CN102392149B - Method for microwave sintering preparation of nano-metric rare earth modified steel-bonded hard alloy - Google Patents
Method for microwave sintering preparation of nano-metric rare earth modified steel-bonded hard alloy Download PDFInfo
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- CN102392149B CN102392149B CN201110339838XA CN201110339838A CN102392149B CN 102392149 B CN102392149 B CN 102392149B CN 201110339838X A CN201110339838X A CN 201110339838XA CN 201110339838 A CN201110339838 A CN 201110339838A CN 102392149 B CN102392149 B CN 102392149B
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Abstract
A method for microwave sintering preparation of nano-metric rare earth modified steel-bonded hard alloy includes the following steps: 1, dosing; 2, ball-milling mixing, that is, properly dosed powder is put into a ball-milling jar to be ball-milled; 3, press forming, that is, the properly mixed powder is made into a pressed blank at certain pressure; 4, sintering before microwaving, that is, the pressed blank and microwaving auxiliary heating materials are placed in a polycrystalline mullite fiber heat-preserving barrel, and the heat-preserving barrel is placed into a microwave sintering furnace; and 5, microwave sintering, that is, after the hearth of the furnace is vacuumized to be below 0.5Pa, highly pure argon is filled for protection, the output power of the microwave sintering furnace is controlled, sintering is carried out at certain temperature rise speed, sintering temperature and heat-preserving time, and ideal steel-bonded hard alloy is obtained simply after cooling. The present invention has the technical effects of reasonable technology, convenient operation, short sintering period, small energy consumption, good properties of TiB2 steel-bonded hard alloy obtained by sintering, high compactness, small granularity, even tissues and suitability for industrial production.
Description
Technical field
The present invention relates to a kind of method for preparing wimet, relate in particular to the method that a kind of microwave sintering prepares nano rare earth modification Steel Bond Hard Alloy.
Background technology
Steel Bond Hard Alloy comes across the U.S. of phase earlier 1960s the earliest.It is a uniform distribution 30-50% hard particles on the basis of steel alloy, forms through oversintering, thereby has both had high firmness, HS, the high-wearing feature as the wimet, but have the cold and hot working performance of steel alloy again.In recent years, Steel Bond Hard Alloy is developed as a kind of novel tool die material, and it also can be used as wear part, mechanical component and cutlery etc. simultaneously.At present, homemade Steel Bond Hard Alloy is also very restricted in production application, and major cause is to receive the restriction of making this alloy prior, thereby product stability is poor, durability is not high.But the variety of steel matrix and lower price also make the application of Steel Bond Hard Alloy in aviation and automotive industry come into one's own day by day.
TiB
2Powder is grey or grey black, has the crystalline structure of six sides (AlB2).Its fusing point is 2980 ℃, and very high hardness is arranged.TiB2 oxidation resistance temperature in air can reach 1000 ℃, and is stable in HCl and HF acid.TiB2 is mainly used in the preparation composite ceramic articles.Since its can anti-molten metal corrosion, can be used for the manufacturing of molten metal crucible and electrolytic cell electrode.TiB
2Steel Bond Hard Alloy is TiB
2Particle is the hard phase, and as the bonding phase, through one type of new engineering material that powder metallurgy process is prepared from, optimum is worked under the environment of heavy lift and high frictional wear with steel, therefore requires HS, high-wearing feature and enough toughness.
Microwave sintering is to utilize in the microwave electromagnetic field dielectric loss of material to make material monolithic be heated to sintering temperature and realize sintering and densification.Compare with normal sintering and to have lot of advantages;, rate of heating low like sintering temperature material compactness fast, that obtain is good etc.; Microwave sintering has quickened the mass transfer process of material simultaneously; Thereby can obtain fine-grained material, microwave sintering is technological thereby be described as " revolution of sintering technology ", has great development potentiality and researching value.At present, it is a lot of that relevant microwave sintering prepares stupalith research report, and microwave sintering is mainly used in sintering to stupalith (like TiO both at home and abroad
2, Al
2O
3Deng ceramic post sintering); And preparing the research of metallic substance, microwave sintering still is in the exploratory stage; Dinesh professor Agrawal like Pennsylvania State Univ-Univ Park USA has carried out microwave sintering research to nano WC-Co; Domestic also have only Central South University and these two universities of Wuhan University of Technology that microwave sintering is prepared wimet the research report was arranged; And all concentrate on the microwave sintering research of WC-Co wimet, and microwave sintering prepares the research of nano rare earth modification Steel Bond Hard Alloy and does not appear in the newspapers both at home and abroad.For this reason, the present invention is with TiB
2Particle is a wild phase, and iron powder is a matrix, nanometer Y
2O
3Doping vario-property is through ball milling, compression moulding, with microwave sintering technology preparation nano rare earth modification Steel Bond Hard Alloy.
