field current density value is as it is shown in figure 1, the effective work function of this negative electrode calculates as shown in Figure 2 at each temperature.
Embodiment 2
The thick carbonization zirconium powder of 10g is put in high energy ball mill and grind, ratio of grinding media to material 5:1, using dehydrated alcohol as process inorganic agent, solid-to-liquid ratio 5:1, rotating speed 500r/min, keep 4 hours.Zirconium carbide powder after being ground by 7g is put in grinding tool, adopts discharge plasma sintering technique sintering, and heating rate is 4 DEG C/s, and 1350 DEG C of insulation 5min, pressure limit is 40MPa～55MPa, subsequently furnace cooling.To obtain, thickness is the zirconium carbide cylindrical piece of 11.954mm, and adopting metallographic pre-grinding, line cutting, locomotive machining, metallurgical polishing method to be processed into diameter is 9.010mm, and thickness is the cylinder of 1.497mm.In unactivated situation, test its emitting performance.Zero-field emission electric current density under each temperature conditions is as shown in table 1, and the effective work function value of this negative electrode is as shown in table 2.
Embodiment 3
The thick carbonization zirconium powder of 10g is put in high energy ball mill and grind, ratio of grinding media to material 5:1, using dehydrated alcohol as process inorganic agent, solid-to-liquid ratio 5:1, rotating speed 800r/min, keep 8 hours.Zirconium carbide powder after being ground by 7g is put in grinding tool, adopts discharge plasma sintering technique sintering, and heating rate is 2 DEG C/s, and 1350 DEG C of insulation 10min, pressure limit is 50MPa～60MPa, subsequently furnace cooling.To obtain, thickness is the zirconium carbide cylindrical piece of 11.520mm, and adopting metallographic pre-grinding, line cutting, locomotive machining, metallurgical polishing method to be processed into diameter is 8.868mm, and thickness is the cylinder of 1.5mm.In unactivated situation, test its emitting performance.Zero-field emission electric current density under each temperature conditions is as shown in table 1, and the effective work function value of this negative electrode is as shown in table 2.
The pure zirconium carbide negative electrode of table 1 zero field current density value (A cm at different temperatures-2)
| Temperature | 1200℃ | 1250℃ | 1300℃ |
| Example 1 | 0.24 | 0.34 | 0.48 |
| Example 2 | 0.31 | 0.43 | 0.63 |
| Example 3 | 0.35 | 0.49 | 0.72 |
The effective work function value of the pure zirconium carbide negative electrode of table 2 (eV)
| Example 1 | Example 2 | Example 3 | |
| Work function (eV) | 2.823 | 2.843 | 2.886 |
Claims (1)
1. the preparation method of zirconium carbide hot cathode material, it is characterised in that zirconium carbide purity >=99.8%, containing the free carbon of≤0.2% mass；Including following step:
(1) zirconium carbide coarse granule raw material is put in high energy ball mill and grind, rotating speed 300～800r/min, grinds 4～10 hours, crosses 100～300 eye mesh screens；
(2) ground zirconium carbide fine powder is put in mould, adopt the method for discharge plasma sintering to be sintered molding, die mould pressure 30～60MPa, temperature range 1300～1500 DEG C, 2～4 DEG C/s of heating rate scope, be incubated 8～15min；
(3) adopt line cutting, turnery processing, metallurgical polishing method obtain the zirconium carbide negative electrode of required size and surface-brightening.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310528681.4A CN103560060B (en) | 2013-10-30 | 2013-10-30 | A kind of zirconium carbide hot cathode material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310528681.4A CN103560060B (en) | 2013-10-30 | 2013-10-30 | A kind of zirconium carbide hot cathode material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103560060A CN103560060A (en) | 2014-02-05 |
| CN103560060B true CN103560060B (en) | 2016-06-29 |
Family
ID=50014278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310528681.4A Active CN103560060B (en) | 2013-10-30 | 2013-10-30 | A kind of zirconium carbide hot cathode material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103560060B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0637046A1 (en) * | 1993-07-29 | 1995-02-01 | Nec Corporation | Thermoionic emissive cathode method of fabricating the same thermoionic emissive cathode and electron beam apparatus |
