CN103113096A - Manufacturing method of high-power yttrium/gadolinium garnet ferrite material - Google Patents

Manufacturing method of high-power yttrium/gadolinium garnet ferrite material Download PDF

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CN103113096A
CN103113096A CN2013100541385A CN201310054138A CN103113096A CN 103113096 A CN103113096 A CN 103113096A CN 2013100541385 A CN2013100541385 A CN 2013100541385A CN 201310054138 A CN201310054138 A CN 201310054138A CN 103113096 A CN103113096 A CN 103113096A
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韩志全
王天进
张方远
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DONGYANG FUSHITE MAGNETIC INDUSTRY Co Ltd
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Abstract

The invention discloses a manufacturing method of a high-power yttrium/gadolinium garnet ferrite material, which comprises the following steps: 1) calculating the amount of raw materials according to a chemical formula of the composition; 2) burning; 3) weighing all the raw materials, placing the weighed raw materials and burned Y2O3 and Gd2O3 into a ball milling tank, and performing ball milling; 4) drying the raw material pulp, screening, placing in a furnace having an oxidizing atmosphere, and presintering; 5) performing secondary ball milling until the average particle size of the powder is not more than 1.2mu m, and discharging; 6) drying, and granulating; 7) pressing into a required product blank; and 8) sintering at 1000-1550 DEG C, and keeping the temperature for 4-50 hours. According to the invention, a small amount of Cu<2+> substitution is used in the formula design, and the Cu<2+> substitution can achieve the effects of promoting solid-phase reaction, increasing density and lowering sintering temperature, thereby favorably ensuring that the product can achieve a high-density fine-grained microstructure at a low sintering temperature.

Description

A kind of manufacture method of superpower yttrium gadolinium ferrogarnet material
Technical field
The invention belongs to microwave technology and field of magnetic material, be specifically related to garnet microwave ferrite material technology.
Background technology
In the making of the High-Power Microwave ferrite circulator/shield retaining that bears high-peak power, the serious problems such as the insertion loss that the superpower non-linear effect due to material causes sharply increases, mis-behave often can appear.In the continuous wave high-power component that bears high-average power was made, saturation magnetization descended due to the temperature rise that also often can occur to cause because of spillage of material, and then brings the problem of device frequency drift.The superpower ability to bear of material can be by superpower non-linear effect critical magnetic field h cOr self-rotating wave linewidth Δ H kCharacterize [1]High-power component is mainly 1 to the requirement of microwave ferrite material) self-rotating wave linewidth Δ H kHigh; 2) lossy microwave is low, is mainly ferromagnetic resonance line width Δ H or effective line width Δ H effLow; 3) saturation magnetization M sLower; 4) the high or M of Curie temperature sTemperature factor low.
Improve material self-rotating wave linewidth Δ H kTwo approach are arranged, the one, mix the fast relaxation foreign ions such as rare earth, the 2nd, grain refining [1]Improve Δ H with rare earth doped method k, must bring ferromagnetic resonance line width Δ H and effective line width Δ H effEnlarge markedly; The method of employing grain refining but can be with less Δ H and Δ H effChange and bring larger Δ H kIncrease [1]In order to ensure the low loss characteristic of high-power component, except will take into account self-rotating wave linewidth Δ H in formulating of recipe kRaising and Δ H and Δ H effReduction beyond, also to manage crystal grain thinning.Yet the refinement of crystal grain often is attended by a large amount of pores increases Δ H, the heat pressing process of numerous and diverse, the inefficiency of external employing equipment usually for this reason, and we need to look for another way.
