CN1302707A - Plasma technology for activating sintered material - Google Patents
Plasma technology for activating sintered material Download PDFInfo
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- CN1302707A CN1302707A CN 01107084 CN01107084A CN1302707A CN 1302707 A CN1302707 A CN 1302707A CN 01107084 CN01107084 CN 01107084 CN 01107084 A CN01107084 A CN 01107084A CN 1302707 A CN1302707 A CN 1302707A
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Abstract
A process for sintering material by plasma activation includes such steps as laoding material in plasma-activation sintering furnace, applying coaxial pressure to material, applying pulse voltage under constant pressure to generate plasma for activating surface of powder particles, cutting off pulse voltage, applying direct current under constant pressure to heat material to needed temp. for a certain time, and stopping heating and removing pressure. Its advantages are low sintering temp. to suppress growth of crystal grains and high performance of sintered material.
Description
Plasma technology for activating sintered material, a kind of powdered metallurgical material preparation, the new technology of processing.
Sintering is one of operation the most basic in the powder metallurgy production process.Sintering is a high temperature action, generally will also suitable protective atmosphere will be arranged through the long time.Therefore, consider from economic angle that the consumption of sintering circuit is the pith that constitutes product cost, improves operation and agglomerating plant, reduces the consumption of material and energy, as reducing sintering temperature, shortening sintering time etc., meaning economically is very big.
Known sintering method has: traditional pressureless sintering method, hot pressing sintering method, microwave sintering method, plasma sintering method (as microwave plasma, direct-current plasma) but all have outside its deficiency.No matter long, poor, the energy consumption height of properties of product of tradition pressureless sintering method process time adopts the fuel heating still to adopt electrical heating, all makes cost up, is therefore replaced by some novel sintering methods gradually.Though hot pressing sintering method has adopted pressure, in the sintering process activation degree (being dynamic process) of sample still needed and further improve, and apparatus expensive and process-cycle are long.And microwave waters connection and the plasma sintering method is improved aspect activation, shortened sintering time, reduced sintering temperature, suppressed growing up of dusty material particle, but experimental condition such as temperature is difficult to control in the sintering process, particularly cause the thermal runaway effect easily in the microwave sintering process, dusty material is produced inhomogeneous heating, thereby influenced the various performances of sintered products, thereby a kind of new method that can improve above-mentioned sintering process shortcoming of in the preparation of dusty material and process, still needing.
Plasma activated sintering dusty material new technology, abroad start to walk since the nineties, because it melts plasma-activated, hot pressing, resistance heated is an one, have advantages such as sintering time weak point, temperature precise control, the relative theory density that only in minutes just makes dusty material is near 100%, and can effectively improve the various performances of material, thereby the research of plasma activated sintering and being applied in abroad emerges rapidly, becomes the new focus of dusty material research.
What essential distinction do plasma activated sintering and plasma sintering have so? plasma sintering is placed on material in the plasma atmosphere and carries out.Mainly contain the discharge of direct current cathode cavity, high-frequency induction, three kinds of methods that produce high-temperature plasma of microwave-excitation at present.The device that these three kinds of methods adopt all has a cover to keep the system of vacuum and control gas pressure and flow, and different mainly is the power mode that produces plasma.The essence of this technology is that the high-temperature plasma that utilize to produce heats material, and the heat exchange by material and high-temperature plasma realizes sintering, promptly plasma as thermal source, material is carried out sintering.But shortcoming is: sample is easy to generate cracking, and along with the rising of temperature, the volatilization of material also aggravates, and technology and theory are all immature.
And the plasma activated sintering method is the micro discharge phenomenon of utilizing between powder particle that the gap produced, by the plasma strike and the intergranular contact portion of heating powder of discharging and being produced, can make the material of contact portion produce evaporation, thereby reach the purpose of purification and activated powder particle, more effectively promoted the carrying out of sintering.It melts plasma, hot pressing, Fast Heating is one, has sintering time weak point, temperature precise control, easy advantage such as industrialization.
The present invention is needing to impose pulse voltage on the dusty material of sintering, produce plasma with activated powder material granule surface, passing to direct current heats up to the dusty material Fast Heating, exert pressure again with sintering and curing powder material, it is even to reach that sintering time is short, the temperature precise control is sintered material granule, improves the purpose of material property.
