CN108746656A - Prealloy powder and preparation method thereof for diamond composition - Google Patents
Prealloy powder and preparation method thereof for diamond composition Download PDFInfo
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- CN108746656A CN108746656A CN201810621942.XA CN201810621942A CN108746656A CN 108746656 A CN108746656 A CN 108746656A CN 201810621942 A CN201810621942 A CN 201810621942A CN 108746656 A CN108746656 A CN 108746656A
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- 239000000843 powder Substances 0.000 title claims abstract description 75
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 41
- 239000010432 diamond Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000203 mixture Substances 0.000 title claims abstract description 22
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000002243 precursor Substances 0.000 claims abstract description 42
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 15
- 239000013049 sediment Substances 0.000 claims abstract description 15
- -1 hydrazine compound Chemical class 0.000 claims abstract description 14
- 238000001556 precipitation Methods 0.000 claims abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 3
- 229910052718 tin Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 11
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- WXOBLSRQYOWIBF-UHFFFAOYSA-N butylhydrazine;oxalic acid Chemical class CCCCNN.OC(=O)C(O)=O WXOBLSRQYOWIBF-UHFFFAOYSA-N 0.000 claims description 4
- DUMHBFMURBWDPC-UHFFFAOYSA-N ethylhydrazine;oxalic acid Chemical class CCNN.OC(=O)C(O)=O DUMHBFMURBWDPC-UHFFFAOYSA-N 0.000 claims description 4
- ATXLENZWWDUZLH-UHFFFAOYSA-N oxalic acid;propylhydrazine Chemical class CCCNN.OC(=O)C(O)=O ATXLENZWWDUZLH-UHFFFAOYSA-N 0.000 claims description 4
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000006193 liquid solution Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 31
- 238000005245 sintering Methods 0.000 abstract description 17
- 238000005275 alloying Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 238000004364 calculation method Methods 0.000 description 45
- 230000000052 comparative effect Effects 0.000 description 19
- 229910052760 oxygen Inorganic materials 0.000 description 19
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 9
- 238000013019 agitation Methods 0.000 description 9
- 238000005352 clarification Methods 0.000 description 9
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 9
- 238000009826 distribution Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910008986 Sn—Ni—La Inorganic materials 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 3
- 229910001000 nickel titanium Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 150000002171 ethylene diamines Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910002555 FeNi Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The prealloy powder and preparation method thereof that the present invention relates to a kind of for diamond composition, belongs to the technical field of diamond tool.The preparation method of the present invention, includes the following steps：Preparation includes that the strong acid salt of Cu, Fe, Sn, Ni are configured to precursor solution；Prepare the precipitant solution being made of oxalic acid and hydrazine compound；Precursor solution is mixed with precipitant solution, ammonium hydroxide is added and adjusts pH value, and diamine compound progress precipitation reaction is added and obtains sediment；Sediment is calcined to obtain calcined product；Reduction treatment is carried out to the calcined product under reducing atmosphere, then crushes, sieve the prealloy powder that can be can be obtained for diamond composition.The prealloy powder powder size being prepared using the above method is thin, and alloying level is high, and sintering activity is high, advantageously reduces sintering temperature, and there is good binding force with diamond particles, so as to effectively improve the utilization rate of diamond particles and the processing efficiency of diamond tool.
Description
Technical field
The present invention relates to the technical fields of diamond tool, it is more particularly related to a kind of made of stones for Buddha's warrior attendant
Prealloy powder of product and preparation method thereof.
Background technology
With the development of Diamond Tools Industry, requirement of the processing enterprise to diamond tool performance is continuously improved, conventional
With elemental metals powder mixing based on carcass material, cannot meet the requirement for preparing high-performance diamond tool.20
The nineties in century, Belgian Umicore companies first proposed the technology solution that ultra-fine prealloy powder is used in diamond tool
Certainly scheme.Prealloy powder powder be " it is a kind of to be made of two or more element, occur in the manufacturing process of powder
Alloying, and all particles keep the metal powder of the component consistent with nominal content ".It is carried since the 1990s
Since going out prealloy powder concept, domestic and international researcher has carried out numerous studies to prealloy powder, and prealloy powder has it significant
Advantage：Prealloy powder is evenly distributed than mechanical mixture powdered elemental, fundamentally avoids component segregation, keeps carcass tissue equal
Even, a degree of alloying occurs in preparation process for prealloy powder, and carcass is made to have high hardness and high impact strong
Degree, can be improved the hold of diamond.It is pre-alloyed to greatly reduce swashing needed for the diffusion of metallic atom in sintering process
Energy living, to reduce sintering temperature, shortens sintering time, and this aspect is conducive to avoid the high-temperature damage to diamond,
On the other hand graphite jig dosage and power consumption can be reduced.
