CN105541337A - Multi-metal silicide powder and preparing method thereof - Google Patents
Multi-metal silicide powder and preparing method thereof Download PDFInfo
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Abstract
The invention relates to multi-metal silicide powder and a preparing method thereof. The preparing method comprises: uniformly mixing, drying and sieving first metal with silicon powder of a corresponding ratio, and performing first thermal treatment at first temperature under the protection of an inertia gas to obtain first metal silicide powder; uniformly mixing, drying and sieving second metal with silicon powder of a corresponding ratio and the first metal silicide powder, and performing second thermal treatment at second temperature under the protection of the inertia gas to obtain multi-metal silicide powder containing the first metal silicide and second metal silicide, wherein a melting point of the first metal silicide is larger than that of the second metal silicide, and the first temperature is higher than the second temperature. Multiple silicide particles are synthesized by a manner of thermal treatment step by step, and forming components and ratios of the silicide particles can be controlled. The obtained multiple silicides are bound together in a solid solution or mutual wrapping manner, and can be directly introduced into a sintering process, a welding process and other processes for use.
Description
Technical field
The present invention relates to one kind of multiple silicide solid solutions or coated powder formed single-size powder with and preparation method thereof.This powder structure is even, not remaining elemental metal or silicon grain, mean particle size 0.1 ~ 30 μm, and silicide component ratio can design adjustment, can be used for being directly used in the fields such as the additive in ceramic post sintering, the solder in welding or auxiliary agent.
Background technology
Silicide with directly in the sinter additives of the potteries such as silicon nitride, silicon carbide, aluminum oxide, can improve ceramic densifying, improve ceramic pattern, improve the performance of pottery, also can be used in welding as solder or auxiliary agent.
Single silicide is often restricted on the calorifics such as thermal expansivity, Young's modulus or mechanical property, can not meet practical application needs.And mix multiple silicide according to ratio and may the thermal expansivity, Young's modulus etc. of silicide after mixing be regulated, be expected to obtain calorifics or mechanical properties that single silicide cannot meet, in sintering, be more conducive to the raising of ceramic over-all properties, in welding, be beneficial to the comprehensive raising of strength of joint, thermal expansion matching and other performances.
But, if multiple silicide powder is mixed simply, between different silicide, bonding strength is not high, different silicides is easily caused to be separated from each other in adding in matrix (as ceramic post sintering raw material) mixing process of later stage, cannot play the distinctive performance of silicide composite grain, when silicide total amount content is not high, separated phenomenon is particularly serious.Owing to there is difference between different silicide synthesis temperature; difference is there is between different silicide fusing point; difference is there is between the fusing point of the synthesis material of different silicide; by multiple silicide or silicide raw material mixed sintering simply; often because the silicide that above-mentioned difference causes the silicide of some low melting points to be agglomerated into macrobead or high synthesis temperature does not synthesize completely, evenly tiny silicide mixed powder and its performance had can not be obtained.
Such as, Kyoto Ceramic Co., Ltd is apt in great river abundant grade (patent No. ZL200480024471.0) and designs the silicon nitride plastid simultaneously containing the silicide of Fe, Cr, Mn etc. and the silicide of W, Mo etc., require in silicon nitride plastid between silicide formed parcel or adjacent phase, avoid the gap on single silicide Young's modulus and thermal expansivity cause stress concentration or heat shock resistance poor.And when two kinds of Formation of silicide parcels or adjacent particle, the coefficient of expansion and Young's modulus can decrease relative to the maximum of single silicide, two kinds of silicides play oneself advantage respective on acceleration of sintering and high temperature toughness simultaneously.But its silicide incorporation way adopts oxide compound or carbide and silica flour in-situ preparation, and not only introduce the impurity such as oxygen, carbon, nitrogenize heat treatment time is long.Meanwhile, the metallic compound content of interpolation is very low, and different metal silicide is easily scatter in batch mixing process, and in sintered compact, silicide is in separate stage.If just there are not the problems referred to above in the silicide solid solution or the parcel composite grain that directly add iron and tungsten.And it can be applicable in pressureless sintering, gas pressure sintering, hot pressed sintering and HIP sintering.
Summary of the invention
For prior art Problems existing, aim to provide a kind of preparation technology of improvement to obtain many metal silications powder of excellent performance.
