CN109023262A - The metallization process and welding method of graphite - Google Patents
The metallization process and welding method of graphite Download PDFInfo
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- CN109023262A CN109023262A CN201710437226.1A CN201710437226A CN109023262A CN 109023262 A CN109023262 A CN 109023262A CN 201710437226 A CN201710437226 A CN 201710437226A CN 109023262 A CN109023262 A CN 109023262A
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- pyrolytic graphite
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- film
- graphite
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a kind of metallization process of graphite and welding methods, it is related to vacuum device technology, the method for metallising, using vacuum arc deposition technology in pyrolytic graphite matrix surface deposited plating layer, the welding method is by pyrolytic graphite part and to need the component that welds to be placed in hydrogen furnace to weld.The method of the present invention, by pyrolytic graphite matrix surface metallize, allow to it is good welded with ceramic or other metals, reach hermetic seal, solve technical problem present in sealing-in, the development of microwave electron tube is greatly facilitated.
Description
Technical field
The present invention relates to vacuum device technical fields, are the metallization process and welding method of a kind of graphite.
Background technique
Travelling-wave tubes is a kind of microwave electron tube, has the characteristics that highly reliable, broadband, efficient.Electronic countermeasure,
The fields such as radar, satellite communication have a wide range of applications.As vacuum electron device, it is constantly subjected to semiconductor devices for many years
Great challenge and threat, for very especially in terms of middle low power.But in high-power, especially super high power field, vacuum electric
Sub- device still has highly significant advantage so far.
The deposition of pyrolytic graphite is the chemical vapour deposition reaction carried out under high temperature, vacuum condition, works as hydrocarbon
After gas and diluent gas are mixed into heating furnace according to a certain percentage, hydrocarbon gas will decompose in furnace, single original of decomposition
Sub- Carbon deposition is on the hot surface of graphite matrix.The residual air of reaction is continuously extracted out by vacuum pump, and carbon atom constantly deposits and shape
At certain thickness.It is down to room temperature to furnace temperature, since base shrinks amount is much larger than pyrolytic graphite, can easily be shelled from matrix
From lower pyrolytic graphite product.
Summary of the invention
The object of the present invention is to provide a kind of metallization process of graphite and welding methods, to solve pyrolytic graphite material
The problem of material connects with ceramics or other metal air-tight seals.
In order to achieve the above objectives, the technical solution of the invention is as follows:
A kind of metalization technological process of pyrolytic graphite comprising step:
A) pyrolyzing graphite material is processed into specific part, forms matrix；
B) surface preparation is carried out to pyrolytic graphite matrix；
C) using vacuum arc deposition technology in pyrolytic graphite matrix surface deposited plating layer；
D) through the post-processing of coating, finished product is obtained.
The metalization technological process of the pyrolytic graphite, the b) step are:
1) pyrolytic graphite piece surface is polished: after 500 mesh, abrasive paper for metallograph polishing, ultrasonic wave is carried out with alcohol
Cleaning 2~4 minutes, is then carried out dehydrating using acetone, the impurity and greasy dirt on surface is removed with this；
2) in vacuum ion membrane plating tank, under vacuum degree≤9 × 10-3Pa, ion is carried out to pyrolytic graphite piece surface and is banged
It hits, bias 1000V adds 1 minute, and 400V adds 1 minute；
3) it then, is cleaned with Ar gas, between back bias voltage 350V~450V, the time 3 minutes or so；
4) recalescence light cleans: with Ar gas, between bias 800V~1000V, and the time 3 minutes or so.
The metalization technological process of the pyrolytic graphite, the c) step are:
1) high-purity Cr target is selected to carry out plating Cr film deposition to pyrolytic graphite piece surface, deposition parameter: voltage 150V~
Between 250V, the time 20 minutes or so；
2) select high-purity N i target to deposit Ni film on newly formed Cr film again, deposition parameter: voltage 100V~200V it
Between, the time 30~50 minutes.