The present invention is achieved by the following technical solutions.
Fig. 1 is the installation drawing of plasma activated sintering of the present invention, and 1 is Pulased power supply unit among the figure, the 2nd, and resistive heating device, the 3,4,5,6, the 11st, the axial pressure device, the 12, the 10th, the sintering mould, 9 and 13 is upper and lower drifts etc.The dusty material that needs sintering is placed mould and imposes homoaxial pressure, in dusty material, produce the particle surface of plasma with pulse voltage with activated material, be heated by resistive device then and impose direct current, material is carried out Fast Heating, therefore to finish activated sintering to dusty material.(plasma activated sintering device, the existing description in the utility application that the applicant proposes on January calendar year 2001 13).
Fig. 2 is temperature, the pressure schematic diagram of above-mentioned sintering process four-stage.Sintering divides four-stage to carry out: the phase I, the dusty material that is sintered is slightly executed homoaxial pressure; Second stage keeps constant pressure, and adds pulse voltage, produces plasma, and particle surface is activated, and supervenes a spot of heat; Phase III, close pulse power supply circuit, continue to improve pressure, under the constant voltage effect, be heated to temperature required and the time to material with direct current; The quadravalence section stops the D.C. resistance heating, eliminates pressure.Applied pressure, temperature and pulse voltage need to decide according to the dusty material and the sintered products performance that are sintered.
Fig. 3 is Pulased power supply unit and resistive heating device circuit theory diagrams
When the three phase sine alternating current becomes Rectified alternating current, obtains HVDC after by capacitor filtering through three-phase bridge rectification, this high voltage direct current is sent into the power switch inverter, become the square wave alternating current, after intermediate-frequency transformer downgrades required voltage, behind switching and rectifying, inductor filter, can obtain working direct current again.It is that a kind of contravariant external characteristics is that voltage falls suddenly, the constant-current type electric current.
For guaranteeing the constant set-point of direct current of resistive heating device output, in Circuits System, be provided with current regulation control circuit and Current Feedback Control circuit in technological requirement; For the pulse direct current that guarantees Pulased power supply unit output satisfies technological requirement, be provided with the modulator loop that pulse frequency modulation and pulse-width modulation circuit constitute especially, in order to the low frequency dc pulse voltage is modulated on the direct current of output.
Pulased power supply unit, resistive heating device, desired parameters will generally can be controlled in according to the difference of agglomerated material and sintered products performance requirement is set during the work of axial pressure device: (1) pulse voltage 5～100V, pulse current 100～250A, pulse turn-on time 10～90ms, pulse 10～80ms breaking time, overall pulse time 20～100s; (2) resistance heated voltage 5～120V, electric current 100～1200A, power-efficient are greater than 80%, and power factor (PF) is greater than 0.9; (3) temperature range is 200～1600 ℃.
Compare advantage and good effect that the present invention exists with known technology:
(1) to the dusty material pressurization accurately, steadily controlled;
(2) Pulased power supply unit and resistive heating device stability is high, continuity is good, and adjustable extent is big, and dynamic response is fast;
(3) owing to the activation of plasma, new technology can realize low-temperature sintering, has so just suppressed growing up of crystal grain, from having improved the performance of sintered body in essence.
(4) sintering time is short, compares with the several hrs of conventional sintering, has saved the energy, has reduced the loss of equipment.
This new technology also can make up configuration respectively with Medium frequency induction or AC resistance stove, also can carry out plasma-activated-Medium frequency induction sintering, plasma-activated-indirect resistance heat-agglomerating etc.
This new technology also can be used for exploring the different process process of the activated sintering of the activated sintering of different types of dusty material or preferred dusty material of the same race, also can adopt first activation, back pressurization, the technical process such as knot of reburning.
Fig. 1 is an installation drawing of the present invention, and 1 is Pulased power supply unit among the figure, the 2nd, and resistive heating device, the 3,4,5,6,11,12, be the axial pressure device, the 10th, the sintering mould, 9 and 13 is upper and lower drifts.Fig. 2 is temperature, the pressure schematic diagram of sintering process quadravalence section.Fig. 3 is Pulased power supply unit and resistive heating device circuit theory diagrams.