First the present invention provides a kind of many metal silicides raw powder's production technology, and the chemical constitution of described many metal silications powder comprises at least two kinds of metal silicides, and described preparation method comprises:
By silica flour Homogeneous phase mixing, the drying of corresponding with it for the first metal ratio, sieve, carry out the first thermal treatment in the first temperature under protection of inert gas and obtain the first metal silication powder;
By the silica flour of corresponding with it for the second metal ratio and described first metal silication powder Homogeneous phase mixing, drying, sieve, under protection of inert gas, carry out in the second temperature heat many metal silications powder that the second process obtains comprising the first metal silicide and the second metal silicide;
Wherein the fusing point of the first metal silicide is greater than the fusing point of the second metal silicide, and the first temperature is higher than the second temperature.
The present invention synthesizes multiple silicide particle by the heat treated mode of substep, and can control its formation component and ratio.By the adjustment to multiple silicide particle ratio, the single silicide powder unappeasable mechanics of institute and thermal property can be solved, as coefficient of thermal expansion, Young's modulus, toughness, hardness etc.And by substep repeatedly heat treated mode solved in the past between different silicide, between different metal because fusing point difference is large, it is large that silicide generates temperature difference, and the ordinary heat treatment caused is difficult to the problem of synthesizing even fine powder.And the multiple silicide obtained is bonded together by modes such as solid solution or mutual parcels, even if also can not by the combination of different silicide separately in the use procedure be uniformly mixed.The silicide mixture generated can be introduced directly in the techniques such as sintering, welding and use.
In the present invention, the metallic element in described many metal silications powder is selected from least two kinds in Fe, Cr, Mn, Ti, Sc, Zn, Zr, Cu, W, Mo, Ti, V, Ni, Y, La, Hf, Zr, Nb, Ta, Re, Os, Ir, Pt, Pd, Co, Rh, Ru, Tc.The metallic element scope that the present invention uses is wide, can obtain many metal silications powder that composition is different, applied widely.
Preferably, described first metal is selected from least one in W, Mo, V, Hf, Ta, described second metal is selected from least one in Fe, Mn, Cu, Ni, Co, Pd, Ti, Pt, Cr, described first temperature is 1300 ~ 1800 DEG C, described second temperature is 800 ~ 1400 DEG C, and the first temperature is higher than the second temperature.Further, described first metal can be selected from least one in W, Mo.Described second metal can be selected from least one in Fe, Cr, Mn.
Preferably, described first metal and/or bimetallic mean particle size can be 0.2 ~ 20 μm.
Preferably, the mean particle size of described silica flour can be 0.5 ~ 20 μm.
Preferably, described preparation method also comprises:
By the silica flour of the 3rd metal ratio corresponding to it and comprise the first metal silicide and the second metal silicide many metal silications powder Homogeneous phase mixing, drying, sieve; carry out in the 3rd temperature heat many metal silications powder that the 3rd process obtains comprising the first metal silicide, the second metal silicide and the 3rd metal silicide under protection of inert gas; the fusing point of described 3rd metal silicide is lower than the fusing point of described second metal silicide, and described 3rd temperature is 600 ~ 1200 DEG C and lower than described second temperature.
Method batch heat of the present invention is not limited to twice or three times, can heat-treat several times according to the height of the kind of the metal silicide contained according to fusing point, namely the metal first adding the silicide of peak melting point corresponding is heat-treated, and then adds metal corresponding to the silicide of the fusing point that takes second place, carries out successively like this.
Preferably, described first thermal treatment, the second thermal treatment and/or the 3rd heat treated treatment time are respectively 0.5 ~ 5 hour.
Many metal silications powder that the present invention also provides a kind of aforesaid method to prepare, the median size of described many metal silications powder is 0.1 ~ 30 μm, and wherein at least two kinds of metal silicides combine closely with the form of solid solution or mutual parcel.
Many metal silications powder provided by the invention, uniform particles, and multiple silicide is bonded together by modes such as solid solution or mutual parcels, and not remaining elemental metal or silicon grain, even if also can not by the combination of different silicide separately in the use procedure be uniformly mixed, and mechanics and thermal property can be realized, as coefficient of thermal expansion, Young's modulus, toughness, hardness performance is adjustable, can be introduced directly in the techniques such as sintering, welding and use.
Accompanying drawing explanation
Fig. 1 Fig. 1 is method schematic process flow diagram of the present invention;
Fig. 2 is the XRD diffracting spectrum of powder prepared by embodiment 1;
Fig. 3 is powdered elemental Surface scan power spectrum prepared by embodiment 1;
Fig. 4 is that powder SEM prepared by embodiment 1 schemes, and wherein 1 represent iron silicide, 2 represent tungsten silicide;
Fig. 5 is that powder SEM prepared by comparative example schemes, and wherein 1 represent iron silicide, 2 represent tungsten silicide.
