CN101736211B - SiC crystal whisker reinforced and toughened Mo2FeB2 matrix metal ceramic and preparation method thereof - Google Patents
SiC crystal whisker reinforced and toughened Mo2FeB2 matrix metal ceramic and preparation method thereof Download PDFInfo
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- 239000002184 metal Substances 0.000 title claims abstract description 43
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000013078 crystal Substances 0.000 title claims abstract description 14
- 239000011159 matrix material Substances 0.000 title abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 33
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- 238000012986 modification Methods 0.000 claims abstract description 8
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
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- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 2
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Abstract
The invention discloses SiC crystal whisker reinforced and toughened Mo2FeB2 matrix metal ceramic and a preparation method thereof, belonging to the technical field of metal matrix composite materials. The metal ceramic comprises the following components in parts by weight: 30-36 parts of Fe, 0.3-1.2 parts of SiC, 45-52 parts of Mo, 5.3-6.5 parts of B, 0.4-1.0 part of C, 2.5-4.5 parts of Ni, 2.0-4.0 parts of Cr, and 2.0-10.0 parts of Mn. The preparation method is characterized by comprising the following steps of: firstly carrying out surface modification treatment on SiC crystal whiskers by adopting plasmas, then ultrasonically dispersing, adding the SiC crystal whiskers as an additive into a mixture, preparing the mixture according with a component requirement, and sequentially carrying out the steps of mixing materials, molding, degreasing, and vacuum sintering to obtain a metal ceramic sintered body. The material has the advantages of high hardness, high bending strength, high fracture toughness and the like.
Description
Technical field
The invention belongs to stupalith and preparation method thereof, relate to silicon carbide whisker and strengthen toughness reinforcing Mo
2FeB
2Based ceramic metal and preparation method thereof.
Background technology
Metal boride has high rigidity, high-melting-point, higher heat conductivity and high-temperature stability, thereby the agglomerated material (boride-base cerment) of itself and metal composite has great potential and wide application prospect as tool die material and wear-resisting, corrosion-resistant and high-temperature material.Compare with the WC-Co Wimet, have following advantage: (1) as tool and mould, and in the course of the work, the abrasion loss of himself abrasion loss and machined material is all smaller; (2) high temperature resistant and corrosion resistance nature is more excellent; During (3) as the coating of steel matrix, and the bonding strength between the matrix is higher; (4) density only is 3/5ths of Wimet; (5) have the favorable conductive rate, be fit to be processed into complicated shape; (6) do not contain this strategic material of Co, also do not contain this more expensive compound of WC, used starting material are element commonly used, that easily obtain, and its manufacturing cost is cheap more many than Wimet.What study morely at present is with TiB
2, ZrB
2Etc. the binary boride is the sintering metal of base.Such sintering metal is when sintering, and matrix metal is not good to the wettability of boride particle, and coking property is relatively poor, be difficult to obtain fine and close sintered compact, and boride also can react generation fragility mutually with matrix metal mutually when sintering.In addition, all be high-purity starting material owing to what adopt, thereby manufacturing cost is higher.Above-mentioned reason makes that the development of high-density high-strength boride-base cerment is very difficult, and for this reason, people have tested multiple sintering aid, make the over-all properties of this material obtain raising to a certain degree, but its comprehensive mechanical property are still lower.Adopt the activated sintering method, make binary boride and metal reaction generate ternary boride, can obtain the ternary boride-based metal pottery that boride crystal grain is tiny and be evenly distributed, be expected to address the above problem.In recent years, country such as Japan, America and Europe is more and more to the research of ternary boride-based metal pottery, is applied in field such as wear-resisting, corrosion-resistant.At present, mainly carried out Mo
2NiB
2, Mo
2FeB
2, several individual system such as WCoB based ceramic metal research, wherein to Mo
2FeB
2Based ceramic metal is studied at most.Be the further performance that improves material, method commonly used at present is to optimize the composition of material, improvement sintering process, crystal grain thinning.The representative Mo that table 1 is developed for Japan
2FeB
2The performance of based ceramic metal (Takagi K.Development and application of high strength ternary boride base cermets.J Solid State Chem 2006; 179:2809-18.).The Mo that has developed at present
2FeB
2The problem that based ceramic metal in use reflects is that hardness is generally on the low side, in other words, if make material keep higher hardness, can't make it have higher intensity and toughness simultaneously.
The Mo of table 1 Japan development
2FeB
2The physicals of based ceramic metal
Domestic scholars mainly is on abroad the research basis, to utilize Mo
2FeB
2Based ceramic metal and steel good binding performance prepare Mo on steel matrix
2FeB
2The based ceramic metal coating.But, for Mo
2FeB
2The alloying of based ceramic metal and technology of preparing itself are studied seldom, and be bigger with external gap, and prepared material obdurability is obviously on the low side.
