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
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- 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
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- heated filament
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- electrovacuum
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- 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
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.
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| 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 |
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| 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 |
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| CN109518258A true CN109518258A (en) | 2019-03-26 |
| CN109518258B CN109518258B (en) | 2021-01-26 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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 |
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