CN102876951B - Method for preparing pure metal ceramic Cr7C3 block - Google Patents
Method for preparing pure metal ceramic Cr7C3 block Download PDFInfo
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- CN102876951B CN102876951B CN201210378657.2A CN201210378657A CN102876951B CN 102876951 B CN102876951 B CN 102876951B CN 201210378657 A CN201210378657 A CN 201210378657A CN 102876951 B CN102876951 B CN 102876951B
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- powder
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- graphite
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Abstract
The invention discloses a method for preparing a pure metal ceramic Cr7C3 block. The method includes the steps: converting pure Cr powder and pure graphite powder into a weight ratio according to the atomic ratio in a carbide Cr7C3 molecular formula and the atomic weight of elements, placing the powder into a milling tank after weighing, adding phenolic resin with the weight not more than 3% of the overall weight of the Cr powder and the graphite powder, vacuumizing the milling tank and performing ball-milling for 5-20 hours to mix raw materials; filling mixture discharged out of the tank into a graphite mould, placing the graphite mould into a sintering furnace for vacuum hot pressed sintering at the temperature of 1200-1500 DEG C, and keeping the temperature for 10-60 minutes; and cooling the sintered graphite mould along with the furnace and taking out a sintered body in the graphite mould to obtain the pure metal ceramic Cr7C3 block.
Description
Technical field
The present invention relates to a kind of preparation method of sintering metal block materials.
Background technology
Cr
7c
3be to there is orthohormbic structure transition metal carbide, there is ceramic character.Its hardness is high, wear resistance good, and preferably toughness, the good advantage such as oxidation-resistance and thermostability can be applied in the component of machine surface of low cost steel grade, improves surface abrasion performance and resistance to high temperature corrosion.In theory, Chinese scholars is mainly applied first principle and has been calculated Cr
7c
3the mechanical property such as microhardness, Young's modulus, its result and trial value are close.Domestic scholars is mainly applied plasma and is covered molten technology and prepare one deck with Cr at steel surface
7c
3for the compound coating of hard phase, in coating structure, remove Cr
7c
3, also have matrix as austenite structure etc. outward, and the thinner thickness of this layer of coating, in practical engineering application, still cannot meet the requirement of high life.Foreign scholar prepares single-phase Cr at present
7c
3main method of attempting has: (a) by the method for thermospray, prepare one deck Cr
7c
3film; (b) plasma activated sintering; (c) self-propagating high-temperature reaction is synthetic; (d) vacuum non-pressure sintering; Wherein (b) method has made and has organized comparatively ideal non-pure single-phase Cr
7c
3block tissue.
Iran scholar S.Sharafi, the people such as S.Gomari, (sintering temperature is 1100 ℃ to utilize the method for mechanical ball milling and vacuum (applying argon gas) pressureless sintering; Soaking time is 1 hour) prepared block Cr
7c
3.The block tissue obtaining in this report is apart from Cr
7c
3also has Cr outward,
2o
3phase is not obviously pure single Cr
7c
3compound block.
Japanese scholars Ken Hirota etc., after the wet-milling of Cr and carbon powder machinery is mixed, have prepared single-phase block Cr with spark plasma sintering
7c
3.Its performance is as shown in table 1.Although Main Mechanical index is more satisfactory, equally do not obtain pure single Cr yet
7c
3compound block.
Non-pure Cr under the different sintering temperatures of table 1
7c
3specifeca tion speeification
Summary of the invention
The object of the present invention is to provide a kind of toughness better, the pure single Cr of high-temperature corrosion resistance
7c
3the preparation technology of compound block.
For reaching above object, the present invention adopts following technical scheme to be achieved:
A kind of clean metal pottery Cr
7c
3the preparation method of block, is characterized in that, comprises the following steps:
(1) pure Cr powder and pure Graphite Powder 99 are pressed to carbide Cr
7c
3the nucleidic mass of molecular formula Atom ratio and each element is converted into weight ratio, after weighing, packs in grinding jar, adds the resol of no more than Cr powder and Graphite Powder 99 gross weight 3% simultaneously, vacuumizes:
(2) ball grinder is put into ball mill start and rotated 5-20 hour, complete raw material and mix;
(3) mixture going out after tank is filled in graphite jig;
(4) graphite jig of filling mixture is put into sintering oven and carry out vacuum heating-press sintering, sintering temperature is 1200 ℃～1500 ℃; Be incubated 10～60 minutes;
(5) graphite jig after sintering is together cooling with sintering oven, takes out the sintered compact in graphite jig, obtains clean metal pottery Cr
7c
3block.