In view of the foregoing, be necessary Mo
2FeB
2Base metal-ceramic material is is further researched and developed, and makes it when having premium propertiess such as very high hardness, wear resistance, red hardness, corrosion resistance nature, also has very high intensity and toughness.Only in this way, this kind material is found application on the tool and mould market at home, and apply it under the harsh service condition such as high temperature, burn into wearing and tearing, replace a large amount of at present WC-Co Wimet that use, be widely used in industries such as machinery, metallurgy, automobile, petrochemical industry, mine.
Summary of the invention
The objective of the invention is present situation, provide a kind of with low cost, not only have very high hardness, and have higher intensity and the toughness reinforcing Mo of flexible silicon carbide whisker enhancing at prior art
2FeB
2Based ceramic metal and preparation method thereof.
Realize the crystal whisker reinforced and toughened Mo of this SiC of the present invention
2FeB
2Based ceramic metal is characterized in that: its composition mass fraction is: Fe is 30～36, and the SiC whisker is 0.3～1.2, and Mo is 45～52, and B is 5.3～6.5, and C is 0.4～1.0, and Ni is 2.5～4.5, and Cr is 2.0～4.0, and Mn is 2.0～10.0.
The present invention is the crystal whisker reinforced and toughened Mo of SiC as previously mentioned
2FeB
2The preparation method of based ceramic metal in turn includes the following steps:
(1) first using plasma carries out surface modification treatment to the SiC whisker, in the glow discharge plasma stove, carry out, in the glow discharge plasma treating processes, used purity of argon 〉=99.0%, charging into the interior argon pressure of furnace chamber is 20-100Pa, operating voltage is 500-700V, and working current is 0.1-0.3A, and the treatment time is 90-180min; Carry out ultra-sonic dispersion then;
(2) preparation meets the compound of following requirement, and its composition mass fraction is: Fe is 30～36, and the SiC whisker is 0.3～1.2, and Mo is 45～52, and B is 5.3～6.5, and C is 0.4～1.0, and Ni is 2.5～4.5, and Cr is 2.0～4.0, and Mn is 2.0～10.0;
(3) batch mixing, compounding process carry out in planetary ball mill;
(4) add forming agent, the forming agent that is added is a polyvinyl alcohol, and additional proportion is the 3mass%-8mass% of compound;
(5) compression moulding, used pressing pressure are 120-250MPa;
(6) degreasing is carried out in vacuum tightness is higher than the vacuum oven of 10Pa, and the heat-up rate between 200-400 ℃ is 0.3-0.5 ℃/min;
(7) vacuum sintering is carried out in vacuum sintering furnace, and vacuum tightness is higher than 5.0 * 10
-2Pa, sintering temperature is 1160-1250 ℃, soaking time is 20-60min.
For realizing this purpose, in composition, add a spot of SiC whisker and a certain amount of Mn.Preparation method's characteristics are: first using plasma carries out surface modification treatment to the SiC whisker, carry out ultra-sonic dispersion then, with it as additive, join in the compound, preparation meets the compound of composition requirement, obtains the sintering metal sintered compact through batch mixing, moulding, degreasing, vacuum sintering successively.The SiC whisker is by behind the plasma bombardment, its surfactivity strengthens, and the whisker that twines is dispersed, and combine with the interface of sintering metal matrix to be improved behind sintering, and to turn to mechanism that material is strengthened toughness reinforcing for final main extract bridging and crackle by whisker; Add an amount of Mn in this sintering metal, liquid phase formation temperature when having reduced sintering has improved the wettability of liquid phase to solid phase, thereby has improved the density of sintered compact, simultaneously part Mn also can solid solution in ceramic phase Mo
2FeB
2In, substitute part Fe atom, changed the valence electron structure of this phase, improved the intrinsic fragility of this phase, thereby made the obdurability of sintering metal sintered compact be able to further raising.
The Mo that SiC of the present invention is crystal whisker reinforced and toughened
2FeB
2Based ceramic metal, its hardness HRA 〉=90.5, bending strength σ
b〉=2100MPa, fracture toughness property K
IC〉=19MNm
-3/2This material not only have higher hardness, wear resistance, erosion resistance, excellent chemical stability, and non-ferrous metal such as copper, zinc and alloy thereof between advantage such as extremely low avidity and frictional coefficient, and its obdurability is also very good, can be used for making the instrument that is used for conventional engineering material processing, be particularly suitable for making the instrument that is used for non-ferrous metal processing.Compare with Wimet, when being used to cut General Structural Steel, it can allow the depth of cut to improve 1-3 doubly, and cutting speed improves more than 1 times; When cutting copper alloy, its durability all improves more than 4 times; When as mold hot extruding copper alloy section bar, compare with existing sintered-carbide die work-ing life and improved 5～20 times.This material also is suitable for making injection mold, automobile valve heat and forges the self-lubricating cylinder liner of mould, air compressor and hydrogen pump, sea-water pump bearing etc.In addition, the crystal whisker reinforced and toughened Mo of SiC of the present invention
2FeB
2The bonding strength of based ceramic metal and steel is than higher, and this material also can be widely used in fields such as wearing piece, high temperature resistant, corrosion barrier.