Embodiment
Below, further illustrate the present invention with reference to accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
The present invention provides a kind of even fine powder body and the preparation technology that contain multiple silicide at this, is mutually linked together closely in this powder between each silicide by solid solution or parcel.This powder can be used for the sintering of pottery, the fields such as welding.
In the metal silicide that the present invention selects, metallic element is in the silicide of Fe, Cr, Mn, Ti, Sc, Zn, Zr, Cu, W, Mo, Ti, V, Ni, Y, La, Hf, Zr, Nb, Ta, Re, Os, Ir, Pt, Pd, Co, Rh, Ru, Tc etc. at least two kinds.Adopt metal simple-substance and elementary silicon as raw material, can not introduce as prior art and such as introduce the impurity such as oxygen, carbon.
The kind of the metallic element contained according to many metal silicides is heat-treated several times according to the height of fusing point, and the metal namely first adding peak melting point is heat-treated, and then adds the metal of the fusing point that takes second place, carries out successively like this.
Such as; see Fig. 1; can by silica flour Homogeneous phase mixing corresponding with it for first metal (the first metal), dry, sieve, thermal treatment under inert protective atmosphere (the first thermal treatment) obtains the first synthetic powder (the first metal silication powder).Here, using metal corresponding for the metal silicide of peak melting point in many metal silicides such as, as the first metal, W, Mo, V, Hf, Ta etc.First heat treated temperature can set according to the generation temperature of the fusing point of the fusing point of the first metal, the first metal silicide and the first metal silicide, such as, choose 1300 ~ 1800 DEG C.First heat treated time can be 0.5 ~ 5 hour fully to synthesize the first metal silicide so that kish simple substance or silica flour simple substance are not as the criterion.The ratio of the first metal and silica flour can set according to desired metal silication species, and the molar ratio of such as metallic element and element silicon can be between 1:3 to 5:1, preferably, between 1:2 to 2:1.
Then; by the silica flour three Homogeneous phase mixing of the first synthetic powder (the first metal silication powder), second batch metal (the second metal) and correspondence; dry, sieve, thermal treatment under inert protective atmosphere (the second thermal treatment) obtains the second synthetic powder (mixed powder containing the first metal silicide and the second metal silicide).Here, using metal corresponding compared with the metal silicide of low melting point in many metal silicides such as, as the second metal, Fe, Mn, Cu, Ni, Co, Pd, Ti, Pt, Cr etc.Second heat treated temperature can set according to the generation temperature of the fusing point of bimetallic fusing point, the first and second metal silicides and the second metal silicide, such as, choose 800 ~ 1400 DEG C.Second heat treated time can be 0.5 ~ 5 hour fully to synthesize the second metal silicide so that kish simple substance or silica flour simple substance are not as the criterion.The ratio of the second metal and silica flour also can set according to desired metal silication species.
Then; as required can also by the silica flour three Homogeneous phase mixing of the second synthetic powder (mixed powder containing the first metal silicide and the second metal silicide), the 3rd batch of metal (the 3rd metal) and correspondence; dry, sieve, thermal treatment under inert protective atmosphere (the 3rd thermal treatment) obtains the 3rd synthetic powder (mixed powder containing the first metal silicide, the second metal silicide and the 3rd metal silicide).Here, should understand and heat-treat several times according to the height of the fusing point of metal silicide, be not limited to twice or three thermal treatment, as long as the metal that the metal silicide first adding peak melting point is corresponding is heat-treated, then add metal corresponding to the metal silicide of the fusing point that takes second place, carry out successively like this ..., until all metals and corresponding silicide all add and thermal treatment.Such as W, Mo, V, Hf, Ta etc. self and the mixing of its silicide fusing point higher metal preliminary planning, thermal treatment 0.5 ~ 5h under waiting comparatively high temps and inert protective atmosphere at 1300 ~ 1800 DEG C.And Fe, Mn, Cu, Ni, Co, Pd, Ti, Pt, Cr etc. self and the lower metal of its silicide fusing point are placed on later stage participation mixing, thermal treatment 0.5 ~ 5h under waiting lesser temps and inert protective atmosphere at 800 ~ 1400 DEG C.But be not limited thereto, that is, also by such as the many metal silicides containing these three kinds of elements of Mo, Co, Ni, can consider that the metal simple-substance Mo first adding peak melting point carries out the first thermal treatment, then add the metal Co that fusing point takes second place and carry out the second thermal treatment, finally add Ni again.By means of this, in earlier stage higher temperature ensures that the metal that fusing point is higher fully reacts, and generates required silicide.And later stage thermal treatment temp is lower, the silicide avoiding fusing point lower melt cause together particle coarsening.