In the prior art, early stage prealloy powder is mainly produced using conventional atomization, the prealloy powder of atomization production
Last alloying level is high, good fluidity, and production efficiency is high, but atomization process is higher to equipment requirement, is not easy to adjustment carcass
Ingredient, and high oxygen content, powder is spherical in shape, and loose specific weight is big, is unfavorable for the granulation of carcass powder and diamond mixture.Altogether
Since it has the characteristics that fine size, sintering activity are high, the application in diamond tool is more and more weighed the precipitation method
Depending on.But the research of the prealloy powder to being used to prepare diamond tool metallic bond focuses primarily upon FeCoCu bases at present
Plinth system, not only bending strength is high but also good to the wetability of carbon material and carbide, caking property by Co therein, but cobalt is not only
It is of high cost, and scarcity of resources,
Invention content
In order to solve above-mentioned technical problem in the prior art, it is made of stones for Buddha's warrior attendant that the purpose of the present invention is to provide one kind
Prealloy powder of product and preparation method thereof.
In order to achieve the above-mentioned object of the invention, present invention employs following technical schemes：
The preparation method of a kind of prealloy powder for diamond composition, it is characterised in that include the following steps：
(1) prepare to include Cu, Fe, Sn, Ni and the optionally strong acid salt of intensified element, be dissolved in the water and be configured to presoma
Solution；
(2) prepare precipitant solution, the precipitant solution is made of oxalic acid and hydrazine compound；
(3) precursor solution is mixed with precipitant solution, it is 4.0~8.0 that ammonium hydroxide, which is added, and adjusts pH value, and two amine compounds are added
Object carries out precipitation reaction and obtains sediment；
(4) sediment is calcined to obtain calcined product, calcination temperature is 450~650 DEG C；
(5) reduction treatment is carried out to the calcined product under reducing atmosphere, the temperature of reduction treatment is 400~550 DEG C；So
After crush, sieve.
Wherein, the intensified element includes at least one of Ti, Mn, W, Zr, Cr, V, Nb, Al, Mg, La or Ce.
Wherein, the one kind of the strong acid salt in hydrochloride, sulfate or nitrate.
Wherein, the hydrazine compound is selected from least one of ethyl hydrazine oxalates, propyl hydrazine oxalates or butyl hydrazine oxalates.
Wherein, the weight ratio of the hydrazine compound and the oxalic acid is 1:5~20.Oxalic acid in the precipitant solution contains
Amount is 72~160g/L.
Wherein, the diamine compound is selected from least one of ethylenediamine, 1,3- propane diamine or Putriscine.
Wherein, the content of the diamine compound is 2~30g/L, preferably 2~20g/L, more preferably 3~15g/L.
Wherein, the reducing atmosphere is the reducing atmosphere comprising hydrogen and/or carbon monoxide.
Wherein, in the precursor solution, with Cu ionometer contents for 12.5~63g/L, preferably 38~64g/L；With
Fe ionometer contents are 11.2~56g/L, preferably 22.4~56g/L；Sn ionometer contents are 5.9~17.7g/L, preferably
5.9~11.8g/L；Contain 5.8~17.4g/L with Ni ionometers；Contain 0~30g/L, preferably 0 with the ion of intensified element
~20g/L.
The second aspect of the present invention further relates to a kind of prealloy for diamond composition obtained by above-mentioned preparation method
Powder.
Compared with prior art, the prealloy powder for diamond composition of the invention has the advantages that：
The prealloy powder powder size that preparation method using the present invention is prepared is thin, and alloying level is high, and sintering activity is high,
Sintering temperature is advantageously reduced, damage when reducing sintering to diamond particles, so as to effectively improve diamond particles
The processing efficiency of utilization rate and diamond tool.
Description of the drawings
Fig. 1 is the XRD diffraction patterns of prealloy powder prepared by embodiment 1.
Fig. 2 is the XRD diffraction patterns of prealloy powder prepared by comparative example 1.
Specific implementation mode
The prealloy powder for diamond composition of the present invention is further elaborated below with reference to specific embodiment,
To help those skilled in the art to have more complete, accurate and deep understanding to the inventive concept of the present invention, technical solution.
