CN113336201A - Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive - Google Patents
Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive Download PDFInfo
- Publication number
- CN113336201A CN113336201A CN202110656231.8A CN202110656231A CN113336201A CN 113336201 A CN113336201 A CN 113336201A CN 202110656231 A CN202110656231 A CN 202110656231A CN 113336201 A CN113336201 A CN 113336201A
- Authority
- CN
- China
- Prior art keywords
- parts
- nitride
- vanadium
- chromium
- composite powder
- 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.)
- Pending
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 93
- 239000000843 powder Substances 0.000 title claims abstract description 81
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title claims abstract description 67
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 239000011812 mixed powder Substances 0.000 claims abstract description 21
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 20
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001935 vanadium oxide Inorganic materials 0.000 claims abstract description 19
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 27
- 238000004321 preservation Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 239000010432 diamond Substances 0.000 claims description 10
- 229910003460 diamond Inorganic materials 0.000 claims description 10
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 10
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 8
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 8
- 229960000892 attapulgite Drugs 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000007767 bonding agent Substances 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 8
- 239000003822 epoxy resin Substances 0.000 claims description 8
- 239000010433 feldspar Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 239000012948 isocyanate Substances 0.000 claims description 8
- 150000002513 isocyanates Chemical class 0.000 claims description 8
- 229910052625 palygorskite Inorganic materials 0.000 claims description 8
- 229920000647 polyepoxide Polymers 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 239000003082 abrasive agent Substances 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 4
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 5
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000011257 shell material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 33
- 239000011651 chromium Substances 0.000 description 22
- 238000006722 reduction reaction Methods 0.000 description 14
- 230000009467 reduction Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 6
- 125000004429 atom Chemical group 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910003470 tongbaite Inorganic materials 0.000 description 5
- -1 Transition metal nitrides Chemical class 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 238000005121 nitriding Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009768 microwave sintering Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
- B24D3/28—Resins or natural or synthetic macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/062—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention relates to the technical field of grinding, in particular to a preparation method of vanadium nitride/chromium nitride composite powder and application of the vanadium nitride/chromium nitride composite powder in a polymeric abrasive. S1, ball-milling and uniformly mixing the carbon reducing agent, the nano vanadium oxide and the nano chromium oxide to obtain mixed powder; s2, drying the mixed powder obtained in the step S1; s3, microwave heating the mixed powder obtained in the step S2 for 30-120 min in the atmosphere of nitrogen, wherein the microwave heating power is 600-1100W. The vanadium nitride/chromium nitride composite powder prepared by the gradient microwave heating method has high purity and uniform particles; the abrasive is applied to the polymeric abrasive as a shell material, so that the breaking strength is greatly improved, the grinding efficiency is further improved, and the service life of the polymeric abrasive is prolonged.
Description
Technical Field
The invention relates to the technical field of grinding, in particular to a preparation method of vanadium nitride/chromium nitride composite powder and application of the vanadium nitride/chromium nitride composite powder in a polymeric abrasive.
Background
Transition metal nitrides are a class of intermetallic filling compounds that have the properties of covalent compounds, ionic crystals and transition metals. Most of the nitrides have the properties of high hardness, excellent thermal stability, excellent corrosion resistance and the like, and the properties are greatly different from those of metal materials and tend to those of ceramic materials. However, such materials have metal-like electrical and magnetic properties and tend to have good electrical conductivity. Due to these special properties, such materials are widely used in high strength tool coating materials, drilling materials, cutting materials and catalytic materials.
However, the traditional preparation of vanadium (chromium) nitride often requires high temperature (more than 1300 ℃) and longer nitriding time (more than 10h), and the whole preparation process is long in period and high in energy consumption. Moreover, long-term high-temperature reaction processes often lead to rapid growth of powder particles. Therefore, it is often difficult to prepare nitride powders of nanometer order by the conventional preparation method. Currently commercially available vanadium (chromium) nitride powders are typically in the micron scale and a single vanadium (chromium) nitride powder cannot meet its stringent needs in the modern industry.
