CN101403054A - Method for generating TiB2/Fe based composite material with reaction in-situ - Google Patents
Method for generating TiB2/Fe based composite material with reaction in-situ Download PDFInfo
- Publication number
- CN101403054A CN101403054A CNA2008100465412A CN200810046541A CN101403054A CN 101403054 A CN101403054 A CN 101403054A CN A2008100465412 A CNA2008100465412 A CN A2008100465412A CN 200810046541 A CN200810046541 A CN 200810046541A CN 101403054 A CN101403054 A CN 101403054A
- Authority
- CN
- China
- Prior art keywords
- powder
- ball milling
- titanium
- boron
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention relates to a method for generating TiB2/Fe base composite materials by reaction in-situ, which has the following process steps of: (1) batching, ferrotitanium powder and ferroboron powder, or iron powder and ferroboron powder, or boron powder and ferrotitanium powder, or ferrotitanium powder, ferroboron powder and iron powder, or titanium powder, ferroboron powder and iron powder, or boron powder, ferrotitanium powder and iron powder, or titanium powder, boron powder and iron powder are adopted as the material; the batching is conducted according to the content of the titanium and the boron in the material and the chemometry of the generated TiB2; (2) ball milling, the material prepared in the step (1) undergoes ball milling, wherein the ratio of the ball to the material is at least 1: 1, and the ball milling time is in the limit of milling the material into mixed powder with equal to or less than micron-size grain diameter; and (3) sintering, the mixed powder undergoing ball milling is loaded into a die and then put in a discharge plasma sintering device or an induction sintering device or a microwave plasma sintering device to be sintered under the pressure of at least 10MPa, at the sintering temperature of 950-1300 DEG C and the holding time of at least 5 seconds.
Description
Technical field
The invention belongs to the preparation method of Fe based composites, particularly a kind of with TiB
2Preparation method for the Fe based composites of strengthening phase.
Background technology
TiB
2It is unique stable compound of transiting group metal elements Ti and B, mutually with covalent bonds, its crystalline network is a close-packed hexagonal structure, boron atomic plane and titanium atom hand-deliver are for occurring, wherein the boron atom forms the two-dimensional network structure with covalent bonds, other contains very most of metalloid key, and this makes it have the special physicochemical performance, is a kind of very stable ultra hard ceramic material.TiB
2The hardness height is only second to diamond, cube BN and B
4C, fusing point are up to 3225 ℃, and be not only high temperature resistant, wear-resistant, corrosion-resistant, and have the favorable conductive heat conductivility.Therefore, TiB
2Receive much attention.
Traditional preparation TiB
2The method of/metal-base composites is mainly powder metallurgic method and smelting process.Powder metallurgic method is with after metal-powder and the ceramic powder mixing, compression moulding, and heat preservation sintering obtains TiB at a certain temperature then
2/ metal-base composites, the TiB that this method makes
2Not only there is certain hole in/metal-base composites, and has strengthening phase TiB in preparation process
2And the interface pollution problem between metallic matrix, and sintering time is longer, the energy consumption height.Smelting process is earlier with the metallic substance fusing, then with TiB
2Join in the liquid metal, not only there is TiB in this method
2Problem pockety, and have the interface pollution problem, influence TiB
2Reinforced effects.In addition, because TiB
2/ iron base composite material has good wear resisting property, also has process for treating surface such as adopting laser melting coating to generate TiB in the iron-based surface
2The report of wear-resistant coating, but there is complex process in process for treating surface, coat-thickness is limited, and with problem, prepared TiB such as matrix bond is not firm
2/ Fe based composites exists in the use and easily comes off, and microtexture, performance are inhomogeneous, component segregation, and the cladding area unrelieved stress is big, defective such as easily cracks.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of reaction in to generate TiB
2The method of/Fe based composites, this kind method not only technology is simple, and required time is short, and the TiB of original position formation
2Surface cleaning is pollution-free, and particle is tiny, is evenly distributed in matrix.
