CN108682601A - A kind of preparation method of vacuum X-ray tube electrode - Google Patents
A kind of preparation method of vacuum X-ray tube electrode Download PDFInfo
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- CN108682601A CN108682601A CN201810609094.0A CN201810609094A CN108682601A CN 108682601 A CN108682601 A CN 108682601A CN 201810609094 A CN201810609094 A CN 201810609094A CN 108682601 A CN108682601 A CN 108682601A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
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Abstract
The invention discloses a kind of preparation methods of vacuum X-ray tube electrode, include the following steps：(a) it using silver ingot as raw material, places it in the graphite crucible of direct current-arc plasma device, be filled with hydrogen, argon gas and device is vacuumized into sealing with vacuum pump, preparation forms silver powder I；(b) dispersant is prepared：The silver powder I that step (a) is obtained is added in alcohol, and oleic acid and ten dihydroxystearic acids are then added, silver powder II is centrifugally separating to obtain after ultrasonic disperse；(c) after carrying out vacuum drying treatment to silver powder made of step (b) II, glass powder is added and organic carrier prepares conductive silver paste；(d) conductive silver paste made from step (c) is coated in ray tube, it is placed in sintering kiln roasting and is formed by curing electrode conductor, the present invention selects volatile organic carrier, surface modification is carried out to silver powder by dispersant, experimental implementation is simple, it is at low cost, silver electrode good conductivity is obtained, there is good weldability.
Description
Technical field
The invention belongs to vacuum X-ray tube electrode material and preparing technical field, more particularly to a kind of vacuum X-ray tube
With the preparation method of electrode.
Background technology
Nano-silver powder is generally used as conductive, Heat Conduction Material because it is with higher conduction, thermal conductivity, the conduction of preparation
Slurry is more to be used in envelope, connection aspect；In addition microelectronic element micromation also be unable to do without nano-silver powder.It is produced in conductor paste
Sintering prepares the electrode product with conducting function after silver powder is added in production process, can form conducting wire.
Currently, nano-silver powder is prepared usually using chemical reduction method, the method introduces layer of surface activity on silver powder surface
Agent, and then the performance of the electrode of its electric conductivity and preparation can be influenced.Simultaneously as nano particle itself has large specific surface area
Characteristic results in nano particle and is easy to form aggregate during preparation, storage, transport etc..Due to the presence of aggregate, greatly
The big stability for reducing nanometer products, weakens the conductive effect of conductive silver slurry.In order to improve nano-silver powder in conductive paste
Stability in material can be prepared nano-silver powder by direct current arc plasma, and glass is added during preparing electrocondution slurry
Glass powder and organic carrier to obtain the conductive silver slurry of excellent properties, and then are prepared by sintering process with excellent properties
Electrode.
Used in cathode-ray tube electrode method has been reported at present.Chinese patent CN98123428.3 discloses one kind and passing through sheet metal
The method for manufacturing the electron gun electrodes of cathode-ray tube, it is described to be assembled in glass rays pipe than electrode, it is formed fixed
Assembled state and composition electron gun.Electrode process prepared by the method it is complicated and should in can be formed and assemble the optics of electron beam
Tou Tang are generated when electron gun works as finished product in cathode-ray tube during being manufactured and assembled due to electrode itself
Mechanical stress and thermal stress and by electron beam generate thermal stress influence, the distortion of electron beam trace can be caused, finally
Lead to the decline of cathode-ray tube quality.Therefore, ray pipe electrode is manufactured, can be led in the circumferential section use of electron beam through-hole
Electric silver paste forms the electrode of lower thickness to meet design requirement, while reducing thermal stress during electrode use after solidification.
Invention content
The present invention prepares difficult and is easy the problem of being distorted affected by environment, to prepare one for used in cathode-ray tube electrode
For kind using high-purity silver powder as conductive phase, glass powder is binder, and is penetrated to the X for being sintered formation after the adjusting of slurry by organic solvent
Spool electrode, realizing electrode discharge can inhibit to evaporate and generate highly resistance sputtering ability in the process.