Embodiment 1
The present embodiment is related to the preparation of Fe-Cu-Sn-Ni-Ce prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 40g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 40g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 7g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 12g2·6H2O is weighed with Ce3+
Weight calculation amount is the CeCl of 1g3·7H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 105g's
Oxalic acid, 12g ethyl hydrazine oxalates be dissolved in the water and be configured to the precipitant solution of 1L, it is spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.5,10g ethylenediamines are added and carry out precipitation reaction about 30 minutes, obtained sediment is cleaned after clarification, is then placed in
It is dried to obtain precursor in vacuum drying chamber.Precursor is calcined in Muffle furnace, calcination temperature 500
DEG C, the time is 1 hour.Reduction treatment finally is carried out to calcined product in a hydrogen atmosphere, the temperature of reduction treatment is 550 DEG C,
Time is 2 hours, then crushes, sieves.The pattern for the prealloy powder that SEM photograph is shown is small very much
The aggregate of grain, particle size uniformity is preferable, measures its size distribution at 1.0~12.6 μm using laser particle size analyzer, Fei Shi
Granularity is 5.2 μm.The oxygen content of product is 0.79wt%.
Embodiment 2
The present embodiment is related to the preparation of Fe-Cu-Sn-Ni-La prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 35g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 50g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 5g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 8g2·6H2O is weighed with La3+
Weight calculation amount is the LaCl of 2g3·7H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 112g's
Oxalic acid, 7g propyl hydrazine oxalates be dissolved in the water and be configured to the precipitant solution of 1L, it is spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.0,1, the 3- propane diamine that 12g is added carries out precipitation reaction about 30 minutes, is cleaned to obtained sediment after clarification, so
After be put into vacuum drying chamber and be dried to obtain precursor.Precursor is calcined in Muffle furnace, calcination temperature
It it is 500 DEG C, the time is 1 hour.Reduction treatment, the temperature of reduction treatment finally are carried out to calcined product under carbon monoxide atmosphere
Degree is 550 DEG C, and the time is 2 hours, then crushes, sieves.The pattern for the prealloy powder that SEM photograph is shown
For many short grained aggregates, particle size uniformity is preferable, using laser particle size analyzer measure its size distribution 1.5~
13.7 μm, Fisher particle size is 5.8 μm.The oxygen content of product is 0.83wt%.
Embodiment 3
The present embodiment is related to the preparation of Fe-Cu-Sn-Ni-Ti prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 50g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 30g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 8g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 10g2·6H2O is weighed with Ti3+
Weight calculation amount is the TiCl of 2g3·6H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 100g's
Oxalic acid, 15g butyl hydrazine oxalates be dissolved in the water and be configured to the precipitant solution of 1L, it is spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.5, the Putriscine that 15g is added carries out precipitation reaction about 30 minutes, is cleaned to obtained sediment after clarification, so
After be put into vacuum drying chamber and be dried to obtain precursor.Precursor is calcined in Muffle furnace, calcination temperature
It it is 500 DEG C, the time is 1 hour.Reduction treatment finally is carried out to calcined product under the mixed atmosphere of carbon monoxide and hydrogen,
The temperature of reduction treatment is 550 DEG C, and the time is 2 hours, then crushes, sieves.SEM photograph is shown pre-
The pattern of alloyed powder is many short grained aggregates, and particle size uniformity is preferable, its granularity is measured using laser particle size analyzer
1.5~14.8 μm are distributed in, Fisher particle size is 6.3 μm.The oxygen content of product is 0.72wt%.
Comparative example 1
This comparative example is related to the preparation of Fe-Cu-Sn-Ni-Ce prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 40g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 40g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 7g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 12g2·6H2O is weighed with Ce3+
Weight calculation amount is the CeCl of 1g3·7H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 105g's
Dissolving oxalic acid is configured to the precipitant solution of 1L in water, spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.5,10g ethylenediamines are added and carry out precipitation reaction about 30 minutes, obtained sediment is cleaned after clarification, is then placed in
It is dried to obtain precursor in vacuum drying chamber.Precursor is calcined in Muffle furnace, calcination temperature 500
DEG C, the time is 1 hour.Reduction treatment finally is carried out to calcined product in a hydrogen atmosphere, the temperature of reduction treatment is 550 DEG C,
Time is 2 hours, then crushes, sieves.The pattern for the prealloy powder that SEM photograph is shown is small very much
The aggregate of grain, particle size uniformity is preferable, measures its size distribution at 1.5~13.5 μm using laser particle size analyzer, Fei Shi
Granularity is 5.5 μm.The oxygen content of product is 0.80wt%.