Embodiment
Further specify technique effect of the present invention below in conjunction with example.The raw material that following example adopted is FeB, FeMo, Fe, Mn, Ni, Cr, graphite, SiC whisker.
Table 2 is compounds of 4 kinds of component prescriptions.Adopt different processing parameters that it is prepared into Mo
2FeB
2Based ceramic metal, and measure its hardness, bending strength and fracture toughness property respectively.
The composition proportion of 4 kinds of compounds of table 2
Embodiment 1:
In the glow discharge plasma stove, using plasma carries out surface modification treatment to the SiC whisker.Charging into the interior argon pressure of furnace chamber is 20Pa, and operating voltage is 500V, and working current is 0.1A, and the treatment time is 180min;
Batch mixing, compounding process carry out in planetary ball mill, and drum's speed of rotation is 160rpm, and the time is 24h;
The add-on of forming agent polyvinyl alcohol is 3mass%, and the used pressure of compression moulding is 120MPa;
Degreasing process is higher than in vacuum tightness under the condition of 10Pa and carries out, and the heat-up rate between 200-400 ℃ is 0.3 ℃/min;
The vacuum tightness of vacuum sintering is higher than 5.0 * 10
-2Pa, sintering temperature is 1250 ℃, soaking time is 20min.
Under above-mentioned preparation process condition, the ceramic-metallic performance of heterogeneity proportioning sees Table 3.
The performance of the different metal pottery that table 3 adopting process 1 is prepared
Embodiment 2:
In the glow discharge plasma stove, using plasma carries out surface modification treatment to the SiC whisker.Charging into the interior argon pressure of furnace chamber is 50Pa, and operating voltage is 600V, and working current is 0.2A, and the treatment time is 120min;
Batch mixing, compounding process carry out in planetary ball mill, and drum's speed of rotation is 180rpm, and the time is 20h;
The add-on of forming agent polyvinyl alcohol is 5mass%, and the used pressure of compression moulding is 160MPa;
Degreasing process is higher than in vacuum tightness under the condition of 10Pa and carries out, and the heat-up rate between 200-400 ℃ is 0.4 ℃/min;
The vacuum tightness of vacuum sintering is higher than 5.0 * 10
-2Pa, sintering temperature is 1160 ℃, soaking time is 60min.
Under above-mentioned preparation process condition, the ceramic-metallic performance of heterogeneity proportioning sees Table 4.
The performance of the different metal pottery that table 4 adopting process 2 is prepared
Embodiment 3:
In the glow discharge plasma stove, using plasma carries out surface modification treatment to the SiC whisker.Charging into the interior argon pressure of furnace chamber is 80Pa, and operating voltage is 700V, and working current is 0.3A, and the treatment time is 90min;
Batch mixing, compounding process carry out in planetary ball mill, and drum's speed of rotation is 220rpm, and the time is 12h;
The add-on of forming agent polyvinyl alcohol is 5mass%, and the used pressure of compression moulding is 200MPa;
Degreasing process is higher than in vacuum tightness under the condition of 10Pa and carries out, and the heat-up rate between 200-400 ℃ is 0.5 ℃/min;
The vacuum tightness of vacuum sintering is higher than 5.0 * 10
-2Pa, sintering temperature is 1190 ℃, soaking time is 40min.
Under above-mentioned preparation process condition, the ceramic-metallic performance of heterogeneity proportioning sees Table 5.
The performance of the different metal pottery that table 5 adopting process 3 is prepared
Embodiment 4:
In the glow discharge plasma stove, using plasma carries out surface modification treatment to the SiC whisker.Charging into the interior argon pressure of furnace chamber is 100Pa, and operating voltage is 700V, and working current is 0.3A, and the treatment time is 90min;
Batch mixing, compounding process carry out in planetary ball mill, and drum's speed of rotation is 200rpm, and the time is 12h;
The add-on of forming agent polyvinyl alcohol is 8mass%, and the used pressure of compression moulding is 250MPa;
Degreasing process is higher than in vacuum tightness under the condition of 10Pa and carries out, and the heat-up rate between 200-400 ℃ is 0.3 ℃/min;
The vacuum tightness of vacuum sintering is higher than 5.0 * 10
-2Pa, sintering temperature is 1220 ℃, soaking time is 30min.
Under above-mentioned preparation process condition, the ceramic-metallic performance of heterogeneity proportioning sees Table 6.
