CN105821392B - The preparation method of tungsten resistance tube heater - Google Patents
The preparation method of tungsten resistance tube heater Download PDFInfo
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- CN105821392B CN105821392B CN201610273694.5A CN201610273694A CN105821392B CN 105821392 B CN105821392 B CN 105821392B CN 201610273694 A CN201610273694 A CN 201610273694A CN 105821392 B CN105821392 B CN 105821392B
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/02—Local etching
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/40—Heating elements having the shape of rods or tubes
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Resistance Heating (AREA)
Abstract
The invention belongs to reactor engineering technical field, discloses a kind of preparation method of the tungsten resistance tube heater for the outer power generation test of reactor.This method be using chemical vapor deposition and Wire EDM combination method it is prepared by tungsten resistance tube heater, including the step of be：The selection and surface preparation of basal body pipe, chemical vapor deposition tungsten coating, the Precision Machining of tungsten red copper multiple tube, chemolysis, ultrasonic cleaning and the annealing steps of basal body pipe.This method can solve the problem that the tungsten resistance tube of intensive fluting prepares problem, and the tungsten resistance tube heater purity height of preparation, residual stress are small.
Description
Technical field
The invention belongs to reactor engineering technical field, and in particular to a kind of tungsten electricity for the outer power generation test of reactor
Hinder the preparation method of pipe heater.
Background technology
Need to make using tungsten electric heater in the out-pile power generation test of certain high-temperature reactor power supply fuel element development stage
For heat release part, to simulate the heat release operating mode in nuclear fuel active region temperature field.Wherein tungsten resistance tube heater is tungsten electric heater
Crucial high-temperature component, and most complicated and most important part in tungsten electric heater manufacturing process.Tungsten resistance tube heater is
Circumference is provided with the path thin-wall tungsten pipe structure of resistance groove, and diameter only has more than ten millimeter, and wall thickness only has 0.3~0.5mm, in addition also
Circumferentially to open resistance groove.A diameter of 14mm of tungsten resistance tube heater as needed for a certain high-temperature reactor, wall thickness only have
0.4mm, in order to increase resistance value, it is necessary to tungsten pipe surface process vertically 126 width be 0.3mm resistance groove, every
Resistance groove is circumferentially divided into three sections, leaves 2mm linkage section between every section, circumferentially mutually wrong between adjacent two resistance grooves
60 ° of angles, spacing 2mm.Because the fusing point of tungsten material is high, hardness and fragility are all very big, can not use conventional machining process
Cutting is realized, therefore, the complexity of structure and the particularity of material bring great difficulty to the manufacture of tungsten resistance tube heater,
The preparation method of tungsten resistance tube heater is problem generally acknowledged in the world.
Traditional tungsten pipe manufacturing method includes extrusion, hubbing, spinning process, tungsten coiled sheet connect, powder metallurgy, vapour deposition
Deng.
Extrusion refers to the pipe after heating being put into recipient, and extrusion die, the other end are placed in one end of recipient
Apply with pressure, force metal to be flowed out from nib, it is produced section decrement, the increased plastic deformation method of length.
Hubbing refers under external force, force metal stock by nib, to obtain respective shapes, gauge articles
Plastic processing method.Through carrying out the drawing of tungsten pipe after extruding and annealing, typically using the bimetallic pulling method of deformable plug,
When this farad stretches tungsten pipe the diameter of tungsten pipe and wall thickness can compression simultaneously, but tube wall thickness is uneven.
Spinning process is that hollow blank is fixed on the mould of spinning machine, while blank is with lathe main axis, is used
Spinning roller stresses on blank, is allowed to produce local plastic deformation, makees jointly in the feed motion of spinning roller and the rotary motion of blank
Under, local plastic deformation is progressively expanded to all surfaces of blank, and be close to mould, the spinning for completing pipe fitting adds
Work.A diameter of 9~12mm is produced on roller type or steel-ball type thermal spinning press at present, wall thickness is 0.25~0.3mm, length
Seamless W pipe more than 600mm, resistance of deformation is big during spinning tungsten pipe, selects the pass that suitable plug material is tungsten pipe rotary pressure technology
Key, it is necessary to try to prevent that plug softens in spinning process.