Comparative example 2
This comparative example is related to the preparation of Fe-Cu-Sn-Ni-Ce prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 40g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 40g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 7g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 12g2·6H2O is weighed with Ce3+
Weight calculation amount is the CeCl of 1g3·7H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 105g's
Oxalic acid, 12g ethyl hydrazine oxalates be dissolved in the water and be configured to the precipitant solution of 1L, it is spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.5 carry out precipitation reaction about 30 minutes, are cleaned to obtained sediment after clarification, are then placed in vacuum drying chamber and carry out
It is dried to obtain precursor.Precursor is calcined in Muffle furnace, calcination temperature is 500 DEG C, and the time is 1 hour.Most
Reduction treatment is carried out to calcined product in a hydrogen atmosphere afterwards, the temperature of reduction treatment is 550 DEG C, and the time is 2 hours, then
It crushes, sieve.The pattern for the prealloy powder that SEM photograph is shown is that polygonal small particles are assembled,
Grain is not of uniform size, measures its size distribution at 2.1~25.7 μm using laser particle size analyzer, Fisher particle size is 9.8 μm.Production
The oxygen content of object is 0.85wt%.
Comparative example 3
This comparative example is related to the preparation of Fe-Cu-Sn-Ni-La prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 35g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 50g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 5g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 8g2·6H2O is weighed with La3+
Weight calculation amount is the LaCl of 2g3·7H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 118g's
Dissolving oxalic acid is configured to the precipitant solution of 1L in water, spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.0,1, the 3- propane diamine that 12g is added carries out precipitation reaction about 30 minutes, is cleaned to obtained sediment after clarification, so
After be put into vacuum drying chamber and be dried to obtain precursor.Precursor is calcined in Muffle furnace, calcination temperature
It it is 500 DEG C, the time is 1 hour.Reduction treatment, the temperature of reduction treatment finally are carried out to calcined product under carbon monoxide atmosphere
Degree is 550 DEG C, and the time is 2 hours, then crushes, sieves.The pattern for the prealloy powder that SEM photograph is shown
For many short grained aggregates, particle size uniformity is preferable, using laser particle size analyzer measure its size distribution 1.5~
15.5 μm, Fisher particle size is 6.3 μm.The oxygen content of product is 0.81wt%.
Comparative example 4
This comparative example is related to the preparation of Fe-Cu-Sn-Ni-La prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 35g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 50g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 5g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 8g2·6H2O is weighed with La3+
Weight calculation amount is the LaCl of 2g3·7H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 112g's
Oxalic acid, 7g propyl hydrazine oxalates be dissolved in the water and be configured to the precipitant solution of 1L, it is spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.0 carry out precipitation reaction about 30 minutes, are cleaned to obtained sediment after clarification, are then placed in vacuum drying chamber and carry out
It is dried to obtain precursor.Precursor is calcined in Muffle furnace, calcination temperature is 500 DEG C, and the time is 1 hour.Most
Reduction treatment is carried out to calcined product under carbon monoxide atmosphere afterwards, the temperature of reduction treatment is 550 DEG C, and the time is 2 hours,
Then it crushes, sieve.The pattern for the prealloy powder that SEM photograph is shown for polygonal small particles are assembled and
At granular size differs, and measures its size distribution at 2.3~23.2 μm using laser particle size analyzer, Fisher particle size is 9.6 μ
m.The oxygen content of product is 0.83wt%.
Comparative example 5
This comparative example is related to the preparation of Fe-Cu-Sn-Ni-Ti prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 50g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 30g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 8g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 10g2·6H2O is weighed with Ti3+
Weight calculation amount is the TiCl of 2g3·6H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 100g's
Dissolving oxalic acid is configured to the precipitant solution of 1L in water, spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.5, the Putriscine that 15g is added carries out precipitation reaction about 30 minutes, is cleaned to obtained sediment after clarification, so
After be put into vacuum drying chamber and be dried to obtain precursor.Precursor is calcined in Muffle furnace, calcination temperature
It it is 500 DEG C, the time is 1 hour.Reduction treatment finally is carried out to calcined product under the mixed atmosphere of carbon monoxide and hydrogen,
The temperature of reduction treatment is 550 DEG C, and the time is 2 hours, then crushes, sieves.SEM photograph is shown pre-
The pattern of alloyed powder is many short grained aggregates, and particle size uniformity is preferable, its granularity is measured using laser particle size analyzer
1.5~16.9 μm are distributed in, Fisher particle size is 6.7 μm.The oxygen content of product is 0.75wt%.
