CN114340124B - Sodium ion emitter and preparation method thereof - Google Patents
Sodium ion emitter and preparation method thereof Download PDFInfo
- Publication number
- CN114340124B CN114340124B CN202111668067.9A CN202111668067A CN114340124B CN 114340124 B CN114340124 B CN 114340124B CN 202111668067 A CN202111668067 A CN 202111668067A CN 114340124 B CN114340124 B CN 114340124B
- Authority
- CN
- China
- Prior art keywords
- tungsten
- powder
- sodium
- porous
- sodium aluminosilicate
- 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
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 38
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 132
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 100
- 239000010937 tungsten Substances 0.000 claims abstract description 100
- 229910000503 Na-aluminosilicate Inorganic materials 0.000 claims abstract description 54
- 235000012217 sodium aluminium silicate Nutrition 0.000 claims abstract description 54
- 239000000429 sodium aluminium silicate Substances 0.000 claims abstract description 54
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000758 substrate Substances 0.000 claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 51
- 238000010438 heat treatment Methods 0.000 claims description 38
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012466 permeate Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 230000035515 penetration Effects 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 11
- 238000005336 cracking Methods 0.000 description 6
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 239000011268 mixed slurry Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 150000002431 hydrogen Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000006138 lithiation reaction Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Abstract
The invention provides a sodium ion emitter and a preparation method thereof, which have compact structures and greatly increase the thickness of a sodium aluminosilicate coating and the adhesion strength of the whole structure. The sodium ion emitter adopts tungsten as a framework, a porous structure formed by sintering a 1:1 mixture of tungsten powder with the diameter of 10 microns and tungsten powder with the diameter of 100 microns is used as a substrate, the bonding force of two materials is greatly increased by a chamfer structure of the framework, and falling off can not occur under the action of high temperature and electrostatic force. The porous tungsten with the porosity of 25% is sintered together with the surface-attached emitting material along with the penetration of the emitting slurry, so that the adhesion strength of the emitting material and the whole structure is further enhanced, and the coating is ensured not to be peeled off under the action of electrostatic force under the action of high voltage. The enhancement of the adhesive force of the emission coating can greatly increase the thickness of the coating, further increase the emission capability and the service life of a sodium ion source, and the sodium ion emitter is more than 10 times of the service life of the original lithium ion source, and the beam current density is more than 2 times of the lithium ion source.
Description
Technical Field
The invention relates to a sodium ion emitter for generating alkali metal plasma, processing materials and an ion accelerator, in particular to a sodium ion emitter and a preparation method thereof.
Background
Sodium ions at high ion temperatures are important tools for plasma generation and studying ion interactions with the plasma. Obtaining boundary plasma density and potential distribution without interference is an important physical quantity essential for researching plasma. The international use of high-energy sodium neutral beams to measure plasma electron density and potential distribution at a non-interfering site is becoming a hotspot. The lithium ion source used at present is limited by the problems of poor spatial resolution, short service life, cracking of the emission material caused by negative thermal expansion coefficient of the coating material, stripping of the emission material from the porous tungsten substrate and the like. To solve these problems, it is often achieved by reducing the coating thickness and reducing the current emission capability. Thinner emission coating results in poor ion emission capability of the ion source, short service life, frequent maintenance, and greatly increased system operation cost. The weaker current emission capability results in a system with poor signal to noise ratio and is more difficult to operate effectively under lithiated wall processing conditions.
Therefore, to solve the above problems, substitution of the lithium ion beam with the sodium ion beam is one of the most effective solutions. The service life of the sodium ion emitter manufactured by the method is more than 10 times that of the original lithium ion emitter, cracking and stripping phenomena caused by thermal shrinkage of the emitting material are avoided, the yield of the alkali metal emitter is improved by more than three times, the sodium ion emitter can be effectively used under the condition of wall treatment of a Tokat Ma Keli, the signal to noise ratio is improved by more than 50 times, and the boundary plasma information can be accurately measured.
