CN109518258A - A kind of preparation method of electrovacuum insulation heated filament - Google Patents
A kind of preparation method of electrovacuum insulation heated filament Download PDFInfo
- Publication number
- CN109518258A CN109518258A CN201811629584.3A CN201811629584A CN109518258A CN 109518258 A CN109518258 A CN 109518258A CN 201811629584 A CN201811629584 A CN 201811629584A CN 109518258 A CN109518258 A CN 109518258A
- Authority
- CN
- China
- Prior art keywords
- heated filament
- mixed
- electrovacuum
- preparation
- solution
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Insulating Materials (AREA)
- Insulated Conductors (AREA)
Abstract
The invention discloses a kind of preparation methods for electrovacuum insulation heated filament for belonging to electrovacuum component manufacturing technology field.Electrovacuum insulation heated filament is made using electrophoretic deposition in heated filament surface depositing insulating layer, after sintering by the present invention；Electrophoresis liquid is mixed to get by mixed oxide and mixed solution in electrophoretic deposition, and the mixed oxide includes aluminium oxide, silica, magnesia, calcium oxide, yttrium oxide；The mixed solution includes cotton solution, ceric ammonium nitrate solution, ethyl alcohol.Preparation method of the present invention is simple and efficient, and the insulation heated filament surfacing of preparation, thickness is uniform, insulating properties is higher, thickness of insulating layer is easy to regulate and control, and is able to satisfy the high requirement of the vacuum devices such as interior hot type air suction element and cathode filament.
Description
Technical field
The invention belongs to electrovacuum component manufacturing technology field, in particular to the preparation side of a kind of electrovacuum insulation heated filament
Method.
Background technique
Interior hot type getter is a kind of important application form of getter, with the miniaturization of vacuum device, in industry
More stringent requirements are proposed in terms of heated current for internal heated getter agent, is to heater strip in getter accordingly
The coherence request of insulation heated filament is also higher and higher.
Currently, there are two types of the conventional preparation techniques of insulation heated filament.One kind is vapor deposition, that is, utilizes in gas phase and physics occurs
Or chemical process forms insulating coating on heated filament surface, the preparation for complicated shape insulation heated filament, vapour deposition process is difficult
Guarantee the insulating properties on its surface.Second is artificial coating, and after insulating layer is prepared into slurry, it is right to be manually applied to heated filament surface
After be sintered, the insulation heated filament external form consistency of this method preparation is very poor, and thickness is difficult to control, and the consistency of heating is also difficult to full
The demand of the present industry of foot.
Summary of the invention
The purpose of the present invention is to provide a kind of electrovacuum preparation method of insulation heated filament, specific technical solution is as follows:
A kind of electrovacuum is, using electrophoretic deposition in heated filament surface depositing insulating layer, to burn with the preparation method of insulation heated filament
Electrovacuum insulation heated filament is made after knot；
Electrophoresis liquid is mixed to get by mixed oxide and mixed solution in the electrophoretic deposition, and the mixed oxide includes
Aluminium oxide, silica, magnesia, calcium oxide, yttrium oxide；The mixed solution includes cotton solution, ceric ammonium nitrate solution, second
Alcohol.
By percentage to the quality, the mixed oxide includes 80%~95% aluminium oxide, 2%~10% magnesia, 2%
~8% silica, 0.5%~0.8% calcium oxide, 0.1%~0.5% yttrium oxide.
With volume percentage, the mixed solution is molten including 1%~3% cotton solution, 0.1%~2% ammonium ceric nitrate
Liquid, 90%~98% ethyl alcohol.
The cotton solution is mixed to get by nitrocellulose, butyl acetate, and content of the nitrocellulose in cotton solution is
(5~10g)/L；
The ceric ammonium nitrate solution is mixed to get by ammonium ceric nitrate powder, ethyl alcohol, and ammonium ceric nitrate is in ceric ammonium nitrate solution
Content be 60g/L.