Summary of the invention
The object of the present invention is to provide a kind of microwave sintering to prepare the method for nano rare earth modification Steel Bond Hard Alloy; Microwave sintering method is easy to operate, the sintering period is short, energy consumption is few, and it is high to obtain density, and crystal grain is tiny; Homogeneous microstructure, the TiB that mechanical property is good
2Steel Bond Hard Alloy.
The present invention realizes like this, comprises the steps:
Step 1: batching, with purity greater than 99.99%, granularity is less than the nanometer Y of 50 nm
2O
3, purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, the Cr powder, the Ni powder, Graphite Powder 99 is by the certain mass percent batching;
Step 2: ball mill mixing, the powder for preparing is put into ball grinder carry out ball milling;
Step 3: compression moulding, the powder that mixes is processed pressed compact under certain pressure;
Step 4: before the microwave sintering, gained pressed compact and microwave-assisted heating material are positioned in the polycrystalline mullite fibre insulated tank, insulated tank is put into microwave agglomerating furnace;
Step 5: microwave sintering; After vacuum tightness is evacuated to and is lower than 0.5 Pa in the furnace chamber, and charge into high-purity argon gas protection, the output rating of controlled microwave sintering oven; Carry out sintering with certain heat-up rate, sintering temperature, soaking time, promptly obtain the ideal Steel Bond Hard Alloy after the cooling.
The said batching mass percent of said step 1 is 0 ~ 40%TiB
2, 0 ~ 1.0% Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus; Surplus Fe is by forming for massfraction 70% reduced iron powder and 30% carbonyl iron dust.
The said ball mill device of said step 2 is a stainless steel jar mill, and ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1, rotating speed 150 ~ 300 r/min, times 6 ~ 12 h.
The said compression moulding pressure of said step 3 is 200 ~ 500 MPa.
The said polycrystalline mullite fibre insulated tank of said step 4 plays insulation effect, and the microwave-assisted heating material is green SiC powder, and add-on is 100 ~ 300 g.
The said high-purity argon gas purity of said step 5 is 99.999%, output rating 0 ~ 3 KW of microwave agglomerating furnace.
15 ~ 60 ℃/min of the said microwave sintering control heat-up rate of said step 5,1200 ~ 1400 ℃ of sintering temperatures, soaking time 10 ~ 30 min.
Table 1 is microwave sintering and normal sintering contrast.From table, can draw, microwave sintering can improve the homogeneity of temperature distribution in the object, has shortened heating, soaking time, has reduced sintering temperature, finally makes sintered compact have the tiny and uniform grain structure, and product has excellent more physics, mechanical property.The microwave sintering technology has and distinct thermal behavior and the thermograde of adding of normal sintering mode; Shortcomings such as the heating object surface temperature of avoiding routine to add pining for occurring is high, the loss of sintering motivating force is big; Simultaneously; The selectivity that the microwave sintering technology also has the thing phase heats, is easy to control and advantages such as sintering temperature is low, with short production cycle, energy utilization rate is high, safety non-pollution in the above rate of heating quickening of critical temperature, microwave heating zone, has become quick preparation high quality novel material and has had the important technical of the traditional material of new capability.
Table 1 microwave sintering and normal sintering contrast
Table 2 is rare earth modified microwave sintering to be prepared the Steel Bond Hard Alloy performance impact.There is table to know, adds density and mechanical property that the proper amount of rare-earth modification can improve Steel Bond Hard Alloy, add more excellence of nano rare earth effect simultaneously.
Table 2 is rare earth modified to prepare the Steel Bond Hard Alloy performance impact to microwave sintering
Technique effect of the present invention is: the TiB that technology is reasonable, easy to operate, the sintering period is short, energy consumption is few, sintering obtained
2The Steel Bond Hard Alloy performance is good, and density is high, and crystal grain is tiny, and homogeneous microstructure is suitable for suitability for industrialized production.
Embodiment
Embodiment one:
This embodiment microwave sintering prepares the method for nano rare earth modification Steel Bond Hard Alloy to carry out according to the following steps: step 1: batching, with purity greater than 99.99%, granularity is less than the nanometer Y of 50 nm
2O
3, purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, the Cr powder, the Ni powder, Graphite Powder 99 is by the certain mass percent batching, the mass percent of specifically preparing burden is 40%TiB
2, 1.0% Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus; Surplus Fe is by forming for massfraction 70% reduced iron powder and 30% carbonyl iron dust.