Patent documentation about microwave ferrite material and manufacture method is existing, and the ferrogarnet chemical formula described in present published CN1286127C is: Y xGd 3-xAl 0.5Fe 4.5O 12And Y 3Fe (5-5y)Al 5yO 12The chemical formula of the garnet material described in CN 1600741A is: Y 3- xGd xFe T-2y-zCo ySi yAl zO 12, Y 3-x-uGd xCa uCo ySi yAl zFe T-2y-u-zO 12And Y 3-xGd xFe T-2y-v-zCo ySi yIn vAl zO 12Described in CN 1719658.A the garnet material chemical formula be: (Y wGd xCa q) (Fe 8-w-x-y-3zIn yV z) O 12The described ferrogarnet of above patent mostly belongs to yttrium gadolinium series pomegranate stone (YGdIG).For the current superpower gyromagnetic material market requirement, high power performance (the Δ H of the described garnet material of above patent kAnd h c) and ferromagnetic resonance line width (Δ H) etc. remain in deficiency.
At present, microwave ferrite superpower garnet material adopts yttrium gadolinium series pomegranate stone (YGdIG) usually.High performance High-Power Microwave Ferrite Material generally will be selected yttrium gadolinium ettringite garnet (YGdCaVIG) material.In YGdIG or YGdCaVIG, Gd 3+Ion is improved Δ H kAnd improve M sThe effect of temperature factor, but it also brings ferromagnetic resonance line width Δ H and effective line width Δ H simultaneously effIncrease, must adopt In in order to reduce Δ H 3+, Sn 4+Deng replacement octahedral position Fe 3+Ion, and Curie temperature also can obviously descend thereupon; Also need use V in order to obtain low magnetic moment 5+, Ge 4+, Al 3+Fe etc. non magnetic ionic replacement four sides position 3+, they also can make Curie temperature descend.Wherein, V 5+Other ion of Curie temperature suppression ratio that ion brings want much less [1]So low magnetic moment superpower garnet adopts yttrium gadolinium ettringite garnet more.We find, if just use above-mentioned replacement ion, are difficult to make product performance to satisfy high-power component to low-loss requirement.
Summary of the invention
The present invention is mainly in existing superpower yttrium gadolinium ettringite garnet Ferrite Material, the problem that loss is bigger than normal, high power capacity is on the low side that exists, provide a kind of copper that contains, the formula of the high power low loss garnet microwave ferrite material of titanium and be convenient to the manufacture method of suitability for industrialized production.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of manufacture method of superpower yttrium gadolinium ferrogarnet material comprises the steps:
1) according to the constitutional chemistry formula
Y 3-y-2z-p+x-q-q 'Gd yCa 2z+p-x+q+q 'Cu xV zGe pSn qTi q′In q″Al wMn w′Fe 5-x-z-p-q-q '-w-w '-δO 12Calculate respectively required various starting material amounts, wherein iron deficiency amount δ be chosen as 0≤δ≤0.5, use the Y of purity 〉=99.9% 2O 3, Gd 2O 3With analytically pure Fe 2O 3, CaCO 3, In 2O 3, V 2O 5, GeO 2, SnO 2, TiO 2, Al (OH) 3, MnCO 3For starting material wherein: 0≤x≤1.30; 0≤y≤3.00; 0≤z≤1.50,0≤p≤1.30,0≤q≤0.70,0≤q '≤0.70,0≤q "≤0.70,0≤w≤1.30,0≤w '≤0.50, δ is the iron deficiency amount, 0≤δ≤0.50;
2) according to step 1) calculate required Y 2O 3, Gd 2O 3Material quantity carry out calcination and process, the calcination treatment temp is 850～1200 ℃, and is stand-by after furnace cooling;
3) according to step 1) calculate required material quantity, take respectively various raw materials with the balance of thousandth gram precision; And the Y that the raw material that takes and calcination were processed 2O 3, Gd 2O 3Put into ball grinder, in expecting: ball: the ratio of thinner=1: 2～5: 0.4～2.0 is carried out ball milling of wet method or is carried out ball milling of dry method;
4) with step 3) sieve after the mixed raw material slurry oven dry of ball milling, to make bulk or powdery and pack in corundum crucible, the stove of putting into oxidizing atmosphere carries out pre-burning, and calcined temperature is 800～1350 ℃;
5) with step 4) Preburning material broken, sieve after, carry out secondary ball milling in pack into ball grinder or sand mill, and by material: ball: the ratio of thinner=1: 2～5: 0.4～2.0 is carried out secondary ball milling, is milled to discharging when expecting powder median size≤1.2 μ m;
6) with step 5) slip carry out drying-granulating, should add cementing agent during granulation;
7) with step 6) particulate material put into forming mould and be pressed into required product blank, typed pressure is 50～150MPa, or further adopts cold isostatic compaction again;
8) blank of compression moulding, the stove of putting into oxidizing atmosphere are carried out sintering, sintering temperature is 1000～1550 ℃, is incubated 4～50 hours.