Mixed solution often contains 100ml ethyl alcohol in the electrophoresis liquid, needs 10~20g mixed oxide.
Voltage used in the electrophoretic deposition is 10~50V.
The sintering temperature is 1200~1600 DEG C.
The preparation method of electrovacuum insulation heated filament the following steps are included:
(1) electrophoresis liquid configures: by alumina powder, SiO 2 powder, magnesium oxide powder, lime powder, yttrium oxide
Powder is uniformly mixed with cotton solution, ceric ammonium nitrate solution, ethyl alcohol, ball milling obtains electrophoresis liquid；
(2) electrophoretic deposition: the electrophoresis liquid that step (1) configures is poured into electrophoresis tank, the heated filament of coiling is placed in electrophoresis liquid
In, it is powered and carries out electrophoretic deposition；
(3) heated filament is sintered: heated filament obtained by step (2) being placed in hydrogen-burning stove and is sintered, insulation heated filament is made.
Ball-milling Time >=10 hour in the step (1).
In the present invention heater material be heater material commonly used in the art, as Mo, MoLa, W, WRe, it is other using Mo, W as base
Alloy.
The invention has the benefit that
(1) using the method for the present invention preparation the surfacing of insulation heated filament, thickness uniformly, insulating properties it is higher, surface insulation
Layer can be controlled in 30~150 μm, and dimensional accuracy is high and is easy to regulate and control, and suitable for the preparation of various complicated shape heated filaments, and can protect
The consistency for demonstrate,proving external form and heated current, effectively overcomes the deficiency of uneven thickness etc. in conventional preparation techniques；It is able to satisfy
The high requirement of the vacuum devices such as interior hot type air suction element and cathode filament；
(2) preparation process in the present invention only includes with three electrophoresis liquid, electrophoresis, sintering processes, simple process, production effect
Rate is higher, at low cost.
Specific embodiment
The present invention provides a kind of electrovacuum with insulation heated filament preparation method, below with reference to embodiment to the present invention do into
The explanation of one step.
Embodiment 1
As steps described below in heated filament surface depositing insulating layer:
(1) electrophoresis liquid configures
By 80g alumina powder, 2g SiO 2 powder, 2.5g magnesium oxide powder, 0.5g lime powder, 0.3g oxidation
Yttrium powder end is uniformly mixed with 10ml cotton solution, 2.5ml ceric ammonium nitrate solution, 500ml ethyl alcohol, wherein is nitrified in cotton solution
Fiber content 6g/L, ammonium ceric nitrate content is 60g/L in ceric ammonium nitrate solution；By ball milling after obtained mixed liquor loading ball grinder
20h obtains electrophoresis liquid；
(2) electrophoretic deposition
The electrophoresis liquid for taking 50mL step (1) to configure is poured into electrophoresis tank, and the diameter 0.3mmWRe heated filament of preparatory coiling is set
In electrophoresis liquid, the electrophoresis 1min under the voltage of 10V；
(3) heated filament is sintered
Heated filament obtained by step (2) is placed in molybdenum box, is then placed in hydrogen-burning stove and is sintered, temperature is 1550 DEG C, has been sintered
Insulation heated filament is obtained after.
By the heated filament of preparation observe under the microscope without cracking and hole defect, surfacing, thickness of insulating layer be 70~
76μm。
Embodiment 2
As steps described below in heated filament surface depositing insulating layer:
(1) electrophoresis liquid configures
By 80g alumina powder, 4g SiO 2 powder, 5g magnesium oxide powder, 0.6g lime powder, 0.4g yttrium oxide
Powder is uniformly mixed with 16ml cotton solution, 4ml ceric ammonium nitrate solution, 800ml ethyl alcohol, wherein nitrocellulose in cotton solution
Content 8g/L, ammonium ceric nitrate content is 60g/L in ceric ammonium nitrate solution；By obtained mixed liquor be packed into ball grinder after ball milling 18h,
Obtain electrophoresis liquid；
(2) electrophoretic deposition
The electrophoresis liquid for taking 50mL step (1) to configure is poured into electrophoresis tank, and the Mo silk of the diameter 0.3mm of preparatory coiling is placed in
In electrophoresis liquid, the electrophoresis 2min under the voltage of 20V；
(3) heated filament is sintered
Heated filament obtained by step (2) is placed in molybdenum box, is then placed in hydrogen-burning stove and is sintered, temperature is 1480 DEG C, has been sintered
Insulation heated filament is obtained after.