Disclosure of Invention
The invention aims to provide a sodium ion emitter and a preparation method thereof. The method is a large-area sodium ion emitter preparation method suitable for alkali metal plasma generation and sodium beam emission spectrum, so as to realize longer service life of the sodium ion emitter and solve the problems that cracking and stripping occur due to thermal shrinkage of a lithium ion emitting material and thermal expansion of a substrate at high temperature, and the signal-to-noise ratio of a lithium beam is poor in a lithiation wall treatment mode, so that boundary plasma information cannot be accurately obtained.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a sodium ion emitter comprising: a round cup-shaped tungsten bottom plate, a porous tungsten substrate layer, a sodium aluminosilicate emitting material layer and a heating body; wherein,
the heating body comprises aluminum oxide and a conical tungsten wire, and the conical tungsten wire is positioned in the aluminum oxide;
the round cup-shaped tungsten bottom plate is provided with a top concave cavity at the top and a bottom concave cavity at the bottom;
the porous tungsten substrate layer and the sodium aluminosilicate emitting material layer are sequentially stacked in the top concave cavity from the bottom of the concave cavity outwards;
in the bottom pocket, the heating body is placed.
Further, the sodium ion emitter is a monolithic structure formed by heat treatment; preferably, the heat treatment is sintering.
Preferably, the porous tungsten substrate layer is formed by pressing and sintering a mixture formed by mixing tungsten powders with different diameters.
Preferably, the thickness of the porous tungsten substrate is 2-2.5mm. Preferably, the thickness of the emissive material layer of sodium aluminosilicate is 2-3mm.
For example, the top cavity depth is 3mm, 4mm, 5mm, or 6mm. The top cavity diameter is 15mm, 16mm, 17mm, 18mm, 19mm, 20mm, 21mm, 22mm, 23mm, 24mm or 25mm.
For example, the depth of the bottom cavity is 15-20 mm. For example, the bottom cavity depth is 15mm, 16mm, 17mm, 18mm, 19mm or 20mm. The bottom cavity diameter is 20mm, 21mm, 22mm, 23mm, 24mm, 25mm, 26mm, 27mm, 28mm or 29mm.
Further, an annular step is arranged around the concave cavity at the top of the round cup-shaped tungsten bottom plate, and a chamfer is formed along the annular step and is used for fixing the porous tungsten substrate. For example, the step diameter is 25mm, 26mm, 27mm or 28mm, and the height is 2mm, 3mm or 4mm. Preferably, the chamfer is 45 °. Optionally, the depth of the chamfer structure is 1mm.
A method for preparing sodium ion emitter comprises the following steps,
(1) Providing a round cup-shaped tungsten bottom plate, wherein the top of the round cup-shaped tungsten bottom plate is provided with a top concave cavity, and the bottom of the round cup-shaped tungsten bottom plate is provided with a bottom concave cavity;
(2) Mixing tungsten powders with different diameters to form a mixture, pressing the mixture into the top concave cavity, and sintering the mixture into a porous tungsten substrate layer;
(3) Dropping sodium aluminosilicate powder slurry on the surface of the porous tungsten substrate layer to enable sodium aluminosilicate powder to permeate into the porous tungsten substrate layer;
(4) Further filling sodium aluminosilicate powder on the surface of the porous tungsten substrate layer in the top concave cavity to obtain a first sodium ion emitter precursor;
(5) Heating and cooling the first sodium ion emitter precursor in vacuum to obtain a second sodium ion emitter precursor;
(6) Adding a raw material comprising aluminum oxide powder into a bottom concave cavity of a round cup-shaped tungsten bottom plate of a second sodium ion emitter precursor, placing a conical tungsten wire into the aluminum oxide powder, and drying to obtain the sodium ion emitter.
Further, in the step (2), the tungsten powders with different diameters are respectively tungsten powder with the diameter of 10 micrometers and tungsten powder with the diameter of 100 micrometers. In the mixture, the mass ratio of the tungsten powder with the diameter of 10 microns to the tungsten powder with the diameter of 100 microns is 1:1.
The purity of the sodium aluminosilicate in the invention is more than 99.5%.