Comparative example 6
This comparative example is related to the preparation of Fe-Cu-Sn-Ni-Ti prealloy powder.
It weighs with Cu2+Weight calculation amount is the CuCl of 50g2·2H2O, it weighs with Fe2+Weight calculation amount is the FeCl of 30g2·4H2O、
It weighs with Sn2+Weight calculation amount is the SnCl of 8g2·2H2O, it weighs with Ni2+Weight calculation amount is the NiCl of 10g2·6H2O is weighed with Ti3+
Weight calculation amount is the TiCl of 2g3·6H2O, be dissolved in the water the precursor solution for being configured to that volume is 1L, spare.Weigh 100g's
Oxalic acid, 15g butyl hydrazine oxalates be dissolved in the water and be configured to the precipitant solution of 1L, it is spare.
The precursor solution of above-mentioned configuration is mixed with precipitant solution, ammonium hydroxide adjusting pH value is added under agitation is
5.5 carry out precipitation reaction about 30 minutes, are cleaned to obtained sediment after clarification, are then placed in vacuum drying chamber and carry out
It is dried to obtain precursor.Precursor is calcined in Muffle furnace, calcination temperature is 500 DEG C, and the time is 1 hour.Most
Reduction treatment is carried out to calcined product under the mixed atmosphere of carbon monoxide and hydrogen afterwards, the temperature of reduction treatment is 550 DEG C,
Time is 2 hours, then crushes, sieves.The pattern for the prealloy powder that SEM photograph is shown is polygonal
Small particles are assembled, and granular size differs, and are measured its size distribution at 1.8~27.2 μm using laser particle size analyzer, are taken
Family name's granularity is 10.2 μm.The oxygen content of product is 0.73wt%.
The prealloy powder that Examples 1 to 3 and comparative example 1~6 are prepared is sintered experiment.By above-mentioned prealloy
It is 300kg/cm that powder, which is installed in the graphite jig of 55mm × 10mm × 10mm in pressure,2Pressure condition under in different temperatures
Under be sintered, sintering time is 200 seconds, and measures the relative density of sintered product, and the results are shown in Table 1.
Table 1
The result shows that the prealloy powder that the embodiment of the present invention 1~3 is prepared is sintered i.e. under 700~750 DEG C of temperature condition
It can be obtained fine and close sintered body, thus the present invention prealloy powder that is prepared is recommended when being used to prepare diamond composition
Sintering range is 700~750 DEG C, and the prealloy powder that comparative example 1,3,5 is prepared is needed at 800 DEG C, or even
Relatively compact sintered body can be just obtained under 850 DEG C of temperature condition.
The tyre-e/or performance prepared for diamond composition is sintered to the prealloy powder that Examples 1 to 3 is prepared.
It is 300kg/cm that above-mentioned prealloy powder, which is installed in the graphite jig of 55mm × 10mm × 10mm in pressure,2, temperature 750
It is sintered under conditions of DEG C, sintering time is 200 seconds, then tests bending strength, impact flexibility and the HRB hardness of carcass.
The prealloy powder that comparative example 1,3,5 is prepared is sintered the tyre-e/or performance prepared for diamond composition.It will
It is 300kg/cm that above-mentioned prealloy powder, which is installed in the graphite jig of 55mm × 10mm × 10mm in pressure,2, temperature be 800 DEG C
Under conditions of be sintered, sintering time be 200 seconds, then test carcass bending strength, impact flexibility and HRB hardness.
The specimen size of bending strength test is the bar shaped of 5mm × 5mm × 40mm, is measured in Material Testing Machine,
Fulcrum spacing is 30mm.
The specimen size of impact flexibility is 55mm × 10mm × 10mm, and the grooving at test specimen midpoint is 2mm × 2mm.In pendulum-type
Impact test aircraft measurements, using 30~60J pendulums.
The specimen size of HRB hardness is the bar shaped of 5mm × 5mm × 40mm, chooses 5 sample points and takes its average value (four house
Five enter to a position).
Test result is as shown in table 2.