By the heated filament of preparation observe under the microscope without cracking and hole defect, surfacing, thickness of insulating layer be 65~
68μm。
Embodiment 3
As steps described below in heated filament surface depositing insulating layer:
(1) electrophoresis liquid configures
By 85g alumina powder, 5.7g SiO 2 powder, 8g magnesium oxide powder, 0.8g lime powder, 0.5g oxidation
Yttrium powder end is uniformly mixed with 12ml cotton solution, 5ml ceric ammonium nitrate solution, 800ml ethyl alcohol, wherein is nitrified in cotton solution fine
Dimension hplc 9g/L, ammonium ceric nitrate content is 60g/L in ceric ammonium nitrate solution；By ball milling after obtained mixed liquor loading ball grinder
For 24 hours, electrophoresis liquid is obtained；
(2) electrophoretic deposition
The electrophoresis liquid for taking 50mL step (1) to configure is poured into electrophoresis tank, and the W silk of the diameter 0.3mm of preparatory coiling is placed in
In electrophoresis liquid, the electrophoresis 2min under the voltage of 30V；
(3) heated filament is sintered
Heated filament obtained by step (2) is placed in molybdenum box, is then placed in hydrogen-burning stove and is sintered, temperature is 1450 DEG C, has been sintered
Insulation heated filament is obtained after.
By the heated filament of preparation observe under the microscope without cracking and hole defect, surfacing, thickness of insulating layer be 85~
90μm。
Claims (9)
1. a kind of electrovacuum preparation method of insulation heated filament, which is characterized in that deposited absolutely using electrophoretic deposition on heated filament surface
Electrovacuum insulation heated filament is made in edge layer after sintering；
Electrophoresis liquid is mixed to get by mixed oxide and mixed solution in the electrophoretic deposition, and the mixed oxide includes oxidation
Aluminium, silica, magnesia, calcium oxide, yttrium oxide；The mixed solution includes cotton solution, ceric ammonium nitrate solution, ethyl alcohol.
2. the electrovacuum according to claim 1 preparation method of insulation heated filament, which is characterized in that with mass percent
Meter, the mixed oxide include 80%~95% aluminium oxide, 2%~10% magnesia, 2%~8% silica, 0.5%
~0.8% calcium oxide, 0.1%~0.5% yttrium oxide.
3. the electrovacuum according to claim 1 preparation method of insulation heated filament, which is characterized in that with percent by volume
Meter, the mixed solution include 1%~3% cotton solution, 0.1%~2% ceric ammonium nitrate solution, 90%~98% ethyl alcohol.
4. the electrovacuum according to claim 3 preparation method of insulation heated filament, which is characterized in that the cotton solution by
Nitrocellulose, butyl acetate are mixed to get, and content of the nitrocellulose in cotton solution is (5~10g)/L；
The ceric ammonium nitrate solution is mixed to get by ammonium ceric nitrate powder, ethyl alcohol, ammonium ceric nitrate containing in ceric ammonium nitrate solution
Amount is 60g/L.
5. the electrovacuum according to claim 1 preparation method of insulation heated filament, which is characterized in that mixed in the electrophoresis liquid
It closes solution and often contains 100ml ethyl alcohol, need 10~20g mixed oxide.
6. the electrovacuum according to claim 1 preparation method of insulation heated filament, which is characterized in that the electrophoretic deposition institute
Voltage is 10~50V.