Further, in the step (2), the sintering temperature is 1800-2000 ℃; the sintering atmosphere is hydrogen, and the pressure is 0.01-1.0 pa; the sintering time is 1-2 hours.
Further, in step (3), the sodium aluminosilicate powder slurry is a sodium aluminosilicate powder and deionized water mixture.
Further, in the step (3), the sodium aluminosilicate powder slurry is dropped on the surface of the porous tungsten substrate layer, so that sodium aluminosilicate powder permeates into the porous tungsten substrate layer, and the process is performed as follows: mixing sodium aluminosilicate powder with deionized water to form slurry, uniformly coating the slurry on the surface of a porous tungsten substrate, and keeping vibrating on an ultrasonic vibration platform for 10-20 minutes to enable the sodium aluminosilicate powder to permeate into the porous tungsten substrate; preferably, 2 drops of slurry are applied per square centimeter of porous tungsten substrate surface.
Further, in the step (4), sodium aluminosilicate powder is uniformly covered on the porous tungsten substrate layer, the thickness is kept between 2 and 3mm, and the thickness is kept between 150 and 200kg/cm 2 The powder is compacted under pressure and the surface is kept even and smooth.
Further, the step (5) specifically includes: the heating is performed in a vacuum furnace. The heating and cooling comprises the steps of raising the air pressure to the highest temperature of 1110-1120 ℃ at the speed of 9-10 ℃ per minute in the range of 0.01-1pa, maintaining the highest temperature for 5-10 minutes, then cooling to the room temperature at the speed of 15-20 ℃ per minute, and then charging nitrogen at the speed of 1000-2000 pa/min until the air pressure is raised to 1 atmosphere, thus the manufacturing of the emission coating is completed. The emission coating is an emission material layer of sodium aluminosilicate.
Further, the step (6) specifically includes: pouring the mixture of the alumina powder and the ceramic glue into a concave cavity with the depth of 15-20 mm of the round cup-shaped tungsten bottom plate, and immersing the conical tungsten wire into the mixture of the alumina powder and the ceramic glue.
Further, in step (6), the drying, heat treatment includes: after injecting the mixture of the alumina powder and the ceramic glue, standing for 24 hours, drying, and then placing the whole structure in a vacuum oven, baking for 5 hours at 100 ℃ to release residual moisture, and then heating to 300 ℃ to bake for 10 hours.
In the present invention, high purity means a purity of more than 99.5%.
Further, the main components of the sodium ion emitter include: a high mechanical strength round cup-shaped tungsten bottom plate, a porous tungsten substrate layer which is formed by mixing, pressing and sintering tungsten powder with the diameter of 10 microns and tungsten powder with the diameter of 100 microns according to the mass ratio of 1:1, a high-purity sodium aluminosilicate (purity of more than 99.5%) emitting material layer, and a heating body which consists of aluminum oxide and conical tungsten wires.
In an alternative embodiment, the porous tungsten substrate layer has a porosity of 25%.
Further, the porous tungsten substrate layer has a thermal expansion coefficient close to that of sodium aluminosilicate, and can not cause coating stripping phenomenon due to different expansion sizes at the using temperature of 1000-1100 ℃.
Further, the sodium aluminosilicate powder and deionized water mixture is adopted to vibrate on an ultrasonic platform for a long time, so that sodium aluminosilicate can enter porous tungsten to form a compact structure, and the sodium aluminosilicate powder and deionized water mixture cannot fall off under the action of electrostatic force in the use process.
Furthermore, the annular chamfer of the tungsten supporting bottom plate can enable the combination of the porous tungsten and the tungsten supporting bottom plate to be more firm, and a larger gap or separation phenomenon can not be generated due to slight difference of thermal expansion coefficients of two materials.
Further, sodium aluminosilicate is uniformly covered on the surface of the porous tungsten substrate by adopting dry powder, and the diameter of the sodium aluminosilicate is 2-10 microns, so that a large number of micro holes can be generated, sodium ions can be facilitated to overflow the surface of the emitter as soon as possible, sodium ions are generated, and the emission capacity of the emitter is improved.