Step 2: ball mill mixing, the powder for preparing to be put into ball grinder carry out ball milling, ball mill device is a stainless steel jar mill, ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1, rotating speed 300 r/min, times 12 h.
Step 3: compression moulding, the powder that mixes is processed pressed compact under 500 MPa pressure;
Step 4: before the microwave sintering, gained pressed compact and microwave-assisted heating material are positioned in the polycrystalline mullite fibre insulated tank, insulated tank is put into microwave agglomerating furnace; The polycrystalline mullite fibre insulated tank plays insulation effect, and the microwave-assisted heating material is green SiC powder, and add-on is 300 g.
Step 5: after vacuum tightness is evacuated to and is lower than 0.5 Pa in the microwave sintering, furnace chamber, and charge into the high-purity argon gas protection; The output rating of controlled microwave sintering oven is carried out sintering with certain heat-up rate, sintering temperature, soaking time, promptly obtains the ideal Steel Bond Hard Alloy after the cooling; High-purity argon gas purity is 99.999%, output rating 0 ~ 3 KW of microwave agglomerating furnace, 60 ℃/min of said microwave sintering control heat-up rate; 1400 ℃ of sintering temperatures, soaking time 30 min.
Embodiment two:
This embodiment microwave sintering prepares the method for nano rare earth modification Steel Bond Hard Alloy to carry out according to the following steps: step 1: batching, with purity greater than 99.99%, granularity is less than the nanometer Y of 50 nm
2O
3, purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, the Cr powder, the Ni powder, Graphite Powder 99 is by the certain mass percent batching, the mass percent of specifically preparing burden is 20%TiB
2, 0.5% Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus; Surplus Fe is by forming for massfraction 70% reduced iron powder and 30% carbonyl iron dust.
Step 2: ball mill mixing, the powder for preparing to be put into ball grinder carry out ball milling, ball mill device is a stainless steel jar mill, ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1, rotating speed 200 r/min, times 10 h.
Step 3: compression moulding, the powder that mixes is processed pressed compact under 300 MPa pressure;
Step 4: before the microwave sintering, gained pressed compact and microwave-assisted heating material are positioned in the polycrystalline mullite fibre insulated tank, insulated tank is put into microwave agglomerating furnace; The polycrystalline mullite fibre insulated tank plays insulation effect, and the microwave-assisted heating material is green SiC powder, and add-on is 200 g.
Step 5: after vacuum tightness is evacuated to and is lower than 0.5 Pa in the microwave sintering, furnace chamber, and charge into the high-purity argon gas protection; The output rating of controlled microwave sintering oven is carried out sintering with certain heat-up rate, sintering temperature, soaking time, promptly obtains the ideal Steel Bond Hard Alloy after the cooling; High-purity argon gas purity is 99.999%, output rating 0 ~ 2 KW of microwave agglomerating furnace, 40 ℃/min of said microwave sintering control heat-up rate; 1300 ℃ of sintering temperatures, soaking time 20 min.
Embodiment three:
This embodiment microwave sintering prepares the method for nano rare earth modification Steel Bond Hard Alloy to carry out according to the following steps: step 1: batching, with purity greater than 99.99%, granularity is less than the nanometer Y of 50 nm
2O
3, purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, the Cr powder, the Ni powder, Graphite Powder 99 is by the certain mass percent batching, the mass percent of specifically preparing burden is 10%TiB
2, 0 .1% Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus; Surplus Fe is by forming for massfraction 70% reduced iron powder and 30% carbonyl iron dust.
Step 2: ball mill mixing, the powder for preparing to be put into ball grinder carry out ball milling, ball mill device is a stainless steel jar mill, ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1, rotating speed 150 r/min, times 6 h.
Step 3: compression moulding, the powder that mixes is processed pressed compact under 200MPa pressure;
Step 4: before the microwave sintering, gained pressed compact and microwave-assisted heating material are positioned in the polycrystalline mullite fibre insulated tank, insulated tank is put into microwave agglomerating furnace; The polycrystalline mullite fibre insulated tank plays insulation effect, and the microwave-assisted heating material is green SiC powder, and add-on is 100 g.