| CN102184818A (en) * | 2011-04-02 | 2011-09-14 | 北京工业大学 | Lanthanum-carbide-tungsten hot cathode material and preparation method thereof |
-
2013
- 2013-10-30 CN CN201310528681.4A patent/CN103560060B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0637046A1 (en) * | 1993-07-29 | 1995-02-01 | Nec Corporation | Thermoionic emissive cathode method of fabricating the same thermoionic emissive cathode and electron beam apparatus |
| CN102184818A (en) * | 2011-04-02 | 2011-09-14 | 北京工业大学 | Lanthanum-carbide-tungsten hot cathode material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| Certain refractory compounds as thermionic emitters;D.L.Goldwater等;《Journal of Applied Physics》;19510131;第22卷(第1期);第70-73页 * |
| Preparation and characterization of zirconium carbide field emitters;William A.Mackie等;《IEEE Transactions on Electron Devices》;19891130;第36卷(第11期);第2697-2702页 * |
| Single-crystal zirconium carbide as a high-temperature thermionic cathode material;William A.Mackie等;《IEEE Transactions on Electron Devices》;19890131;第36卷(第1期);第220-224页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103560060A (en) | 2014-02-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101962297B (en) | Preparation method of silicon nitride ceramics ring for polysilicon reduction furnace | |
| CN103639408B (en) | A kind of method preparing Intermatallic Ti-Al compound with titantium hydride Al alloy powder short route | |
| CN104293291B (en) | A kind of superhard abrasive compound and preparation method thereof | |
| CN102717086B (en) | Method for preparing high-niobium titanium-aluminum alloy spherical micro powder in short process | |
| CN103572087B (en) | The preparation method of boron carbide particles reinforced aluminum matrix composites | |
| CN107746983B (en) | Preparation method of hard alloy with high and uniform distribution of crystal grains | |
| CN102071346A (en) | Method for preparing compact nanocrystalline WC-Co hard alloy block material with small grain size | |
| CN104911380A (en) | Preparation method of ultrafine-grain Ti-6Al-4V alloy | |
| CN109371274A (en) | A kind of preparation method of high-performance powder metallurgy TZM molybdenum alloy | |
| CN104651652B (en) | A kind of preparation method inhaling hydrogen element | |
| CN102363289A (en) | Preparation technology of metal ceramic bonding agent diamond/ cubic boron nitride (CBN) grinding wheel | |
| CN104525956A (en) | Method for preparing hydrogenated titanium alloy powder | |
| CN103093916A (en) | Neodymium iron boron magnetic materials and preparation method of the same | |
| CN103194629A (en) | Method for preparing tungsten molybdenum copper composite material | |
| CN104131208A (en) | Aluminium oxide-titanium carbide micron composite ceramic cutter material and microwave sintering method thereof | |
| CN103310972A (en) | Method for preparing high-performance sintered Nd-Fe-B magnet | |
| CN103537688A (en) | Method for preparing Fe-Al alloy by using nano-powder | |
| CN104232961B (en) | A kind of high-strength height hard Cu-Cr composite and its preparation method and application | |
| CN107244918A (en) | A kind of TiB TiC TiB2‑B4The fast preparation method of C Al composite ceramicses | |
| CN103560060B (en) | A kind of zirconium carbide hot cathode material and preparation method thereof | |
| CN104162661B (en) | Microwave sintering method of Al2O3-TiC-TiN micron composite ceramic cutter material | |
| CN105575684A (en) | Silver based electrical contact composite material and preparation method thereof | |
| CN104402450A (en) | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature | |
| CN108034875A (en) | A kind of Mo-Si-B alloys of rare earth doped oxide and preparation method thereof | |
| CN110788318B (en) | Preparation method of high-density rare earth tungsten electrode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Jinshu Inventor after: Dong Liran Inventor after: Liu Wei Inventor after: Wang Qiang Inventor after: Li Jieming Inventor after: Zhou Meiling Inventor after: Zuo Tieyong Inventor before: Wang Jinshu Inventor before: Liu Wei Inventor before: Dong Liran Inventor before: Wang Qiang Inventor before: Li Jieming Inventor before: Zhou Meiling Inventor before: Zuo Tieyong |
|
| COR | Change of bibliographic data | ||
| GR01 | Patent grant |