Table 2
It is above-mentioned the experimental results showed that the carcass that the prealloy powder of the embodiment of the present invention is sintered under conditions of 750 DEG C can obtain
Good mechanical performance, simultaneously because sintering temperature is relatively low, when preparing diamond tool such as saw blade tip or drill bit pair
The damage of diamond particles is small, reduces degree of graphitization when sintering, can give full play to the grinding performance of diamond particles.
In order to analyze Examples 1 to 3 and difference of the comparative example 1,3,5 in sintering character and mechanical performance, with embodiment 1, comparison
X-ray diffraction analysis has been carried out for the prealloy powder that example 1 is prepared, and as a result as shown in Fig. 1~2, finds 1 He of embodiment
The prealloy powder that comparative example 1 is prepared can obtain the characteristic peak of the alloys phase such as (FeNi), (CuNiSn), (CuSn), but real
The characteristic peak for applying Fe in the prealloy powder that example 1 is prepared is relatively low, illustrates that the alloying level of the prealloy powder of embodiment 1 is high,
And contain the Fe of more non-alloying in comparative example 1, so that the prealloy powder of the present invention has lower sintering temperature,
And better mechanical performance.
To those skilled in the art, specific embodiment has only carried out exemplary retouch to technical scheme of the present invention
It states, but protection scope of the present invention is not subject to the restrictions described above, as long as using each of technical scheme of the present invention progress
The improvement of kind of unsubstantiality, or it is not improved technical scheme of the present invention is directly applied into other occasions, be regarded as
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of prealloy powder for diamond composition, it is characterised in that include the following steps：
Preparation includes Cu, Fe, Sn, Ni and the optionally strong acid salt of intensified element, is dissolved in the water and is configured to precursor solution；
Prepare precipitant solution, the precipitant solution is made of oxalic acid and hydrazine compound；
Precursor solution is mixed with precipitant solution, be added ammonium hydroxide adjust pH value be 4.0 ~ 8.0, and be added diamine compound into
Row precipitation reaction obtains sediment；
Sediment is calcined to obtain calcined product, calcination temperature is 450 ~ 650 DEG C；
Reduction treatment is carried out to the calcined product under reducing atmosphere, the temperature of reduction treatment is 400 ~ 550 DEG C；Then into
Row is crushed, is sieved.
2. the preparation method of the prealloy powder according to claim 1 for diamond composition, it is characterised in that：It is described strong
It includes at least one of Ti, Mn, W, Zr, Cr, V, Nb, Al, Mg, La or Ce to change element.
3. the preparation method of the prealloy powder according to claim 1 for diamond composition, it is characterised in that：It is described strong
The one kind of hydrochlorate in hydrochloride, sulfate or nitrate.
4. the preparation method of the prealloy powder according to claim 1 for diamond composition, it is characterised in that：The hydrazine
Compound is selected from least one of ethyl hydrazine oxalates, propyl hydrazine oxalates or butyl hydrazine oxalates.
5. the preparation method of the prealloy powder according to claim 1 for diamond composition, it is characterised in that：The hydrazine
Compound and the weight ratio of the oxalic acid are 1:5~20.
6. the preparation method of the prealloy powder according to claim 1 for diamond composition, it is characterised in that：Described two
Amine compounds are selected from least one of ethylenediamine, 1,3- propane diamine or Putriscine.
7. the preparation method of the prealloy powder according to claim 6 for diamond composition, it is characterised in that：Described two
The content of amine compounds is 2 ~ 30 g/L.
8. the preparation method of the prealloy powder according to claim 1 for diamond composition, it is characterised in that：It is described to go back
Originality atmosphere is the reducing atmosphere comprising hydrogen and/or carbon monoxide.
9. the preparation method of the prealloy powder according to claim 1 for diamond composition, it is characterised in that：Before described
It drives in liquid solution, with Cu ionometer contents for 12.5 ~ 63g/L, with Fe ionometer contents for 11.2 ~ 56g/L, is contained with Sn ionometers
Amount is 5.9 ~ 17.7g/L, contains 5.8 ~ 17.4g/L with Ni ionometers；Contain 0 ~ 30g/L with the ion of intensified element.
10. a kind of prealloy powder for diamond composition, it is characterised in that：It is prepared by claim 1 ~ 9 any one of them
Method is prepared.
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| CN112725674A (en) * | 2021-03-19 | 2021-04-30 | 中南大学 | Diamond composite material and preparation method and application thereof |
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| CN115805305A (en) * | 2022-12-13 | 2023-03-17 | 北京有研粉末新材料研究院有限公司 | Spherical composite powder and preparation method thereof |
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