The present invention is achieved by the following technical solutions：
A kind of preparation method of vacuum X-ray tube electrode, includes the following steps：
(a) it using silver ingot as raw material, places it in the graphite crucible of direct current-arc plasma device, is filled with hydrogen, argon gas simultaneously
Device is vacuumized into sealing with vacuum pump, the silver ingot is heated rapidly fusing by plasma, evaporation formed metallic vapour and with
The recyclegas that wind turbine generates disperses forms silver powder I into receipts powder room；
(b) dispersant is prepared：The silver powder I that step (a) is obtained is added in alcohol, and oleic acid is then added and ten dihydroxy are stearic
Acid is centrifugally separating to obtain silver powder II after ultrasonic disperse；
(c) after carrying out vacuum drying treatment to silver powder made of step (b) II, glass powder is added and organic carrier prepares conduction
Silver paste；
(d) conductive silver paste made from step (c) is coated in ray tube, is placed in sintering kiln roasting and is formed by curing electrode
Conductor.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
The purity of silver ingot is 99.95wt% in the step (a).
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
The cathode current of direct current-arc plasma device is 100-700A in the step (a), and vacuum pump the blowing pressure is 0.01-
0.06MPa, the ratio for being filled with hydrogen and argon gas is 1:6-1:2.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
Step (b) dispersant is formulated as：In terms of mass parts, often prepares 100 parts of alcohol and need 10-15 parts of silver powder I, 0.3-0.5
Part oleic acid and ten dihydroxystearic acid of 0.3-0.5 parts.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
The vacuum drying temperature of the step (c) is 30-100 DEG C；In terms of mass parts, the conductive silver paste by 40-60 parts of silver powder II,
0.4-1.5 parts of glass powders and 39-60 parts of organic carriers are prepared.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
The organic carrier includes terpinol, ethyl cellulose, Span -85, rilanit special, neck dibatyl phithalate, diethyl two
Alcohol ether acetate, ethyl acetate, butyl carbitol and butyl carbitol acetate.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
In terms of mass parts, the organic carrier includes 35-70 parts of terpinols, 2-5 parts of ethyl celluloses, 5-6 parts of Spans -85,1-2 parts of hydrogen
Change castor oil, 15 parts of neck dibatyl phithalates, 2-3 parts of diethylene glycol ether acetic acid esters, 0-38 parts of ethyl acetate.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
In terms of mass parts, the organic carrier includes 34 parts of terpinols, 2-5 parts of ethyl celluloses, 5-6 parts of Spans -85,1-2 parts of hydrogenations
Castor oil, 15 parts of neck dibatyl phithalates, 2-3 parts of diethylene glycol ether acetic acid esters, 18 parts of butyl carbitols and 18 parts of butyl
Carbitol acetate.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
Calcination temperature is 500-600 DEG C in the step (d), roasting time 15-30min.
A kind of preparation method of vacuum X-ray tube electrode of the present invention, the technical solution further solved be,
Thickness of electrode prepared by the step (d) is 20-80 μm.
Beneficial effects of the present invention are：
1. a kind of preparation method of vacuum X-ray tube electrode of the present invention, selects volatile organic carrier, passes through dispersant
Surface modification is carried out to silver powder, the preparation of nano-silver powder is realized using direct current arc plasma, the present invention obtains silver electrode
It is low to be less electrically conductive than resistivity, ranging from 5 × 10-4Ω•cm~1.3×10-5Ω•cm；Solderability is good, is 86% ~ 95% solderability,
Vacuum degree in X-ray tube keeps 5 × 10-7Pa is without decline.
2. electrode silver content prepared by the present invention is high, good conductivity, dispersant used is at low cost, dispersed height, while can
With the viscosity by adjusting electrocondution slurry to achieve the effect that the thickness for controlling silver electrode, experimental implementation is simple, at low cost.
