CN102876951A - Method for preparing pure metal ceramic Cr7C3 block - Google Patents
Method for preparing pure metal ceramic Cr7C3 block Download PDFInfo
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- CN102876951A CN102876951A CN2012103786572A CN201210378657A CN102876951A CN 102876951 A CN102876951 A CN 102876951A CN 2012103786572 A CN2012103786572 A CN 2012103786572A CN 201210378657 A CN201210378657 A CN 201210378657A CN 102876951 A CN102876951 A CN 102876951A
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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 have the orthohormbic structure transition metal carbide, have the character of pottery.Its hardness is high, wear resistance good, and preferably toughness, good advantages such as oxidation-resistance and thermostability can be applied in the component of machine surface of low-cost steel grade, improve surface abrasion performance and resistance to high temperature corrosion.In theory, Chinese scholars is mainly used 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 used plasma and is covered molten technology and prepare one deck with Cr at steel surface
7C
3Be the compound coating of hard phase, remove Cr in the coating structure
7C
3, also have matrix such as austenite structure etc. outward, and the thinner thickness of this layer coating, in practical engineering application, still can't satisfy the requirement of high life.The foreign scholar prepares single-phase Cr at present
7C
3Main method of attempting has: (a) method by thermospray prepares one deck Cr
7C
3Film; (b) plasma activated sintering; (c) the 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
3The block 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
3Resulting block tissue is except Cr is arranged in this report
7C
3Also has Cr outward,
2O
3Phase is not pure single Cr obviously
7C
3The compound block.
Japanese scholars Ken Hirota etc. behind Cr and carbon powder machinery wet-milling mixing, have prepared single-phase block Cr with spark plasma sintering
7C
3Its performance is as shown in table 1.Although the Main Mechanical index is more satisfactory, equally do not obtain pure single Cr yet
7C
3The compound 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 purpose, 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, may further comprise the steps:
(1) pure Cr powder and pure Graphite Powder 99 are pressed carbide Cr
7C
3The molecular formula Atom is converted into weight ratio than the nucleidic mass with each element, in the grinding jar of packing into after weighing, adds simultaneously the resol of no more than Cr powder and Graphite Powder 99 gross weight 3%, vacuumizes:
(2) ball grinder is put into the ball mill start and rotated 5-20 hour, finish raw material and mix;
The mixture that (3) will go out behind the tank is filled in the 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 behind the sintering together cools off with sintering oven, takes out the sintered compact in the graphite jig, namely obtains clean metal pottery Cr
7C
3Block.
In the aforesaid method, the purity of the described Cr powder of step (1) and Graphite Powder 99 is 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.
Described the vacuumizing of step (1), 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 ℃/second; Pressure 0-150Mpa.
Advantage of the present invention is that preparation process is simple, resulting pure single Cr
7C
3Compound block relative density is higher, and the Main Mechanical index is better, and not only be suitable for wear-resisting field occasion, and can also be used for anti-corrosion field, and wear-resisting, anti-corrosion mutual field.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1
At first, with 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) press Cr
7C
3The molecular formula Atom than and the nucleidic mass of each element be converted into weight ratio, in the stainless steel jar mill of packing into after weighing, add simultaneously the resol of Cr powder and Graphite Powder 99 gross weight 0.5%, vacuumize that (vacuum tightness is 10
-1Pa).
Then, ball grinder is put into ball mill start rotate, ball milling is after 20 hours, and the mixture of Cr powder, Graphite Powder 99 and resol is filled in the graphite jig.
At last, the graphite jig of filling Cr powder, Graphite Powder 99 and resol mixture is put into vacuum sintering funace carry out sintering, the vacuum tightness 10 of vacuum oven during sintering
-1Pa; The heat-up rate of sintering oven is 5 ℃/second; Pressure is 0MPa; Sintering temperature is 1200 ℃; Soaking time is 10 minutes, together cools off with sintering oven after sintering is complete, takes out the sintered compact in the graphite jig, namely 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 wherein are slightly different:
1) Cr powder purity and granularity are 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 is 5 hours.
3) vacuum tightness 10 of vacuum oven during sintering
-2Pa; The heat-up rate of sintering oven is 10 ℃/second; Pressure is 150MPa; Sintering temperature is 1350 ℃; Soaking time is 30 minutes.
Gained clean metal pottery Cr among this embodiment
7C
3The block 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 wherein are slightly different:
1) Cr powder purity and granularity are 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 is 15 hours.
