CN102921948B - Sintering technology for cemented carbide extrusion bar - Google Patents
Sintering technology for cemented carbide extrusion bar Download PDFInfo
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- CN102921948B CN102921948B CN201210512844.5A CN201210512844A CN102921948B CN 102921948 B CN102921948 B CN 102921948B CN 201210512844 A CN201210512844 A CN 201210512844A CN 102921948 B CN102921948 B CN 102921948B
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Abstract
The invention discloses a sintering technology for a cemented carbide extrusion bar. The sintering technology comprises four continuous processes of positive-pressure hydrogen dewaxing, partial-pressure sintering, high-pressure and high-temperature sintering, and cooling. At a normal temperature, hydrogen is filled into an empty sintering furnace, the furnace temperature is gradually boosted to 600 DEG C stage by stage in 490 minutes, the hydrogen is cut off, a mechanical pump is used for controlling the vacuum degree in the furnace to be about 10 pascals of the inner pressure of a sintering box, argon is then filled into the sintering box so as to ensure that the inner pressure of the sintering box is between 300 and 600 pascals, the furnace temperature is gradually increased to 1410 DEG C in 235 minutes stage by stage under the pressure of 300-600 pascals, the furnace is kept at the temperature of 1410 DEG C for 60 minutes, high-pressure argon of 60 bars is filled into the furnace for 20 minutes after the thermal insulation at 1410 DEG C is maintained for 30 minutes, the high pressure of the argon is maintained for 10 minutes, the pressure maintaining and temperature maintaining are finished at the same time, and then, the furnace begins to be cooled. Under the condition of fully filling the high-pressure argon in the furnace, the furnace is naturally cooled to 900 DEG C and is then quickly cooled to below 50 DEG C after about 300 minutes. The sintering technology can be used for effectively improving the bending percent of pass of the thin cemented carbide extrusion bars with the diameter of no more than phi 6 millimeters.
Description
Technical field
The present invention relates to a kind of sintering process of carbide alloy extruded bars, it can improve the crooked qualification rate of carbide alloy extruded rod, especially can improve the once friendship inspection qualification rate of thin footpath carbide alloy extruded bars.
Background technology
The in the situation that of diameter D≤Ф 6mm, there is the phenomenon that linearity first-time qualification rate is lower in the sintering of carbide alloy extruded bars conventionally.The forming agent of carbide alloy extruded rod mainly contains paraffin, cellulose etc., and this forming agent all can remove completely in the dewaxing of hydrogen malleation.But, in follow-up vacuum-sintering and pressure sintering, all there is more or less crooked phenomenon, wherein the extruded alloy bar ratio in thin footpath is maximum, and in pressure sintering furnace, sintering buckling problem is also particularly to give prominence to.This be because, in at present general alloy sintering technique, the forming agent of product removes after end, is all generally to enter the vacuum-sintering stage then in 1350 degree left and right, just to start to enter dividing potential drop sintering, be filled with the argon gas of minute pressure pressure, the evaporation of liquid phase cobalt while preventing sintering.Like this, in the vacuum-sintering stage of stove, carbide alloy extruded rod will be subject to the impact of the interior original paper of the stoves such as inboard wall of burner hearth, graphite heat-preservation cylinder and body of heater leakage, and the carbide alloy extruded rod rate of curving after sintering is improved greatly.
Summary of the invention
The sintering process that the object of this invention is to provide a kind of carbide alloy extruded bars, it can improve the crooked qualification rate of carbide alloy extruded rod, the once friendship inspection qualification rate of especially thin footpath carbide alloy extruded bars.
For this reason, the invention provides a kind of sintering process of carbide alloy extruded bars, it is characterized in that, this sintering process comprises hydrogen malleation dewaxing step, dividing potential drop sintering step, high pressure-temperature sintering step and cooling step successively,
In hydrogen malleation dewaxing step, under normal temperature condition, hydrogen is filled with in emptying sintering furnace, within first heating-up time of 480-500 minute, progressively, by stages furnace temperature is risen to the first heating-up temperature 590-610 degree, then turn off hydrogen, vacuum degree control in stove is arrived to sintering box internal pressure 9-11Pa;
At dividing potential drop sintering step, in graphite sintering box inside, start to be filled with argon gas, guarantee sintering box internal pressure 300-600Pa, under 300-600Pa pressure condition, through second heating-up time of 230-240 minute, be warmed up to progressively, stage by stage the second heating-up temperature 1400-1420 degree;
At high pressure-temperature sintering step, in the second heating-up temperature, be incubated the first temperature retention time 55-65 minute, after being incubated the second temperature retention time 25-35 minute, the second heating-up temperature is filled with high pressure argon gas 40-100bar, wherein filling the high pressure argon gas time is 1/3 of the first temperature retention time, and the high pressure dwell time is 1/6 of the first temperature retention time;
At cooling step, pressurize finishes simultaneously and begins to cool down with insulation, is full of under the condition of high pressure argon gas in stove, naturally cools to the first chilling temperature 890-910 degree, then 290-310 minute the first cool time, from the first chilling temperature, is chilled to soon below 50 degree.