Should be understood that in order to avoid bringing impurity into, above-mentioned thermal treatment all should be carried out under protection of inert gas, to avoid oxidation or the nitrogenize of metal and silicon.If containing nitrogen in protective atmosphere, then silica flour or metal powder generating portion or all nitrogenize.Use metal oxide can form silica impurity as in raw material then product.Rare gas element can select argon gas etc.
Should be understood that the mode that above-mentioned mixing can adopt ball milling to mix is carried out, to mix as standard.Abrading-ball can adopt silicon nitride ball or alumina balls, and ball-milling medium can adopt dehydrated alcohol etc., and Ball-milling Time can be 1 ~ 5 hour.
Preferably, above-mentioned each heat treatment process is this powder of thermal treatment under loose condition (of surface) after sizing, more easily obtains the even fine powder of easily dispersion.
The purity of metal simple-substance powder used in the present invention is preferably more than 98%, and mean particle size is preferably 0.2 ~ 20 μm.Silica flour used is preferably more than 98%, and mean particle size is preferably 0.5 ~ 20 μm.
The present invention obtains multiple silicide powder, and each silicide wraps up uniformly or is solid-solubilized in (see Fig. 4) together, mixes even if add in other powder, and each silicide can not be separated separately.
Below some exemplary embodiments are listed further better the present invention to be described.Should understand; the above-mentioned embodiment that the present invention describes in detail; and following examples are only not used in for illustration of the present invention and limit the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.In addition, concrete proportioning, time etc. in following processing parameter are also only exemplary, and those skilled in the art can select suitable value in the scope of above-mentioned restriction.
Embodiment 1
Embodiment 1:
Twice thermal treatment synthesis m
wSi2: m
feSi2the WSi of=1:1
2/ FeSi
2adjacent or package structure powder
1) first time mixing: by tungsten powder and silica flour according to atomic ratio 1:2 mixing 100g, adds silicon nitride ball or alumina balls and adds 45g dehydrated alcohol and mix, ball milling 1.5h;
2) dried and screened: 40 DEG C of forced air drying 3h, cross 60 mesh sieves;
3) first time thermal treatment: argon atmosphere 1450 DEG C of thermal treatment 3h;
4) second time mixing: powder thermal treatment obtained adds iron powder and the silica flour that 100g atomic ratio is 1:2,100g silicon nitride ball or alumina balls, and 120g dehydrated alcohol mixes, ball milling 2h;
5) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
6) second time thermal treatment: argon atmosphere 1250 DEG C of thermal treatment 5h, obtains the powder needed;
The XRD figure of resultant is shown in Fig. 2, and Fig. 3 is shown in the energy spectrum analysis of element Surface scan, and SEM shape appearance figure is shown in Fig. 4.As shown in Figure 2, generate the metal silicide that we need, do not find the residual of metal simple-substance or elementary silicon.As shown in Figure 3, iron silicide and tungsten silicide are uniformly dispersed, and are mutually bundled together closely.As shown in Figure 4, the silicide powder granule obtained is even, and great majority, between 5 ~ 15 μm, seldom have the particle more than 25 μm.
Embodiment 2:
Twice thermal treatment synthesis m
moSi2: m
feSi2the MoSi of=1:2
2/ FeSi
2adjacent or package structure powder
1) first time mixing: by molybdenum powder and silica flour according to atomic ratio 1:2 mixing 60g, adds silicon nitride ball or alumina balls and adds 45g dehydrated alcohol and mix, ball milling 1.5h;
2) dried and screened: 40 DEG C of forced air drying 3h, cross 60 mesh sieves;
3) first time thermal treatment: argon atmosphere 1300 DEG C of thermal treatment 5h;
4) second time mixing: powder thermal treatment obtained adds iron powder and the silica flour that 120g atomic ratio is 1:2,100g silicon nitride ball or alumina balls, and 120g dehydrated alcohol mixes, ball milling 2h;
5) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
6) second time thermal treatment: argon atmosphere 1200 DEG C of thermal treatment 5h, obtains the powder needed.