Tungsten coiled sheet connection, which produces tungsten pipe heater and tungsten plate Mass Cracking easily occurs, scraps, and recovery rate is low, the pipe shape being rolled into
Shape is non-round, the problems such as the radial strength difference of pipe.In addition, although pipe crimping can be controlled strictly with the wall thickness tolerance of tungsten plate, cigarette
Afterwards because the influence of weld seam, the uniformity of pipe wall thickness are undesirable.
The obtained tungsten product tissue of powder metallurgic method is not fine and close, is also easy to produce pin hole, and is cold-pressed green relative density and is only
60%~65%, volume contraction is up to 30%~40% in subsequent high temperature sintering process, causes thin-walled or Irregular Shaped Parts
The problems such as producing gross distortion, cracking or avalanche.And then the production cycle was long, forming efficiency is low the methods of physical vapour deposition (PVD), add
Work cost is sufficiently expensive.
Chemical vapor deposition is a kind of method of vapor-phase growing for preparing material, and it is one or more of compounds, simple substance
Gas is passed through the reative cell for being placed with base material, by space gas-phase chemical reaction on matrix surface depositing solid films or coating
Technology.
The above method fails to disclose how the method for preparing tungsten pipe especially tungsten resistance heating tube.
The content of the invention
(1) goal of the invention
According to the problems of prior art, a kind of tungsten resistance tube purity provided by the invention is high, stress is small, cutting
Technique is fine, the preparation method of tungsten resistance tube heater simple to operate.
(2) technical scheme
In order to solve the problems of prior art, technical scheme provided by the invention is as follows：
The preparation method of tungsten resistance tube heater, this method are combined using chemical vapor deposition and Wire EDM
Method is prepared to tungsten resistance tube heater, and it comprises the following steps：
(1) selection and surface preparation of basal body pipe
It is more than required tungsten resistance tube heating as basal body pipe, the length of copper tube from the copper tube that wall thickness is 0.8~1mm
The center section of the length of body, wherein copper tube is to chemical vapor deposition tungsten coating；The external diameter of copper tube center section and institute
Need the internal diameter of tungsten resistance tube consistent and the external diameter at copper tube both ends is more than the external diameter of center section；
(2) chemical vapor deposition tungsten coating
Whole copper tube is stood on vertically in evacuated chemical vapor deposition unit, then pass to WF6And H2Gas
Reduction reaction is carried out, goes out high-purity tungsten coating in copper tube outside deposition, the wherein thickness of tungsten coating is more than tungsten electricity to be prepared
The thickness of pipe is hindered, obtains tungsten-red copper multiple tube；
The method that the chemical vapor deposition processes use interior heating, penetrates electrical heating wire with to copper tube inside copper tube
Outer surface heat, and control red copper tube outer surface temperature be 490~680 DEG C；
(3) Precision Machining of tungsten-red copper multiple tube
The tungsten that step (2) is obtained-red copper multiple tube is cut according to required length, then using the inner circle of copper tube as base
Standard, support plug is penetrated, both ends endoporus is loaded fixation with one heart, the tungsten pipe using alundum wheel to tungsten-red copper composite pipe
Cylindrical carry out fine gtinding, reaches requirement of the tungsten resistance tube to wall thickness；
Workpiece after grinding cuts out resistance vertically using Wire EDM mode in the compound pipe surface of tungsten-red copper
Groove, each electroplating bath circumferential angle and position are determined using dividing head in cutting process；
(4) chemolysis of basal body pipe
The chemolysis is divided into two steps,
Step is 1.：Using the nitric acid that volume fraction is 40% by the red copper basal body pipe corrosion in tungsten-red copper multiple tube；
Step is 2.：Boiled and washed with the sodium hydroxide solution heating of volume fraction 20%；
(5) it is cleaned by ultrasonic
The tungsten resistance tube that step (4) obtains is cleaned by ultrasonic using deionized water, dehydration of alcohol is utilized after cleaning and is dried up；
(6) anneal
Stress relief annealing process is carried out to tungsten resistance tube heater in vacuum high temperature furnace, to reduce the remnants of tungsten resistance tube
Stress, obtain required tungsten resistance tube heater；Vacuum is better than 5 × 10 wherein in vacuum high temperature furnace-3Pa, temperature be 800~
1000 DEG C, time 30min.
Preferably, copper tube described in the step (1) is also needed before chemical vapor deposition tungsten coating by annealing
Step.
Preferably, electrical heating wire is tungsten bar described in the step (2), positioned at the radial center position of red copper basal body pipe.