Embodiment
(1) plasma activated sintering of alumina in Nano level
Packed in the sintering mould in the nano-alumina powder end, at first powder is activated, be rapidly heated subsequently and powder exerted pressure and carry out sintering with pulse current.Pulse current 850A wherein, pulse turn-on time 60ms, breaking time 30ms, plasma-activated time 90s, pressure 40MPa, 1250～1350 ℃ of heating-up temperatures.
(2) plasma activated sintering of Hardmetal materials WC+CO
Pack into after WC powder (purity is 99.9%) and CO powder (purity is 99.8%) evenly mixed in proportion in the sintering mould, at first powder is activated, be rapidly heated subsequently and powder exerted pressure and carry out sintering with pulse current.
(a), the optimum process condition of WC-6%CO dusty material: pulse current 600A, pulse turn-on time 40ms, plasma-activated time 30s, pressure is 30.5MPa, 1350 ℃ of following sintering 5 minutes, hardness reached HRA92, and the relative theory density value is 99.83%.
(b), the sintering of WC-10%
The optimum process condition of sintering WC-10%CO: pulse current 500A, pulse turn-on time is 40ms, be 60ms breaking time, the plasma-activated time is 25s, pressure is 26.3MPa, and heating-up temperature 300-1350 ℃, sintering time is 4 minutes, just reach 99.65% with solid density, Rockwell hardness reaches 91.
(c), the sintering of WC-15%CO
The optimum process condition of sintering WC-15%CO dusty material: Pulse Electric is annotated 450A, and pulse turn-on time is 40ms, and be 60ms breaking time, the plasma-activated time was 20s, and pressure is 21.6MPa, 1300 ℃ of following sintering 5 minutes, hardness reaches HRA90, and the relative theory density value is 99.90%.
(d) sintering of WC-20%CO
The optimum process condition of sintering WC-20%COO dusty material: pulse current 400A, pulse turn-on time is 20ms, be 80ms breaking time, the plasma-activated time is 30s, heating-up temperature 1250-1300 ℃, pressure was 17.6MPa, 1300 ℃ of following sintering 5 minutes, hardness reaches HRA89, and the relative theory density value is 99.93%.
(3) nanoscale ZrO
2Plasma activated sintering
With nano level ZrO
2Powder is packed in the sintering mould, at first with pulse current powder is activated, and is rapidly heated subsequently and powder exerted pressure to carry out sintering.Optimum process condition is: pulse current 700A, pulse turn-on time 45ms, breaking time 30ms, plasma-activated time 60s, pressure 30MPa, heating-up temperature 1300-1400 ℃, sintering time is 7 minutes, and Vickers hardness reaches 15.4GPa, and relative theory density is near 100%.
(4) plasma activated sintering of Cu powder
Technological parameter is: pulse current 2500A, pulse paths time are 40ms, breaking time is 60ms, adopted D.C. resistance heat-agglomerating to 600 ℃ again, and total activated sintering time is 15s, reduces to room temperature subsequently.Institute's applied pressure is 5MPa in the process, and after activated sintering, the solid density of sample reaches 99.6%, and the process time only is 15s.
Claims (3)
1, a kind of plasma technology for activating sintered material is characterized in that: sintering divides four-stage to carry out, and the phase I, the dusty material particle is slightly granted its homoaxial pressure; Second stage keeps constant pressure, and adds pulse voltage, produces plasma, and the dusty material particle surface is activated; Phase III, close pulse power supply circuit, continue to improve pressure, under the constant voltage effect, be heated to temperature required and the time to material with direct current; The quadravalence section stops the D.C. resistance heating, eliminates pressure.
2, plasma technology for activating sintered material according to claim 1 is characterized in that: pulse power supply circuit is an impulse modulation loop that comprises that pulse frequency modulation and pulsewidth modulation constitute.
