CN105689699B - A kind of process units and technique for producing hypoxemia dusty material - Google Patents
A kind of process units and technique for producing hypoxemia dusty material Download PDFInfo
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- CN105689699B CN105689699B CN201610055174.7A CN201610055174A CN105689699B CN 105689699 B CN105689699 B CN 105689699B CN 201610055174 A CN201610055174 A CN 201610055174A CN 105689699 B CN105689699 B CN 105689699B
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- reduction furnace
- crucible
- dusty material
- furnace tube
- hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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Abstract
The invention provides a kind of process units and technique for producing hypoxemia dusty material, including vertical vacuum tube furnace, the reduction furnace tube of insertion vertical vacuum tube furnace top and bottom is vertically installed in vertical vacuum tube furnace, the bottom of reduction furnace tube is connected with hydrogen gas tank and nitrogen pot, and the top of reduction furnace tube is connected with gas recovery pipe；Sample rack is installed in reduction furnace tube, the crucible for holding dusty material is placed with sample rack, described crucible includes the crucible body of both ends open, crucible body bottom is arranged on bin stock bottom plate, and multiple gas passages being evenly arranged of insertion bin stock bottom plate are machined with bin stock bottom plate；The inner chamber of described crucible body is less than the bottom internal diameter of crucible body for frustum and the top internal diameter of crucible body.There is provided vertical reduction furnace tube, coordinates with crucible, adds the contact area of hydrogen and dusty material, improve reduction efficiency so that hydrogen consumption is few, reduces production cost.
Description
Technical field
The invention belongs to field of powder material, is related to hypoxemia dusty material, and in particular to one kind produces hypoxemia dusty material
Process units and technique.
Background technology
CuCr alloys are the contact materials for being widely used in manufacture vacuum circuit breaker both at home and abroad.CuCr alloy raw materials Cr
The height of the quality of powder, particularly oxygen content is the deciding factor for influenceing CuCr alloy mass down to end-use properties.
At present, China using electrolysis the methods of obtained Cr powder oxygen content it is high, typically in more than 5000ppm.Use this
Kind of Cr powder, no matter with the reduction of Vacuum Heat carbon or vacuum sintering method, the oxygen content of obtained CuCr alloys is very high, generally
2000ppm or so.The contact manufactured with this hyperoxia CuCr alloys, vacuum interrupter can be made in manufacture, storage and using process
Middle vacuum degradation.In order to based on the CuCr alloys that hypoxemia is produced with domestic raw material, it is necessary to first to hyperoxia Cr powder
Reduction treatment is carried out, reduces the oxygen content of Cr powder as far as possible.Although the method for reducing Cr powder is a lot, such as with high-purity H2 reduction, use
Al etc. is living to dial metal reduction, the reduction of Vacuum Heat carbon etc..But how most economical most effectively to select suitable method to obtain satisfied
Effect, it is always the key problem in technology for preparing Cu-Cr alloy contact materials.
In the prior art, the method that oxygen content in power reduces mainly has：
(A) hot carbon reduction method：The technique mixes powder with appropriate graphite powder, then carries out heating treatment, obtains oxygen
The relatively low powder of content, this method technique is simple, and cost is low, but can not produce high-purity powder, and the addition of graphite powder is not
Good control, graphite can not be totally consumed in heat treatment process, have residual impurity to cause the purity of powder situation not up to standard.
(B) hydrogen reduction method：This method can be used for the dusty material for producing low oxygen content, but hydrogen density only has
0.0899g/L, when hydrogen is flowed into common box, tube furnace, gas can cause stove because be flowed out along furnace wall the reason for density
The problems such as interior H2 contacts deficiency with dusty material, and hydrogen consumption is big, and reduction efficiency is low, and production cost is high.
In summary, existing hydrogen reducing law technology is used for the dusty material for producing low oxygen content, faces low production efficiency,
Gas consumption is big, the problem such as manufacturing cost height.
The content of the invention
In view of the deficienciess of the prior art, it is an object of the present invention to provide a kind of life for producing hypoxemia dusty material
Device and technique are produced, hydrogen reduction method is solved and produces that hypoxemia powder efficient utilization is low, and consumption is big, the technical barrier such as production cost height.
It is achieved in order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of process units for producing hypoxemia dusty material, including vertical vacuum tube furnace, erect in vertical vacuum tube furnace
To the reduction furnace tube for being provided with insertion vertical vacuum tube furnace top and bottom, bottom and hydrogen gas tank and the nitrogen of reduction furnace tube
Tank is connected, and the top of reduction furnace tube is connected with gas recovery pipe；
Sample rack is installed in reduction furnace tube, the crucible for holding dusty material is placed with sample rack,
Described crucible includes the crucible body of both ends open, and crucible body bottom is arranged on bin stock bottom plate, processed on bin stock bottom plate
There are multiple gas passages being evenly arranged of insertion bin stock bottom plate；
The inner chamber of described crucible body is less than in the bottom of crucible body for frustum and the top internal diameter of crucible body
Footpath.