Preferably, Y described step 2) 2O 3And Gd 2O 3Calcination temperature be 950～1150 ℃.
Preferably, described step 3) or 5) in to carry out ball milling ball grinder used be stainless cylinder of steel, steel ball used is Stainless Steel Ball, thinner used is alcohol.
Preferably, described step 3) in, ball milling of wet method is according to material: ball: the ratio of thinner=1: 3: 1 adds starting material, steel ball and alcohol, and Ball-milling Time is 12 hours.
Preferably, described step 5) according to material: ball: the ratio of thinner=1: 3: 0.9 adds starting material, steel ball and alcohol, and Ball-milling Time is 30 hours.
Preferably, described step 6), cementing agent is the polyvinyl alcohol aqueous solution that contains 4～15wt%.
Preferably, described iron deficiency amount δ is chosen as 0≤δ≤0.3.
Preferably, in described step 6), drying-granulating is mist projection granulating or mechanical pelleting, and in described step 7), forming pressure is 98MPa, the temperature difference of the sintering temperature in described step 8) should be controlled at ± 5 ℃ in.
The present invention considers that the fusing point of CuO is low, is commonly used for sintering agent in ferritic preparation, and effect is very good.So, adopted a small amount of Cu in formulating of recipe 2+Replace.Cu 2+Replacement can be played the effect that promotes solid state reaction, raising density, reduces sintering temperature, obtains high-density, compact grained microstructure thereby be conducive to product under lower sintering temperature.That is, Cu under suitable sintering condition 2+Replacement can guarantee high-density again by crystal grain thinning; Both can improve self-rotating wave linewidth Δ H kCan reduce again pore to live width Δ H and effective line width Δ H effContribution, taken into account the high Δ H of device to material kWith low Δ H and low Δ H effRequirement.
Cu 2+Be weak magnetic ion, tend to replace the Fe of octahedral position in garnet 3+, on impact and the non magnetic ion In of magnetic moment 3+, Sn 4+Etc. close, just more weak.The Cu of divalence 2+Ion can be used to part and substitutes Ca 2+, play in formula the non magnetic ion V of high price z 5+, Ge 4+, Sn 4+Deng the electricity price poising action.The introducing of Cu also helps and reduces sintering temperature and energy consumption in addition.
In addition, from material property, home products is compared with U.S. Trans-Tech company product, DIELECTRIC CONSTANT ε ' generally on the low side [1,2]Ti 4+Ion has the effect that improves specific inductivity, simultaneously Ti 4+To octahedral position Fe 3+Replacement also can reduce crystal anisotropy constant K 1, reduce anisotropy broadening Δ H EachFor this reason, adopt In in formula 3+, Sn 4+, Ti 4+Plasma is to octahedral position Fe 3+The associating replacement, be conducive to DIELECTRIC CONSTANT ε ' raising.
Embodiment
Below by example and subordinate list, technical scheme of the present invention is described in further detail.
Manufacturing process flow is: 1) raw material disposal → 2) by formula calculation and weighing → 3) ball milling → 4) pre-burning → 5) secondary ball milling → 6) drying-granulating → 7) compression moulding → 8) sintering.