The metalization technological process of the pyrolytic graphite, the d) step are:
1) it by the pyrolytic graphite part after depositional coating, is put into hydrogen furnace, under hydrogen protection, is slowly heated to 850
DEG C~1000 DEG C, 5 minutes or so are kept the temperature, then furnace cooling；
2) after coming out of the stove, finished product is obtained；
3) fabricated part is put into thermo-humidistat cabinet and is saved, prevent from aoxidizing and polluted.
The metalization technological process of the pyrolytic graphite, the c) step, first with Cr target in pyrolytic graphite matrix table
Then Ni target as sputter is used in face bottoming, the film thickness of Cr film and Ni film is with the control of activity duration length, to guarantee securely to tie with matrix
It closes and is connect with other metals.
A kind of welding method of the metallization pyrolytic graphite is:
A) component that pyrolytic graphite part and needs weld is placed in hydrogen furnace, is carried out under hydrogen protection；
B) solder used in is silver-copper brazing alloy；
C) its welding condition are as follows: welding temperature is 810 DEG C~820 DEG C, heat preservation 3~after five minutes, it is naturally cooling to
200 DEG C or less；
D) it is lower than 50 DEG C to temperature, takes out weldment and get product.
The welding method of the metallization pyrolytic graphite, the silver-copper brazing alloy, copper content is between 72-28%.
The metallization process and welding method of a kind of graphite of the invention, using vacuum ionic coating technology in pyrolytic graphite base
Cr film and Ni film is deposited in body surface face, to be modified to pyrolytic graphite surface, allows pyrolytic graphite and ceramics or other gold
Category is reliably welded, and realizes hermetic seal, the development of microwave electron tube is greatly facilitated.
Detailed description of the invention
Fig. 1 is the nucleation and growth course schematic diagram of pyrolytic graphite deposition.
Specific embodiment
The metallization process and welding method of a kind of graphite of the invention, main contents include:
1, the method for metallising and technological parameter of pyrolytic graphite.
The method of pyrolytic graphite metallization carries out the surface deposition of pyrolytic graphite using vacuum arc deposition technology.Ion
Plating is to ionize the plating material particle fraction being evaporated under the conditions of low pressure discharge, forms ion, atom, molecule and other
Neutral particle group bombards using diffusion and electric field action, is deposited on the matrix (workpiece) for being applied with back bias voltage, Huo Zheyu
Substrate is nearby activated, is decomposed, the reaction gas of ionization interacts, and goes out the technology of compound film in deposition on substrate.Multi sphere
Ion plating category physical gas phase deposition technology has ionization level high, and ion energy is big, and deposition rate is high, adhesive force is good, film layer causes
Feature close, easily controllable, adaptability is wide.Most Metal and Alloy materials can be deposited, are widely used in film deposition.
It needs to carry out surface preparation to pyrolytic graphite matrix before deposition, specifically include that
1) pyrolytic graphite is processed into specific part, piece surface is polished, and carries out ultrasonic cleaning 2 using alcohol
It to 4 minutes, is then carried out dehydrating using acetone, the impurity and greasy dirt on surface is removed with this；
2) ion bombardment is carried out to material surface, so that vacuum degree≤9 of vacuum chamber × 10-3Pa；The cleaning of Ar gas, negative bias
Press 350V between 450V, the time 3 minutes or so；Aura cleaning: Ar gas, bias 800V is between 1000V, a 3 minutes time left side
It is right；
3) high-purity Cr target is selected to carry out plating Cr film deposition to pyrolytic graphite surface, deposition parameter selects voltage 150V extremely
Between 250V, the time 20 minutes or so；
4) Ni film is deposited on the basis of selecting high-purity N i target in newly formed Cr film, deposition parameter selects 100V to 200V
Between, the time 30 to 50 minutes；
5) post-depositional film layer needs to carry out postprocessing working procedures appropriate, mainly in hydrogen furnace, is slowly heated to 850
DEG C to 1000 DEG C, 5 minutes are kept the temperature, then furnace cooling, using this postprocessing working procedures is mainly to increase the attachment of film layer and matrix
Power enables film layer to be firmly combined with matrix；
6) it needs for the part after plating to be put into thermo-humidistat cabinet after coming out of the stove and save, prevent from aoxidizing and pollute.