Preferably, WF described in step (2)6And H2Gas is high-purity gas of the purity more than 99.9%.
Preferably, the Wire EDM described in step (3) is to cut out 126 vertically in the compound pipe surface of tungsten-red copper
Road width 0.3mm resistance groove, every resistance groove circumferentially divide equally three sections, 2mm linkage sections are left between every section, are in circumferentially
Three-point support structure, cutting position between adjacent two resistance grooves circumferentially mutual wrong 60 ° of angles, spacing 2mm.
Preferably, carried out finely in the step (3) using alundum wheel is cylindrical to the tungsten pipe of tungsten-red copper composite pipe
The cutting output of grinding is 0.05mm/ times.
Preferably, the step in step (4) is 1. corrosion at room temperature 30~60 minutes using nitric acid corrosion.
Preferably, the heating of the step in step (4) 2. boils that to wash existed using the sodium hydroxide solution of volume fraction 20%
Heating, which is boiled, under conditions of 100 DEG C washes 10 minutes.
(3) beneficial effect
The preparation method of the tungsten resistance tube heater provided using the application, solves the thin wall type high purity tungsten of intensive fluting
Resistance tube prepares problem, specifically has the beneficial effect that：
(1) tungsten resistance tube heater is prepared using chemical gaseous phase depositing process, the tungsten pipe purity of preparation is high.
(2) it is 0.8~1mm red copper matrix tube outer surfaces by the way that tungsten is deposited on into wall thickness, is advantageous to follow-up tungsten resistance tube
Precision Machining.By the method for chemolysis and process conditions by copper tube corrosion without by tungsten corrosion, there is unstressed, nothing
Pollution, matrix remove the advantages of thorough and simple to operate, avoid the processing difficulties problem brought because tungsten hardness and brittleness are big.
The wall thickness selection of copper tube and the technical scheme that applicant considers mechanical strength and stress is made, copper tube
Wall thickness, which is thinner than 0.8mm, can cause mechanical strength small；Wall thickness is more than 1mm then can produce stress in thermal expansion process to tungsten.
(3) heating process is interior heating in chemical vapor deposition processes, and heater strip is the tungsten bar positioned at matrix tube hub,
Heating is more uniform, is advantageous to chemical vapor deposition and forms the equally distributed tungsten coating of thickness.
(4) annealing process step has all been carried out to basal body pipe and tungsten pipe in tungsten resistance tube preparation process, reduce further
The stress of tungsten resistance tube heater.
Brief description of the drawings
Fig. 1 is the cross-sectional view for the tungsten resistance tube heater that embodiment 1 provides；Wherein 1 is resistance groove.
Embodiment
Below in conjunction with specific embodiment and Figure of description, the present invention is further elaborated.
Embodiment 1
Tungsten resistance tube heater needed for a certain high-temperature reactor, as shown in figure 1, a diameter of 14mm, wall thickness 0.4mm,
In order to increase resistance value, it is necessary to process the resistance groove that 126 width are 0.3mm, every resistance groove vertically in tungsten pipe surface
Three sections are circumferentially divided into, leaves 2mm linkage section between every section, circumferentially mutual wrong 60 ° of angles between adjacent two resistance grooves
Degree, spacing 2mm, is prepared, this method is to utilize chemical gas using method provided by the invention to the tungsten resistance tube heater
Mutually the method for deposition and Wire EDM is prepared to tungsten resistance tube heater, and it comprises the following steps：
(1) selection and surface preparation of basal body pipe
From the copper tube that wall thickness is 0.8mm as basal body pipe, the length of copper tube is more than the length of required tungsten resistance tube,
Wherein the center section of copper tube is to chemical vapor deposition tungsten coating；The external diameter of copper tube center section and required tungsten resistance tube
Internal diameter is consistent and the external diameter at copper tube both ends is more than the external diameter of center section；
(2) chemical vapor deposition tungsten coating
Copper tube is made annealing treatment, whole copper tube stood on vertically in evacuated chemical vapor deposition unit,
Then pass to the %WF that purity is 99.956And H2Gas carries out reduction reaction, goes out high-purity tungsten coating in copper tube outside deposition,
Wherein the thickness of tungsten coating is more than the thickness of tungsten resistance tube to be prepared, obtains tungsten-red copper multiple tube；
The method that the chemical vapor deposition processes use interior heating, penetrates electrical heating wire with to copper tube inside copper tube
Outer surface heat, and control red copper tube outer surface temperature be 500 DEG C；
(3) Precision Machining of tungsten-red copper multiple tube
The tungsten that step (2) is obtained-red copper multiple tube is cut according to required length, then using the inner circle of copper tube as base
Standard, penetrate support plug, both ends endoporus be loaded fixation with one heart, using alundum wheel with the cutting output of 0.05mm/ times to tungsten-
The cylindrical carry out fine gtinding of tungsten pipe of red copper composite pipe, reaches requirement of the tungsten resistance tube to wall thickness；
Workpiece after grinding cuts out resistance vertically using Wire EDM mode in the compound pipe surface of tungsten-red copper
Groove, each electroplating bath circumferential angle and position are determined using dividing head in cutting process；Described Wire EDM be tungsten-
The compound pipe surface of red copper cuts out 126 width 0.3mm resistance groove vertically, and every resistance groove circumferentially divides equally three sections, often
2mm linkage sections are left between section, circumferentially in three-point support structure, the cutting position between adjacent two resistance grooves is circumferentially
Mutually 60 ° of angles of mistake, spacing 2mm.