Example one
1.
Figure BDA00002843773500051
According to chemical formula
Y 3-y-2z-p+x-q-q′Gd yCa 2z+p-x+q+q′Cu xV zGe pSn qTi q′In q″Al wMn w′Fe 5-x-z-p-q-q′-w-w′-δO 12
Get: x=0.05; Y=1.00; Z=0.32; P=0.10; Q=0; Q '=0.03; Q "=0.27; W=0.05; W '=0 calculates required raw material.Use the Y after purity 〉=99.9% and process calcination are processed 2O 3, Gd 2O 3And analytically pure CuO, Fe 2O 3, CaCO 3, V 2O 5, GeO 2, TiO 2, In 2O 3, Al (OH) 3Be starting material, weigh up the starting material of corresponding weight.2. the raw material that weighs up is packed in ball grinder, and in material: ball: the ratio of alcohol=1: 3: 1 adds steel ball and alcohol, ball milling discharging after 12 hours.Cross 30 mesh sieves after the slurry drying, in the special-purpose corundum crucible of packing into.The stove that the corundum crucible that 3. powder will be housed is put into oxidizing atmosphere carries out pre-burning, and calcined temperature is 1200 ℃, is incubated 5 hours.4. Preburning material is first pulverized 30 mesh sieves, then put into ball grinder, and in material: ball: the ratio of alcohol=1: 3: 0.9 adds steel ball and alcohol, secondary ball milling discharging after 30 hours.5. with the oven dry of secondary ball abrasive material, add the cementing agent of 8wt%, mix and make 40 order particulate material.6. particulate material is put into forming mould and be pressed into required product blank, typed pressure is 98MPa.7. the stove of the blank of compression moulding being put into oxidizing atmosphere carries out sintering, and sintering temperature is 1280 ℃～1310 ℃, is incubated and cools to room temperature with the furnace after 5 hours.
The sample that obtains is made and is measured required bead and spillikin through mill processing, carries out parameter testing.Measuring result is as shown in table 1.
The electromagnetic performance parameter of table 1 example one superpower garnet material
Figure BDA00002843773500052
Figure BDA00002843773500061
Example two
1. according to chemical formula
Y 3-y-2z-p+x-q-q′Gd yCa 2z+p-x+q+q′Cu xV zGe pSn qTi q′In q″Al wMn w′Fe 5-x-z-p-q-q′-w-w′-δO 12
Get: x=0.05; Y=1.20; Z=0.26; P=0.10; Q=0; Q '=0.05; Q "=0.30; W=0; W '=0 calculates desired raw material.Use the Y after purity 〉=99.9% and process calcination are processed 2O 3, Gd 2O 3With analytically pure CuO, Fe 2O 3, CaCO 3, GeO 2, V 2O 5, In 2O 3, TiO 2Be raw material, weigh up the raw material of corresponding weight.2. the raw material that weighs up is packed in ball grinder, and in material: ball: the ratio of alcohol=1: 3: 1.0 adds steel ball and alcohol, ball milling discharging after 12 hours.To cross 30 mesh sieves after the slurry oven dry, in the corundum crucible of packing into.The stove that the corundum crucible that 3. powder will be housed is put into air atmosphere carries out pre-burning, and calcined temperature is 1200 ℃, is incubated 5 hours.4. Preburning material is first carried out coarse reduction and cross 30 mesh sieves, then put into ball grinder, and in material: ball: the ratio of water=1: 3: 0.9 adds steel ball and alcohol, secondary ball milling discharging after 30 hours.5. with the oven dry of secondary ball milling slurry, add the cementing agent of 8wt%, mix and make 40 order particulate material.6. particulate material is put into forming mould and be pressed into required product blank, typed pressure is 98MPa.7. with the blank of compression moulding, the stove of putting into oxidizing atmosphere carries out sintering, and sintering temperature is 1300 ℃～1330 ℃, is incubated and cools to room temperature with the furnace after 5 hours.