The present invention also has following distinguishing feature：
Preferably, the taper of the inner chamber of crucible body is 20 °~60 °.
Preferably, a diameter of 0.01mm~0.02mm of gas passage.
A kind of crucible for producing hypoxemia dusty material, includes the crucible body of both ends open, and crucible body bottom is arranged on
On bin stock bottom plate, on bin stock bottom plate on be machined with insertion bin stock bottom plate multiple gas passages being evenly arranged；
The inner chamber of described crucible body is less than in the bottom of crucible body for frustum and the top internal diameter of crucible body
Footpath.
T-slot is additionally provided with described bin stock bottom plate, the bottom of crucible body is coordinated by T-slot is arranged on bin stock bottom
Detachable location and installation is realized on plate.
A kind of production technology for producing hypoxemia dusty material, the production technology use hydrogen reduction method, it is characterised in that：Should
Production technology uses process units as described above.
Described production technology specifically includes following steps：
Step 1, dusty material is dried, be then charged into crucible, sample rack crucible being placed in reduction furnace tube
On, vacuumized in reduction furnace tube, then pass to hydrogen, then vacuumize again；
Step 2, vertical vacuum tube furnace heating heating so that the environment temperature in reduction furnace tube reaches 400~1500
DEG C, 2~3 hours are incubated, room temperature is then naturally cooling to, continues to be passed through hydrogen 2~3 hours, then pass to nitrogen 0.5 hour,
Obtain hypoxemia dusty material.
Described dusty material is chromium powder powder material or copper powder powder material.
The oxygen volume content of described hypoxemia dusty material is less than or equal to 350ppm.
In described step one, the pressure after being vacuumized in reduction furnace tube is less than or equal to -0.01MPa, and hydrogen is passed through shrinkage
For 2L/min, continue half an hour.
In described step two, the heating rate in former boiler tube is 250~360 DEG C/h.
In described step two, air pressure is in 1.2~1.3 standard atmospheric pressures in stove when hydrogen is passed through in former boiler tube.
The present invention compared with prior art, has the following technical effect that：
The process units of the present invention is provided with vertical reduction furnace tube, coordinates with crucible, adds hydrogen and dusty material
Contact area, improve reduction efficiency so that hydrogen consumption is few, reduces production cost.
The crucible of the present invention is used for the contact area for increasing hydrogen and dusty material, by changing the taper of crucible body,
The reduction requirement to different size dusty material can be achieved.It is applied widely, there is powdered, the granular substance of certain fluidity
Material.
The production technology of the present invention coordinates process units, has device simple, easily operated, stable and reliable for performance, adapts to
The features such as property is strong.
Brief description of the drawings
Fig. 1 is the overall structure diagram of the present invention.
Fig. 2 is the complete section structural representation of the crucible of the present invention.
Fig. 3 is the overlooking the structure diagram of the bin stock bottom plate of the present invention.
The implication of each label is in figure：1- vertical vacuum tube furnaces, 2- reduction furnace tubes, 3- hydrogen gas tanks, 4- nitrogen pots, 5-
Gas recovery pipe, 6- sample racks, 7- dusty materials, 8- crucibles, (8-1)-crucible body, (8-2)-bin stock bottom plate, (8-
3)-gas passage, (8-4)-T-slot.
Explanation is further explained in detail to the particular content of the present invention with reference to embodiments.
Embodiment
Specific embodiment of the invention given below is, it is necessary to which explanation is that the invention is not limited in implement in detail below
Example, all equivalents done on the basis of technical scheme each fall within protection scope of the present invention.
Embodiment 1：
The present embodiment provides a kind of crucible for producing hypoxemia dusty material, includes the crucible body 8-1 of both ends open, crucible
Body 8-1 bottoms are arranged on bin stock bottom plate 8-2, and insertion bin stock bottom plate 8-2 multiple uniform cloth are machined with bin stock bottom plate 8-2
The gas passage 8-3 put；
Described crucible body 8-1 inner chamber is less than crucible body 8-1 for frustum and crucible body 8-1 top internal diameter
Bottom internal diameter.
T-slot 8-4 is additionally provided with bin stock bottom plate 8-2, crucible body 8-1 bottom is coordinated by T-slot 8-4 to be arranged on
Detachable location and installation is realized on bin stock bottom plate 8-2.The taper of crucible body 8-1 inner chamber is 20 °~60 °.Gas passage 8-3
A diameter of 0.01mm~0.02mm.