Specific implementation mode
The invention content of the present invention is further described with reference to embodiment.
Silver ingot purity is 99.95wt%；Butyl carbitol, butyl carbitol acetate, ten dihydroxystearic acids, adjacent benzene two
Formic acid dibutyl ester, ethyl acetate come from one factory of Nanjing chemical reagent；Oleic acid, ethyl cellulose have from Chinese medicines group chemical reagent
Limit company；Rilanit special comes from Shanghai Ling Feng chemical reagent Co., Ltd；Span -85, alcohol are tried from Chinese medicines group chemistry
Agent Co., Ltd；Diethylene glycol ether acetic acid esters comes from Shanghai Nuo Chen International Trading Company Ltd；Terpinol is from sub- safe joint
Chemical industry；It is that analysis is pure.
Embodiment 1
The preparation of silver powder I：200g silver ingots are chosen, are placed it in the graphite crucible in direct current-arc plasma device, according to 1:3
Ratio be passed through hydrogen and argon gas and vacuumize and be sealed, control cathode current is 300A, the blowing pressure 0.02MPa, silver
Ingot is heated rapidly fusing by plasma, and evaporation forms metallic vapour and the recyclegas generated with wind turbine disperses to receipts powder room,
The average grain diameter for preparing the silver powder I of gained is 100nm.
Embodiment 2
(1) 100 parts of alcohol are added in I, the 0.5 part of oleic acid of silver powder and 0.5 part of ten dihydroxystearic acid prepared 10 parts of embodiments 1
In, it is centrifuged after ultrasonic disperse, is placed in vacuum drying chamber and is dried, obtain high dispersancy nano silver powder II；Control
Drying temperature processed is 50 DEG C；
(2) glass powder and 59.6 parts of organic carriers for weighing 40 parts of II, 0.4 part of silver powder prepare conductive silver paste；
(3) conductive silver paste in above-mentioned (2) is coated in inside the ray tube of glass material, is placed in high temperature sintering furnace 500 DEG C
Roasting keeps the temperature 30min, electrode is formed after solidification；
Organic carrier formula is in wherein above-mentioned (2)：35 parts of terpinols, 38 parts of ethyl acetate, 2 parts of ethyl celluloses, 6 parts of departments
Class -85,2 parts of rilanit specials, 15 parts of dibutyl phthalates, 2 parts of diethylene glycol ether acetic acid esters.
20 μm of its thickness of electrode after tested, resistivity are 5 × 10-4Ω cm, solderability 86%, the vacuum in X-ray tube
Degree keeps 5 × 10-7Pa is without decline.
Embodiment 3
(1) 100 parts of alcohol are added in I, the 0.3 part of oleic acid of silver powder and 0.3 part of ten dihydroxystearic acid prepared 10 parts of embodiments 1
In, it is centrifuged after ultrasonic disperse, is placed in vacuum drying chamber and is dried, obtain high dispersancy nano silver powder II；Control
Drying temperature processed is 50 DEG C；
(2) glass powder and 59 parts of organic carriers for weighing 50 parts of II, 1 part of silver powder prepare conductive silver paste；
(3) conductive silver paste in above-mentioned (2) is coated in inside the ray tube of glass material, is placed in high temperature sintering furnace 550 DEG C
Roasting keeps the temperature 20min, electrode is formed after solidification；
Organic carrier formula is in wherein above-mentioned (2)：35 parts of terpinols, 35 parts of ethyl acetate, 5 parts of ethyl celluloses, 6 parts of departments
Class -85,2 parts of rilanit specials, 15 parts of dibutyl phthalates, 2 parts of diethylene glycol ether acetic acid esters.
30 μm of its thickness of electrode after tested, resistivity are 5.9 × 10-5Ω cm, solderability 90% are true in X-ray tube
Reciprocal of duty cycle keeps 5 × 10-7Pa is without decline.