Reaction in of the present invention generates TiB
2The method of/Fe based composites, processing step is as follows:
(1) batching
With titanium-iron powder and ferro-boron powder, or titanium valve and ferro-boron powder, or boron powder and titanium-iron powder, or titanium-iron powder, ferro-boron powder and iron powder, titanium valve, ferro-boron powder and iron powder, or boron powder, titanium-iron powder and iron powder, or titanium valve, boron powder and iron powder be raw material, according to the content of titanium in the raw material and boron, according to generating TiB
2Stoichiometry prepare burden;
(2) ball milling
The raw material that step (1) is equipped with carries out ball milling, and ratio of grinding media to material was at least 1: 1, the ball milling time with raw material become≤mixed powder of micron order particle diameter exceeds;
(3) sintering
With the mould of packing into of the mixed powder behind the ball milling, put into then in discharge plasma agglomerating plant or induction sintering equipment or the microwave plasma sintering equipment, be at least sintering under the 10MPa at pressure, sintering temperature is 950 ℃～1300 ℃, soaking time was at least for 5 seconds, promptly made the TiB that reaction in generates
2/ Fe based composites.
Simplify in order to make charging at sintering step, can after the ball milling step of aforesaid method, before the sintering step, increase the precompressed step, described precompressed is the mixed powder behind the ball milling to be packed in the precompressed mould into (pressure is at least 10MPa in extrusion forming, time was at least for 5 seconds), the cavity shape of the cavity shape of precompressed mould and size and sintering mould and measure-alike.
The rare gas element that prevents the raw material oxidation for the oxidation inhibitor that prevents from the raw material oxidation, can add to prevent the raw material oxidation or feeding during ball milling.Oxidation inhibitor be in the mechanical milling process not with the liquid organic material of raw material generation chemical reaction, preferred acetone or dehydrated alcohol, the add-on of acetone or dehydrated alcohol is to flood abrading-ball and raw material exceeds.Preferred argon gas of rare gas element or helium.
The present invention has following beneficial effect:
1, the TiB of the method for the invention original position formation
2Surface cleaning is pollution-free, and particle is tiny, is evenly distributed in matrix, helps the raising of composite materials property.
2, the method for the invention adopts discharge plasma sintering or induction sintering or microwave plasma sintering, thereby can shorten preparation time greatly, and save energy reduces preparation cost.
3, the method for the invention is simple, and raw material is easy to obtain, and is convenient to suitability for industrialized production.
Description of drawings
Fig. 1 is the TiB with the method for the invention preparation
2The X-ray diffractogram of/Fe based composites.
Embodiment
Embodiment 1
Present embodiment is that the titanium-iron powder (titaniferous 41.23wt%) of FeTi40-A and ferro-boron powder (boracic 18.15wt%) that the trade mark is FeB17C0.1 are raw material with the trade mark, adopts the discharge plasma sintering, and processing step is as follows:
(1) batching
According to the atomic ratio of Ti and B is to prepare burden at 1: 2, takes by weighing titanium-iron powder 64.2g, ferro-boron powder 65.8g.
(2) ball milling
Adopt YMJ-II type ball mill, the raw material that step (1) is equipped with is put into stainless steel jar mill, ratio of grinding media to material is 1: 1, adds oxidation inhibitor acetone, and the add-on of acetone is to flood abrading-ball and raw material exceeds, 6 hours ball milling time.After ball milling finishes ball grinder is opened, treat the acetone volatilization after, the mixed powder after grinding vacuum plastic sealing is standby.