(4) chemolysis of basal body pipe
The chemolysis is divided into two steps,
Step is 1.：By tungsten-red copper multiple tube using the nitric acid that volume fraction is 40% by red copper basal body pipe corrosion；In room temperature
Lower corrosion 30~60 minutes.
Step is 2.：Heat to boil under conditions of 100 DEG C using the sodium hydroxide solution of volume fraction 20% and wash 10 minutes.
(5) it is cleaned by ultrasonic
The tungsten resistance tube that step (4) obtains is cleaned by ultrasonic using deionized water, dehydration of alcohol is utilized after cleaning and is dried up；
(6) anneal
Stress relief annealing process is carried out to tungsten resistance tube heater in vacuum high temperature furnace, to reduce the remnants of tungsten resistance tube
Stress, obtain required tungsten resistance tube heater；Vacuum is better than 5 × 10 wherein in vacuum high temperature furnace-3Pa, temperature are 800 DEG C, when
Between be 30min.
Described in the step (1) preferably, electrical heating wire is tungsten bar described in the step (2), positioned at red copper matrix
The radial center position of pipe.
Embodiment 2
As different from Example 1, the wall thickness of basal body pipe is 1mm.Chemical vapor deposition processes control red copper tube outer surface
Temperature be 620 DEG C；Annealing temperature is 900 DEG C in step (6).
Embodiment 3
As different from Example 1, the wall thickness of basal body pipe is 0.9mm.Chemical vapor deposition processes control copper tube appearance
The temperature in face is 680 DEG C；Annealing temperature is 1000 DEG C in step (6).
Embodiment 4
A diameter of 18mm, wall thickness 0.5mm are prepared using method provided by the invention, tungsten pipe surface is processed vertically
Go out the resistance groove that 130 width are 0.4mm, every resistance groove is circumferentially divided into three sections, 2mm connection is left between every section
Section, circumferentially mutual wrong 60 ° of angles between adjacent two resistance grooves, spacing 3mm.