Further, the sintering temperature is 1100 ℃ and is maintained for 20 minutes, sodium aluminosilicate is not fully changed into liquid while being sintered together, a large number of micro hole structures of the emission material are reserved, stress caused by heating expansion is released, and cracking of the emission material caused by expansion is effectively restrained.
In the invention, the porous tungsten substrate layer is in a porous tungsten cake structure.
The beneficial effects are that:
1. according to the invention, a cavity with a circular depth of 5mm is processed on the top of a firm and high-temperature-resistant circular cup-shaped tungsten skeleton, chamfering processing is carried out on the bottom of the cavity, tungsten powder with a diameter of 10 microns and tungsten powder with a diameter of 100 microns are mixed in a ratio of 1:1, and the mixture is pressed and sintered together with a tungsten base to form a porous tungsten cake structure with a porosity of 25% and a thickness of 2mm, so that the problem that cracks or falling phenomena are generated at high temperature due to different thermal expansion coefficients of tungsten and porous tungsten can be effectively solved.
2. The mixed slurry of sodium aluminosilicate powder with the diameter of 2-10 microns and deionized water can go deep into a porous tungsten substrate under the action of ultrasonic vibration, and the mixed slurry and the sodium aluminosilicate powder on the surface can be sintered together to increase the adhesive force of the surfaces of the two materials, so that the mixed slurry cannot be peeled off under the action of electrostatic force.
3. Sodium aluminosilicate powder is uniformly paved on the surface of the substrate, and the concave cavity with the depth of about 3mm is filled up, and the pressure is 200kg/cm 2 The porous structure of the emission material coating is formed after sintering at 1100 ℃ by compacting under pressure, so that the stress caused by thermal expansion can be effectively released, and further, the phenomena of cracking or partial falling of powder caused by expansion are avoided.
4. The thermal expansion coefficient of the porous tungsten cake is smaller than that of tungsten and is close to that of sodium aluminosilicate with a porous structure, so that the problem that contact surface materials are broken due to stress caused by thermal expansion and cold contraction of two materials can be effectively solved.
5. The tungsten heating wire and alumina ceramic integrated structure is adopted, so that insulation of the heating wire is realized, and meanwhile, the original heat radiation heating structure is changed into a heat conduction heating emitter, so that the heating efficiency is higher.
Drawings
FIG. 1 is a cross-sectional view of the structure of the present invention;
fig. 2 is an exploded view of a sodium ion emitter.
Wherein: 1 is a tungsten skeleton, 2 is a chamfer, 3 is a porous tungsten substrate, 4 is a sodium aluminosilicate cake, 5 is an alumina ceramic body, and 6 is a tungsten heating wire.
Detailed Description
The technical scheme of the invention is described in detail below with reference to the attached drawings.
As shown in fig. 1-2, a sodium ion emitter (i.e., sodium ion source) suitable for ion accelerator, material treatment and plasma generation comprises a tungsten skeleton 1 with high mechanical strength, a porous tungsten substrate 3 obtained by pressing and sintering a tungsten powder mixture with a diameter of 10 micrometers and 100 micrometers in a mass ratio of 1:1, a tungsten skeleton chamfer 2 used for fixing the porous tungsten substrate 3, a high-purity sodium aluminosilicate sintered ceramic body (high purity means purity of more than 99.5%), a tungsten heating wire 6 for realizing heating and insulating functions and a columnar alumina ceramic body 5. The tungsten heating wire 6 is positioned in the columnar alumina ceramic body 5, and the tungsten heating wire 6 and the columnar alumina ceramic body 5 form a heating body. The tungsten heating wire 6 is a conical tungsten wire. The distance between the tungsten heating wire 6 and the tungsten framework 1 is more than 2mm, and two ends of the tungsten heating wire are connected with a heating power supply.
The ceramic body sintered by the high-purity sodium aluminosilicate is a sodium aluminosilicate cake 4. The sodium aluminosilicate cake 4 is a sintered ceramic body of sodium aluminosilicate with purity greater than 99.5%.