(3) precompressed
Take by weighing step (2) mixed powder after grinding 10g, put into the mould of Φ 20, apply the pressure pre-molding of 50MPa, the time was 5 seconds;
(4) sintering
With pack into the graphite jig of Φ 20 of the blank of step (3) pre-molding, (agglomerating plant is SPS-1050 to put the discharge plasma agglomerating plant then into, Japan helps friendly coal mining industry Co., Ltd. to make) in, under pressure 50MPa, heat-up rate with 50 ℃/min rises to 10 minutes postcooling of 950 ℃ of insulations to room temperature with temperature, promptly makes the TiB that reaction in generates
2/ Fe based composites.
Embodiment 2
Present embodiment is that the titanium-iron powder (titaniferous 26.75wt%) of FeTi30-A and ferro-boron powder (boracic 20.06wt%) that the trade mark is FeB22C0.1 are raw material with the trade mark, adopts the discharge plasma sintering, and processing step is as follows:
(1) batching
According to the atomic ratio of Ti and B is to prepare burden at 1: 2, takes by weighing titanium-iron powder 81.1g, ferro-boron powder 48.9g.
(2) ball milling
Adopt YMJ-II type ball mill, the raw material that step (1) is equipped with is put into stainless steel jar mill, ratio of grinding media to material is 3: 1, adds the oxidation inhibitor dehydrated alcohol, and the add-on of dehydrated alcohol is to flood abrading-ball and raw material exceeds, 1 hour ball milling time.After ball milling finishes ball grinder is opened, treat absolute ethanol volatilizes after, the mixed powder after grinding vacuum plastic sealing is standby.
(3) precompressed
Take by weighing step (2) mixed powder after grinding 10g, put into the mould of Φ 20, apply the pressure pre-molding of 40MPa, the time is 1 minute;
(4) sintering
With pack into the graphite jig of Φ 20 of the blank of step (3) pre-molding, (agglomerating plant is SPS-1050 to put the discharge plasma agglomerating plant then into, Japan helps friendly coal mining industry Co., Ltd. to make) in, under pressure 30MPa, heat-up rate with 80 ℃/min rises to 5 minutes postcooling of 1050 ℃ of insulations to room temperature with temperature, promptly makes the TiB that reaction in generates
2/ Fe based composites, its X-ray diffractogram as shown in Figure 1.
Embodiment 3
Present embodiment is that the ferro-boron powder (boracic 20.06wt%) of FeB22C0.1 is a raw material with the industrial titanium valve (titaniferous 97.00wt%) and the trade mark, adopts the discharge plasma sintering, and processing step is as follows:
(1) batching
According to the atomic ratio of Ti and B is to prepare burden at 1: 2, takes by weighing titanium valve 40.8g, ferro-boron powder 89.2g.
(2) ball milling
Adopt YMJ-II type ball mill, the raw material that step (1) is equipped with is put into stainless steel jar mill, ratio of grinding media to material is 2: 1, feeds argon gas in ball grinder, and the feeding amount is 1 standard atmospheric pressure.3 hours ball milling time, ball milling after finishing is opened ball grinder, and the mixed powder after grinding vacuum plastic sealing is standby.
(3) sintering
Mixed powder behind step (2) ball milling is taken by weighing pack into the graphite jig of Φ 20 of 10g, (agglomerating plant is SPS-1050 to put the discharge plasma agglomerating plant then into, Japan helps friendly coal mining industry Co., Ltd. to make) in, under pressure 30MPa, heat-up rate with 100 ℃/min rises to 1 minute postcooling of 1100 ℃ of insulations to room temperature with temperature, promptly makes the TiB that reaction in generates
2/ Fe based composites.
Embodiment 4
Present embodiment is that ferro-boron powder (boracic 20.06wt%) and the technical pure iron powder of FeB22C0.1 is raw material with industrial titanium valve (titaniferous 97.00wt%), the trade mark, adopts the discharge plasma sintering, and processing step is as follows:
(1) batching
According to the atomic ratio of Ti and B is to prepare burden at 1: 2, takes by weighing titanium valve 27.7g, ferro-boron powder 60.5g, iron powder 41.8g.