Sintered sample is made required bead and the spillikin of measurement and is carried out parameter testing through mill processing, and measuring result is as shown in table 2.
The electromagnetic performance parameter of table 2 example two superpower garnet materials
Figure BDA00002843773500062
Figure BDA00002843773500071
Example three
1.
Figure BDA00002843773500072
According to chemical formula
Y 3-y-2z-p+x-q-q 'Gd yCa 2z+p-x+q+q 'Cu xV zGe pSn qTi q′In q″Al wMn w′Fe 5-x-z-p-q-q '-w-w '-δO 12Get: x=0.05; Y=1.00; Z=0.32; P=0.10; Q=0; Q '=0.03; Q "=0.27; W=0.05; W '=0.04 calculates required raw material.Use the Y after purity 〉=99.9% and process calcination are processed 2O 3, Gd 2O 3And analytically pure CuO, Fe 2O 3, CaCO 3, V 2O 5, GeO 2, In 2O 3, Al (OH) 3, MnCO 3Be starting material, weigh up the starting material of corresponding weight.2. the raw material that weighs up is packed in ball grinder, and in material: ball: the ratio of alcohol=1: 3: 1 adds steel ball and alcohol, ball milling discharging after 12 hours.Cross 30 mesh sieves after the slurry drying, in the special-purpose corundum crucible of packing into.The stove that the corundum crucible that 3. powder will be housed is put into oxidizing atmosphere carries out pre-burning, and calcined temperature is 1200 ℃, is incubated 5 hours.4. Preburning material is pulverized 30 mesh sieves in advance, then put into ball grinder, and in material: ball: the ratio of alcohol=1: 3: 0.9 adds steel ball and alcohol, secondary ball milling discharging after 30 hours.5. with the oven dry of secondary ball abrasive material, add the cementing agent of 8wt%, mix and make 40 order particulate material.6. particulate material is put into forming mould and be pressed into required product blank, typed pressure is 98MPa.7. the stove of the blank of compression moulding being put into oxidizing atmosphere carries out sintering, and sintering temperature is 1320 ℃～1350 ℃, is incubated and cools to room temperature with the furnace after 5 hours.
The sample that obtains is made and is measured required bead and spillikin through mill processing, carries out parameter testing.Measuring result is as shown in table 3.
The electromagnetic performance parameter of table 3 example three superpower garnet materials
Figure BDA00002843773500073
Figure BDA00002843773500081
Material of the present invention has the advantages that power is born in low-loss, low-temperature coefficient, height, has solved preferably the problem that loss is bigger than normal or high power performance is not good enough of general superpower garnet material.In addition, because composition and engineering material reasonable in design has advantages of that also sintering temperature is low, energy consumption is low, production cost is low.In a word, the invention provides a kind of be convenient to suitability for industrialized production take into account Δ H kWith Δ H, Δ H effHigh power low loss microwave ferrite material formula and the manufacture method thereof of performance.