2, the connection side of pyrolytic graphite and metal material (material can be commonly cut down in the electron tube that the present invention uses)
Method and technological parameter.
The connection for being mainly after pyrolytic graphite metallization and can commonly cutting down metal material in electron tube, can cut down material
Surface needs to plate Ni pretreatment process, this is technique more conventional together.The mainly optimization of welding condition.
1) using welding under hydrogen shield, welding process is used in program-controlled hydrogen the welding method of pyrolytic graphite and metal material
It is carried out in steam stove；
2) using AgCu (72-28%) solder common in electron tube preparation process as connection solder；
3) since (anisotropy is pyrolyzed graphite: the face a-b 1.8x10-6 to the coefficient of expansion of pyrolytic graphite at room temperature；The face C
23.4x10-6；Isotropism pyrolytic graphite: 7.7x10-6) with can cut down material (about 1.4x10-6 at 100 DEG C, at 600 DEG C about
Coefficient of expansion 10.94x10-6) has differences, and the heating and temperature lowering curve in welding process select relatively slow parameter, makes
Heating rate≤20 DEG C/min is obtained, 3 to 5 minutes need to be kept the temperature between 800 DEG C~830 DEG C after solder fusing, then can drop naturally
Temperature, hereinafter, to temperature lower than 50 DEG C, can take out weldment to 200 DEG C.
Embodiment:
1. a pair pyrolytic graphite matrix pre-processes:
1) 500 mesh abrasive paper for metallograph are polished, and alcohol ultrasonic cleaning 3 minutes, acetone dehydration；
2) vacuumizing makes the vacuum degree in multiple arc vacuum ionic plating tank reach 9 × 10-3Pa；
3) cleaned using aura: Ar gas, bias 1000V add 1 minute；
4) icon bombardment cleaning: Ar gas is carried out, back bias voltage 400V, 1 minute；
2. carrying out the deposition of transition film layer (Cr layers) and superficial film (Ni layers):
1) Cr film deposition uses parameter: voltage 200V, and 20 minutes；
2) Ni film deposition uses parameter: voltage 150V, and 40 minutes；
3. pair coating post-processes:
1) in hydrogen furnace, with 10 DEG C/min of heating rate, 950 DEG C is heated to, keeps the temperature 5 minutes, then furnace cooling；
2) it needs for the part after plating to be put into thermo-humidistat cabinet after coming out of the stove and save.
4. the welding of pyrolytic graphite and metal material:
1) material surface can be cut down and carry out conventional electroplated Ni processing；
2) using welding under hydrogen shield, welding process carries out welding method in program-controlled hydrogen furnace；
3) use solder for AgCu (72-28%) solder；
4) welding condition: heating rate≤10 DEG C/min, keep the temperature 3 minutes, then can drop naturally by 810 DEG C~820 DEG C
Temperature is to 200 DEG C or less；
5) it is lower than 50 DEG C to temperature, takes out weldment.
So far, the metallization process of pyrolytic graphite of the invention and welding process terminate, can be with the operation of this solution process
Obtain the soldering good seam of effect.
Claims (6)
1. a kind of metalization technological process of pyrolytic graphite, which is characterized in that comprising steps of
A) pyrolyzing graphite material is processed into specific part, forms matrix；
B) surface preparation is carried out to pyrolytic graphite matrix；
C) using vacuum arc deposition technology in pyrolytic graphite matrix surface deposited plating layer；
D) through the post-processing of coating, finished product is obtained.
2. the metalization technological process of pyrolytic graphite as described in claim 1, which is characterized in that the b) step is:
1) pyrolytic graphite piece surface is polished: after 500 mesh, abrasive paper for metallograph polishing, ultrasonic cleaning 2 is carried out with alcohol
It~4 minutes, is then carried out dehydrating using acetone, the impurity and greasy dirt on surface is removed with this；
2) in vacuum ion membrane plating tank, under vacuum degree≤9 × 10-3Pa, ion bombardment is carried out to pyrolytic graphite piece surface,
Bias 1000V adds 1 minute, and 400V adds 1 minute；
3) it then, is cleaned with Ar gas, between back bias voltage 350V~450V, the time 3 minutes or so；
4) recalescence light cleans: with Ar gas, between bias 800V~1000V, and the time 3 minutes or so.