(2) ball milling
Adopt YMJ-II type ball mill, the raw material that step (1) is equipped with is put into stainless steel jar mill, ratio of grinding media to material is 3: 1, feeds helium in ball grinder, and the feeding amount is 1 standard atmospheric pressure.2 hours ball milling time, ball milling after finishing is opened ball grinder, and the mixed powder after grinding vacuum plastic sealing is standby.
(3) precompressed
Take by weighing step (2) mixed powder after grinding 10g, put into the mould of Φ 20, apply the pressure pre-molding of 10MPa, the time is 2 minutes;
(4) sintering
With pack into the graphite jig of Φ 20 of the blank of step (3) pre-molding, (agglomerating plant is SPS-1050 to put the discharge plasma agglomerating plant then into, Japan helps friendly coal mining industry Co., Ltd. to make) in, under pressure 30MPa, heat-up rate with 150 ℃/min rises to 1200 ℃ of insulation postcooling in 5 second to room temperature with temperature, promptly makes the TiB that reaction in generates
2/ Fe based composites.
Embodiment 5
Present embodiment is that the titanium-iron powder (titaniferous 26.75wt%) of FeTi30-A and ferro-boron powder (boracic 20.06wt%) that the trade mark is FeB22C0.1 are raw material with the trade mark, adopts the Medium frequency induction sintering, and processing step is as follows:
(1) batching
According to the atomic ratio of Ti and B is to prepare burden at 1: 2, takes by weighing titanium-iron powder 81.1g, ferro-boron powder 48.9g.
(2) ball milling
Adopt YMJ-II type ball mill, the raw material that step (1) is equipped with is put into stainless steel jar mill, ratio of grinding media to material is 3: 1, adds oxidation inhibitor acetone, and the add-on of acetone is to flood abrading-ball and raw material exceeds, 2 hours ball milling time.After ball milling finishes ball grinder is opened, treat the acetone volatilization after, the mixed powder after grinding vacuum plastic sealing is standby.
(3) precompressed
Take by weighing step (2) mixed powder after grinding 10g, put into the mould of Φ 20, apply the pressure pre-molding of 40MPa, the time is 1 minute;
(4) sintering
With pack into the graphite jig of Φ 20 of the blank of step (3) pre-molding, put into then in the Medium frequency induction agglomerating plant, under pressure 40MPa, with the heat-up rate of 160 ℃/min temperature is risen to 3 minutes postcooling of 1250 ℃ of insulations to room temperature, promptly make the TiB that reaction in generates
2/ Fe based composites.
Embodiment 6
Present embodiment is that the titanium-iron powder (titaniferous 26.75wt%) of FeTi30-A and ferro-boron powder (boracic 20.06wt%) that the trade mark is FeB22C0.1 are raw material with the trade mark, adopts microwave plasma sintering, and processing step is as follows:
(1) batching
According to the atomic ratio of Ti and B is to prepare burden at 1: 2, takes by weighing titanium-iron powder 81.1g, ferro-boron powder 48.9g.
(2) ball milling
Adopt YMJ-II type ball mill, the raw material that step (1) is equipped with is put into stainless steel jar mill, ratio of grinding media to material is 4: 1, adds the oxidation inhibitor dehydrated alcohol, and the add-on of dehydrated alcohol is to flood abrading-ball and raw material exceeds, 1.5 hours ball milling time.After ball milling finishes ball grinder is opened, treat absolute ethanol volatilizes after, the mixed powder after grinding vacuum plastic sealing is standby.
(3) precompressed
Take by weighing step (2) mixed powder after grinding 10g, put into the mould of Φ 20, apply the pressure pre-molding of 40MPa, the time is 1 minute;
(4) sintering
With pack into the graphite jig of Φ 20 of the blank of step (3) pre-molding, put into then in the microwave plasma sintering equipment, under pressure 10MPa, with the heat-up rate of 130 ℃/min temperature is risen to 1300 ℃ of insulation postcooling in 30 second to room temperature, promptly make the TiB that reaction in generates
2/ Fe based composites.
