CN107265515B - A kind of High Content Chromium doped ferroferric oxide raw powder's production technology - Google Patents
A kind of High Content Chromium doped ferroferric oxide raw powder's production technology Download PDFInfo
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- CN107265515B CN107265515B CN201710638499.2A CN201710638499A CN107265515B CN 107265515 B CN107265515 B CN 107265515B CN 201710638499 A CN201710638499 A CN 201710638499A CN 107265515 B CN107265515 B CN 107265515B
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- 239000011651 chromium Substances 0.000 title claims abstract description 89
- 239000000843 powder Substances 0.000 title claims abstract description 66
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 26
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000005516 engineering process Methods 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 21
- 239000011888 foil Substances 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000004062 sedimentation Methods 0.000 claims abstract description 15
- 238000000748 compression moulding Methods 0.000 claims abstract description 14
- 238000004448 titration Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 238000005253 cladding Methods 0.000 claims abstract description 10
- 230000001376 precipitating effect Effects 0.000 claims abstract description 10
- 239000013049 sediment Substances 0.000 claims abstract description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 238000000975 co-precipitation Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 20
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 16
- 239000010453 quartz Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000003708 ampul Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 229910000963 austenitic stainless steel Inorganic materials 0.000 abstract description 5
- 238000010301 surface-oxidation reaction Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000013456 study Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 description 7
- 230000002285 radioactive effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229910003430 FeCr2O4 Inorganic materials 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 229910003265 NiCr2O4 Inorganic materials 0.000 description 1
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009390 chemical decontamination Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
- G21C3/02—Fuel elements
- G21C3/04—Constructional details
- G21C3/16—Details of the construction within the casing
- G21C3/18—Internal spacers or other non-active material within the casing, e.g. compensating for expansion of fuel rods or for compensating excess reactivity
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention relates to a kind of High Content Chromium doped ferroferric oxide raw powder's production technology, the molecular formula of the material is Fe3‑xCrxO4, which adulterates Fe the following steps are included: step (1), using coprecipitation preparation Cr3O4Front axle shell: precipitating reagent is slowly dropped to the FeSO in stirring4With Cr2(SO4)3In mixed solution, sediment is dried in natural sedimentation after the completion of titration, is taken out grinding and is uniformly obtained front axle shell；Step (2), by above-mentioned front axle shell compression moulding, using vacuum-sintering is carried out after the first Fe foil cladding, taking-up is pulverized, and step (3) adds Fe in above-mentioned powder2O3Powder, compression moulding after grinding uniformly take out grinding uniformly with vacuum-sintering is carried out after the 2nd Fe foil cladding, the Fe of as required high-content Cr doping3O4Powder Fe3‑xCrxO4, wherein x=1-1.5, the present invention provides the high-content Cr that a kind of prior art can not be prepared to adulterate Fe3O4Powder CrxFe3‑xO4Method, so as to easily study the performance of nuclear power plant's primary heat transport system Austenitic stainless steel pipe wall surface oxidation film.
Description
Technical field
The invention belongs to nuclear industry fields, are related to the preparation method of oxide powder, and in particular to a kind of High Content Chromium is mixed
Miscellaneous ferroso-ferric oxide raw powder's production technology.
Background technique
Nuclear power plant is after running some cycles, and the radioactive pollutant of meeting depositing dosed quantities, gives on primary heat transport system tube wall
The personnel of equipment inspection and maintenance cause certain radiation.The radioactive pollutant of wherein most is mainly due to corrosion product
Caused by being activated in reactor core.Corrosion product is influenced constantly to move in system by temperature, pressure, flow velocity and chemical environment of water
It moves and deposits, it will usually combine closely with Austenitic stainless steel pipe wall surface oxidation film.Chemical decontamination is removal major loop radiation
Property sediment pollution reduce dose of radiation effective means.
Austenitic stainless steel is widely used in PWR nuclear power plant nuclear island and nuclear auxiliary building, it is considered that its surface oxidation
Film has internal dense lamella and external oxidation sedimentary, and composition is a kind of similar Fe with spinel structure3O4Substance
(NixCryFe3-x-yO4), about 0.4~2.5 μm of oxide thickness.By the synthesis of the factors such as material, chemical environment of water, runing time
It influences, under presurized water reactor reproducibility water-chemical regime, the common chemical composition of oxide specifically has Fe3O4、NiFe2O4With
FeCr2O4, NiCr2O4, Fe2CrO4Deng.Make the inside and outside oxygen on washer surface by chemical methodes such as oxidation, reduction, complexings
Change layer all to dissolve, so that removal is deposited on the radioactive substance of equipment surface.
It in order to be effectively removed radionuclide, while avoiding injuring basis material, to being deposited on oxidation film Radionuclide
Existing forms and protective oxide film Forming Mechanism carry out research and are necessary.In these above-mentioned oxide components, Cr doping
Fe3O4(CrxFe3-xO4) due to its dissolubility it is poor, be even more important to the research of this oxide.In CrxFe3-xO4The preparation of powder
Aspect, existing document report is prepared for the Fe of low Cr content (Cr atomic ratio < 20%) doping using chemical method both at home and abroad3O4Sample.
But since the activity of Cr element is big, high-content CrxFe3-xO4The preparation of powder be it is very difficult, there is presently no correlative studys
The report of work.
Summary of the invention
The purpose of the invention is to overcome the deficiencies of the prior art and provide a kind of High Content Chromium doped ferroferric oxide powder
The preparation method of body.
In order to achieve the above objectives, a kind of the technical solution adopted by the present invention are as follows: High Content Chromium doped ferroferric oxide powder
Preparation method, comprising the following steps:
Step (1) adulterates Fe using coprecipitation preparation Cr3O4Front axle shell A: precipitating reagent is slowly dropped in stirring
FeSO4With Cr2(SO4)3In mixed solution, sediment is dried in natural sedimentation after the completion of titration, is taken out before grinding uniform obtain
Drive powder A；
The front axle shell A compression moulding is taken out grinding using vacuum-sintering is carried out after the first Fe foil cladding by step (2)
Obtain powder B；
Step (3) adds Fe in the powder B2O3Powder, grinding uniformly obtain powder C, the powder C are pressed into
Type is taken out grinding and obtains powder D, the powder D is required high-content Cr with vacuum-sintering is carried out after the 2nd Fe foil cladding
The Fe of doping3O4Powder Fe3-xCrxO4。
Further, the precipitating reagent is KOH solution or NaOH solution.
Further, the precipitating reagent is the mixed liquor of KOH solution and NaOH solution.
Further, the FeSO4With Cr2(SO4)3Mixed solution according to the atomic ratio of Fe and Cr be 1:1-2:1 carry out
It prepares.
Further, in the step (1), the rate of titration of the precipitating reagent is 0.03-0.05cm3/ min, it is described
FeSO4With Cr2(SO4)3The mixing speed of mixed solution is 200-400r/min, and precipitation temperature is room temperature, and the sedimentation time, 3-5 was small
When, the natural sedimentation time is 4-6 hours after the completion of titration, the sediment is filtered and wash, by the sediment after washing
Be placed in a vacuum drying oven 40 DEG C heat preservation 20-24 hours.
Further, in the step (2), by the first quartz of front axle shell A merging after the first Fe foil cladding
Vacuum Package is carried out in pipe, is then sintered 6 hours at 1000 DEG C, and the vacuum degree in first quartz ampoule is less than 10-2Pa。
Further, in the step (3), the powder B after the 2nd Fe foil cladding is placed in the second quartz ampoule
Middle carry out Vacuum Package, then 1000 DEG C sintering 6-8 hours, the vacuum degree in second quartz ampoule is less than 10-2Pa。
Further, in the compression moulding pressure and the step (3) of the front axle shell A in the step (2)
The compression moulding pressure of the powder B is 100Mpa.
Further, Fe described in the step (3)2O3The additive amount of powder is the 1% of the powder B mass.
Further, in the step (3), 1≤x≤1.5.
The present invention provides the high-content Cr that a kind of prior art can not be prepared to adulterate Fe3O4Powder CrxFe3-xO4Side
Method, thus facilitate researcher study nuclear power plant's primary heat transport system Austenitic stainless steel pipe wall surface oxidation film performance, be
It removes the pollution of major loop radioactive deposite and effective means is provided.
Detailed description of the invention
Fe when attached drawing 1 is x=1 in the present invention3-xCrxO4Powder microscopic appearance figure；
Fe when attached drawing 2 is x=1 in the present invention3-xCrxO4The X-ray diffraction pattern of powder.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment the invention will be further described.
The present invention provides a kind of High Content Chromium doped ferroferric oxide raw powder's production technology, it the following steps are included:
Step (1) adulterates Fe using coprecipitation preparation Cr3O4Front axle shell A: KOH solution is slowly dropped in stirring
FeSO4With Cr2(SO4)3In mixed solution, wherein FeSO4With Cr2(SO4)3Mixed solution is 1:1- according to the atomic ratio of Fe and Cr
2:1 is prepared.Rate of titration is controlled in 0.03-0.05cm3/ min, mixing speed 200-400r/min, precipitation temperature are
Room temperature, sedimentation time 3-5 hour.Natural sedimentation 4-6 hours after the completion of titration.Vacuum oven is put into after sediment is washed,
40 DEG C heat preservation 20-24 hours, then take out grinding and uniformly obtain front axle shell A.
Step (2), the front axle shell A compression moulding under 100Mpa pressure that will be obtained, is coated with the first Fe foil, is enclosed
(vacuum degree is less than 10 in first quartz ampoule-2Pa), it is sintered 6 hours for 1000 DEG C, takes out grinding and obtain powder B.
Step (3), the Fe that addition mass percent is 1% in the powder B that above-mentioned steps (2) are obtained2O3Powder, grinding are equal
It is even to obtain powder C, powder C compression moulding under 100Mpa pressure is coated with the 2nd Fe foil, is enclosed in the second quartz ampoule
(vacuum degree is less than 10-2Pa), 1000 DEG C sintering 6-8 hours take out grinding and obtain powder D, and powder D is what high-content Cr was adulterated
Fe3O4Powder Fe3-xCrxO4, wherein 1≤x≤1.5.
KOH solution in above-mentioned steps (1) can also use the mixed liquor of NaOH solution or KOH solution and NaOH solution
Instead of.
Front axle shell A Fe foil is coated in above-mentioned steps (2), and vacuum enclose the first quartz ampoule after be sintered and step
(3) Fe that mass percent is 1% is added in powder B2O3Powder coats powder C Fe foil, and vacuum encloses the second stone
It is sintered after English pipe, aforesaid operations are for obtaining pure Cr doping Fe3O4Powder Fe3-xCrxO4。
Embodiment 1:
Step (1) adulterates Fe using coprecipitation preparation Cr3O4Front axle shell, raw material FeSO4, Cr2(SO4)3And KOH,
FeSO4With Cr2(SO4)3Proportion is carried out for 2:1 according to the atomic ratio of Fe and Cr, and mixed solution is made.KOH solution is slowly dropped to
FeSO in stirring4With Cr2(SO4)3In mixed solution, wherein the concentration of KOH solution is 40%w/v, FeSO4With Cr2(SO4)3
The concentration of mixed solution is 0.1mol/L, and rate of titration is controlled in 0.04cm3/ min, mixing speed 400r/min, precipitation temperature
For room temperature, the sedimentation time 5 hours.Natural sedimentation 4 hours after the completion of titration.After washing, sediment is put into vacuum oven, 40
DEG C heat preservation 24 hours, then grinding uniformly obtained front axle shell.
Step (2), front axle shell compression moulding under 100Mpa pressure that step (1) is obtained, is coated with Fe foil, envelope
Enter in quartz ampoule that (vacuum degree is less than 10-2Pa), it is sintered 6 hours for 1000 DEG C.Taking-up is pulverized.
Step (3) adds the Fe that mass percent is 1% in the powder that above-mentioned steps (2) obtain2O3Powder, grinding are equal
Even, the compression moulding under 100Mpa pressure is coated with Fe foil, and (vacuum degree is less than 10 in enclosed quartz ampoule-2Pa), 1000 DEG C
Sintering 6 hours.Taking-up is pulverized, the Fe of as high-content Cr doping3O4Powder Fe3-xCrxO4, wherein x=1, Cr atom account for
The ratio of Fe atom is 50%.
The Fe of above-mentioned x=13-xCrxO4The microscopic appearance of powder as shown in Figure 1, its X-ray diffraction pattern as shown in Fig. 2, by scheming
2 it is found that its peak shape of resulting powder is Fe after having adulterated3O4The peak shape of crystal structure, does not occur Cr after having adulterated3O2Peak shape,
As it can be seen that Cr is fully doped into Fe3O4In.And it since the atomic radius of Fe atom and Cr atom differs very little, thus adulterates
Caused Fe afterwards3O4Cell parameter variation less, distortion of lattice very little, thus adulterate afterwards resulting Fe3-xCrxO4Powder its
The diffraction maximum of crystal structure compares pure Fe3O4The diffraction maximum offset of crystal structure is unobvious.
Embodiment 2:
Step (1) adulterates Fe using coprecipitation preparation Cr3O4Front axle shell, raw material FeSO4, Cr2(SO4)3And KOH,
FeSO4With Cr2(SO4)3Proportion is carried out for 3:2 according to the atomic ratio of Fe and Cr, and mixed solution is made.KOH solution is slowly dropped to
FeSO in stirring4With Cr2(SO4)3In mixed solution, wherein the concentration of KOH solution is 30%w/v, FeSO4With Cr2(SO4)3
The concentration of mixed solution is 0.2mol/L, and rate of titration is controlled in 0.05cm3/ min, mixing speed 200r/min, precipitation temperature
For room temperature, the sedimentation time 3 hours.Natural sedimentation 5 hours after the completion of titration.After washing, it is put into vacuum oven, 40 DEG C of heat preservations 20
Hour, then grinding uniformly obtains front axle shell.
Step (2) is sintered front axle shell using the method in 1 step of embodiment (2).
Step (3) adds the Fe that mass percent is 1% in the powder that above-mentioned steps (2) obtain2O3Powder, grinding are equal
Even, the compression moulding under 100Mpa pressure is coated with Fe foil, and (vacuum degree is less than 10 in enclosed quartz ampoule-2Pa), 1000 DEG C
Sintering 8 hours.Taking-up is pulverized.The Fe of high-content Cr doping can be obtained3O4Powder Fe3-xCrxO4, wherein x=1.2, Cr
The ratio that atom accounts for Fe atom is 66.67%.
Embodiment 3:
Step (1) adulterates Fe using coprecipitation preparation Cr3O4Front axle shell, raw material FeSO4, Cr2(SO4)3And NaOH,
FeSO4With Cr2(SO4)3Proportion is carried out for 1:1 according to the atomic ratio of Fe and Cr, and mixed solution is made.NaOH solution is slowly dropped to
FeSO in stirring4With Cr2(SO4)3In mixed solution, wherein the concentration of KOH solution is 40%w/v, FeSO4With Cr2(SO4)3
The concentration of mixed solution is 0.15mol/L, and the drop speed is controlled in 0.03cm3/ min, speed of agitator 300/min, precipitating temperature
Spending is room temperature, the sedimentation time 4 hours.Natural sedimentation 6 hours after the completion of titration.After washing, it is put into vacuum oven, 40 DEG C of heat preservations
22 hours, then grinding uniformly obtained front axle shell.
Step (2) is sintered front axle shell using the method in 1 step of embodiment (2).
Step (3) obtains adding the Fe that mass percent is 1% in powder in above-mentioned steps (2)2O3Powder, grinding is uniform,
The compression moulding under 100Mpa pressure is coated with Fe foil, and (vacuum degree is less than 10 in enclosed quartz ampoule-2Pa), 1000 DEG C of burnings
Knot 7 hours.Taking-up is pulverized.The Fe of high-content Cr doping finally can be obtained3O4Powder Fe3-xCrxO4, wherein x=1.5,
The ratio that Cr atom accounts for Fe atom is 100%.
The present invention provides the high-content Cr that a kind of prior art can not be prepared to adulterate Fe3O4Powder CrxFe3-xO4Side
Method, the x value in various embodiments of the present invention is nominal component, and the x value in actual sample is obtained by energy spectrometer analysis, from
Experimental result sees that actual x value and nominal component are almost the same.Cr by preparing high-content adulterates Fe3O4Powder CrxFe3- xO4, it may be convenient to the performance of nuclear power plant's primary heat transport system Austenitic stainless steel pipe wall surface oxidation film is studied, thus for removal
The pollution of major loop radioactive deposite provides effective means.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology, which comprises the following steps:
Step (1) adulterates Fe using coprecipitation preparation Cr3O4Front axle shell A: precipitating reagent is slowly dropped to the FeSO in stirring4With
Cr2(SO4)3In mixed solution, sediment is dried in natural sedimentation after the completion of titration, is taken out grinding and is uniformly obtained front axle shell A；
The front axle shell A compression moulding is taken out grinding and obtained by step (2) using vacuum-sintering is carried out after the first Fe foil cladding
Powder B；
Step (3) adds Fe in the powder B2O3Powder, grinding uniformly obtain powder C, and the powder C compression moulding is used
Vacuum-sintering is carried out after 2nd Fe foil cladding, grinding is taken out and obtains powder D, the powder D is required high-content Cr doping
Fe3O4Powder Fe3-xCrxO4。
2. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
The precipitating reagent is KOH solution or NaOH solution.
3. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
The precipitating reagent is the mixed liquor of KOH solution and NaOH solution.
4. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
The FeSO4With Cr2(SO4)3Mixed solution according to Fe and Cr atomic ratio be 1:1-2:1 prepared.
5. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
In the step (1), the rate of titration of the precipitating reagent is 0.03-0.05cm3/ min, the FeSO4With Cr2(SO4)3It mixes molten
The mixing speed of liquid is 200-400r/min, and precipitation temperature is room temperature, sedimentation time 3-5 hour, natural sedimentation after the completion of titration
Time is 4-6 hours, filters and washs the sediment, the sediment after washing is placed in a vacuum drying oven at 40 DEG C
Heat preservation 20-24 hours.
6. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
In the step (2), the front axle shell A after the first Fe foil cladding is placed in the first quartz ampoule and carries out Vacuum Package,
Then it is sintered 6 hours at 1000 DEG C, the vacuum degree in first quartz ampoule is less than 10-2Pa。
7. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
In the step (3), the powder B after the 2nd Fe foil cladding is placed in the second quartz ampoule and carries out Vacuum Package, so
Afterwards 1000 DEG C sintering 6-8 hours, the vacuum degree in second quartz ampoule is less than 10-2Pa。
8. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
The compression moulding pressure of the front axle shell A and being pressed into for the powder B in the step (3) in the step (2)
Type pressure is 100MPa.
9. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1, it is characterised in that:
Fe described in the step (3)2O3The additive amount of powder is the 1% of the powder B mass.
10. a kind of High Content Chromium doped ferroferric oxide raw powder's production technology according to claim 1 or 4, feature
It is: in the step (3), 1≤x≤1.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710638499.2A CN107265515B (en) | 2017-07-31 | 2017-07-31 | A kind of High Content Chromium doped ferroferric oxide raw powder's production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710638499.2A CN107265515B (en) | 2017-07-31 | 2017-07-31 | A kind of High Content Chromium doped ferroferric oxide raw powder's production technology |
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| Publication Number | Publication Date |
|---|---|
| CN107265515A CN107265515A (en) | 2017-10-20 |
| CN107265515B true CN107265515B (en) | 2019-02-01 |
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