The porous tungsten substrate 3 is a porous tungsten cake. The porosity of the porous tungsten substrate 3 was 25%. The porous tungsten cake with the porosity of 25% and the sodium aluminosilicate ceramic body have similar thermal expansion coefficients, so that the adhesiveness of the emitting material on the substrate is ensured, and the emitting material can be prevented from cracking due to thermal expansion. The tungsten framework and the porous tungsten sintered together by the chamfer structure ensure that the two materials cannot fall off at high temperature due to different thermal expansion coefficients, and the porous tungsten cake cannot be peeled off due to the action of electrostatic force in the discharging process.
The tungsten skeleton with high mechanical strength is made of high-hardness tungsten material and is in a round cup shape. The top of the tungsten skeleton is provided with a top concave cavity and an annular chamfer structure. The top cavity is a cavity with the diameter of 20mm and the depth of 5mm. The bottom of the tungsten framework 1 is provided with a bottom concave cavity with the diameter of 25mm and the depth of 20mm. The annular chamfer structure is arranged as follows: an annular step is arranged around the top concave cavity, the diameter of the step is 28mm, the height of the step is 3mm, and a chamfer angle 2 is formed along the annular step to form an annular chamfer angle structure which is used for being fixed with an auxiliary structure of the ion source so as to ensure good electric contact of the ion source. Optionally, the chamfer 2 is 45 °, and the depth of the chamfer structure is 1mm. In the top concave cavity, a porous tungsten substrate 3 and a sodium aluminosilicate cake 4 are sequentially stacked outwards from the bottom of the concave cavity. In the bottom pocket, the heating body is placed.
Mixing tungsten powder with the diameter of 10 microns and tungsten powder with the diameter of 100 microns according to the mass ratio of 1:1 to form mixed powder, wherein the mixed powder is formed at the temperature of 10T/cm 2 The mixed powder is pressed into the top cavity under pressure, the structure is placed in an atmosphere of 0.01pa of hydrogen at 2000 ℃ for firing for 2 hours until the substrate with the porous structure is formed by sintering, and then the temperature is slowly reduced to room temperature, so that the porous tungsten substrate 3 with the porosity of about 25% is formed. The tungsten skeleton 1 and the porous tungsten substrate 3 are sintered together, and the tungsten skeleton 1 and the porous tungsten substrate 3 have the same composition, so that the expansion coefficients are close, and the separation of the skeleton and the substrate caused by the difference of the thermal expansion coefficients is facilitated to be relieved. The thickness of the porous tungsten substrate was 2.5mm.
0.5 g sodium aluminosilicate powder with purity more than 99.5% is stirred by 2ml deionized water to form a slurry body, the slurry body is dripped on the surface of the porous tungsten substrate 3, 2 drops are dripped per square centimeter, the slurry body is uniformly smeared and placed on an ultrasonic vibration platform, and vibration is kept for 20 minutes, so that the sodium aluminosilicate powder can permeate into the porous tungsten body. Mixing deionized water and dry sodium aluminosilicate powder in the mass ratio of 1:10, stirring uniformly, filling into a cavity at the top of a tungsten skeleton, and stirring at a speed of 200kg/cm 2 The powder is compacted under pressure to the same height as the surface of the cavity and to keep the surface even and smooth. With such a knotThe thickness of the surface sodium aluminosilicate coating can reach 2-3mm. The current emission capability is higher because it is proportional to the coating thickness. And (3) in the room temperature environment, the surface coating is slowly dried in the shade for 48 hours, so that the powder coating cannot crack, and the ion source framework is prepared.
The prepared ion source framework is put into a vacuum furnace, and the air pressure is maintained at about 0.01pa, so that the evaporation of sodium aluminosilicate at high temperature is inhibited. The skeleton structure was slowly heated with a temperature rise rate of 10 degrees celsius/min, and after the temperature reached 1110 degrees celsius, it was maintained at this temperature for 10 minutes until a liquid glass-like body formed on the surface, and then the vacuum oven was slowly cooled at 20 degrees celsius/min until a room temperature state. The vacuum chamber was purged with nitrogen at a rate of 1000pa/min until it was raised to 1 atmosphere, and through the above steps, the firing of the emissive coating was completed. The emissive coating is sodium aluminosilicate cake 4. The thickness of the emissive coating was 3mm.