3. the metalization technological process of pyrolytic graphite as described in claim 1, which is characterized in that the c) step is:
1) high-purity Cr target is selected to carry out plating Cr film deposition, deposition parameter: voltage 150V~250V to pyrolytic graphite piece surface
Between, the time 20 minutes or so；
2) high-purity N i target is selected to deposit Ni film on newly formed Cr film again, deposition parameter: between voltage 100V~200V, when
Between 30~50 minutes.
4. the metalization technological process of pyrolytic graphite as described in claim 1, which is characterized in that the d) step is:
1) by the pyrolytic graphite part after depositional coating, be put into hydrogen furnace, under hydrogen protection, be slowly heated to 850 DEG C~
1000 DEG C, 5 minutes or so are kept the temperature, then furnace cooling；
2) after coming out of the stove, finished product is obtained；
3) fabricated part is put into thermo-humidistat cabinet and is saved, prevent from aoxidizing and polluted.
5. a kind of welding method of metallization pyrolytic graphite as described in claim 1, which is characterized in that
A) component that pyrolytic graphite part and needs weld is placed in hydrogen furnace, is carried out under hydrogen protection；
B) solder used in is silver-copper brazing alloy；
C) its welding condition are as follows: welding temperature is 810 DEG C~820 DEG C, heat preservation 3~after five minutes, it is naturally cooling to 200 DEG C
Below；
D) it is lower than 50 DEG C to temperature, takes out weldment and get product.
6. the metalization technological process of pyrolytic graphite as described in claim 1, which is characterized in that the c) step first uses Cr target
Then material uses Ni target as sputter in pyrolytic graphite matrix surface bottoming, the film thickness of Cr film and Ni film with the control of activity duration length,
To guarantee to be firmly combined with matrix and be connect with other metals；The silver-copper brazing alloy, copper content is between 72-28%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710437226.1A CN109023262A (en) | 2017-06-12 | 2017-06-12 | The metallization process and welding method of graphite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710437226.1A CN109023262A (en) | 2017-06-12 | 2017-06-12 | The metallization process and welding method of graphite |
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| CN109023262A true CN109023262A (en) | 2018-12-18 |
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ID=64629150
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| CN201710437226.1A Withdrawn CN109023262A (en) | 2017-06-12 | 2017-06-12 | The metallization process and welding method of graphite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110195211A (en) * | 2019-05-09 | 2019-09-03 | 西安交通大学 | A kind of preparation method of controllable polymorphic type chromium carbide modified graphite |
| CN112091375A (en) * | 2020-09-14 | 2020-12-18 | 武汉育辰飞光电科技有限公司 | Process for solving oxidation problem of resistance seal welding by adding nitrogen |
| CN112708854A (en) * | 2020-12-19 | 2021-04-27 | 合肥开泰机电科技有限公司 | Vacuum coating structure for large-area brazing |
-
2017
- 2017-06-12 CN CN201710437226.1A patent/CN109023262A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110195211A (en) * | 2019-05-09 | 2019-09-03 | 西安交通大学 | A kind of preparation method of controllable polymorphic type chromium carbide modified graphite |
| CN110195211B (en) * | 2019-05-09 | 2022-02-22 | 西安交通大学 | Preparation method of controllable multi-type chromium carbide modified graphite |
| CN112091375A (en) * | 2020-09-14 | 2020-12-18 | 武汉育辰飞光电科技有限公司 | Process for solving oxidation problem of resistance seal welding by adding nitrogen |
| CN112708854A (en) * | 2020-12-19 | 2021-04-27 | 合肥开泰机电科技有限公司 | Vacuum coating structure for large-area brazing |
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Application publication date: 20181218 |