Embodiment 4：
(1) 100 parts of alcohol are added in I, the 0.3 part of oleic acid of silver powder and 0.3 part of ten dihydroxystearic acid prepared 15 parts of embodiments 1
In, it is centrifuged after ultrasonic disperse, is placed in vacuum drying chamber and is dried, obtain high dispersancy nano silver powder II；Control
Drying temperature processed is 60 DEG C；
(2) glass powder and 39 parts of organic carriers for weighing 60 parts of II, 1 part of silver powder prepare conductive silver paste；
(3) conductive silver paste in above-mentioned (2) is coated in inside the ray tube of glass material, is placed in high temperature sintering furnace 600 DEG C
Roasting keeps the temperature 15min, electrode is formed after solidification；
Organic carrier formula is in wherein above-mentioned (2)：70 parts of terpinols, 5 parts of ethyl celluloses, 6 parts of Spans -85,2 part hydrogenate castor
Sesame oil, 15 parts of dibutyl phthalates, 2 parts of diethylene glycol ether acetic acid esters.
50 μm of its thickness of electrode after tested, resistivity are 3.8 × 10-5Ω cm, solderability 90% are true in X-ray tube
Reciprocal of duty cycle keeps 5 × 10-7Pa is without decline.
Embodiment 5：
(1) 100 parts of alcohol are added in I, the 0.3 part of oleic acid of silver powder and 0.3 part of ten dihydroxystearic acid prepared 15 parts of embodiments 1
In, it is centrifuged after ultrasonic disperse, is placed in vacuum drying chamber and is dried, obtain high dispersancy nano silver powder II；Control
Drying temperature processed is 60 DEG C；
(2) glass powder and 39 parts of organic carriers for weighing 60 parts of II, 1.5 part of silver powder prepare conductive silver paste；
(3) conductive silver paste in above-mentioned (2) is coated in inside the ray tube of glass material, is placed in high temperature sintering furnace 600 DEG C
Roasting keeps the temperature 15min, electrode is formed after solidification；
Organic carrier formula is in wherein above-mentioned (2)：34 parts of terpinols, 18 parts of butyl carbitols, 18 parts of butyl carbitol acetic acid
Ester, 5 parts of ethyl celluloses, 6 parts of Span -85,2 part rilanit specials, 15 parts of dibutyl phthalates, 2 parts of diethylene glycol second
Ether acetic acid ester.
70 μm of its thickness of electrode after tested, resistivity are 1.3 × 10-5Ω cm, solderability 95% are true in X-ray tube
Reciprocal of duty cycle keeps 5 × 10-7Pa is without decline.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection domain.
Claims (10)
1. a kind of preparation method of vacuum X-ray tube electrode, which is characterized in that include the following steps：
(a) it using silver ingot as raw material, places it in the graphite crucible of direct current-arc plasma device, is filled with hydrogen, argon gas simultaneously
Device is vacuumized into sealing with vacuum pump, the silver ingot is heated rapidly fusing by plasma, evaporation formed metallic vapour and with
The recyclegas that wind turbine generates disperses forms silver powder I into receipts powder room；
(b) dispersant is prepared：The silver powder I that step (a) is obtained is added in alcohol, and oleic acid is then added and ten dihydroxy are stearic
Acid is centrifugally separating to obtain silver powder II after ultrasonic disperse；
(c) after carrying out vacuum drying treatment to silver powder made of step (b) II, glass powder is added and organic carrier prepares conduction
Silver paste；
(d) conductive silver paste made from step (c) is coated in ray tube, is placed in sintering kiln roasting and is formed by curing electrode
Conductor.
2. a kind of preparation method of vacuum X-ray tube electrode according to claim 1, which is characterized in that the step
(a) purity of silver ingot is 99.95wt% in.
3. a kind of preparation method of vacuum X-ray tube electrode according to claim 1, which is characterized in that the step
(a) cathode current of direct current-arc plasma device is 100-700A in, and vacuum pump the blowing pressure is 0.01-0.06MPa, is filled with
The ratio of hydrogen and argon gas is 1:6-1:2.