Preferably, the cobalt content 5-15wt% of carbide alloy extruded bars.
Preferably, the first heating-up time was 490 minutes, and the first heating-up temperature is 600 degree; The second heating-up time was 235 minutes, and the first heating-up temperature is 1410 degree; The first temperature retention time is 60 minutes; The second temperature retention time is 30 minutes; Be filled with high pressure argon gas 60bar; Filling the high pressure argon gas time is 20 minutes; The high pressure dwell time is 10 minutes; The first chilling temperature is 900 degree; Be 300 minutes the first cool time.
Preferably, described dividing potential drop sintering step is the step of pressure-fired heating and heat preservation, uses mechanical pump to control vacuum in stove, and sintering box internal pressure is 10Pa.
Preferably, in the described hydrogen malleation dewaxing stage, the intensification of each time phase is allocated as follows: within first 40 minutes, from 20 degree, be warmed up to 150 degree; Within 120 minutes next, be warming up to 260 degree, 260 degree insulations 60 minutes; Through 60 minutes, be warming up to 370 degree, 370 degree insulations 60 minutes; Through 60 minutes, be warming up to 450 degree, 450 degree insulations are after 30 minutes; Through 60 minutes, be warming up to 600 degree, 600 degree are not incubated.
Preferably, in the described dividing potential drop sintering stage, the intensification of each time phase is allocated as follows: temperature in stove was warming up to 1320 degree in first 175 minutes, 1320 degree insulations 30 minutes; Through 30 minutes, be warming up to 1410 degree, 1410 degree insulations 60 minutes, wherein, it is 300-600Pa that dividing potential drop sintering divides pressure pressure, minute pressure pressure, since 600 intensifications, remains to 1410 degree insulations after 30 minutes always.
Preferably, in the described HTHP sintering stage, temperature distribution is as follows: temperature is warmed up to after 1410 degree, divide under pressure pressure and be incubated 30 minutes, then start to be filled with high pressure argon gas, inflationtime 20 minutes, during inflation, temperature keeps 1410 degree constant, inflated rear high-pressure pressurize 10 minutes, during high pressure pressurize, temperature 1410 is constant.
Preferably, at described cooling stage, the temperature and time in its each stage is allocated as follows: in stove, be full of under the condition of high pressure argon gas, within 180 minutes, be cooled to 900 degree, then about 240 minutes, from 900 degree, be chilled to soon below 50 degree.
Beneficial effect: the present invention can guarantee product sintering atmosphere in sintering box, has improved the interior atmosphere evenness of sintering box of carbide alloy extruded rod sintering, and then improves the once friendship inspection qualification rate of carbide alloy extruded rod bending.
Accompanying drawing explanation
Fig. 1 is the structural principle schematic diagram according to the sintering furnace of carbide alloy extruded bars of the present invention.
The specific embodiment
As shown in Figure 1, according to a kind of sintering furnace of carbide alloy extruded bars, at least comprise: furnace shell 10; Heat-insulation layer 20, it is arranged on the inwall of furnace shell 10; Sintering box 30, it is arranged in heat-insulation layer 20, and is provided with temperature sensor and pressure sensor; Hydrogen charging device 31 and argon gas charging device 32, it is communicated with the inner chamber of sintering box 30 respectively, and is communicated with sources of hydrogen and argon gas source respectively; Master controller 100, it controls at least one time controller 35, at least one temperature controller 34, at least one pressure controller 33.Various controllers can adopt controller well-known to those having ordinary skill in the art to implement.
The invention provides a kind of sintering process of cobalt content 5-15wt% carbide alloy extruded bars, sintering process comprises the dewaxing of hydrogen malleation, and pressure-fired heats up, insulation, high pressure-temperature sintering, and cooling four continuous process form.In wherein said hydrogen malleation dewaxing 490 minutes, progressively, stage by stage furnace temperature is risen to 600 degree, turn off argon gas, then use mechanical pump that vacuum degree control in stove is arrived to sintering box internal pressure 10Pa left and right, then start to be filled with argon gas and guarantee sintering box internal pressure 300-600Pa, under 300-600Pa press strip part through 235 minutes progressively, be warmed up to stage by stage 1410 degree, 1410 degree insulation 60 minutes, in 1410 insulations, after 30 minutes, be filled with high pressure argon gas 60bar, wherein fill 20 minutes high pressure argon gas time, high pressure pressurize 10 minutes, pressurize finishes simultaneously and begins to cool down with insulation.In stove, be full of under the condition of high pressure argon gas, naturally cool to 900 degree, then about 300 minutes, from 900 degree, be chilled to soon below 50 degree.