Embodiment 2：
As shown in Figure 1 to Figure 3, the present embodiment provides a kind of process units for producing hypoxemia dusty material, including vertical true
Empty tube furnace 1, it is characterised in that：The top of insertion vertical vacuum tube furnace 1 and bottom are vertically installed in vertical vacuum tube furnace 1
Reduction furnace tube 2, the bottom of reduction furnace tube 2 is connected with hydrogen gas tank 3 and nitrogen pot 4, and top and the gas of reduction furnace tube 2 return
Closed tube 5 is connected；
Sample rack 6 is installed in reduction furnace tube 2, the earthenware for holding dusty material 7 is placed with sample rack 6
Crucible 8, described crucible 8 is using the crucible for producing hypoxemia dusty material provided in embodiment 1.
Embodiment 3：
The present embodiment provides a kind of production technology for producing hypoxemia dusty material, and dusty material 7 is chromium powder powder material, the life
Production. art is using process units as described in example 2 above.Chromium powder powder material needs to be located in advance before entering in reduction furnace tube 2
Reason, specific preprocessing process are as follows：
It is 0.11% to weigh the oxygen volumetric concentration in Cr powder 100g, Cr powder, and particle diameter is 150 μm.Cr powder is put to box dry
In dry case, it is dried at a temperature of 50~80 DEG C, after being kept for 48~72 hours, obtains dried Cr powder.
Specific production technology comprises the following steps：
Step 1, dusty material 7 is dried, be then charged into crucible 8, the sample that crucible 8 is placed in reduction furnace tube 2 is put
Put on frame 6, vacuumized in reduction furnace tube 2, then pass to hydrogen, then vacuumize again, wherein：After being vacuumized in reduction furnace tube 2
Pressure be less than or equal to -0.01MPa, it is 2L/min that hydrogen, which is passed through speed, continue half an hour.
Step 2, the heating heating of vertical vacuum tube furnace 1 so that the environment temperature in reduction furnace tube 2 reaches 1000~
1500 DEG C, the heating rate in reduction furnace tube 2 is 250~360 DEG C/h, is incubated 2~3 hours, is then naturally cooling to room temperature, after
It is continuous to be passed through hydrogen 2~3 hours, wherein in the heating, during insulation and cooling, hydrogen is continually fed into, and reduce
Air pressure is 1.2~1.3 standard atmospheric pressures in stove when hydrogen is passed through in boiler tube 2, then passes to nitrogen 0.5 hour, obtains low
Oxygen dusty material.
Powder-product is taken out in blow-on, using the oxygen content in nitrogen oxygen analyzer analysed for powder, by test, oxygen volume content
350ppm is dropped to from 1100ppm.
Embodiment 4：
The present embodiment provides a kind of production technology for producing hypoxemia dusty material, and dusty material 7 is copper powder powder material, the life
Production. art is using process units as described in example 2 above.Copper powder powder material needs to be located in advance before entering in reduction furnace tube 2
Reason, specific preprocessing process are as follows：
It is 0.36% to weigh the oxygen volumetric concentration in Cu powder 100g, Cu powder, and particle diameter is 200 μm.Cu powder is put to box dry
In dry case, it is dried at a temperature of 50~80 DEG C, after being kept for 48~72 hours, obtains dried Cu powder.
Specific production technology comprises the following steps：
Step 1, dusty material 7 is dried, be then charged into crucible 8, the sample that crucible 8 is placed in reduction furnace tube 2 is put
Put on frame 6, vacuumized in reduction furnace tube 2, then pass to hydrogen, then vacuumize again, wherein：After being vacuumized in reduction furnace tube 2
Pressure be less than or equal to -0.01MPa, it is 2L/min that hydrogen, which is passed through speed, continue half an hour.
Step 2, the heating heating of vertical vacuum tube furnace 1 so that the environment temperature in reduction furnace tube 2 reaches 400~700
DEG C, the heating rate in reduction furnace tube 2 is 250~360 DEG C/h, is incubated 2~3 hours, is then naturally cooling to room temperature, continues to lead to
Enter hydrogen 2~3 hours, wherein in the heating, during insulation and cooling, be continually fed into hydrogen, and reduction furnace tube 2
Air pressure is 1.2~1.3 standard atmospheric pressures in stove when being inside passed through hydrogen, then passes to nitrogen 0.5 hour, obtains hypoxemia powder
Material.
Powder-product is taken out in blow-on, using the oxygen content in nitrogen oxygen analyzer analysed for powder, by test, oxygen volume content
260ppm is dropped to from 3600ppm.