Claims (8)

1. the manufacture method of a superpower yttrium gadolinium ferrogarnet material,
It is characterized in that comprising the steps:
1) according to the constitutional chemistry formula
Y 3-y-2z-p+x-q-q 'Gd yCa 2z+p-x+q+q 'Cu xV zGe pSn qTi q′In q″Al wMn w′Fe 5-x-z-p-q-q '-w-w '-δO 12Calculate respectively required various starting material amounts, wherein iron deficiency amount δ be chosen as 0≤δ≤0.5, use the Y of purity 〉=99.9% 2O 3, Gd 2O 3With analytically pure Fe 2O 3, CaCO 3, In 2O 3, V 2O 5, GeO 2, SnO 2, TiO 2, Al (OH) 3, MnCO 3For starting material wherein: 0≤x≤1.30; 0≤y≤3.00; 0≤z≤1.50,0≤p≤1.30,0≤q≤0.70,0≤q '≤0.70,0≤q "≤0.70,0≤w≤1.30,0≤w '≤0.50, δ is the iron deficiency amount, 0≤δ≤0.50;
2) according to step 1) calculate required Y 2O 3, Gd 2O 3Material quantity carry out calcination and process, the calcination treatment temp is 850～1200 ℃, and is stand-by after furnace cooling;
3) according to step 1) calculate required material quantity, take respectively various raw materials with the balance of thousandth gram precision; And the Y that the raw material that takes and calcination were processed 2O 3, Gd 2O 3Put into ball grinder, in expecting: ball: the ratio of thinner=1: 2～5: 0.4～2.0 is carried out ball milling of wet method or is carried out ball milling of dry method;
4) with step 3) sieve after the mixed raw material slurry oven dry of ball milling, to make bulk or powdery and pack in corundum crucible, the stove of putting into oxidizing atmosphere carries out pre-burning, and calcined temperature is 800～1350 ℃;
5) with step 4) Preburning material broken, sieve after, carry out secondary ball milling in pack into ball grinder or sand mill, and by material: ball: the ratio of thinner=1: 2～5: 0.4～2.0 is carried out secondary ball milling, is milled to discharging when expecting powder median size≤1.2 μ m;
6) with step 5) slip carry out drying-granulating, should add cementing agent during granulation;
7) with step 6) particulate material put into forming mould and be pressed into required product blank, typed pressure is 50～150MPa, or further adopts cold isostatic compaction again;
8) blank of compression moulding, the stove of putting into oxidizing atmosphere are carried out sintering, sintering temperature is 1000～1550 ℃, is incubated 4～50 hours.
2. the manufacture method of superpower yttrium gadolinium ferrogarnet material according to claim 1, is characterized in that: Y described step 2) 2O 3And Gd 2O 3Calcination temperature be 950～1150 ℃.
3. the manufacture method of superpower yttrium gadolinium ferrogarnet material according to claim 1, it is characterized in that: described step 3) or 5) in to carry out ball milling ball grinder used be stainless cylinder of steel, steel ball used is Stainless Steel Ball, and thinner used is alcohol.
4. the manufacture method of superpower yttrium gadolinium ferrogarnet material according to claim 3, it is characterized in that: described step 3) ball milling of wet method according to: material: ball: the ratio of thinner=1: 3: 1 adds starting material, steel ball and alcohol, and Ball-milling Time is 12 hours.
5. the manufacture method of superpower yttrium gadolinium ferrogarnet material according to claim 3, it is characterized in that: described step 5) according to: material: ball: the ratio of thinner=1: 3: 0.9 adds starting material, steel ball and alcohol, and Ball-milling Time is 30 hours.
6. the manufacture method of superpower yttrium gadolinium ferrogarnet material according to claim 1 is characterized in that: described step 6), cementing agent is the polyvinyl alcohol aqueous solution that contains 4～15wt%.
7. the manufacture method of superpower yttrium gadolinium ferrogarnet material according to claim 1, it is characterized in that: described iron deficiency amount δ is chosen as 0≤δ≤0.3.
8. the manufacture method of superpower yttrium gadolinium ferrogarnet material according to claim 1; it is characterized in that: in described step 6), drying-granulating is mist projection granulating or mechanical pelleting; in described step 7), forming pressure is 98MPa, the temperature difference of the sintering temperature in described step 8) should be controlled at ± 5 ℃ in.
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CN105272196A (en) * 2015-11-19 2016-01-27 南京国睿微波器件有限公司 Garnet ferrite material applied to high-power phase shifter and preparing method thereof
CN108360062A (en) * 2018-02-02 2018-08-03 北京中材人工晶体研究院有限公司 A kind of method that multistep is synthetically prepared rear-earth-doped gadolinium gallium aluminium crystal raw material repeatedly
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Application publication date: 20130522