3) vacuum tightness 10 of vacuum oven during sintering
-2Pa; The heat-up rate of sintering oven is 8 ℃/second; Pressure is 70MPa; Sintering temperature is 1450 ℃; Soaking time is 60 minutes.
Gained clean metal pottery Cr among this embodiment
7C
3The block 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, easy attached the combining on the ball milling tank skin of Graphite Powder 99 in this process, the main purpose that adopts resol be the anchor stone ink powder in the Cr powder, thereby make Cr powder and Graphite Powder 99 atomic ratio as 7:3 to guarantee that carbon does not lose.
Claims (4)
1. clean metal pottery Cr
7C
3The preparation method of block is characterized in that, may further comprise the steps:
(1) pure Cr powder and pure Graphite Powder 99 are pressed carbide Cr
7C
3The molecular formula Atom is converted into weight ratio than the nucleidic mass with each element, in the grinding jar of packing into after weighing, adds simultaneously the resol of no more than Cr powder and Graphite Powder 99 gross weight 3%, vacuumizes:
(2) ball grinder is put into the ball mill start and rotated 5-20 hour, finish raw material and mix;
The mixture that (3) will go out behind the tank is filled in the 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 behind the sintering together cools off with sintering oven, takes out the sintered compact in the graphite jig, namely obtains clean metal pottery Cr
7C
3Block.
2. clean metal as claimed in claim 1 pottery Cr
7C
3The preparation method of block is characterized in that, the purity of the described Cr powder of step (1) and Graphite Powder 99 is 99.9%, granularity all≤200 μ m.
3. clean metal as claimed in claim 1 pottery Cr
7C
3The preparation method of block is characterized in that, described the vacuumizing of step (1), vacuum tightness≤10
-1Pa).
4. the described vacuum heating-press sintering of step (4), its processing parameter is: vacuum tightness≤10
-1Pa; Heat-up rate 5-10 ℃/second; Pressure 0-150Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210378657.2A CN102876951B (en) | 2012-10-09 | 2012-10-09 | Method for preparing pure metal ceramic Cr7C3 block |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210378657.2A CN102876951B (en) | 2012-10-09 | 2012-10-09 | Method for preparing pure metal ceramic Cr7C3 block |
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| Publication Number | Publication Date |
|---|---|
| CN102876951A true CN102876951A (en) | 2013-01-16 |
| CN102876951B CN102876951B (en) | 2014-04-23 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451462A (en) * | 2013-08-01 | 2013-12-18 | 西安交通大学 | Method for improving abrasion resistance of block Cr7C3 by using rare earth |
| CN103467100A (en) * | 2013-08-01 | 2013-12-25 | 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 |
| CN111118375A (en) * | 2020-01-16 | 2020-05-08 | 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176224A (en) * | 1996-09-06 | 1998-03-18 | 汪兆泉 | Production process of chromium carbide |
| JP2003013169A (en) * | 2001-04-27 | 2003-01-15 | Allied Material Corp | WC-Co FINE-PARTICULATE CEMENTED CARBIDE SUPERIOR IN OXIDATION RESISTANCE |
| CN102154581A (en) * | 2011-03-23 | 2011-08-17 | 北京矿冶研究总院 | Preparation method of nano chromium carbide composite powder |
-
2012
- 2012-10-09 CN CN201210378657.2A patent/CN102876951B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1176224A (en) * | 1996-09-06 | 1998-03-18 | 汪兆泉 | Production process of chromium carbide |
| JP2003013169A (en) * | 2001-04-27 | 2003-01-15 | Allied Material Corp | WC-Co FINE-PARTICULATE CEMENTED CARBIDE SUPERIOR IN OXIDATION RESISTANCE |
| CN102154581A (en) * | 2011-03-23 | 2011-08-17 | 北京矿冶研究总院 | Preparation method of nano chromium carbide composite powder |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451462A (en) * | 2013-08-01 | 2013-12-18 | 西安交通大学 | Method for improving abrasion resistance of block Cr7C3 by using rare earth |
| CN103467100A (en) * | 2013-08-01 | 2013-12-25 | 西安交通大学 | Preparation method for corrosion-resistant and abrasion-resistant Cr7C3 |
| CN103467100B (en) * | 2013-08-01 | 2015-04-29 | 西安交通大学 | Preparation method for corrosion-resistant and abrasion-resistant Cr7C3 |
| 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 |
| 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 |
| CN111118375A (en) * | 2020-01-16 | 2020-05-08 | 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 |
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| Publication number | Publication date |
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| CN102876951B (en) | 2014-04-23 |
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Granted publication date: 20140423 Termination date: 20161009 |