7. the electrovacuum according to claim 1 preparation method of insulation heated filament, which is characterized in that the sintering temperature is
1200~1600 DEG C.
8. the preparation method of described in any item electrovacuums insulation heated filament according to claim 1~7, which is characterized in that including
Following steps:
(1) electrophoresis liquid configures: by alumina powder, SiO 2 powder, magnesium oxide powder, lime powder, yttrium oxide powder
It is uniformly mixed with cotton solution, ceric ammonium nitrate solution, ethyl alcohol, ball milling obtains electrophoresis liquid；
(2) electrophoretic deposition: the electrophoresis liquid that step (1) configures being poured into electrophoresis tank, the heated filament of coiling is placed in electrophoresis liquid, is led to
Electricity carries out electrophoretic deposition；
(3) heated filament is sintered: heated filament obtained by step (2) being placed in hydrogen-burning stove and is sintered, insulation heated filament is made.
9. the electrovacuum according to claim 8 preparation method of insulation heated filament, which is characterized in that in the step (1)
Ball-milling Time >=10 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811629584.3A CN109518258B (en) | 2018-12-28 | 2018-12-28 | Preparation method of insulating hot wire for electric vacuum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811629584.3A CN109518258B (en) | 2018-12-28 | 2018-12-28 | Preparation method of insulating hot wire for electric vacuum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109518258A true CN109518258A (en) | 2019-03-26 |
| CN109518258B CN109518258B (en) | 2021-01-26 |
Family
ID=65797183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811629584.3A Active CN109518258B (en) | 2018-12-28 | 2018-12-28 | Preparation method of insulating hot wire for electric vacuum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109518258B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110820031A (en) * | 2019-11-19 | 2020-02-21 | 有研工程技术研究院有限公司 | Preparation method of miniature getter |
| CN111800896A (en) * | 2019-12-24 | 2020-10-20 | 有研工程技术研究院有限公司 | Preparation method of high-temperature heating wire |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1487125A (en) * | 2003-08-27 | 2004-04-07 | 京东方科技集团股份有限公司 | Painting method of zirconium powder coating for electrophoretic grid |
| CN1505062A (en) * | 2002-11-27 | 2004-06-16 | 北京有色金属研究总院 | Insulation material for heating wire, method for making same and use thereof |
| CN201138649Y (en) * | 2007-12-26 | 2008-10-22 | 彩虹集团电子股份有限公司 | Apparatus for coating electrophoresis on hot wire |
| CN102832090A (en) * | 2012-08-29 | 2012-12-19 | 安徽华东光电技术研究所 | Heater assembly for space traveling wave tube and preparation method thereof |
| CN104008940A (en) * | 2014-04-28 | 2014-08-27 | 安徽华东光电技术研究所 | Method for performing electrophoresis on X-band space traveling-wave tube cathode filament |
| CN105931932A (en) * | 2016-04-26 | 2016-09-07 | 北京科技大学 | Preparation method of aluminum nitride insulation layer cathode hot wire |
| CN107768210A (en) * | 2017-09-04 | 2018-03-06 | 湖北汉光科技股份有限公司 | Large power long life-span cathode heater sub-assembly preparation method |
-
2018
- 2018-12-28 CN CN201811629584.3A patent/CN109518258B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1505062A (en) * | 2002-11-27 | 2004-06-16 | 北京有色金属研究总院 | Insulation material for heating wire, method for making same and use thereof |
| CN1487125A (en) * | 2003-08-27 | 2004-04-07 | 京东方科技集团股份有限公司 | Painting method of zirconium powder coating for electrophoretic grid |
| CN201138649Y (en) * | 2007-12-26 | 2008-10-22 | 彩虹集团电子股份有限公司 | Apparatus for coating electrophoresis on hot wire |