In aforesaid method, the Cr powder that step (1) is described and the purity of Graphite Powder 99 are 99.9%, granularity all≤200 μ m.The add-on of resol is the 0.5-3% of Cr powder and Graphite Powder 99 gross weight.
What step (1) was described vacuumizes, vacuum tightness≤10
-1pa).
The described vacuum heating-press sintering of step (4), its processing parameter is: vacuum tightness≤10
-1pa; Heat-up rate 5-10 ℃/sec; Pressure 0-150Mpa.
Advantage of the present invention is that preparation process is simple, the pure single Cr obtaining
7c
3compound block relative density is higher, and Main Mechanical index is better, and be not only suitable for wear-resisting field occasion, and can also be used for anti-corrosion field, and wear-resisting, anti-corrosion mutual field.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
First, by pure Cr powder (purity and granularity are respectively: 99.9% and 200 μ m) and Graphite Powder 99 (purity and granularity are respectively: 99.9% and 200 μ m) by Cr
7c
3molecular formula Atom than and the nucleidic mass of each element be converted into weight ratio, after weighing, pack in stainless steel jar mill, add the resol of Cr powder and Graphite Powder 99 gross weight 0.5% simultaneously, vacuumize that (vacuum tightness is 10
-1pa).
Then, ball grinder is put into ball mill start and rotate, ball milling, after 20 hours, is filled to the mixture of Cr powder, Graphite Powder 99 and resol in graphite jig.
Finally, the graphite jig of filling Cr powder, Graphite Powder 99 and resol mixture is put into vacuum sintering funace and carry out sintering, the vacuum tightness 10 of vacuum oven during sintering
-1pa; The heat-up rate of sintering oven is 5 ℃/sec; Pressure is 0MPa; Sintering temperature is 1200 ℃; Soaking time is 10 minutes, together cooling with sintering oven after sintering, takes out the sintered compact in graphite jig, obtains clean metal pottery Cr
7c
3block.The main performance index of the present embodiment is as shown in table 2.
Embodiment 2
The processing step of the present embodiment is identical with embodiment 1, but some processing parameters are wherein slightly different:
1) Cr powder purity and granularity be respectively 99.9%, 150 μ m; Graphite Powder 99 purity and granularity are respectively 99.9%, 150 μ m.The add-on of resol is 2.5% of Cr powder and Graphite Powder 99 gross weight.The vacuum tightness that grinding jar vacuumizes is 10
-2pa.
2) Ball-milling Time 5 hours.
3) vacuum tightness 10 of vacuum oven during sintering
-2pa; The heat-up rate of sintering oven is 10 ℃/sec; Pressure is 150MPa; Sintering temperature is 1350 ℃; Soaking time is 30 minutes.
Gained clean metal pottery Cr in this embodiment
7c
3block main performance index is as shown in table 2.
Embodiment 3
The processing step of the present embodiment is identical with embodiment 1, but some processing parameters are wherein slightly different:
1) Cr powder purity and granularity be respectively 99.9%, 50 μ m; Graphite Powder 99 purity and granularity are respectively
99.9%、90μm）。The add-on of resol is 3% of Cr powder and Graphite Powder 99 gross weight.
2) Ball-milling Time 15 hours.
3) vacuum tightness 10 of vacuum oven during sintering
-2pa; The heat-up rate of sintering oven is 8 ℃/sec; Pressure is 70MPa; Sintering temperature is 1450 ℃; Soaking time is 60 minutes.
Gained clean metal pottery Cr in this embodiment
7c
3block main performance index is as shown in table 2.
Clean metal pottery Cr under the different sintering temperatures of table 2 the present invention
7c
3the salient features of block
In mechanical milling process because Cr powder and Graphite Powder 99 all belong to crumbly mass, easily attached combining on ball milling tank skin of Graphite Powder 99 in this process, adopt the main purpose of resol be anchor stone ink powder in Cr powder, thereby to guarantee that carbon does not lose, make Cr powder and Graphite Powder 99 atomic ratio as 7:3.