In view of the defects in the prior art, the inventor develops a preparation method of vanadium nitride/chromium nitride composite powder and application thereof in a polymerization grinding material based on years of abundant experience and professional knowledge of the materials, and combines theoretical analysis and research innovation, and obtains the nano-scale vanadium nitride/chromium nitride composite powder with higher purity and uniform shape by adopting a gradient microwave heating method while reducing the synthesis temperature.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of vanadium nitride/chromium nitride composite powder, which adopts a gradient microwave heating mode to obtain nano-scale vanadium nitride/chromium nitride powder with higher purity and more uniform shape.
The technical purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of vanadium nitride/chromium nitride composite powder, which comprises the following operation steps:
s1, ball-milling and uniformly mixing the carbon reducing agent, the nano vanadium oxide and the nano chromium oxide to obtain mixed powder;
s2, drying the mixed powder obtained in the step S1;
s3, microwave heating the mixed powder obtained in the step S2 for 30-120 min in the atmosphere of nitrogen, wherein the microwave heating power is 600-1100W.
The invention takes nano vanadium oxide and nano chromium oxide as vanadium and chromium sources, takes nano carbon black as a carbon source, and adopts a microwave heating in-situ reduction nitridation process to synthesize nano vanadium nitride/chromium powder. The nano material has high chemical activity and can accelerate the carbothermic reduction nitridation reaction because the raw material is nano powder which has high specific surface area, large contact area between particles, more interface atoms and high diffusion coefficient of atoms in an interface area. In addition, microwave heating has the advantages of high heating speed, uniform heating, high thermal efficiency, safety, cleanness, no pollution and the like, and is one of the best heating ways. Meanwhile, vanadium pentoxide and various forms of carbon are good wave-absorbing materials, and the nano powder has large surface atomic number, lacks adjacent atoms around the surface atoms, has a plurality of dangling bonds, has unsaturated properties, is easy to combine with other atoms to be stably released, and has great chemical activity; and the diameter of the nano particles is small, so that the diffusion distance of carbon and nitrogen atoms to the inside of the matrix is reduced, and the reaction is accelerated under the action of microwave heating non-thermal effect, so that the reaction temperature is reduced.
Further, the microwave heating in step S3 is divided into three gradient heating. Because the reaction of chromium nitride and vanadium nitride generated by chromium oxide and vanadium oxide in the presence of the carbon reducing agent is a gradual reduction reaction, different heating temperatures are required in different reduction stages, and the reaction is influenced in the forward direction if the temperature is too high or too low, the whole reduction reaction process can be carried out at the optimum temperature by adopting a gradient heating mode, the generation of mixed crystals is avoided, the purity of the chromium nitride/vanadium nitride composite powder is improved, and the energy is saved.
Further, the first gradient of microwave heating in the step S3 is microwave heating of 600-800W, and heat preservation is carried out for 10-20 min; the second gradient is microwave heating at 1000-1100W, and heat preservation is carried out for 50-80 min; the third gradient is microwave heating at 800-900W, and heat preservation is carried out for 10-30 min.
Due to VO2And V2O3Is relatively low in formation temperature, and V2O5Has a melting point of 675 ℃ and is strongly volatilized when the temperature is higher than 700 ℃ to cause serious raw material loss, so that the temperature is maintained at 600-700 ℃ for a period of time when the microwave heating power of the first gradient is 600-800W to ensure that V is converted into V2O5VO (vanadium suboxide) converted into non-volatile vanadium2And V2O3；V2O3The further reduced product is VO, the conversion temperature of which is higher than V2O3Conversion temperature to VC, i.e. V in the case of excess carbon2O3The carbonization reaction formula is preferentially generated to generate VC, and if VO is generated in the reaction process2Is produced in a large amount and is converted into V2O3Part of (b) can be directly carbonized to VC and the conversion of VC to VN is an exothermic process, but the temperature increase is detrimental to the reaction. However, due to V2O5The reduction and carbonization reaction of (2) is an endothermic reaction, and the gradual reduction of the vanadium oxide is not favored by the temperature reduction. Therefore, under the nitrogen atmosphere, the vanadium oxide is gradually reduced and fully carbonized at a higher temperature, and then the temperature is reduced to a temperature suitable for nitriding, so that the carbide is fully nitrided, the nitrogen content in the final product is increased, and the introduction of VC is avoided.