The method comprises the steps of adding a mixture with the mass ratio of high-purity alumina powder (purity of 99.9%) to inorganic ceramic glue with the temperature resistant of 1400 ℃ to be 2:1 into a tungsten skeleton, injecting the mixture with the thickness of 2mm, drying for 24 hours, placing a conical tungsten heating wire 6 in the center of the bottom concave cavity, injecting the mixture of the alumina powder and the ceramic glue again until the tungsten heating wire 6 is completely covered, standing for 24 hours, drying, placing the whole structure in a vacuum oven, baking at 100 ℃ for 5 hours to release residual moisture, heating to 300 ℃ and baking for 10 hours, discharging residual organic impurities, and hardening the alumina powder condensate. Wherein the alumina powder aggregate is hardened to form columnar alumina ceramic body 5.
When the sodium ion emitter prepared by the invention is used, the ion source is heated to 1000-1100 ℃, and a bias voltage of minus 10 to minus 1kV is applied to the emitter, so that 1-7mA/cm can be led out 2 Sodium ion flow of (2).
While the foregoing has been described in relation to illustrative embodiments thereof, so as to facilitate the understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but is to be construed as limited to the spirit and scope of the invention as defined and defined by the appended claims, as long as various changes are apparent to those skilled in the art, all within the scope of which the invention is defined by the appended claims.
Claims (2)
1. A method for preparing a sodium ion emitter, which is characterized in that the sodium ion emitter consists of a round cup-shaped tungsten bottom plate, a porous tungsten substrate layer, a sodium aluminosilicate emitting material layer and a heating body; wherein,
the heating body comprises aluminum oxide and a conical tungsten wire, and the conical tungsten wire is positioned in the aluminum oxide;
the round cup-shaped tungsten bottom plate is provided with a top concave cavity at the top and a bottom concave cavity at the bottom; the depth of the bottom concave cavity is 15-20 mm;
the porous tungsten substrate layer and the sodium aluminosilicate emitting material layer are sequentially stacked in the top concave cavity from the bottom of the top concave cavity outwards;
in the bottom cavity, the heating body is placed;
an annular step is arranged around the concave cavity at the top of the round cup-shaped tungsten bottom plate and is chamfered along the annular step for fixing the porous tungsten substrate; the thickness of the porous tungsten substrate is 2-2.5mm; the thickness of the emitting material layer of the sodium aluminosilicate is 2-3 mm;
the method comprises the steps of,
(1) Providing a round cup-shaped tungsten bottom plate, wherein the top of the round cup-shaped tungsten bottom plate is provided with a top concave cavity, and the bottom of the round cup-shaped tungsten bottom plate is provided with a bottom concave cavity;
(2) Mixing tungsten powders with different diameters to form a mixture, pressing the mixture into the top concave cavity, and sintering the mixture into a porous tungsten substrate layer;
(3) Dropping sodium aluminosilicate powder slurry on the surface of the porous tungsten substrate layer to enable sodium aluminosilicate powder to permeate into the porous tungsten substrate layer;
(4) Further filling sodium aluminosilicate powder on the surface of the porous tungsten substrate layer in the top concave cavity to obtain a first sodium ion emitter precursor;
(5) Heating and cooling the first sodium ion emitter precursor in vacuum to obtain a second sodium ion emitter precursor;
(6) Adding a raw material comprising aluminum oxide powder into a bottom concave cavity of a round cup-shaped tungsten bottom plate of a second sodium ion emitter precursor, placing a conical tungsten wire into the aluminum oxide powder, drying, and performing heat treatment to obtain the sodium ion emitter;