Claims (4)
1. a clean metal pottery Cr
7c
3the preparation method of block, is characterized in that, comprises the following steps:
(1) pure Cr powder and pure Graphite Powder 99 are pressed to carbide Cr
7c
3the nucleidic mass of molecular formula Atom ratio and each element is converted into weight ratio, after weighing, packs in ball grinder, adds the resol of no more than pure Cr powder and pure Graphite Powder 99 gross weight 3% simultaneously, vacuumizes;
(2) ball grinder is put into ball mill start and rotated 5-20 hour, complete raw material and mix;
(3) mixture going out after tank is filled in graphite jig;
(4) graphite jig of filling mixture is put into sintering oven and carry out vacuum heating-press sintering, sintering temperature is 1200 ℃～1500 ℃; Be incubated 10～60 minutes;
(5) graphite jig after sintering is together cooling with sintering oven, takes out the sintered compact in graphite jig, obtains clean metal pottery Cr
7c
3block.
2. clean metal pottery Cr as claimed in claim 1
7c
3the preparation method of block, is characterized in that, the pure Cr powder that step (1) is described and the purity of pure Graphite Powder 99 are 99.9%, granularity all≤200 μ m.
3. clean metal pottery Cr as claimed in claim 1
7c
3the preparation method of block, is characterized in that, what step (1) was described vacuumizes, vacuum tightness≤10
-1pa.
4. clean metal pottery Cr as claimed in claim 1
7c
3the preparation method of block, is characterized in that, the described vacuum heating-press sintering of step (4), and its processing parameter is: vacuum tightness≤10
-1pa; Heat-up rate 5-10 ℃/sec; Pressure 0-150MPa.
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|---|---|---|---|
| CN201210378657.2A CN102876951B (en) | 2012-10-09 | 2012-10-09 | Method for preparing pure metal ceramic Cr7C3 block |
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|---|---|---|---|
| CN201210378657.2A CN102876951B (en) | 2012-10-09 | 2012-10-09 | Method for preparing pure metal ceramic Cr7C3 block |
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| CN102876951A CN102876951A (en) | 2013-01-16 |
| CN102876951B true CN102876951B (en) | 2014-04-23 |
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| CN201210378657.2A Expired - Fee Related CN102876951B (en) | 2012-10-09 | 2012-10-09 | Method for preparing pure metal ceramic Cr7C3 block |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451462B (en) * | 2013-08-01 | 2016-01-20 | 西安交通大学 | A kind of rare earth improves block Cr 7c 3the method of anti-erosion performance |
| CN103467100B (en) * | 2013-08-01 | 2015-04-29 | 西安交通大学 | Preparation method for corrosion-resistant and abrasion-resistant Cr7C3 |
| CN104480333A (en) * | 2014-11-24 | 2015-04-01 | 海安县鹰球粉末冶金有限公司 | Method of producing cermets by virtue of sintering method |
| CN106829963A (en) * | 2016-12-16 | 2017-06-13 | 吴中区穹窿山福顺生物技术研究所 | A kind of gear nano level metal carbide composite material and preparation method thereof |
| CN111118375B (en) * | 2020-01-16 | 2021-04-06 | 西安石油大学 | Chromium carbide-nickel-chromium metal ceramic block material and preparation method thereof |
| CN113086984A (en) * | 2021-05-27 | 2021-07-09 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of chromium carbide powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176224A (en) * | 1996-09-06 | 1998-03-18 | 汪兆泉 | Production process of chromium carbide |
| CN102154581A (en) * | 2011-03-23 | 2011-08-17 | 北京矿冶研究总院 | Preparation method of nano chromium carbide composite powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003013169A (en) * | 2001-04-27 | 2003-01-15 | Allied Material Corp | WC-Co FINE-PARTICULATE CEMENTED CARBIDE SUPERIOR IN OXIDATION RESISTANCE |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176224A (en) * | 1996-09-06 | 1998-03-18 | 汪兆泉 | Production process of chromium carbide |
| CN102154581A (en) * | 2011-03-23 | 2011-08-17 | 北京矿冶研究总院 | Preparation method of nano chromium carbide composite powder |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2003-13169A 2003.01.15 |
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