The carbothermic reduction reaction mechanism of chromium oxide is two, the first is CO gas generated by Boudouord reaction (gasification reaction of carbon), and the CO gas is adsorbed on the surface of oxide to reduce and carbonize Cr2O3(ii) a The second is Cr2O3Directly reacting with C, and directly contacting carbon atoms with the surface of the oxide through a certain process, so that the carbon black and the oxide can directly perform reduction carbonization reaction when being heated. However, since CO is generated by the carbothermic reduction reaction, both mechanisms occur simultaneously during the reaction. Under the vacuum condition, carbon powder is added according to 99-101% of oxygen content in chromium oxide, and reduction is carried out in two different temperature stages, so that the chromium oxide with the Cr content of more than 99% and the C content of less thanLess than 0.02% of metallic chromium with an oxygen content of less than 0.5%. However, when carbon is used as a reducing agent in a flowing nitrogen atmosphere, Cr2O3Does not contain metallic chromium, but directly generates chromium carbide such as Cr3C2Or a mesophase Cr when the carbon is in excess and the temperature conditions are appropriate3C2-x(x is more than or equal to 0 and less than or equal to 0.5). Therefore, the high-temperature nitriding stage according to the present invention is an oxide Cr of chromium2O3Direct reduction nitridation to CrN or Cr carbide of chromium3C2And Cr3C2-xThen, the carbide is gradually nitrided, and the whole process does not generate nitriding reaction of the metal chromium simple substance. According to the Boudouord reaction mechanism, Cr2O3The change in gibbs free energy at which the carbonization reaction occurs is shown by the following reaction equations:
C(s)+CO2(g)＝2CO(g)，△Gθ＝-117990-84.35T；
3Cr2O3(s)+17CO(g)＝2Cr3C2(s)+13CO2(g)，△Gθ＝-723165-171.00T；
Cr2O3possible chemical formulae in the direct reaction with C are as follows:
3Cr2O3(s)+13C(s)＝2Cr3C2(s)+9CO(g)，△Gθas can be seen from the reaction formula 359410-774.65T, the lower the partial pressure of CO, the more the reaction proceeds in the forward direction. When Cr is present2O3Conversion to Cr3C2When the crystal structure is changed from hexagonal close packing to orthorhombic. Cr (chromium) component3C2The generation temperature is lower, and the reaction temperature is improved, which is beneficial to Cr3C2And (4) generating.
Cr3C2The conversion to CrN can be achieved by the following formula:
2Cr3C2(s)+3N2(g)＝6CrN(s)+4C(s)；
Cr2N(s)+1/2N2(g)＝2CrN(s)，△Gθ＝-261330+212.80T。
at 1220 ℃ or lower, Delta GθThe value of (A) is negative, which indicates that the reaction formula can spontaneously proceed in the positive direction in this temperature range, i.e., Cr2The stability of N is higher than that of CrN. Theoretically Δ GθThe smaller the reaction, the greater the probability that the reaction will occur, and Δ G of this reaction formulaθThe temperature is gradually increased, so that the reaction is inhibited by the temperature increase, and the method of the invention adopting the gradient microwave heating mode is also favorable for generating CrN.
Further, the material addition in the step 1 is as follows according to the parts by weight: 20-26 parts of carbon reducing agent, 37-40 parts of nano chromium oxide and 37-40 parts of nano vanadium oxide.
Further, the carbon reducing agent is nano carbon black.
Furthermore, the nano chromium oxide is nano chromium sesquioxide, and the nano vanadium oxide is nano vanadium pentoxide.
The second purpose of the invention is to provide the application of the vanadium nitride/chromium nitride composite powder in the polymeric abrasive, which improves the flexural strength of the polymeric abrasive and improves the grinding efficiency.
The technical points are as follows:
the application of the vanadium nitride/chromium nitride composite powder in the polymeric abrasive is to polymerize the vanadium nitride/chromium nitride composite powder with the composite abrasive by an in-situ growth method.
Further, the in-situ growth comprises the following operation steps:
a1, uniformly stirring the composite abrasive, and grinding the mixture into composite abrasive micropowder;
a2, adding vanadium nitride/chromium nitride composite powder and a bonding agent into the composite abrasive micro powder for bonding, and then curing, wherein the addition amount of the vanadium nitride/chromium nitride composite powder is 0.8-1.5% of that of the composite abrasive;
a3, crushing the solidified material and sieving the crushed material into the polymeric abrasive with the required grain size.