in the step (2), the sintering temperature is 1800-2000 ℃; the sintering atmosphere is hydrogen, and the pressure is 0.01-1.0 pa; sintering for 1-2 hours;
in the step (3), the sodium aluminosilicate powder slurry is dripped on the surface of the porous tungsten substrate layer, so that sodium aluminosilicate powder permeates into the porous tungsten substrate layer, and the process is carried out by the following steps: mixing sodium aluminosilicate powder with deionized water to form slurry, uniformly coating the slurry on the surface of a porous tungsten substrate, and keeping vibrating on an ultrasonic vibration platform for 10-20 minutes to enable the sodium aluminosilicate powder to permeate into the porous tungsten substrate;
in the step (4), uniformly covering sodium aluminosilicate powder on the porous tungsten substrate layer, wherein the concentration of the sodium aluminosilicate powder is 150-200 kg/cm 2 Compacting the powder under pressure and keeping the surface uniform and smooth;
in step (5), the heating is performed by: raising the air pressure to the highest temperature of 1110-1120 ℃ at the speed of 9-10 ℃ per minute within the range of 0.01-1pa, and maintaining the highest temperature for 5-10 minutes; the cooling is performed as follows: cooling to room temperature at a speed of 15-20 ℃ per minute, and then filling nitrogen at a speed of 1000-2000 pa/min until the pressure is increased to 1 atmosphere;
the step (6) comprises: pouring the mixture of the alumina powder and the ceramic glue into a concave cavity at the bottom of the round cup-shaped tungsten bottom plate, and immersing the conical tungsten wire into the mixture of the alumina powder and the ceramic glue.
2. The method of claim 1, wherein in step (6), the drying, heat treating comprises: after injecting the mixture of the alumina powder and the ceramic glue, standing for 24 hours, drying, and then placing the whole structure in a vacuum oven, baking for 5 hours at 100 ℃ to release residual moisture, and then heating to 300 ℃ to bake for 10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111668067.9A CN114340124B (en) | 2021-12-30 | 2021-12-30 | Sodium ion emitter and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111668067.9A CN114340124B (en) | 2021-12-30 | 2021-12-30 | Sodium ion emitter and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114340124A CN114340124A (en) | 2022-04-12 |
| CN114340124B true CN114340124B (en) | 2024-02-27 |
Family
ID=81021638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111668067.9A Active CN114340124B (en) | 2021-12-30 | 2021-12-30 | Sodium ion emitter and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114340124B (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2216942A (en) * | 1936-12-22 | 1940-10-08 | Zeiss Ikon Ag | Glow cathode for cathode ray tubes |
| US2813220A (en) * | 1954-12-06 | 1957-11-12 | Philips Corp | Indirectly heated cathode |
| FR1174340A (en) * | 1956-04-24 | 1959-03-10 | Egyesuelt Izzolampa | Diffusion cathode with reserve of material and method for its manufacture |
| US4395631A (en) * | 1979-10-16 | 1983-07-26 | Occidental Research Corporation | High density ion source |
| US4928033A (en) * | 1988-11-15 | 1990-05-22 | Environmental Technologies Group, Inc. | Thermionic ionization source |
| CN1046245A (en) * | 1989-04-03 | 1990-10-17 | 菲利浦光灯制造公司 | The negative electrode of discharge tube |
| US5147460A (en) * | 1990-05-21 | 1992-09-15 | Acheson Industries, Inc. | Internal coating materials for a cathode ray tube |
| WO2009110506A1 (en) * | 2008-03-07 | 2009-09-11 | 三井造船株式会社 | Ion source |
| CN105788996A (en) * | 2014-12-22 | 2016-07-20 | 中国电子科技集团公司第十二研究所 | Sub-micron film scandium-tungsten cathode and preparation method thereof |
| CN109979791A (en) * | 2018-12-20 | 2019-07-05 | 中国电子科技集团公司第十二研究所 | A kind of Heater-Cathode assembly and preparation method thereof |
| CN112616233A (en) * | 2020-12-16 | 2021-04-06 | 中国科学院合肥物质科学研究院 | Stable-state high-beam-density long-life lithium ion source suitable for accelerator |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101311480B1 (en) * | 2011-08-03 | 2013-11-13 | 한국생산기술연구원 | manufacturing method of WC sintered-body for friction stir welding(FSW) tool |