Step 5: after vacuum tightness is evacuated to and is lower than 0.5 Pa in the microwave sintering, furnace chamber, and charge into the high-purity argon gas protection; The output rating of controlled microwave sintering oven is carried out sintering with certain heat-up rate, sintering temperature, soaking time, promptly obtains the ideal Steel Bond Hard Alloy after the cooling; High-purity argon gas purity is 99.999%, output rating 0 ~ 1.5 KW of microwave agglomerating furnace, 15 ℃/min of said microwave sintering control heat-up rate; 1200 ℃ of sintering temperatures, soaking time 10min.
Embodiment four:
This embodiment normal sintering prepares the method for nano rare earth modification Steel Bond Hard Alloy to carry out according to the following steps: step 1: batching, with purity greater than 99.99%, granularity is less than the nanometer Y of 50 nm
2O
3, purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, the Cr powder, the Ni powder, Graphite Powder 99 is by the certain mass percent batching, the mass percent of specifically preparing burden is 40%TiB
2, 1.0%Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus; Surplus Fe is by forming for massfraction 70% reduced iron powder and 30% carbonyl iron dust.
Step 2: ball mill mixing, the powder for preparing to be put into ball grinder carry out ball milling, ball mill device is a stainless steel jar mill, ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1, rotating speed 300 r/min, times 12 h.
Step 3: compression moulding, the powder that mixes is processed pressed compact under 500 MPa pressure;
Step 4: after vacuum tightness is evacuated to and is lower than 0.5 Pa in the normal sintering, furnace chamber, and charge into the high-purity argon gas protection; The output rating of control sintering oven is carried out sintering with certain heat-up rate, sintering temperature, soaking time, promptly obtains the ideal Steel Bond Hard Alloy after the cooling; High-purity argon gas purity is 99.999%; 20 ℃/min of said sintering control heat-up rate, 1450 ℃ of sintering temperatures, soaking time 120 min.
Embodiment five:
This embodiment microwave sintering prepares the method for nano rare earth modification Steel Bond Hard Alloy to carry out according to the following steps: step 1: batching, with purity greater than 99.99%, granularity is less than the micron Y of 50 μ m
2O
3, purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, the Cr powder, the Ni powder, Graphite Powder 99 is by the certain mass percent batching, the mass percent of specifically preparing burden is 40%TiB
2, 0.5% Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus; Surplus Fe is by forming for massfraction 70% reduced iron powder and 30% carbonyl iron dust.
Step 2: ball mill mixing, the powder for preparing to be put into ball grinder carry out ball milling, ball mill device is a stainless steel jar mill, ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1, rotating speed 300 r/min, times 12 h.
Step 3: compression moulding, the powder that mixes is processed pressed compact under 500 MPa pressure;
Step 4: before the microwave sintering, gained pressed compact and microwave-assisted heating material are positioned in the polycrystalline mullite fibre insulated tank, insulated tank is put into microwave agglomerating furnace; The polycrystalline mullite fibre insulated tank plays insulation effect, and the microwave-assisted heating material is green SiC powder, and add-on is 300 g.
Step 5: after vacuum tightness is evacuated to and is lower than 0.5 Pa in the microwave sintering, furnace chamber, and charge into the high-purity argon gas protection; The output rating of controlled microwave sintering oven is carried out sintering with certain heat-up rate, sintering temperature, soaking time, promptly obtains the ideal Steel Bond Hard Alloy after the cooling; High-purity argon gas purity is 99.999%, output rating 0 ~ 3 KW of microwave agglomerating furnace, 60 ℃/min of said microwave sintering control heat-up rate; 1400 ℃ of sintering temperatures, soaking time 20 min.
Embodiment six:
This embodiment microwave sintering prepares the method for nano rare earth modification Steel Bond Hard Alloy to carry out according to the following steps: step 1: batching, with purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, the Cr powder, the Ni powder, Graphite Powder 99 is by the certain mass percent batching, the mass percent of specifically preparing burden is 40%TiB
2, 1.0% Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus; Surplus Fe is by forming for massfraction 70% reduced iron powder and 30% carbonyl iron dust.
Step 2: ball mill mixing, the powder for preparing to be put into ball grinder carry out ball milling, ball mill device is a stainless steel jar mill, ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1, rotating speed 300 r/min, times 12 h.
Step 3: compression moulding, the powder that mixes is processed pressed compact under 500 MPa pressure;
Step 4: before the microwave sintering, gained pressed compact and microwave-assisted heating material are positioned in the polycrystalline mullite fibre insulated tank, insulated tank is put into microwave agglomerating furnace; The polycrystalline mullite fibre insulated tank plays insulation effect, and the microwave-assisted heating material is green SiC powder, and add-on is 300 g.