4. a kind of preparation method of vacuum X-ray tube electrode according to claim 1, which is characterized in that the step
(b) dispersant is formulated as：In terms of mass parts, often prepare 100 parts of alcohol and need 10-15 part silver powder I, 0.3-0.5 parts of oleic acid and
Ten dihydroxystearic acid of 0.3-0.5 parts.
5. a kind of preparation method of vacuum X-ray tube electrode according to claim 1, which is characterized in that the step
(c) vacuum drying temperature is 30-100 DEG C；In terms of mass parts, the conductive silver paste by 40-60 parts of silver powder II, 0.4-1.5 parts
Glass powder and 39-60 parts of organic carriers are prepared.
6. the preparation method of any vacuum X-ray tube electrode according to claim 1 or 5, which is characterized in that described
Organic carrier includes terpinol, ethyl cellulose, Span -85, rilanit special, neck dibatyl phithalate, diethylene glycol second
Ether acetic acid ester, ethyl acetate, butyl carbitol and butyl carbitol acetate.
7. a kind of preparation method of vacuum X-ray tube electrode according to claim 6, which is characterized in that with mass parts
Meter, the organic carrier includes 35-70 parts of terpinols, 2-5 parts of ethyl celluloses, 5-6 parts of Spans -85,1-2 parts of hydrogenated castors
Oil, 15 parts of neck dibatyl phithalates, 2-3 parts of diethylene glycol ether acetic acid esters, 0-38 parts of ethyl acetate.
8. a kind of preparation method of vacuum X-ray tube electrode according to claim 6, which is characterized in that with mass parts
Meter, the organic carrier include 34 parts of terpinols, 2-5 parts of ethyl celluloses, 5-6 parts of Spans -85,1-2 parts of rilanit specials, 15
Part neck dibatyl phithalate, 2-3 parts of diethylene glycol ether acetic acid esters, 18 parts of butyl carbitols and 18 parts of butyl carbitol acetic acid
Ester.
9. a kind of preparation method of vacuum X-ray tube electrode according to claim 1, which is characterized in that the step
(d) calcination temperature is 500-600 DEG C in, roasting time 15-30min.
10. a kind of preparation method of vacuum X-ray tube electrode according to claim 1, which is characterized in that the step
(d) thickness of electrode prepared is 20-80 μm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101494150A (en) * | 2009-02-27 | 2009-07-29 | 东南大学 | Cold-cathode focusing type X ray tube |
| CN103137400A (en) * | 2011-11-30 | 2013-06-05 | 高砂热学工业株式会社 | Field emission x-ray generating apparatus |
| CN103258584A (en) * | 2013-01-09 | 2013-08-21 | 深圳市创智材料科技有限公司 | Electric conductive silver paste and manufacturing method thereof |
| CN103440897A (en) * | 2013-08-06 | 2013-12-11 | 浙江光达电子科技有限公司 | Silicon solar cell front silver electrode high-square-resistance slurry and manufacturing method thereof |
-
2018
- 2018-06-13 CN CN201810609094.0A patent/CN108682601A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101494150A (en) * | 2009-02-27 | 2009-07-29 | 东南大学 | Cold-cathode focusing type X ray tube |
| CN103137400A (en) * | 2011-11-30 | 2013-06-05 | 高砂热学工业株式会社 | Field emission x-ray generating apparatus |
| CN103258584A (en) * | 2013-01-09 | 2013-08-21 | 深圳市创智材料科技有限公司 | Electric conductive silver paste and manufacturing method thereof |
| CN103440897A (en) * | 2013-08-06 | 2013-12-11 | 浙江光达电子科技有限公司 | Silicon solar cell front silver electrode high-square-resistance slurry and manufacturing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张小敏等: "纳米铜粉制备及其在乙醇中的分散工艺研究", 《材料工程》 * |
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Application publication date: 20181019 |