3, plasma technology for activating sintered material according to claim 1 is characterized in that: resistive heating device is a contravariant, and external characteristics is that voltage falls suddenly, the constant-current type dc source.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01107084 CN1203946C (en) | 1996-07-12 | 2001-01-20 | Plasma technology for activating sintered material |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NO962936 | 1996-07-12 | ||
| CN 01107084 CN1203946C (en) | 1996-07-12 | 2001-01-20 | Plasma technology for activating sintered material |
Related Child Applications (3)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100520929A Division CN1292865C (en) | 2001-01-20 | 2001-01-20 | Nano aluminium oxide plasma activation sintering method |
| CNB2005100520914A Division CN1292864C (en) | 2001-01-20 | 2001-01-20 | Method for copper powder plasma activated sintering |
| CNB200510052090XA Division CN1292863C (en) | 2001-01-20 | 2001-01-20 | Nano zirconium oxide plasma activation sintering method |
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| Publication Number | Publication Date |
|---|---|
| CN1302707A true CN1302707A (en) | 2001-07-11 |
| CN1203946C CN1203946C (en) | 2005-06-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01107084 Expired - Fee Related CN1203946C (en) | 1996-07-12 | 2001-01-20 | Plasma technology for activating sintered material |
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| CN (1) | CN1203946C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139371A (en) * | 2011-05-04 | 2011-08-03 | 佛山市钜仕泰粉末冶金有限公司 | Tungsten alloy target material and preparation method thereof |
| CN102464494A (en) * | 2010-11-16 | 2012-05-23 | 中国科学院合肥物质科学研究院 | Microwave pressure sintering device |
| US8247039B2 (en) | 2005-06-02 | 2012-08-21 | Institut “Jo{hacek over (z)}ef Stefan” | Method and device for local functionalization of polymer materials |
| WO2013177811A1 (en) * | 2012-05-30 | 2013-12-05 | 深圳市华星光电技术有限公司 | Method for preparing target material for tft-lcd array substrate cu conductor, and target material |
| CN103567440A (en) * | 2013-08-15 | 2014-02-12 | 厦门虹鹭钨钼工业有限公司 | Preparation method for tungsten carbide target material for film coating of oil exploration drill bit |
| CN104630524A (en) * | 2013-11-15 | 2015-05-20 | 核工业西南物理研究院 | Method for preparing beryllium-titanium alloy by carrying out spark plasma sintering |
| CN107096919A (en) * | 2016-02-19 | 2017-08-29 | 泰克纳里阿研究与创新基金 | The equipment for sintering the method for conductive powder and performing methods described |
| CN116655380A (en) * | 2023-05-26 | 2023-08-29 | 香河昆仑新能源材料股份有限公司 | Garnet type solid electrolyte and preparation method and application thereof |
-
2001
- 2001-01-20 CN CN 01107084 patent/CN1203946C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8247039B2 (en) | 2005-06-02 | 2012-08-21 | Institut “Jo{hacek over (z)}ef Stefan” | Method and device for local functionalization of polymer materials |
| CN102464494A (en) * | 2010-11-16 | 2012-05-23 | 中国科学院合肥物质科学研究院 | Microwave pressure sintering device |
| CN102139371A (en) * | 2011-05-04 | 2011-08-03 | 佛山市钜仕泰粉末冶金有限公司 | Tungsten alloy target material and preparation method thereof |
| CN102139371B (en) * | 2011-05-04 | 2013-01-23 | 佛山市钜仕泰粉末冶金有限公司 | Tungsten alloy target material and preparation method thereof |
| WO2013177811A1 (en) * | 2012-05-30 | 2013-12-05 | 深圳市华星光电技术有限公司 | Method for preparing target material for tft-lcd array substrate cu conductor, and target material |
| CN103567440A (en) * | 2013-08-15 | 2014-02-12 | 厦门虹鹭钨钼工业有限公司 | Preparation method for tungsten carbide target material for film coating of oil exploration drill bit |
| CN104630524A (en) * | 2013-11-15 | 2015-05-20 | 核工业西南物理研究院 | Method for preparing beryllium-titanium alloy by carrying out spark plasma sintering |
| CN107096919A (en) * | 2016-02-19 | 2017-08-29 | 泰克纳里阿研究与创新基金 | The equipment for sintering the method for conductive powder and performing methods described |
| CN116655380A (en) * | 2023-05-26 | 2023-08-29 | 香河昆仑新能源材料股份有限公司 | Garnet type solid electrolyte and preparation method and application thereof |
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|---|---|
| CN1203946C (en) | 2005-06-01 |
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