Claims (5)
1, a kind of reaction in generates TiB
2The method of/Fe based composites is characterized in that processing step is as follows:
(1) batching
With titanium-iron powder and ferro-boron powder, or titanium valve and ferro-boron powder, or boron powder and titanium-iron powder, or titanium-iron powder, ferro-boron powder and iron powder, titanium valve, ferro-boron powder and iron powder, or boron powder, titanium-iron powder and iron powder, or titanium valve, boron powder and iron powder be raw material, according to the content of titanium in the raw material and boron, according to generating TiB
2Stoichiometry prepare burden;
(2) ball milling
The raw material that step (1) is equipped with carries out ball milling, and ratio of grinding media to material was at least 1: 1, the ball milling time with raw material become≤mixed powder of micron order particle diameter exceeds;
(3) sintering
With the mould of packing into of the mixed powder behind the ball milling, put into then in discharge plasma agglomerating plant or induction sintering equipment or the microwave plasma sintering equipment, be at least sintering under the 10MPa at pressure, sintering temperature is 950 ℃～1300 ℃, soaking time was at least for 5 seconds, promptly made the TiB that reaction in generates
2/ Fe based composites.
2, reaction in according to claim 1 generates TiB
2The method of/Fe based composites, it is characterized in that after the ball milling step, increase the precompressed step before the sintering step, described precompressed is with the extrusion forming in the precompressed mould of packing into of the mixed powder behind the ball milling, the cavity shape of the cavity shape of precompressed mould and size and sintering mould and measure-alike.
3, reaction in according to claim 1 and 2 generates TiB
2The method of/Fe based composites, adding prevents the oxidation inhibitor of raw material oxidation or the rare gas element that feeding prevents the raw material oxidation when it is characterized in that ball milling.
4, reaction in according to claim 3 generates TiB
2The method of/Fe based composites is characterized in that oxidation inhibitor is acetone or dehydrated alcohol, and the add-on of acetone or dehydrated alcohol is to flood abrading-ball and raw material exceeds.
5, reaction in according to claim 3 generates TiB
2The method of/Fe based composites is characterized in that rare gas element is argon gas or helium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100465412A CN101403054B (en) | 2008-11-13 | 2008-11-13 | Method for generating TiB2/Fe based composite material by in-situ reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100465412A CN101403054B (en) | 2008-11-13 | 2008-11-13 | Method for generating TiB2/Fe based composite material by in-situ reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101403054A true CN101403054A (en) | 2009-04-08 |
| CN101403054B CN101403054B (en) | 2010-10-13 |
Family
ID=40537212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100465412A Active CN101403054B (en) | 2008-11-13 | 2008-11-13 | Method for generating TiB2/Fe based composite material by in-situ reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101403054B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102699495A (en) * | 2011-12-28 | 2012-10-03 | 佳木斯大学 | Method for preparing TiB2 metal ceramic wear-resistant coating |
| CN105950952A (en) * | 2016-07-06 | 2016-09-21 | 昆明理工大学 | Production method for in-situ generation of titanium zirconium boride reinforced high-modulus and high-hardness steel |
| CN109055860A (en) * | 2018-09-07 | 2018-12-21 | 吉林大学 | One specific admixture scale TiCN and TiB2Particle Strengthening and Toughening low-alloy steel and preparation method thereof |
| CN112251676A (en) * | 2020-10-22 | 2021-01-22 | 北京华锦源耐磨材料有限公司 | Composite wear-resistant steel plate and preparation method thereof |
| CN115626859A (en) * | 2022-11-30 | 2023-01-20 | 矿冶科技集团有限公司 | Metal composite boron powder and preparation method thereof |
-
2008