Embodiment 1: start to be filled with argon gas and guarantee sintering box internal pressure 300Pa, be warmed up to progressively, stage by stage 1410 degree under 300Pa press strip part through 235 minutes.
Embodiment 2: start to be filled with argon gas and guarantee sintering box internal pressure 450Pa, be warmed up to progressively, stage by stage 1410 degree under 450Pa press strip part through 235 minutes.
Embodiment 3: start to be filled with argon gas and guarantee sintering box internal pressure 600Pa, be warmed up to progressively, stage by stage 1410 degree under 600Pa press strip part through 235 minutes.
Product linearity result comparing result (take Ф 6mm as example)
| Technique | Common process | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Linearity qualification rate | 85％ | 90％ | 92％ | 95％ |
Claims (10)
1. a sintering process for carbide alloy extruded bars, is characterized in that, this sintering process comprises hydrogen malleation dewaxing step, dividing potential drop sintering step, high pressure-temperature sintering step and cooling step successively,
In hydrogen malleation dewaxing step, under normal temperature condition, hydrogen is filled with in emptying sintering furnace, within first heating-up time of 480-500 minute, progressively, by stages furnace temperature is risen to the first heating-up temperature 590-610 degree, then turn off hydrogen, vacuum degree control in stove is arrived to sintering box internal pressure 9-11Pa;
At dividing potential drop sintering step, in graphite sintering box inside, start to be filled with argon gas, guarantee sintering box internal pressure 300-600Pa, under 300-600Pa pressure condition, through second heating-up time of 230-240 minute, be warmed up to progressively, stage by stage the second heating-up temperature 1400-1420 degree;
At high pressure-temperature sintering step, in the second heating-up temperature, be incubated the first temperature retention time 55-65 minute, after being incubated the second temperature retention time 25-35 minute, the second heating-up temperature is filled with high pressure argon gas 40-100bar, wherein filling the high pressure argon gas time is 1/3 of the first temperature retention time, and the high pressure dwell time is 1/6 of the first temperature retention time;
At cooling step, pressurize finishes simultaneously and begins to cool down with insulation, is full of under the condition of high pressure argon gas in stove, naturally cools to the first chilling temperature 890-910 degree, then 290-310 minute the first cool time, from the first chilling temperature, is chilled to soon below 50 degree.
2. sintering process as claimed in claim 1, is characterized in that, the first heating-up time was 490 minutes, and the first heating-up temperature is 600 degree; The second heating-up time was 235 minutes, and the second heating-up temperature is 1410 degree; The first temperature retention time is 60 minutes; The second temperature retention time is 30 minutes; Be filled with high pressure argon gas 60bar; Filling the high pressure argon gas time is 20 minutes; The high pressure dwell time is 10 minutes; The first chilling temperature is 900 degree; And/or first cool time be 300 minutes.
3. sintering process as claimed in claim 1, is characterized in that, described dividing potential drop sintering step is the step of pressure-fired heating and heat preservation, uses mechanical pump to control vacuum in stove, and sintering box internal pressure is 10Pa.
4. sintering process as claimed in claim 1, is characterized in that, in the described hydrogen malleation dewaxing stage, the intensification of each time phase is allocated as follows: within first 40 minutes, from 20 degree, be warmed up to 150 degree; Within 120 minutes next, be warming up to 260 degree, 260 degree insulations 60 minutes; Through 60 minutes, be warming up to 370 degree, 370 degree insulations 60 minutes; Through 60 minutes, be warming up to 450 degree, 450 degree insulations are after 30 minutes; Through 60 minutes, be warming up to 600 degree, 600 degree are not incubated.
5. sintering process as claimed in claim 1, is characterized in that, in the described dividing potential drop sintering stage, the intensification of each time phase is allocated as follows: temperature in stove was warming up to 1320 degree in first 175 minutes, 1320 degree insulations 30 minutes; Through 30 minutes, be warming up to 1410 degree, 1410 degree insulations 60 minutes, wherein, it is 300-600Pa that dividing potential drop sintering divides pressure pressure, minute pressure pressure, since 600 intensifications, remains to 1410 degree insulations after 30 minutes always.
6. sintering process as claimed in claim 1, it is characterized in that, in the described HTHP sintering stage, temperature distribution is as follows: temperature is warmed up to after 1410 degree, under minute pressure pressure, is incubated 30 minutes, then starts to be filled with high pressure argon gas, inflationtime 20 minutes, during inflation, temperature keeps 1410 degree constant, has inflated rear high-pressure pressurize 10 minutes, and during high pressure pressurize, temperature 1410 is constant.
7. sintering process as claimed in claim 1, it is characterized in that, at described cooling stage, the temperature and time in its each stage is allocated as follows: in stove, be full of under the condition of high pressure argon gas, within 180 minutes, be cooled to 900 degree, then about 240 minutes, from 900 degree, be chilled to soon below 50 degree.
8. sintering process as claimed in claim 1, is characterized in that, the cobalt content 5-15wt% of carbide alloy extruded bars.
9. a sintering furnace for carbide alloy extruded bars, is characterized in that, this sintering furnace at least comprises:
Furnace shell;
Heat-insulation layer, it is arranged on the inwall of furnace shell;
Sintering box, it is arranged in heat-insulation layer, and is provided with temperature sensor and pressure sensor;
Hydrogen charging device and argon gas charging device, it is communicated with the inner chamber of sintering box respectively, and is communicated with sources of hydrogen and argon gas source respectively;
Master controller, it controls at least one time controller, at least one temperature controller, at least one pressure controller,
In hydrogen malleation dewaxing step; master controller drives hydrogen charging device to start working; control time controller and temperature controller; make within first heating-up time of 480-500 minute; progressively, by stages furnace temperature is risen to the first heating-up temperature 590-610 degree, then, master controller quits work hydrogen charging device; controlled pressure controller, arrives sintering box internal pressure 9-11Pa by vacuum degree control in stove;
At dividing potential drop sintering step, master controller drives argon gas charging device to start working, control time controller and temperature controller, guarantee sintering box internal pressure 300-600Pa, under 300-600Pa pressure condition, through second heating-up time of 230-240 minute, be warmed up to progressively, stage by stage the second heating-up temperature 1400-1420 degree;
At high pressure-temperature sintering step, in the second heating-up temperature, be incubated the first temperature retention time 55-65 minute, after being incubated the second temperature retention time 25-35 minute, the second heating-up temperature is filled with high pressure argon gas 40-100bar, wherein filling the high pressure argon gas time is 1/3 of the first temperature retention time, and the high pressure dwell time is 1/6 of the first temperature retention time;
At cooling step, master controller is controlled pressurize and is finished simultaneously and begin to cool down with insulation, in stove, be full of under the condition of high pressure argon gas, naturally cool to the first chilling temperature 890-910 degree, then 290-310 minute the first cool time, from the first chilling temperature, be chilled to soon below 50 degree.
10. sintering furnace as claimed in claim 9, is characterized in that,
In hydrogen malleation dewaxing step; master controller drives hydrogen charging device to start working; control time controller and temperature controller; make within first heating-up time of 490 minutes; furnace temperature is risen to 600 ℃ of the first heating-up temperatures progressively, by stages, then, master controller quits work hydrogen charging device; controlled pressure controller, arrives sintering box internal pressure 10Pa by vacuum degree control in stove;
At dividing potential drop sintering step, master controller drives argon gas charging device to start working, control time controller and temperature controller, guarantee sintering box internal pressure 300-600Pa, under 300-600Pa pressure condition, through second heating-up time of 235 minutes, be warmed up to progressively, stage by stage 1410 ℃ of the second heating-up temperatures;
At high pressure-temperature sintering step, in the second heating-up temperature, be incubated the first temperature retention time 60 minutes, in the second heating-up temperature, be incubated the second temperature retention time and after 30 minutes, be filled with high pressure argon gas 40-100bar, wherein filling the high pressure argon gas time is 1/3 of the first temperature retention time, and the high pressure dwell time is 1/6 of the first temperature retention time;
At cooling step, master controller is controlled pressurize and is finished simultaneously and begin to cool down with insulation, in stove, be full of under the condition of high pressure argon gas, naturally cool to 900 ℃ of the first chilling temperatures, then 300 minutes the first cool times, from the first chilling temperature, be chilled to soon below 50 degree.
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| CN114029487A (en) * | 2021-10-22 | 2022-02-11 | 浙江恒成硬质合金有限公司 | Hard alloy dewaxing method for dewaxing furnace |
| CN114178529A (en) * | 2021-11-03 | 2022-03-15 | 浙江恒成硬质合金有限公司 | Hard alloy degreasing furnace and degreasing method |
| CN117428189B (en) * | 2023-12-19 | 2024-03-08 | 厦门大鸿翰金属材料科技有限公司 | Cemented carbide sintering process |
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Effective date of registration: 20220215 Address after: 330600 Industrial Park, Jing'an County, Yichun City, Jiangxi Province Patentee after: JIANGXI JIANGWU CEMENTED CARBIDE CO.,LTD. Address before: 330046 No. 118 West Beijing Road, Jiangxi, Nanchang Patentee before: JIANGXI RARE EARTH AND RARE METALS TUNGSTEN Group Corp. |
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