Claims (8)
1. the preparation method of tungsten resistance tube heater, it is characterised in that this method is to utilize chemical vapor deposition and wire electric discharge
The method that cutting combines is prepared to tungsten resistance tube heater, and it comprises the following steps：
(1) selection and surface preparation of basal body pipe
It is more than required tungsten resistance tube heater as basal body pipe, the length of copper tube from the copper tube that wall thickness is 0.8~1mm
The center section of length, wherein copper tube is to chemical vapor deposition tungsten coating；The external diameter of copper tube center section and required tungsten
The internal diameter of resistance tube is consistent and the external diameter at copper tube both ends is more than the external diameter of center section；
(2) chemical vapor deposition tungsten coating
Whole copper tube is stood on vertically in evacuated chemical vapor deposition unit, then pass to WF6And H2Gas is carried out
Reduction reaction, go out high-purity tungsten coating in copper tube outside deposition, the wherein thickness of tungsten coating is more than tungsten resistance tube to be prepared
Thickness, obtain tungsten-red copper multiple tube；
The method that the chemical vapor deposition processes use interior heating, penetrates electrical heating wire with to copper tube appearance inside copper tube
Face heat, and control red copper tube outer surface temperature be 490~680 DEG C；
(3) Precision Machining of tungsten-red copper multiple tube
The tungsten that step (2) is obtained-red copper multiple tube is cut according to required length, then on the basis of the inner circle of copper tube, is worn
Enter to support plug, both ends endoporus be loaded fixation with one heart, using alundum wheel it is cylindrical to the tungsten pipe of tungsten-red copper composite pipe enter
Row fine gtinding, reach requirement of the tungsten resistance tube to wall thickness；
Workpiece after grinding cuts out resistance groove vertically using Wire EDM mode in the compound pipe surface of tungsten-red copper,
In cutting process each electroplating bath circumferential angle and position are determined using dividing head；
(4) chemolysis of basal body pipe
The chemolysis is divided into two steps,
Step is 1.：Using the nitric acid that volume fraction is 40% by the red copper basal body pipe corrosion in tungsten-red copper multiple tube；
Step is 2.：Boiled and washed with the sodium hydroxide solution heating of volume fraction 20%；
(5) it is cleaned by ultrasonic
The tungsten resistance tube that step (4) obtains is cleaned by ultrasonic using deionized water, dehydration of alcohol is utilized after cleaning and is dried up；
(6) anneal
Stress relief annealing process is carried out to tungsten resistance tube in vacuum high temperature furnace, obtains required tungsten resistance tube heater；
Wire EDM described in step (3) is to cut out 126 width 0.3mm vertically in the compound pipe surface of tungsten-red copper
Resistance groove, every resistance groove circumferentially divide equally three sections, 2mm linkage sections are left between every section, circumferentially in supported at three point knot
Structure, cutting position between adjacent two resistance grooves circumferentially mutual wrong 60 ° of angles, spacing 2mm.
2. the preparation method of tungsten resistance tube heater according to claim 1, it is characterised in that institute in the step (1)
State copper tube also needs by annealing process step before chemical vapor deposition tungsten coating.
3. the preparation method of tungsten resistance tube heater according to claim 1, it is characterised in that institute in the step (2)
It is tungsten bar to state electrical heating wire, positioned at the radial center position of red copper basal body pipe.
4. the preparation method of tungsten resistance tube heater according to claim 1, it is characterised in that WF described in step (2)6
And H2Gas is high-purity gas of the purity more than 99.9%.
5. the preparation method of tungsten resistance tube heater according to claim 1, it is characterised in that sharp in the step (3)
It it is 0.05mm/ times with the alundum wheel cutting output for carrying out fine gtinding cylindrical to the tungsten pipe of tungsten-red copper composite pipe.
6. the preparation method of tungsten resistance tube heater according to claim 1, it is characterised in that the step in step (4)
1. it is corrosion at room temperature 30~60 minutes using nitric acid corrosion.
7. the preparation method of tungsten resistance tube heater according to claim 1, it is characterised in that the step in step (4)
It is to heat to boil under conditions of 100 DEG C using the sodium hydroxide solution of volume fraction 20% to wash 10 points that 2. described heating, which is boiled and washed,
Clock.
8. the preparation method of tungsten resistance tube heater according to claim 1, it is characterised in that in step (6) at annealing
The vacuum of vacuum high temperature furnace is better than 5 × 10 during reason-3Pa, temperature are 800~1000 DEG C, time 30min.
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| CN201610273694.5A CN105821392B (en) | 2016-04-28 | 2016-04-28 | The preparation method of tungsten resistance tube heater |
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| CN201610273694.5A CN105821392B (en) | 2016-04-28 | 2016-04-28 | The preparation method of tungsten resistance tube heater |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962935A (en) * | 2006-12-08 | 2007-05-16 | 北京工业大学 | Process for preparing high-purity compact profile tungsten products |
| CN102592689A (en) * | 2012-02-06 | 2012-07-18 | 国核华清（北京）核电技术研发中心有限公司 | Composite material heating block, and manufacturing method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7964505B2 (en) * | 2005-01-19 | 2011-06-21 | Applied Materials, Inc. | Atomic layer deposition of tungsten materials |
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2016
- 2016-04-28 CN CN201610273694.5A patent/CN105821392B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962935A (en) * | 2006-12-08 | 2007-05-16 | 北京工业大学 | Process for preparing high-purity compact profile tungsten products |
| CN102592689A (en) * | 2012-02-06 | 2012-07-18 | 国核华清（北京）核电技术研发中心有限公司 | Composite material heating block, and manufacturing method and application thereof |
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