-
2021
- 2021-12-30 CN CN202111668067.9A patent/CN114340124B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2216942A (en) * | 1936-12-22 | 1940-10-08 | Zeiss Ikon Ag | Glow cathode for cathode ray tubes |
| US2813220A (en) * | 1954-12-06 | 1957-11-12 | Philips Corp | Indirectly heated cathode |
| FR1174340A (en) * | 1956-04-24 | 1959-03-10 | Egyesuelt Izzolampa | Diffusion cathode with reserve of material and method for its manufacture |
| US4395631A (en) * | 1979-10-16 | 1983-07-26 | Occidental Research Corporation | High density ion source |
| US4928033A (en) * | 1988-11-15 | 1990-05-22 | Environmental Technologies Group, Inc. | Thermionic ionization source |
| CN1046245A (en) * | 1989-04-03 | 1990-10-17 | 菲利浦光灯制造公司 | The negative electrode of discharge tube |
| US5147460A (en) * | 1990-05-21 | 1992-09-15 | Acheson Industries, Inc. | Internal coating materials for a cathode ray tube |
| WO2009110506A1 (en) * | 2008-03-07 | 2009-09-11 | 三井造船株式会社 | Ion source |
| CN105788996A (en) * | 2014-12-22 | 2016-07-20 | 中国电子科技集团公司第十二研究所 | Sub-micron film scandium-tungsten cathode and preparation method thereof |
| CN109979791A (en) * | 2018-12-20 | 2019-07-05 | 中国电子科技集团公司第十二研究所 | A kind of Heater-Cathode assembly and preparation method thereof |
| CN112616233A (en) * | 2020-12-16 | 2021-04-06 | 中国科学院合肥物质科学研究院 | Stable-state high-beam-density long-life lithium ion source suitable for accelerator |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114340124A (en) | 2022-04-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9597734B2 (en) | Electrostatic chuck and showerhead with enhanced thermal properties and methods of making thereof | |
| JP4476701B2 (en) | Manufacturing method of sintered body with built-in electrode | |
| KR101531726B1 (en) | Electrostatic chuck and method for producing same | |
| JP5225024B2 (en) | Suction board and vacuum suction device | |
| KR20200036791A (en) | Member for semiconductor manufacturing apparatus | |
| CN114340124B (en) | Sodium ion emitter and preparation method thereof | |
| US11837489B2 (en) | Electrostatic chuck device and production method for electrostatic chuck device | |
| KR101457614B1 (en) | Glass composition for solid oxide fuel cell sealant, sealant and the manufacturing method using the same | |
| KR100890414B1 (en) | Electrostatic chuck with heater | |
| KR101165477B1 (en) | Ceramic heater unit | |
| JP2533679B2 (en) | Plate-shaped ceramic heater and method for manufacturing the same | |
| JP5032444B2 (en) | Substrate holder | |
| CN112616233B (en) | Stable-state high-beam-density long-life lithium ion source suitable for accelerator | |
| CN216930353U (en) | Heating plate, ceramic heating plate and chemical vapor deposition equipment | |
| JP3720757B2 (en) | Ceramic bonding apparatus and method for manufacturing ceramic bonded body using the same. | |
| JP7272370B2 (en) | Silicon nitride substrate manufacturing method and silicon nitride substrate | |
| JP6855958B2 (en) | Manufacturing method of electrode plate for plasma processing equipment and electrode plate for plasma processing equipment | |
| JP2015205780A (en) | Method for producing porous silicon carbide sintered compact, and porous silicon carbide sintered compact having protective layer | |
| CN211386900U (en) | Microwave sintering device | |
| CN112750692A (en) | Composite sintered body and method for producing composite sintered body | |
| CN110822899B (en) | Auxiliary heating and heat insulating device for microwave sintering | |
| TWI240985B (en) | Wafer holder for semiconductor manufacturing device and semiconductor manufacturing device in which it is installed | |
| US11869796B2 (en) | Electrode-embedded member and method for manufacturing same, electrostatic chuck, and ceramic heater | |
| JP3688156B2 (en) | Ceramic joined body and manufacturing method thereof | |
| JP2020040865A (en) | Manufacturing method of ceramic member |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |