CN102921948A - Sintering technology for cemented carbide extrusion bar - Google Patents
Sintering technology for cemented carbide extrusion bar Download PDFInfo
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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
In the situation of diameter D≤Ф 6mm, there is the lower phenomenon of linearity first-time qualification rate usually in the sintering of carbide alloy extruded bars.The forming agent of carbide alloy extruded rod mainly contains paraffin, cellulose etc., and this forming agent all can remove in the dewaxing of hydrogen malleation fully.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, the sintering buckling problem also is particularly to give prominence to.This be because, in at present general alloy sintering technique, after the forming agent of product removes end, generally all be to enter the vacuum-sintering stage then about 1350 degree, just to begin to enter the dividing potential drop sintering, be filled with the argon gas of minute pressure pressure, the evaporation of liquid phase cobalt when preventing sintering.Like this, in the vacuum-sintering stage of stove, the 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, so that the carbide alloy extruded rod rate of curving behind the sintering improves greatly.
Summary of the invention
The sintering process that the purpose 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 the emptying sintering furnace, within the 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 the stove is arrived sintering box internal pressure 9-11Pa;
At the dividing potential drop sintering step, begin to be filled with argon gas in graphite sintering box inside, guarantee sintering box internal pressure 300-600Pa, under the 300-600Pa pressure condition, through the 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 the high pressure-temperature sintering step, be incubated the first temperature retention time 55-65 minute in the second heating-up temperature, 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 with insulation and begins to cool down, and is full of in stove under the condition of high pressure argon gas, naturally cools to the first chilling temperature 890-910 degree, then is chilled to soon from the first chilling temperature below 50 degree 290-310 minute the first cool time.
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 vacuum in the mechanical pump control stove, and the sintering box internal pressure is 10Pa.
Preferably, in the described hydrogen malleation dewaxing stage, the intensification of each time phase is allocated as follows: be warmed up to 150 from 20 degree and spend in front 40 minutes; Be warming up to 260 degree in next 120 minutes, 260 degree insulations 60 minutes; Be warming up to 370 degree through 60 minutes, 370 degree insulations 60 minutes; Be warming up to 450 degree through 60 minutes, 450 degree insulations are after 30 minutes; Be warming up to 600 degree through 60 minutes, 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 the stove was warming up to 1320 spends 1320 degree insulations 30 minutes in front 175 minutes; Be warming up to 1410 degree through 30 minutes, 1410 degree insulations 60 minutes, wherein, it is 300-600Pa that the dividing potential drop sintering divides pressure pressure, minute pressure pressure remains to 1410 degree insulations after 30 minutes since 600 intensifications always.
Preferably, in the described HTHP sintering stage, temperature distribution is as follows: after temperature is warmed up to 1410 degree, divide under the pressure pressure and be incubated 30 minutes, then begin to be filled with the high pressure argon gas, inflationtime 20 minutes, temperature keeps 1410 degree constant during inflation, the high-pressure pressurize was 10 minutes after inflation was finished, and temperature 1410 is constant during the high pressure pressurize.
Preferably, at described cooling stage, the temperature and time of its stages is allocated as follows: be full of in stove under the condition of high pressure argon gas, be cooled to 900 degree, and then be chilled to soon below 50 degree from 900 degree about 240 minutes in 180 minutes.
Beneficial effect: the present invention can guarantee product sintering atmosphere in the 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.
Description of drawings
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, the sintering furnace according to a kind of carbide alloy extruded bars comprises at least: furnace shell 10; Heat-insulation layer 20, it is arranged on the inwall of furnace shell 10; Sintering box 30, it is arranged in the 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, and the high pressure-temperature sintering cools off four continuous process and forms.In the 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 the stove is arrived about sintering box internal pressure 10Pa, then begin to be filled with argon gas and guarantee sintering box internal pressure 300-600Pa, under 300-600Pa press strip spare through 235 minutes progressively, be warmed up to stage by stage 1410 degree, 1410 degree insulations 60 minutes, be filled with high pressure argon gas 60bar in 1410 insulations after 30 minutes, wherein fill 20 minutes high pressure argon gas time, high pressure pressurize 10 minutes, pressurize finishes simultaneously with insulation and begins to cool down.In stove, be full of under the condition of high pressure argon gas, naturally cool to 900 degree, then be chilled to soon below 50 degree from 900 degree about 300 minutes.
Embodiment 1: begin to be filled with argon gas and guarantee sintering box internal pressure 300Pa, be warmed up to progressively, stage by stage 1410 through 235 minutes and spend under 300Pa press strip spare.
Embodiment 2: begin to be filled with argon gas and guarantee sintering box internal pressure 450Pa, be warmed up to progressively, stage by stage 1410 through 235 minutes and spend under 450Pa press strip spare.
Embodiment 3: begin to be filled with argon gas and guarantee sintering box internal pressure 600Pa, be warmed up to progressively, stage by stage 1410 through 235 minutes and spend under 600Pa press strip spare.
The product linearity is comparing result (take Ф 6mm as example) as a result
| Technique | Common process | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| The linearity qualification rate | 85％ | 90％ | 92％ | 95％ |
Claims (10)
1. the sintering process of a 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 the emptying sintering furnace, within the 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 the stove is arrived sintering box internal pressure 9-11Pa;
At the dividing potential drop sintering step, begin to be filled with argon gas in graphite sintering box inside, guarantee sintering box internal pressure 300-600Pa, under the 300-600Pa pressure condition, through the 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 the high pressure-temperature sintering step, be incubated the first temperature retention time 55-65 minute in the second heating-up temperature, 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 with insulation and begins to cool down, and is full of in stove under the condition of high pressure argon gas, naturally cools to the first chilling temperature 890-910 degree, then is chilled to soon from the first chilling temperature below 50 degree 290-310 minute the first cool time.
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 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; 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 vacuum in the mechanical pump control stove, and the 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: be warmed up to 150 from 20 degree and spend in front 40 minutes; Be warming up to 260 degree in next 120 minutes, 260 degree insulations 60 minutes; Be warming up to 370 degree through 60 minutes, 370 degree insulations 60 minutes; Be warming up to 450 degree through 60 minutes, 450 degree insulations are after 30 minutes; Be warming up to 600 degree through 60 minutes, 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 the stove was warming up to 1320 spends 1320 degree insulations 30 minutes in front 175 minutes; Be warming up to 1410 degree through 30 minutes, 1410 degree insulations 60 minutes, wherein, it is 300-600Pa that the dividing potential drop sintering divides pressure pressure, minute pressure pressure remains to 1410 degree insulations after 30 minutes since 600 intensifications 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: after temperature was warmed up to 1410 degree, insulation was 30 minutes under minute pressure pressure, then begins to be filled with the high pressure argon gas, inflationtime 20 minutes, temperature keeps 1410 degree constant during inflation, and the high-pressure pressurize was 10 minutes after inflation was finished, and temperature 1410 is constant during the high pressure pressurize.
7. sintering process as claimed in claim 1, it is characterized in that at described cooling stage, the temperature and time of its stages is allocated as follows: in stove, be full of under the condition of high pressure argon gas, be cooled to 900 degree in 180 minutes, then be chilled to soon below 50 degree from 900 degree about 240 minutes.
8. sintering process as claimed in claim 1 is characterized in that, the cobalt content 5-15wt% of carbide alloy extruded bars.
9. the sintering furnace of a carbide alloy extruded bars is characterized in that, this sintering furnace comprises at least:
Furnace shell;
Heat-insulation layer, it is arranged on the inwall of furnace shell;
Sintering box, it is arranged in the 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.
10. sintering furnace as claimed in claim 9 is characterized in that,
In hydrogen malleation dewaxing step, master controller drives the hydrogen charging device and starts working, control time controller and temperature controller, make within first heating-up time of 480-500 minute (preferred 490 minutes), progressively, by stages furnace temperature is risen to the first heating-up temperature 590-610 degree (preferred 600 ℃), then, master controller quits work the hydrogen charging device, the controlled pressure controller arrives sintering box internal pressure 9-11Pa (preferred 10Pa) with vacuum degree control in the stove;
At the dividing potential drop sintering step, master controller drives the argon gas charging device and starts working, control time controller and temperature controller, guarantee sintering box internal pressure 300-600Pa, under the 300-600Pa pressure condition, through second heating-up time of 230-240 minute (preferred 235 minutes), be warmed up to progressively, stage by stage the second heating-up temperature 1400-1420 degree (preferred 1410 ℃);
At the high pressure-temperature sintering step, be incubated the first temperature retention time 55-65 minute (preferred 60 minutes) in the second heating-up temperature, be incubated the second temperature retention time 25-3 minute in the second heating-up temperature and be filled with high pressure argon gas 40-100bar after (preferred 30 minutes), 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 control pressurize finishes simultaneously with insulation and begins to cool down, in stove, be full of under the condition of high pressure argon gas, naturally cool to the first chilling temperature 890-910 degree (preferred 900 ℃), then be chilled to soon from the first chilling temperature below 50 degree in 290-310 minute the first cool time (preferred 300 minutes).
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Cited By (8)
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| CN104353831A (en) * | 2014-10-31 | 2015-02-18 | 东莞理工学院 | Vacuum sintering anti-bending method for hard alloy round bar material |
| CN104357696A (en) * | 2014-12-01 | 2015-02-18 | 技锋精密刀具（马鞍山）有限公司 | Sintering process of products obtained by hard alloy paraffin production process |
| CN104399983A (en) * | 2014-10-31 | 2015-03-11 | 东莞理工学院 | Method for reducing bending rate of hard alloy short bar materials |
| CN109943761A (en) * | 2019-03-13 | 2019-06-28 | 河源富马硬质合金股份有限公司 | A kind of pressing method producing hard alloy bar |
| CN111118376A (en) * | 2019-12-05 | 2020-05-08 | 江西江钨硬质合金有限公司 | High-hardness and high-strength WC-Co-based hard alloy, preparation method thereof and cutting tool |
| 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 |
| CN117428189A (en) * | 2023-12-19 | 2024-01-23 | 厦门大鸿翰金属材料科技有限公司 | Cemented carbide sintering process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104353831A (en) * | 2014-10-31 | 2015-02-18 | 东莞理工学院 | Vacuum sintering anti-bending method for hard alloy round bar material |
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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 |
| CN117428189A (en) * | 2023-12-19 | 2024-01-23 | 厦门大鸿翰金属材料科技有限公司 | Cemented carbide sintering process |
| 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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