The performance of the different metal pottery that table 6 adopting process 4 is prepared
In this power book span, when the addition of Mn in the sintering metal matrix increased, the ceramic-metallic bending strength of gained was relative with fracture toughness property higher.In the preparation technology parameter, sintering temperature is relatively large to Effect on Performance, and when the sintering temperature value of mediating, when being 1190 ℃, the sintering metal comprehensive mechanical property of above-mentioned each component prescription is higher relatively.In a word, in claims span, its influence to material mechanical performance of above-mentioned factor is limited.
Claims (3)
1. Mo that SiC is crystal whisker reinforced and toughened
2FeB
2Based ceramic metal is characterized in that: its composition quality umber is: Fe is 30～36, and the SiC whisker is 0.3～1.2, and Mo is 45～52, and B is 5.3～6.5, and C is 0.4～1.0, and Ni is 2.5～4.5, and Cr is 2.0～4.0, and Mn is 2.0～10.0.
2. the crystal whisker reinforced and toughened Mo of SiC according to claim 1
2FeB
2Based ceramic metal is characterized in that: the raw material that is adopted is FeB, FeMo, Fe, Mn, Ni, Cr, graphite, SiC whisker.
3. Mo that SiC is crystal whisker reinforced and toughened
2FeB
2The preparation method of based ceramic metal in turn includes the following steps:
(1), first using plasma carries out surface modification treatment to the SiC whisker, in the glow discharge plasma stove, carry out, in the glow discharge plasma treating processes, used purity of argon 〉=99.0%, charging into the interior argon pressure of furnace chamber is 20-100Pa, operating voltage is 500-700V, and working current is 0.1-0.3A, and the treatment time is 90-180min; Carry out ultra-sonic dispersion then;
(2), preparation meets the compound of following requirement, its composition quality umber is: Fe is 30～36, the SiC whisker is 0.3～1.2, Mo is 45～52, B is 5.3～6.5, C is 0.4～1.0, Ni is 2.5～4.5, Cr is 2.0～4.0, Mn is 2.0～10.0;
(3), batch mixing, compounding process carries out in planetary ball mill;
(4), add forming agent, the forming agent that is added is a polyvinyl alcohol, additional proportion is the 3mass%-8mass% of compound;
(5), compression moulding, used pressing pressure is 120-250MPa;
(6), degreasing, in vacuum tightness is higher than the vacuum oven of 10Pa, carry out, the heat-up rate between 200-400 ℃ is 0.3-0.5 ℃/min;
(7), vacuum sintering, in vacuum sintering furnace, carry out, vacuum tightness is higher than 5.0 * 10
-2Pa, sintering temperature is 1160-1250 ℃, soaking time is 20-60min.
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|---|---|---|---|
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| CN101948326A (en) * | 2010-09-17 | 2011-01-19 | 哈尔滨工业大学 | SiC whisker toughened ZrC-based ultra-high temperature ceramic composite material and preparation method thereof |
| CN102965602B (en) * | 2012-12-14 | 2014-04-16 | 南昌工程学院 | Wire mesh flexible composite fabric for surface modification and preparation method of wire mesh flexible composite fabric |
| BR112015023290A2 (en) * | 2013-03-15 | 2017-07-18 | Mesocoat Inc | thermal spray powder, method of manufacturing a thermal spray powder, thermal spray coating formed of a thermal spray powder, and method of forming a thermal spray coating on a substrate |
| CN106747330A (en) * | 2016-11-30 | 2017-05-31 | 郑州仁宏医药科技有限公司 | A kind of high-performance abrasion-proof composite cermet material |
| CN106747329A (en) * | 2016-11-30 | 2017-05-31 | 郑州仁宏医药科技有限公司 | A kind of wear-resisting composite cermet material and preparation method thereof |
| CN107868898B (en) * | 2017-10-31 | 2019-09-17 | 武汉科技大学 | A kind of WCoB-TiC-SiC multiphase metal ceramics material and preparation method thereof |
| CN110952043B (en) * | 2019-12-28 | 2021-04-23 | 苏州再超冶金制品有限公司 | SiC whisker reinforced iron-based powder metallurgy material and preparation method thereof |
| CN112556868B (en) * | 2020-10-26 | 2021-11-02 | 南京航空航天大学 | SiC MOSFET junction temperature detection method based on combined thermosensitive electrical parameter sensitivity enhancement |
| CN115786758B (en) * | 2022-11-25 | 2024-05-10 | 西安近代化学研究所 | Mo (molybdenum)2FeB2Preparation method of-TiN-based composite material |
| CN116727924B (en) * | 2023-07-13 | 2024-04-02 | 江苏九洲新材料科技有限公司 | High-hardness high-strength nickel-based alloy flux-cored wire and preparation method thereof |
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