Further, the polymeric abrasive comprises the following components in parts by weight: 30-40 parts of silicon carbide, 10-18 parts of corundum abrasive and 1-3 parts of boron nitride.
Further, the binding agent comprises the following components in parts by weight: 30-40 parts of E-44 epoxy resin, 10-15 parts of polyurethane prepolymer, 1-3 parts of diamond micro powder, 7-10 parts of isocyanate, 21-23 parts of attapulgite, 10-14 parts of feldspar, 20-25 parts of boron glass and 40-45 parts of quartz.
Further, the preparation method of the binding agent is as follows:
b1, sieving the diamond micropowder, then uniformly mixing the E-44 epoxy resin, the polyurethane prepolymer and the isocyanate, and uniformly mixing the diamond micropowder and the mixture for later use;
b2, mixing attapulgite, feldspar, boron glass and quartz, grinding and sieving by a 120-mesh sieve;
b3, heating the prepared mixture to 1200 ℃ at the speed of 10 ℃/min, smelting for 4h, and then water quenching;
b4, drying the water-quenched product at 108 ℃ for 6 hours, grinding, and sieving with a 150-mesh sieve for later use;
b5, uniformly mixing the product obtained in the step B1 and the product obtained in the step B2, pressing the mixture into a blank by using a press, and sintering the blank by using a microwave sintering furnace to obtain the bonding agent.
In conclusion, the invention has the following beneficial effects:
the vanadium nitride/chromium nitride composite powder prepared by the gradient microwave heating method has high purity and uniform particles; the abrasive is applied to the polymeric abrasive as a shell material, so that the breaking strength is greatly improved, the grinding efficiency is further improved, and the service life of the polymeric abrasive is prolonged.
Drawings
FIG. 1 is an XRD pattern of the vanadium nitride/chromium nitride composite powder of examples 1 to 4;
FIG. 2 is an SEM image of the vanadium nitride/chromium nitride composite powder of example 2.
Reference numerals
a. XRD profile of the vanadium nitride/chromium nitride composite powder of example 4, b. XRD profile of the vanadium nitride/chromium nitride composite powder of example 3, c. XRD profile of the vanadium nitride/chromium nitride composite powder of example 2, d. XRD profile of the vanadium nitride/chromium nitride composite powder of example 1.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the detailed description of the preparation method of the vanadium nitride/chromium nitride composite powder and the application thereof in the polymeric abrasive material according to the present invention are as follows.
The materials used in this example are all commercially available.
Example 1
Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive
A preparation method of vanadium nitride/chromium nitride composite powder comprises the following operation steps:
s1, ball-milling and uniformly mixing the carbon reducing agent, the nano vanadium oxide and the nano chromium oxide to obtain mixed powder;
s2, drying the mixed powder obtained in the step S1;
s3, microwave heating the mixed powder obtained in the step S2 for 30-120 min in the atmosphere of nitrogen, wherein the microwave heating power is 600-1100W.
Wherein, the material adding amount in the step S1 is as follows according to the weight portion: 26 parts of carbon reducing agent, 40 parts of nano chromium oxide and 40 parts of nano vanadium oxide.
The application of the vanadium nitride/chromium nitride composite powder in the polymeric abrasive comprises the following operation steps:
a1, uniformly stirring the composite abrasive, and grinding the mixture into composite abrasive micropowder;
a2, adding vanadium nitride/chromium nitride composite powder and a bonding agent into the composite abrasive micro powder for bonding, and then curing, wherein the addition amount of the vanadium nitride/chromium nitride composite powder is 1.0 percent of that of the composite abrasive;
a3, crushing the solidified material and sieving the crushed material into the polymeric abrasive with the required grain size.
Wherein, the polymeric abrasive comprises the following components in parts by weight: 40 parts of silicon carbide, 18 parts of corundum abrasive and 3 parts of boron nitride; the binding agent comprises the following components: 40 parts of E-44 epoxy resin, 15 parts of polyurethane prepolymer, 3 parts of diamond micropowder, 10 parts of isocyanate, 23 parts of attapulgite, 14 parts of feldspar, 25 parts of boron glass and 45 parts of quartz.