Claims (4)
1. a kind of production technology for producing hypoxemia dusty material, the production technology uses hydrogen reduction method, it is characterised in that：The life
Production. art is using the process units for producing hypoxemia dusty material；
The described process units for producing hypoxemia dusty material, including vertical vacuum tube furnace (1), vertical vacuum tube furnace (1)
The interior vertical reduction furnace tube (2) for being provided with insertion vertical vacuum tube furnace (1) top and bottom, the bottom of reduction furnace tube (2) with
Hydrogen gas tank (3) and nitrogen pot (4) are connected, and the top of reduction furnace tube (2) is connected with gas recovery pipe (5)；
Sample rack (6) is installed in reduction furnace tube (2), is placed with sample rack (6) for holding dusty material (7)
Crucible (8), described crucible (8) includes the crucible body (8-1) of both ends open, and crucible body (8-1) bottom is arranged on storage
Expect on bottom plate (8-2), multiple gas passages being evenly arranged of insertion bin stock bottom plate (8-2) are machined with bin stock bottom plate (8-2)
(8-3)；
The inner chamber of described crucible body (8-1) is less than crucible body (8- for the top internal diameter of frustum and crucible body (8-1)
1) bottom internal diameter；
T-slot (8-4) is additionally provided with described bin stock bottom plate (8-2), the bottom of crucible body (8-1) passes through T-slot (8-4)
Coordinate to be arranged on bin stock bottom plate (8-2) and realize detachable location and installation；
Described production technology specifically includes following steps：
Step 1, dusty material (7) is dried, is then charged into crucible (8), crucible (8) is placed on the sample in reduction furnace tube (2)
On product rack (6), vacuumized in reduction furnace tube (2), then pass to hydrogen, then vacuumize again；
Described dusty material (7) is chromium powder powder material or copper powder powder material；
Step 2, vertical vacuum tube furnace (1) heating heating so that the environment temperature in reduction furnace tube (2) reaches 400~1500
DEG C, 2~3 hours are incubated, room temperature is then naturally cooling to, continues to be passed through hydrogen 2~3 hours, then pass to nitrogen 0.5 hour,
Obtain hypoxemia dusty material；
The oxygen volume content of described hypoxemia dusty material is less than or equal to 350ppm.
2. production technology as claimed in claim 1, it is characterised in that：In described step one, vacuumized in reduction furnace tube (2)
Pressure afterwards is less than or equal to -0.01MPa, and it is 2L/min that hydrogen, which is passed through speed, continues half an hour.
3. production technology as claimed in claim 1, it is characterised in that：In described step two, the heating in reduction furnace tube (2)
Speed is 250~360 DEG C/h.
4. production technology as claimed in claim 1, it is characterised in that：In described step two, hydrogen is passed through in reduction furnace tube (2)
Air pressure is 1.2~1.3 standard atmospheric pressures in stove during gas.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610055174.7A CN105689699B (en) | 2016-01-27 | 2016-01-27 | A kind of process units and technique for producing hypoxemia dusty material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610055174.7A CN105689699B (en) | 2016-01-27 | 2016-01-27 | A kind of process units and technique for producing hypoxemia dusty material |
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| Publication Number | Publication Date |
|---|---|
| CN105689699A CN105689699A (en) | 2016-06-22 |
| CN105689699B true CN105689699B (en) | 2018-01-23 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321558A (en) * | 2000-04-30 | 2001-11-14 | 北京科技大学 | Preparation process of superfine carbide powder by direct reduction carbonization in pipe furnace |
| CN103084568A (en) * | 2012-12-05 | 2013-05-08 | 江门富祥电子材料有限公司 | Device used for reducing tantalum powder by using magnesium to reduce oxygen content and provided with cooler and method for reducing tantalum powder by using magnesium to reduce oxygen content |
| CN204329631U (en) * | 2014-11-25 | 2015-05-13 | 北京矿冶研究总院 | Intermediate frequency furnace for sintering multiple volatile substances |
| CN204439488U (en) * | 2015-03-23 | 2015-07-01 | 中国矿业大学 | A kind of thermogravimetric analysis experiment table |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62247003A (en) * | 1986-04-21 | 1987-10-28 | Kobe Steel Ltd | Method and apparatus for reducing metallic powder |
-
2016
- 2016-01-27 CN CN201610055174.7A patent/CN105689699B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321558A (en) * | 2000-04-30 | 2001-11-14 | 北京科技大学 | Preparation process of superfine carbide powder by direct reduction carbonization in pipe furnace |
| CN103084568A (en) * | 2012-12-05 | 2013-05-08 | 江门富祥电子材料有限公司 | Device used for reducing tantalum powder by using magnesium to reduce oxygen content and provided with cooler and method for reducing tantalum powder by using magnesium to reduce oxygen content |
| CN204329631U (en) * | 2014-11-25 | 2015-05-13 | 北京矿冶研究总院 | Intermediate frequency furnace for sintering multiple volatile substances |
| CN204439488U (en) * | 2015-03-23 | 2015-07-01 | 中国矿业大学 | A kind of thermogravimetric analysis experiment table |
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