Step 5: after vacuum tightness is evacuated to and is lower than 0.5 Pa in the microwave sintering, furnace chamber, and charge into the high-purity argon gas protection; The output rating of controlled microwave sintering oven is carried out sintering with certain heat-up rate, sintering temperature, soaking time, promptly obtains the ideal Steel Bond Hard Alloy after the cooling; High-purity argon gas purity is 99.999%, output rating 0 ~ 3 KW of microwave agglomerating furnace, 60 ℃/min of said microwave sintering control heat-up rate; 1400 ℃ of sintering temperatures, soaking time 20 min.
Claims (4)
1. a microwave sintering prepares the method for nano rare earth modification Steel Bond Hard Alloy, it is characterized in that comprising the steps:
Step 1: batching, with purity greater than 99.99%, granularity is less than the nanometer Y of 50 nm
2O
3, purity greater than 99.7%, granularity is less than the TiB of 3.0 μ m
2Powder, purity greater than 99%, granularity is less than 38 μ m reduced iron powders, purity greater than 99. 5%, granularity is less than the carbonyl iron dust of 3 μ m, Cr powder, Ni powder, Graphite Powder 99 are 0 ~ 40%TiB by mass percentage
2, 0 ~ 1.0% Y
2O
3, 1.5%Cr, 1.5%Ni, 0.6%C, Fe surplus batching; Surplus Fe is made up of massfraction 70% reduced iron powder and 30% carbonyl iron dust;
Step 2: ball mill mixing, the powder for preparing is put into ball grinder carry out ball milling;
Step 3: compression moulding, the powder that mixes is processed pressed compact under 200 ~ 500 MPa pressure;
Step 4: before the microwave sintering, gained pressed compact and microwave-assisted heating material are positioned in the polycrystalline mullite fibre insulated tank, insulated tank is put into microwave agglomerating furnace;
Step 5: microwave sintering; After vacuum tightness is evacuated to and is lower than 0.5 Pa in the furnace chamber; And charge into high-purity argon gas protection; The output rating of controlled microwave sintering oven is carried out sintering with 15 ~ 60 ℃/min of heat-up rate, 1200 ~ 1400 ℃ of sintering temperatures, soaking time 10 ~ 30 min, promptly obtains the ideal Steel Bond Hard Alloy after the cooling.
2. microwave sintering according to claim 1 prepares the method for nano rare earth modification Steel Bond Hard Alloy; It is characterized in that: the said ball grinder of step 2 is a stainless steel jar mill, and ball-milling medium is raw spirit or acetone, ball-to-powder weight ratio 6:1; Rotating speed 150 ~ 300 r/min, times 6 ~ 12 h.
3. microwave sintering according to claim 1 prepares the method for nano rare earth modification Steel Bond Hard Alloy; It is characterized in that: the said polycrystalline mullite fibre insulated tank of step 4 plays insulation effect; The microwave-assisted heating material is green SiC powder, and add-on is 100 ~ 300 g.
4. microwave sintering according to claim 1 prepares the method for nano rare earth modification Steel Bond Hard Alloy, it is characterized in that: the said high-purity argon gas purity of step 5 is 99.999%, output rating 0 ~ 3 KW of microwave agglomerating furnace.
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| CN107500784A (en) * | 2016-09-23 | 2017-12-22 | 武汉科技大学 | A kind of magnesite-dolomite refractories based on microwave sintering and preparation method thereof |
| CN108637263B (en) * | 2018-05-31 | 2024-05-24 | 北京科技大学 | Microwave sintering for preparing TiB2Method for producing M cermet powders |
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| CN101760685A (en) * | 2008-12-25 | 2010-06-30 | 北京有色金属研究总院 | Superfine WC-Co cemented carbide containing rare-earth elements and preparation method thereof |
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| CN101760685A (en) * | 2008-12-25 | 2010-06-30 | 北京有色金属研究总院 | Superfine WC-Co cemented carbide containing rare-earth elements and preparation method thereof |
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| Title |
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| 周建等.微波烧结WC-10Co硬质合金的工艺研究.《国外建材科技》.2007,第28卷(第5期),第40-42页. |
| 微波烧结WC-10Co硬质合金的工艺研究;周建等;《国外建材科技》;20071231;第28卷(第5期);第40-42页 * |
| 李永涛等.超细/纳米粉末改进Ti(C N)基金属陶瓷性能研究进展.《材料导报》.2005 |
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