Example 2
Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive
A preparation method of vanadium nitride/chromium nitride composite powder comprises the following operation steps:
s1, ball-milling and uniformly mixing the carbon reducing agent, the nano vanadium oxide and the nano chromium oxide to obtain mixed powder;
s2, drying the mixed powder obtained in the step S1;
s3, performing microwave heating on the mixed powder obtained in the step S2 in the atmosphere of nitrogen, performing first gradient heating and heat preservation for 20min under the power of 600W; the second gradient is heating and heat preservation for 60min under the power of 1100W, and the third gradient is heating and heat preservation for 20min under the power of 900W.
Wherein, the material adding amount in the step S1 is as follows according to the weight portion: 24 parts of carbon reducing agent, 38 parts of nano chromium oxide and 38 parts of nano vanadium oxide.
The application of the vanadium nitride/chromium nitride composite powder in the polymeric abrasive comprises the following operation steps:
a1, uniformly stirring the composite abrasive, and grinding the mixture into composite abrasive micropowder;
a2, adding vanadium nitride/chromium nitride composite powder and a bonding agent into the composite abrasive micro powder for bonding, and then curing, wherein the addition amount of the vanadium nitride/chromium nitride composite powder is 1.5% of the composite abrasive;
a3, crushing the solidified material and sieving the crushed material into the polymeric abrasive with the required grain size.
Wherein, the polymeric abrasive comprises the following components in parts by weight: 30 parts of silicon carbide, 10 parts of corundum abrasive and 1 part of boron nitride; the binding agent comprises the following components: 30 parts of E-44 epoxy resin, 10 parts of polyurethane prepolymer, 1 part of diamond micropowder, 7 parts of isocyanate, 21 parts of attapulgite, 10 parts of feldspar, 20 parts of boron glass and 40 parts of quartz.
Example 3
Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive
A preparation method of vanadium nitride/chromium nitride composite powder comprises the following operation steps:
s1, ball-milling and uniformly mixing the carbon reducing agent, the nano vanadium oxide and the nano chromium oxide to obtain mixed powder;
s2, drying the mixed powder obtained in the step S1;
s3, performing microwave heating on the mixed powder obtained in the step S2 in a nitrogen atmosphere, performing first gradient heating and heat preservation for 10min under the power of 800W; the second gradient is heating and heat preservation for 70min under the power of 1100W, and the third gradient is heating and heat preservation for 20min under the power of 800W.
Wherein, the material adding amount in the step S1 is as follows according to the weight portion: 22 parts of carbon reducing agent, 40 parts of nano chromium oxide and 40 parts of nano vanadium oxide.
The application of the vanadium nitride/chromium nitride composite powder in the polymeric abrasive comprises the following operation steps:
a1, uniformly stirring the composite abrasive, and grinding the mixture into composite abrasive micropowder;
a2, adding vanadium nitride/chromium nitride composite powder and a bonding agent into the composite abrasive micro powder for bonding, and then curing, wherein the addition amount of the vanadium nitride/chromium nitride composite powder is 1.0 percent of that of the composite abrasive;
a3, crushing the solidified material and sieving the crushed material into the polymeric abrasive with the required grain size.
Wherein, the polymeric abrasive comprises the following components in parts by weight: 30 parts of silicon carbide, 10 parts of corundum abrasive and 1 part of boron nitride; the binding agent comprises the following components: 30 parts of E-44 epoxy resin, 10 parts of polyurethane prepolymer, 1 part of diamond micropowder, 7 parts of isocyanate, 21 parts of attapulgite, 10 parts of feldspar, 20 parts of boron glass and 40 parts of quartz.
Example 4
Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive
A preparation method of vanadium nitride/chromium nitride composite powder comprises the following operation steps:
s1, ball-milling and uniformly mixing the carbon reducing agent, the nano vanadium oxide and the nano chromium oxide to obtain mixed powder;
s2, drying the mixed powder obtained in the step S1;
s3, performing microwave heating on the mixed powder obtained in the step S2 in the nitrogen atmosphere, performing first gradient heating and heat preservation for 20min under the power of 700W; the second gradient is heating and heat preservation for 60min under the power of 1000W, and the third gradient is heating and heat preservation for 20min under the power of 900W.
Wherein, the material adding amount in the step S1 is as follows according to the weight portion: 24 parts of carbon reducing agent, 37 parts of nano chromium oxide and 37 parts of nano vanadium oxide.
The application of the vanadium nitride/chromium nitride composite powder in the polymeric abrasive comprises the following operation steps:
a1, uniformly stirring the composite abrasive, and grinding the mixture into composite abrasive micropowder;
a2, adding vanadium nitride/chromium nitride composite powder and a bonding agent into the composite abrasive micro powder for bonding, and then curing, wherein the addition amount of the vanadium nitride/chromium nitride composite powder is 0.8 percent of that of the composite abrasive;
a3, crushing the solidified material and sieving the crushed material into the polymeric abrasive with the required grain size.
Wherein, the polymeric abrasive comprises the following components in parts by weight: 35 parts of silicon carbide, 12 parts of corundum abrasive and 2 parts of boron nitride; the binding agent comprises the following components: 30 parts of E-44 epoxy resin, 10 parts of polyurethane prepolymer, 2 parts of diamond micropowder, 7 parts of isocyanate, 21 parts of attapulgite, 10 parts of feldspar, 20 parts of boron glass and 42 parts of quartz.
The preparation method of the binding agent comprises the following steps:
b1, sieving the diamond micropowder, then uniformly mixing the E-44 epoxy resin, the polyurethane prepolymer and the isocyanate, and uniformly mixing the diamond micropowder and the mixture for later use;
b2, mixing attapulgite, feldspar, boron glass and quartz, grinding and sieving by a 120-mesh sieve;
b3, heating the prepared mixture to 1200 ℃ at the speed of 10 ℃/min, smelting for 4h, and then water quenching;
b4, drying the water-quenched product at 108 ℃ for 6 hours, grinding, and sieving with a 150-mesh sieve for later use;
b5, uniformly mixing the product obtained in the step B1 and the product obtained in the step B2, pressing the mixture into a blank by using a press, and sintering the blank by using a microwave sintering furnace to obtain the bonding agent.
1. XRD (X-ray diffraction) tests are carried out on the vanadium nitride/chromium nitride composite powder obtained in the examples 1-4, and the test results are shown in the attached figures 1-2;
2. the flexural strength of the polymeric abrasives obtained in examples 1-4 was tested and the results are shown in Table 1.
2. The flexural strength of the polymeric abrasives obtained in examples 1-4 was tested and the results are shown in Table 1.
TABLE 1 flexural Strength test results for the polymeric abrasives of examples 1-4
| Flexural strength// MPa | |
| Example 1 | 94.4 |
| Example 2 | 121.9 |
| Example 3 | 119.8 |
| Example 4 | 120.3 |
As shown in FIG. 1, when the microwave power is 900W, the gradient microwave heating method is adopted, the synthesized composite powder has VN and CrN as main diffraction peaks, and relatively weak Cr exists2O3And Cr2N0.39C0.61The diffraction peak of (1). In the case of producing nitrides by the conventional carbothermal reduction nitridation method, the temperature at which VN and CrN are produced is 1200 ℃. VN and CrN are formed after a temperature of 900W is maintained for 1.5h by microwave heating, and the maximum temperature is only 1028 ℃. It can be seen that the microwave heating mode can reduce the synthesis temperature of VN/CrN composite powder by about 200 ℃, which is mainly attributed to the non-thermal effect of microwave heating. And the peak positions of example 3 (curve b) and example 2 (curve c) were substantially the same, but Cr2N0.39C0.61The intensity of the peak of (a) decreases with increasing microwave power. It is explained that when the microwave power is increased to 1000W or more, the oxides in the raw material can be completely reduced, and the N atoms gradually move to Cr with the increase of the power2N0.39C0.61Medium diffusion generates CrN. As is clear from example 1 (curve d), Cr is present in the product6.2C3.5N0.3And Cr2VC2. The two products reduce the nitrogen content in the final composite powder, and in order to reduce the contents of the two substances as much as possible, a gradient microwave heating mode is adopted.
As can be seen from fig. 2, the particle size of the vanadium nitride/chromium nitride composite powder obtained by the gradient microwave heating is uniform.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of vanadium nitride/chromium nitride composite powder is characterized by comprising the following operation steps:
s1, ball-milling and uniformly mixing the carbon reducing agent, the nano vanadium oxide and the nano chromium oxide to obtain mixed powder;
s2, drying the mixed powder obtained in the step S1;
s3, microwave heating the mixed powder obtained in the step S2 for 30-120 min in the atmosphere of nitrogen, wherein the microwave heating power is 600-1100W.
2. The method of claim 1, wherein the microwave heating in step S3 is divided into three gradient heating.
3. The method for preparing vanadium nitride/chromium nitride composite powder according to claim 2, wherein the first gradient of microwave heating in step S3 is 600 to 800W, and the temperature is maintained for 10 to 20 min; the second gradient is microwave heating at 1000-1100W, and heat preservation is carried out for 50-80 min; the third gradient is microwave heating at 800-900W, and heat preservation is carried out for 10-30 min.
4. The method for preparing vanadium nitride/chromium nitride composite powder according to claim 1, wherein the materials added in step S1 are as follows in parts by weight: 20-26 parts of a carbon reducing agent, 37-40 parts of nano chromium oxide and 37-40 parts of nano vanadium oxide.
5. The method for preparing vanadium nitride/chromium nitride composite powder according to any one of claims 1 to 4, wherein the carbon reducing agent is nano carbon black.
6. The method for preparing vanadium nitride/chromium nitride composite powder according to any one of claims 1 to 4, wherein the nano chromium oxide is nano chromium sesquioxide and the nano vanadium oxide is nano vanadium pentoxide.
7. Use of the vanadium nitride/chromium nitride composite powder according to claim 1 in a polymeric abrasive, wherein the composite powder is polymerized with the abrasive by in situ growth.
8. Use of a vanadium nitride/chromium nitride composite powder in a polymeric abrasive according to claim 7, characterized in that said in situ growth comprises the following operative steps:
a1, uniformly stirring the composite abrasive, and grinding the mixture into composite abrasive micropowder;
a2, adding vanadium nitride/chromium nitride composite powder and a bonding agent into the composite abrasive micro powder for bonding, and then curing, wherein the addition amount of the vanadium nitride/chromium nitride composite powder is 0.8-1.5% of that of the composite abrasive;
a3, crushing the solidified material and sieving the crushed material into the polymeric abrasive with the required grain size.
9. The use of the vanadium nitride/chromium nitride composite powder according to claim 7 in polymeric abrasives, wherein the polymeric abrasives comprise the following components in parts by weight: 30-40 parts of silicon carbide, 10-18 parts of corundum abrasive and 1-3 parts of boron nitride.
10. The use of the vanadium nitride/chromium nitride composite powder in a polymeric abrasive according to claim 7, wherein the binder comprises the following components in parts by weight: 30-40 parts of E-44 epoxy resin, 10-15 parts of polyurethane prepolymer, 1-3 parts of diamond micro powder, 7-10 parts of isocyanate, 21-23 parts of attapulgite, 10-14 parts of feldspar, 20-25 parts of boron glass and 40-45 parts of quartz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110656231.8A CN113336201A (en) | 2021-06-11 | 2021-06-11 | Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110656231.8A CN113336201A (en) | 2021-06-11 | 2021-06-11 | Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113336201A true CN113336201A (en) | 2021-09-03 |
Family
ID=77476965
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110656231.8A Pending CN113336201A (en) | 2021-06-11 | 2021-06-11 | Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113336201A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5188130A (en) * | 1989-11-29 | 1993-02-23 | Philip Morris, Incorporated | Chemical heat source comprising metal nitride, metal oxide and carbon |
| CN1562770A (en) * | 2004-04-06 | 2005-01-12 | 湘潭市恒新特种合金厂 | Method for preparing vanadium nitride and device |
| CN102674844A (en) * | 2012-06-04 | 2012-09-19 | 河南工业大学 | Method for preparing nanometer vanadium/chromium carbide composite powder by reduction with microwave method |
| CN203216257U (en) * | 2013-02-01 | 2013-09-25 | 湖南省中晟热能科技有限公司 | Pushed slab kiln for compounding and sintering vanadium nitride through microwave-electric hybrid heating |
| CN111002235A (en) * | 2019-12-24 | 2020-04-14 | 江苏锋芒复合材料科技集团有限公司 | Preparation method of novel polymeric abrasive |
| CN111635236A (en) * | 2020-05-26 | 2020-09-08 | 南京理工大学 | Method for microwave sintering of sialon ceramic material |
| CN112605390A (en) * | 2020-10-19 | 2021-04-06 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of vacuum-grade low-nitrogen metal chromium for preparing high-temperature alloy by using chromium powder |
-
2021
- 2021-06-11 CN CN202110656231.8A patent/CN113336201A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5188130A (en) * | 1989-11-29 | 1993-02-23 | Philip Morris, Incorporated | Chemical heat source comprising metal nitride, metal oxide and carbon |
| CN1562770A (en) * | 2004-04-06 | 2005-01-12 | 湘潭市恒新特种合金厂 | Method for preparing vanadium nitride and device |
| CN102674844A (en) * | 2012-06-04 | 2012-09-19 | 河南工业大学 | Method for preparing nanometer vanadium/chromium carbide composite powder by reduction with microwave method |
| CN203216257U (en) * | 2013-02-01 | 2013-09-25 | 湖南省中晟热能科技有限公司 | Pushed slab kiln for compounding and sintering vanadium nitride through microwave-electric hybrid heating |
| CN111002235A (en) * | 2019-12-24 | 2020-04-14 | 江苏锋芒复合材料科技集团有限公司 | Preparation method of novel polymeric abrasive |
| CN111635236A (en) * | 2020-05-26 | 2020-09-08 | 南京理工大学 | Method for microwave sintering of sialon ceramic material |
| CN112605390A (en) * | 2020-10-19 | 2021-04-06 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of vacuum-grade low-nitrogen metal chromium for preparing high-temperature alloy by using chromium powder |
Non-Patent Citations (1)
| Title |
|---|
| 李俊等: "微波碳热还原法制备氮化钒的研究和实践", 《铁合金》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108840681B (en) | Nano boron carbide and preparation method thereof | |
| CN110436928A (en) | High-performance nano twin boron carbide ceramics block materials and preparation method thereof | |
| CN109437917B (en) | Method for producing titanium nitride and titanium carbonitride by two-stage reduction nitridation | |
| CN112125680A (en) | Boron carbide micro powder purification method, boron carbide ceramic and preparation method of boron carbide ceramic | |
| CN113336201A (en) | Preparation method of vanadium nitride/chromium nitride composite powder and application of vanadium nitride/chromium nitride composite powder in polymeric abrasive | |
| CN101914734B (en) | Method for preparing spinel whisker/aluminum composite block material by in-situ growth in aluminum matrix | |
| CN111172443B (en) | High-comprehensive-performance hard alloy cutter material and preparation method thereof | |
| Dehghanzadeh et al. | Synthesis of nanosize silicon carbide powder by carbothermal reduction of SiO 2 | |
| CN113319742B (en) | Preparation method of abrasive with grinding and polishing functions | |
| Dolukhanyan et al. | Formation of the Ti2Alc Max-Phase in a Hydride Cycle From a Mixture of Titanium and Aluminum Carbohydride Powders | |
| JP4526343B2 (en) | WC-SiC sintered body with high hardness, high Young's modulus, and high fracture toughness | |
| JP2022136391A (en) | Al4SiC4 COMPOSITION OR Al4SiC4 POWDER, AND METHOD OF PRODUCING THE SAME | |
| JPS61117107A (en) | Amorphous boron niride powder and its preparation | |
| CN109650862B (en) | High-temperature-resistant boron nitride-strontium feldspar ceramic matrix composite material and preparation method thereof | |
| JPS58213617A (en) | Production of titanium carbonitride powder | |
| CN111732436A (en) | Easy-to-sinter titanium and tungsten co-doped zirconium carbide powder and preparation method thereof | |
| CN111847458A (en) | Preparation method of high-purity and low-cost molybdenum disilicide | |
| JPS63199833A (en) | Manufacture of high-purity metallic chromium | |
| CN114835124B (en) | Preparation method of nano silicon carbide particles based on ferric nitrate shape regulator | |
| US20220289635A1 (en) | Method for preparing carbon/boron carbide composite material | |
| TWI746329B (en) | Preparation method of carbon/boron carbide composite material | |
| JP4542747B2 (en) | Manufacturing method of high strength hexagonal boron nitride sintered body | |
| RU2789998C1 (en) | Method for obtaining silicon carbide | |
| JPH04321560A (en) | Production of isotropic graphite material having high strength | |
| JPS58213619A (en) | Production of powder of composite carbonitride solid solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210903 |