| CN102832090A (en) * | 2012-08-29 | 2012-12-19 | 安徽华东光电技术研究所 | Heater assembly for space traveling wave tube and preparation method thereof |
| CN104008940A (en) * | 2014-04-28 | 2014-08-27 | 安徽华东光电技术研究所 | Method for performing electrophoresis on X-band space traveling-wave tube cathode filament |
| CN105931932A (en) * | 2016-04-26 | 2016-09-07 | 北京科技大学 | Preparation method of aluminum nitride insulation layer cathode hot wire |
| CN107768210A (en) * | 2017-09-04 | 2018-03-06 | 湖北汉光科技股份有限公司 | Large power long life-span cathode heater sub-assembly preparation method |
Non-Patent Citations (4)
| Title |
|---|
| 姜进红: "热子及热子组合件的常见问题及解决方法", 《真空电子技术》 * |
| 孙慧 等: "硝酸铈铵复盐制备工艺研究", 《无机盐工业》 * |
| 王志义等: "电泳沉积氧化铝陶瓷涂层的制备及耐腐蚀性能", 《电镀与涂饰》 * |
| 管相杰: "金属基陶瓷涂层的制备及耐磨、耐腐蚀性能研究", 《青岛科技大学硕士学位论文》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110820031A (en) * | 2019-11-19 | 2020-02-21 | 有研工程技术研究院有限公司 | Preparation method of miniature getter |
| CN111800896A (en) * | 2019-12-24 | 2020-10-20 | 有研工程技术研究院有限公司 | Preparation method of high-temperature heating wire |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109518258B (en) | 2021-01-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109665834A (en) | The controllable indium gallium zinc target and preparation method thereof of phase composition | |
| CN100358832C (en) | Mullite whisker-mullite composite coating and preparation process thereof | |
| US20180305260A1 (en) | Ceramic component for timepiece | |
| CN109518258A (en) | A kind of preparation method of electrovacuum insulation heated filament | |
| KR20110089348A (en) | Corrosion resistant binders for bonding ceramic components exposed to the plasma | |
| CN101898906B (en) | Preparation method of carbon/carbon composite material SiO2-mullite-Al2O3 gradient outer coating | |
| CN105777204A (en) | Aventurine metallic luster glaze and preparation method thereof | |
| CN111925211A (en) | A kind of A2B2O7 rare earth tantalate ceramic and preparation method thereof | |
| CN104803372A (en) | Graphene film, and making method and use thereof | |
| CN105859272A (en) | Method for preparing nanometer negative expansion ceramic LiAlSiO4 by sintering at low temperature | |
| CN105350294B (en) | A kind of chopped carbon fiber of applying silicon carbide layer and preparation method thereof | |
| JP7165675B2 (en) | Method for manufacturing ceramic parts | |
| CN108620298A (en) | Electrothermal silicon carbide element surface oxidation-resistant coating and preparation method thereof | |
| CN109627050A (en) | A kind of quartz crucible inner surface coating and preparation method thereof | |
| CN1989273A (en) | Conductive element and method of making | |
| CN105199730B (en) | A kind of method for preparing rear-earth-doped oxidation tungsten nano structure membrane | |
| CN109627047A (en) | A kind of compound barium coating quartz crucible of silicon nitride combined silicon carbide and preparation method thereof | |
| CN108893740B (en) | A method for preparing high temperature insulating film by alternating liquid and gas phase deposition | |
| CN105603374B (en) | One kind prepares Si on polysilicon ingot crucible3N4The method of film | |
| CN110627495A (en) | A kind of low thermal conductivity high entropy aluminate ceramics and preparation method thereof | |
| JPH0724258B2 (en) | Solid diffusion source, doped silicon wafer and method of making same | |
| JP2004083376A (en) | Porous ceramic film having simultaneously controlled porosity and film thickness and method for producing the same | |
| CN115322594B (en) | A kind of high infrared radiation magnesium-doped silica coating and preparation method thereof | |
| JP2006205558A (en) | Alumina coating structure and its manufacturing method | |
| CN1238465C (en) | Diolame fluorescent powder and preparing method thereof |
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 |