- 2008-11-13 CN CN2008100465412A patent/CN101403054B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102699495A (en) * | 2011-12-28 | 2012-10-03 | 佳木斯大学 | Method for preparing TiB2 metal ceramic wear-resistant coating |
| CN102699495B (en) * | 2011-12-28 | 2015-06-24 | 佳木斯大学 | Method for preparing TiB2 metal ceramic wear-resistant coating |
| CN105950952A (en) * | 2016-07-06 | 2016-09-21 | 昆明理工大学 | Production method for in-situ generation of titanium zirconium boride reinforced high-modulus and high-hardness steel |
| CN109055860A (en) * | 2018-09-07 | 2018-12-21 | 吉林大学 | One specific admixture scale TiCN and TiB2Particle Strengthening and Toughening low-alloy steel and preparation method thereof |
| CN112251676A (en) * | 2020-10-22 | 2021-01-22 | 北京华锦源耐磨材料有限公司 | Composite wear-resistant steel plate and preparation method thereof |
| CN112251676B (en) * | 2020-10-22 | 2022-05-03 | 北京华锦源耐磨材料有限公司 | Composite wear-resistant steel plate and preparation method thereof |
| CN115626859A (en) * | 2022-11-30 | 2023-01-20 | 矿冶科技集团有限公司 | Metal composite boron powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101403054B (en) | 2010-10-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101880808B (en) | Method for preparing nano oxide dispersion reinforced superfine crystal tungsten-based composite material | |
| CN111992708B (en) | Method for preparing high-performance diamond/copper composite material | |
| CN101403054B (en) | Method for generating TiB2/Fe based composite material by in-situ reaction | |
| CN110257684B (en) | Preparation process of FeCrCoMnNi high-entropy alloy-based composite material | |
| CN103071793B (en) | Molybdenum sputtering target material hot isostatic pressure production method | |
| WO2020042949A1 (en) | Highly oriented nanometer max phase ceramic and preparation method for max phase in-situ autogenous oxide nanocomposite ceramic | |
| CN109338172A (en) | A kind of 2024 aluminum matrix composites and preparation method thereof of high-entropy alloy enhancing | |
| CN106929845B (en) | Method for preparing iron-based amorphous and nanocrystalline coating | |
| CN102703742A (en) | Metal-based composite material with substrate of nano laminated structure and preparation method thereof | |
| CN105272260B (en) | A kind of soap-free emulsion polymeization phase tungsten carbide composite and preparation method thereof | |
| CN103464764B (en) | Metal matrix wear-resistant corrosion-resistant surface coating composite and preparation method thereof | |
| CN110395733B (en) | Titanium-aluminum-carbon material capable of being etched in water, preparation method thereof and preparation method of organ-shaped material | |
| CN107473237B (en) | Preparation method of binary tungsten boride superhard material | |
| CN103726046B (en) | Method for preparing compound coatings through laser shock induced chemical reaction | |
| CN107140987A (en) | A kind of Os2B3Hard material and its preparation and application | |
| CN101508572B (en) | Quick production method for high-compact single-phase TiB2 | |
| Zhang et al. | Preparation and properties of Ti (C, N)-based cermets with graphene nanosheet addition by spark plasma sintering | |
| CN107285329B (en) | Tungsten diboride hard material and preparation method and application thereof | |
| CN104232961A (en) | High-strength high-hardness Cu-Cr composite material as well as preparation method and application thereof | |
| CN104032253A (en) | Ti-B-C-N ceramic coating and preparation method thereof | |
| CN104451325A (en) | Process for preparing Mo2FeB2-based metal ceramic | |
| CN102392149B (en) | Method for microwave sintering preparation of nano-metric rare earth modified steel-bonded hard alloy | |
| Nguyen et al. | Synthesis of YB2C2 by high‐energy ball milling and reactive spark plasma sintering | |
| CN105506330B (en) | Microwave liquid-phase sintering process composite porous high temperature resistant TiAl | |
| CN112813393B (en) | Molybdenum-nickel alloy target and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |