CN109014177A - A kind of preparation method of insulating wrapped composite powder and transformer core - Google Patents
A kind of preparation method of insulating wrapped composite powder and transformer core Download PDFInfo
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- CN109014177A CN109014177A CN201811013657.6A CN201811013657A CN109014177A CN 109014177 A CN109014177 A CN 109014177A CN 201811013657 A CN201811013657 A CN 201811013657A CN 109014177 A CN109014177 A CN 109014177A
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- 239000000843 powder Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- 229910000676 Si alloy Inorganic materials 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 24
- 239000000377 silicon dioxide Substances 0.000 abstract description 23
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 229910052742 iron Inorganic materials 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 6
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000011856 silicon-based particle Substances 0.000 abstract description 2
- 229910000976 Electrical steel Inorganic materials 0.000 description 15
- 238000000151 deposition Methods 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 10
- 229910052681 coesite Inorganic materials 0.000 description 9
- 229910052906 cristobalite Inorganic materials 0.000 description 9
- 229910052682 stishovite Inorganic materials 0.000 description 9
- 229910052905 tridymite Inorganic materials 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention belongs to soft magnetic materials technical field more particularly to the preparation methods of a kind of insulating wrapped composite powder and transformer core.The preparation method of insulating wrapped composite powder and transformer core of the invention can successfully prepare insulating wrapped composite powder and transformer core, in the transformer core of preparation, the encirclement uniform and fine and close by silicon dioxide insulating layer of Fe-6.5wt.%Si particle, realizes the structure of the transformer core to insulate between particle.The excellent electromagnetic properties such as high magnetic strength, high resistivity, good frequency stability, low-coercivity and low iron loss are realized based on transformer core of the invention.Compared to the transformer core of traditional naked layer, resistivity improves two orders of magnitude, while considerably reducing iron loss, and with the increase of test frequency, iron loss fall is bigger, can greatly improve its performance in high frequency equipment；The process flow of this preparation method is simple, and step is few, is conducive to raising production efficiency, reduction into production and rises this and manufacture difficulty.
Description
Technical field
The invention belongs to soft magnetic materials technical field more particularly to a kind of insulating wrapped composite powders and transformer core
Preparation method.
Background technique
The important equipment of power distribution network include in generator, motor, transformer and other electric instruments and apparatus include by
The soft magnetism functional structure of silicon steel production.With the continuous improvement of energy-saving and emission-reduction demand, the devices such as various high efficiency motors are to silicon steel magnetic
The requirement of conductance, iron loss and magnetic anisotropy is higher and higher, is based on the demand, and people start to release Fe-6.5wt.%Si
High silicon steel, high silicon steel can reduce the noise and volume of device, have low energy consumption, low fever, small in size, low noise and height steady
The features such as qualitative.But brittleness is high at room temperature, processing performance is poor for high silicon steel, and pair rolling technology is difficult to high silicon plate and band
Material.The especially raising of doubling network voltage grade and the application of various high frequencies, hyperfrequency power equipment, silicon steel material and
Influence of magnetic electricity performance of the transformer core under medium-high frequency use environment to equipment performance is more prominent.
It is ground although domestic and international researcher has carried out extensive and deep basis for the related various problems of high-silicon electrical steel
Study carefully work, but worldwide only has Nippon Steel engineering holding company to realize high silicon using gas phase reaction under high temperature at present
The large-scale production of electrician's steel sheet, and other technologies or because higher cost or because by environmental constraints or because of technical maturity not
It is enough or constrain it due to stock utilization is lower the problems such as and further apply.
Summary of the invention
The purpose of the invention is, provide a kind of insulating wrapped composite powder with excellent electromagnetic property and
By the preparation method of composite powder production insulating wrapped transformer core.
To achieve the above object, the invention adopts the following technical scheme that.
A kind of preparation method of insulating wrapped composite powder production transformer core, specific preparation step includes, with matter
Amount point calculates:
50 parts of Fe-6.5wt.%Si alloy powder is added to by 450~500 parts of dehydrated alcohols and 10 parts step 1
Distilled water composition mixed solution in；
Step 2 is slowly added 20 parts of silane coupling agent；By above-mentioned solution under 50 DEG C of water-baths, 1~2h of mechanical stirring；
Step 3 is under 50 DEG C of water-baths, while with the strong mechanical stirring of 800rpm revolving speed, uniformly slowly addition 15~
20 parts of ammonium hydroxide is slowly added 5~20 parts of ethyl orthosilicate, until the concentration of ethyl orthosilicate is adjusted up to 0.1~0.4ml/g
Save PH to 8~9；
Step 4 waits for reacting completely, powder after reaction is obtained, after powder after reaction is washed with dehydrated alcohol, in vacuum
Dry 20~the 30h of drying box obtains insulating wrapped composite powder；
Powder after reaction is fabricated to transformer core using discharge plasma sintering technology by step 5: whole in progress
A sintering process applies the uniaxial tension of 30MPa to graphite jig, and control sintering temperature is 950~1050 DEG C, keeps the temperature 10min；
Residual stress is eliminated in finally 700~800 DEG C of annealing in argon atmosphere, and sintering terminates after being cooled to room temperature, takes out graphite mo(u)ld
Tool demoulding obtains transformer core.
A kind of preferred embodiment to above scheme is, in step 3, adjusts the concentration of ethyl orthosilicate to 0.4ml/g.
Specifically, Fe-6.5wt.%Si alloy powder is the gas of 150~300 mesh of granularity, purity >=94 in step 1
Atomized powder.
Specifically, silane coupling agent specifically refers to 3- aminopropyl triethoxysilane in step 2.
The beneficial effect is that:
The preparation method of insulating wrapped composite powder and transformer core of the invention can successfully prepare insulating wrapped
Composite powder and transformer core, in the transformer core of preparation, Fe-6.5wt.%Si particle is equal by silicon dioxide insulating layer
Even and fine and close encirclement realizes the structure of the transformer core to insulate between particle.It is real based on transformer core of the invention
The excellent electromagnetic properties such as high magnetic strength, high resistivity, good frequency stability, low-coercivity and low iron loss are showed.It compares
The transformer core of traditional naked layer, resistivity improves two orders of magnitude, while considerably reducing iron loss, and with survey
The increase of frequency is tried, iron loss fall is bigger, can greatly improve its performance in high frequency equipment；This preparation method work
Skill process is simple, and step is few, is conducive to raising production efficiency, reduction into production and rises this and manufacture difficulty.
Detailed description of the invention
Fig. 1 is preparation flow and reaction principle figure of the invention.
Fig. 2 is no SiO2Relative permeability (the μ of insulating layer transformer core and insulating wrapped transformer core after annealing
R) with test frequency trend chart.
Specific embodiment
It describes in detail below in conjunction with specific embodiment to the present invention.
In the present invention in the preparation process of transformer core with the materials such as Fewt.%Si powder, ethyl orthosilicate be original
Material, based in actual application, the purity of above-mentioned material is by the performance and production technology to transformer core in the present invention
It has some impact on, therefore in a particular embodiment, is all made of the material having determined and is introduced, specifically, following realities
Apply the gas-atomised powders that Fe-6.5wt.%Si used in example is 150~300 mesh of granularity, purity >=94；The gas-atomised powders are
Ferro-silicium ingot is melted to liquid in induction furnace, then cooling into cooling water by high-pressure pump pressurized jet, recycling obtains
Powder；The specific mass component of Fe-6.5wt.%Si powder used in the present embodiment is as shown in table 1:
1 Fe-6.5wt.%Si raw material chemical constituent of table
| Element | Fe | Silicon | C | S | Mn | Al | P | N |
| Ingredient wt.% | 93.18 | 6.61 | 0.003 | 0.006 | 0.01 | 0.01 | 0.18 | 0.0036 |
It is to be calculated with mass fraction in following embodiment.
Embodiment one:
A kind of preparation method of insulating wrapped composite powder production transformer core, specific preparation step include:
50 parts of Fe-6.5wt.%Si alloy powder is added to by 450 parts of dehydrated alcohols and 10 parts of distillation step 1
In the mixed solution of water composition；
The silane coupling agent that step 2 is slowly added 20 parts (specifically refers to 3- aminopropyl-triethoxy silicon in the present embodiment
Alkane)；By above-mentioned solution under 50 DEG C of water-baths, mechanical stirring 2h；
Step 3 is under 50 DEG C of water-baths, while with the strong mechanical stirring of 800rpm revolving speed, uniformly slowly addition 15~
20 parts of ammonium hydroxide is slowly added 15 parts of ethyl orthosilicate, until ethyl orthosilicate concentration reach 0.4ml/g, adjust PH to 8~
9；
Step 4 waits for reacting completely, powder after reaction is obtained, after powder after reaction is washed with dehydrated alcohol, in vacuum
The dry 30h of drying box obtains insulating wrapped composite powder；Its reaction principle is as shown in Figure 1
Powder after reaction is fabricated to transformer core using discharge plasma sintering technology by step 5: whole in progress
A sintering process applies the uniaxial tension of 30MPa to graphite jig, and control sintering temperature is 1050 DEG C, keeps the temperature 10min；Finally exist
Residual stress is eliminated in 800 DEG C of annealing in argon atmosphere, and sintering terminates after being cooled to room temperature, is taken out graphite jig and is demoulded to obtain
Insulating wrapped transformer core sample A.
After waiting processing compared with raw material carry out XRD spectrum to above-mentioned A sample, it can be found that sample A has the property that
A1, by depositing operation treated its powder shape of Fe-6.5wt.%Si alloy powder and change in size very little,
But powder surface is more coarse, the reason is that alloy powder surface iron content is decreased obviously after depositing operation processing, and silicon
Rise with oxygen element content, confirmed by XDR and EDS analysis, the amorphous phase of powder surface deposition is SiO2；It can be inferred that logical
One layer can be deposited uniformly and fine and close amorphous SiO on high si fe alloy powder surface by crossing depositing operation technique2Clad obtains high
Silicon steel/SiO2Core-shell structure powder.Depositing operation technique will not change the phase structure of the high silicon steel as stratum nucleare, further divide
Analysis shows the amorphous SiO as shell2Crystalline state, while SiO can be converted at 985.0 DEG C2Sedimentary size of microcrystal increases.
A2, transformer core consistency with higher and preferable machining property, compared to no SiO2Insulation
The transformer core (high silicon steel) (Ms ≈ 184emu/g) of layer, the value of the Ms of the transformer core of insulating wrapped composite powder production
For 155~165emu/g, about 10.3% is had dropped.
A3, without SiO2The opposite magnetic of the high silicon steel transformer core of insulating layer and insulating wrapped transformer core after C annealing
Conductance (μ r) is with test frequency variation tendency as shown in Fig. 2, combining figure it is found that high when test frequency is increased to 400Hz or more
Silicon steel/SiO2The μ r of transformer core is almost no longer increased with test frequency and is reduced, but without SiO2The high silicon steel transformation of insulating layer
Only after test frequency is more than 50000Hz, the value of μ r just no longer declines device iron core.This shows the A sample transformer fe of preparation
Core has better frequency stability, and perfection is suitble to use in medium-high frequency device.
A4, the resistivity of transformer core is measured, compared to no SiO2The electricity of the high silicon steel transformer core of insulating layer
Resistance rate (9.7*10-7Ω m), the resistivity of A transformer core improves two orders of magnitude, has reached (4.8*10-5Ω m),
This is because in A transformer core, there are SiO2Insulating layer hinders electron transfer, therefore has higher resistivity,
Simultaneously under identical frequency, the iron loss of A1 transformer core is lower, and with the increase of frequency, the iron loss range of decrease is bigger, in middle height
Equipment performance can preferably be improved in frequency device.
Embodiment two
A kind of preparation method of insulating wrapped composite powder production transformer core, specific preparation step include:
50 parts of Fe-6.5wt.%Si alloy powder is added to by 450 parts of dehydrated alcohols and 10 parts of distillation step 1
In the mixed solution of water composition；
The silane coupling agent that step 2 is slowly added 20 parts (specifically refers to 3- aminopropyl-triethoxy silicon in the present embodiment
Alkane)；By above-mentioned solution under 50 DEG C of water-baths, mechanical stirring 1h；
Step 3 is under 50 DEG C of water-baths, while with the strong mechanical stirring of 750rpm revolving speed, uniformly slowly addition 15~
20 parts of ammonium hydroxide is slowly added 10 parts of ethyl orthosilicate, until ethyl orthosilicate concentration reach 0.3ml/g, adjust PH to 8~
9；
Step 4 waits for reacting completely, powder after reaction is obtained, after powder after reaction is washed with dehydrated alcohol, in vacuum
Drying box is dry to obtain insulating wrapped composite powder for 24 hours；
Insulating wrapped composite powder after reaction is fabricated to transformer fe using discharge plasma sintering technology by step 5
Core: entire sintering process is being carried out to the uniaxial tension of graphite jig application 30MPa, control sintering temperature is 950 DEG C, heat preservation
10min；Residual stress is eliminated in finally 700 DEG C of annealing in argon atmosphere, and sintering terminates after being cooled to room temperature, takes out graphite
Mold releasability obtains insulating wrapped transformer core sample B.
After being handled compared with raw material and sample A carry out XRD spectrum etc. above-mentioned B sample, it can be found that sample B has
Following characteristic: compared to sample A, the SiO on alloy powder surface in B transformer core2Insulating layer size and quantity become smaller, and become
The raw alloy powder for rising to 177.5emu/g but be still below raw material of the value of the Ms of depressor iron core, the frequency of sample transformer core
Stability is improved compared to current material；Simultaneously as existing non magnetic SiO between particle2Insulating layer is equivalent to air gap
With demagnetizing field source, the content and thickness of silicon dioxide insulating layer are higher, energy required for needing to complete to magnetize or demagnetize
Higher, the Hc of sample is bigger, therefore sample B, under same working condition, required reaction time and processing prepare iron core
When need heat treatment requirements and time to decline, production cost/difficulty is declined compared with sample A.
Embodiment three
Pass through the property to the material mixture ratio variation in preparation method provided by the invention to transformer core in the present embodiment
Matter influence is introduced, and in preparation method of the invention, the addition concentration of ethyl orthosilicate is to change transformer fe core inner
The major control factors of microstructure,
On the basis of not changing other influences factor, the additive amount of ethyl orthosilicate is followed successively by 5ml, 10ml, 15ml,
20ml and 25ml, corresponding concentration are 0.1ml/g, 0.2ml/g, 0.3ml/g, 0.4ml/g and 0.5ml/g.It is dense in dropwise addition to it
The SEM photograph for spending the composite powder of lower depositing operation preparation compares it can be found that the surface of raw material alloy powder is smooth, but
It is after depositing operation technique, surface becomes more coarse, and increases with concentration, and roughness is higher.When ethyl orthosilicate
When dropwise addition concentration is 0.1ml/g, the silica deposition of nano-scale appears in alloy powder surface.Increase with concentration is added dropwise
Size and number to 0.2ml/g, nanometer grade silica deposit gradually increase.With ethyl orthosilicate dropwise addition concentration after
It is continuous to increase to 0.3ml/g or 0.4ml/g, it can be found that nanometer grade silica deposit forms the titanium dioxide of one layer of dense uniform
Silicon layer is coated on particle surface.It is actually detected the result shows that, be added dropwise concentration increase to 0.4ml/g from 0.1ml/g in the range of,
The average particle diameter size of nanometer grade silica deposit increases with concentration increase is added dropwise.However, be added dropwise concentration after
Continuous to increase to 0.5ml/g, silica starts to occur in the form of free state, the silica of most of free state and high silicon steel
Particle and not in contact with and the average grain diameter of nanometer grade silica deposit is begun to decline.
The insulating wrapped of the depositing operation preparation for the alloy powder in raw material and under different ethyl orthosilicate concentration of table 2 is multiple
The EDS for closing powder analyzes result.Compared to the high si fe alloy powder of raw material, the content of ferro element is decreased obviously, and element silicon and
Oxygen element shows opposite trend.However, continuing to increase to 0.5ml/g, element silicon as concentration is added dropwise in ethyl orthosilicate
8.15wt.% and 3.97wt.% are dropped to respectively with the content of oxygen element, and further detection confirms, dense in the ethyl orthosilicate
Under degree, silica starts to occur in the form of free state, reduces the deposition on alloying pellet surface.With positive silicic acid second
Ester concentration increases, and the amount of coated with silica insulating layer increases, Ms and the density decline of alloy powder.
The EDS result for the insulating wrapped composite powder that under the different ethyl orthosilicate concentration of table 2 prepared by depositing operation
After comprehensively considering, when the dropwise addition concentration of TEOS is 0.3ml/g, cladding of the silicon dioxide insulating layer to alloy powder
Uniformly, silicon dioxide insulating layer thickness is about 800nm, and the comprehensive magnetic of sample can be best, Ms 165emu/g, Hc 12Oe, ρ
It is only 5.8W/kg for 7.6 10-5 Ω m, W1/10k.
Finally it should be noted that above embodiments are only to illustrate the technical solution of the invention, rather than to this hair
It is bright create protection scope limitation, although being explained in detail referring to preferred embodiment to the invention, this field it is general
Lead to it will be appreciated by the skilled person that can be modified or replaced equivalently to the technical solution of the invention, without departing from this
The spirit and scope of innovation and creation technical solution.
Claims (5)
1. the preparation method of a kind of insulating wrapped composite powder and transformer core, which is characterized in that include the following steps, respectively
Component is calculated in step with quality point:
50 parts of Fe-6.5wt.%Si alloy powder is added to by 450~500 parts of dehydrated alcohols and 10 parts of steaming step 1
In the mixed solution of distilled water composition；
Step 2 is slowly added 20 parts of silane coupling agent；By above-mentioned solution under 50 DEG C of water-baths, 1~2h of mechanical stirring；
Step 3 is under 50 DEG C of water-baths, while with the strong mechanical stirring of 800rpm revolving speed, uniformly slowly 15~20 parts of addition
Ammonium hydroxide, 5~20 parts of ethyl orthosilicate is slowly added, until the concentration of ethyl orthosilicate up to 0.1~0.4ml/g, adjusts PH
To 8~9；
Step 4 waits for reacting completely, obtains powder after reaction, after powder after reaction is washed with dehydrated alcohol, is being dried in vacuo
Dry 20~the 30h of case obtains insulating wrapped composite powder；
Powder after reaction is fabricated to transformer core using discharge plasma sintering technology by step 5: entirely being burnt
Knot process applies the uniaxial tension of 30MPa to graphite jig, and control sintering temperature is 950~1050 DEG C, keeps the temperature 10~30min；
Residual stress is eliminated in finally 700~800 DEG C of annealing in argon atmosphere, and sintering terminates after being cooled to room temperature, takes out graphite mo(u)ld
Tool demoulding obtains transformer core.
2. the preparation method of a kind of insulating wrapped composite powder and transformer core, feature exist according to claim 1
In adjusting the concentration of ethyl orthosilicate to 0.4ml/g in step 3.
3. the preparation method of a kind of insulating wrapped composite powder and transformer core, feature exist according to claim 1
In in step 1, Fe-6.5wt.%Si alloy powder is the gas-atomised powders of 150~300 mesh of granularity, purity >=94.
4. the preparation method of a kind of insulating wrapped composite powder and transformer core, feature exist according to claim 1
In in step 2, silane coupling agent specifically refers to 3- aminopropyl triethoxysilane.
5. the preparation method of a kind of insulating wrapped composite powder and transformer core, feature exist according to claim 1
In in step 5, sintering temperature is 985.0 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113363067A (en) * | 2020-03-05 | 2021-09-07 | 中科院广州化学有限公司 | Iron-silicon composite magnetic powder core with surface coating structure and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5227235A (en) * | 1990-05-09 | 1993-07-13 | Tdk Corporation | Composite soft magnetic material and coated particles therefor |
| CN102136331A (en) * | 2010-12-30 | 2011-07-27 | 长春工业大学 | High-efficiency soft magnetic composite material and preparation method thereof |
| CN104078230A (en) * | 2014-07-24 | 2014-10-01 | 武汉科技大学 | Intergranular insulated high-silicon electrical steel core and preparation method thereof |
| CN106041061A (en) * | 2016-07-06 | 2016-10-26 | 同济大学 | High-performance low-loss compound magnetic powder core and preparation method thereof |
| CN106783132A (en) * | 2016-12-26 | 2017-05-31 | 安徽工业大学 | A kind of silicon steel core high insulated between particle and preparation method thereof |
-
2018
- 2018-08-31 CN CN201811013657.6A patent/CN109014177A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5227235A (en) * | 1990-05-09 | 1993-07-13 | Tdk Corporation | Composite soft magnetic material and coated particles therefor |
| CN102136331A (en) * | 2010-12-30 | 2011-07-27 | 长春工业大学 | High-efficiency soft magnetic composite material and preparation method thereof |
| CN104078230A (en) * | 2014-07-24 | 2014-10-01 | 武汉科技大学 | Intergranular insulated high-silicon electrical steel core and preparation method thereof |
| CN106041061A (en) * | 2016-07-06 | 2016-10-26 | 同济大学 | High-performance low-loss compound magnetic powder core and preparation method thereof |
| CN106783132A (en) * | 2016-12-26 | 2017-05-31 | 安徽工业大学 | A kind of silicon steel core high insulated between particle and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113363067A (en) * | 2020-03-05 | 2021-09-07 | 中科院广州化学有限公司 | Iron-silicon composite magnetic powder core with surface coating structure and preparation method thereof |
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