Embodiment 3:
Twice thermal treatment synthesis m
mo5Si3: m
cr3Sithe Mo of=3:1
5si
3/ Cr
3adjacent or the package structure powder of Si
1) first time mixing: by molybdenum powder and silica flour according to atomic ratio 5:3 mixing 150g, 80g silicon nitride ball or alumina balls add 60g dehydrated alcohol and mix, ball milling 1.5h;
2) dried and screened: 40 DEG C of forced air drying 3h, cross 60 mesh sieves;
3) first time thermal treatment: argon atmosphere 1800 DEG C of thermal treatment 0.5h;
4) second time mixing: powder thermal treatment obtained adds chromium powder and the silica flour of 50g atomic ratio 3:1,100g silicon nitride ball or alumina balls, and 120g dehydrated alcohol mixes, ball milling 2h;
5) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
6) second time thermal treatment: argon atmosphere 1400 DEG C of thermal treatment 0.5h, obtains the powder needed.
Embodiment 4:
Twice thermal treatment synthesis m
w5Si3: m
cu3Sithe W of=2:1
5si
3/ Cu
3adjacent or the package structure powder of Si
1) first time mixing: by tungsten powder and silica flour according to atomic ratio 5:3 mixing 120g, add 60g silicon nitride ball or alumina balls, the mixing of 50g dehydrated alcohol, ball milling 1.5h;
2) dried and screened: 40 DEG C of forced air drying 3h, cross 60 mesh sieves;
3) first time thermal treatment: argon atmosphere 1400 DEG C of thermal treatment 2h;
4) second time mixing: powder thermal treatment obtained adds copper powder and the silica flour of 60g atomic ratio 3:1,100g silicon nitride ball or alumina balls, and 120g dehydrated alcohol mixes, ball milling 2h;
5) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
6) second time thermal treatment: argon atmosphere 900 DEG C of thermal treatment 5h, obtains the powder needed.
Embodiment 5:
Twice thermal treatment synthesis m
moSi2: m
(Fe+Mn) 5Si3the MoSi of=1:1
2/ Fe
5si
3/ Mn
5si
3adjacent or package structure powder
1) first time mixing: by molybdenum powder and silica flour according to atomic ratio 1:2 mixing 100g, 50g silicon nitride ball or alumina balls add 50g dehydrated alcohol and mix, ball milling 1.5h;
2) dried and screened: 40 DEG C of forced air drying 3h, cross 60 mesh sieves;
3) first time thermal treatment: argon atmosphere 1500 DEG C of thermal treatment 2h;
4) second time mixing: powder thermal treatment obtained adds 39g iron powder, 38g manganese powder, 24g silica flour, 100g silicon nitride ball or alumina balls, 150g dehydrated alcohol mixes, ball milling 2h;
5) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
6) second time thermal treatment: argon atmosphere 1200 DEG C of thermal treatment 2h, obtains the powder needed.
Embodiment 6:
Twice thermal treatment synthesis m
wSi2: m
niSithe rich WSi of=4:1
2adjacent or the package structure powder of/NiSi
1) first time mixing: by tungsten powder and silica flour according to atomic ratio 1:2 mixing 160g, 70g silicon nitride ball or alumina balls add 70g dehydrated alcohol and mix, ball milling 1.5h;
2) dried and screened: 40 DEG C of forced air drying 3h, cross 60 mesh sieves;
3) first time thermal treatment: argon atmosphere 1400 DEG C of thermal treatment 5h;
4) second time mixing: powder thermal treatment obtained adds nickel powder and the silica flour of 40g atomic ratio 1:1,100g silicon nitride ball or alumina balls, and 120g dehydrated alcohol mixes, ball milling 2h;
5) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
6) second time thermal treatment: argon atmosphere 1000 DEG C of thermal treatment 2h, obtains the powder needed.
Embodiment 7:
Three thermal treatment synthesis m
moSi2: m
coSi: m
niSithe rich MoSi of=1:1:1
2adjacent or the package structure powder of/CoSi/NiSi
1) first time mixing: by molybdenum powder and silica flour according to atomic ratio 1:2 mixing 100g, 50g silicon nitride ball or alumina balls add 50g dehydrated alcohol and mix, ball milling 1.5h;
2) dried and screened: 40 DEG C of forced air drying 3h, cross 60 mesh sieves;
3) first time thermal treatment: argon atmosphere 1500 DEG C of thermal treatment 2h;
4) second time mixing: powder thermal treatment obtained adds cobalt powder and the silica flour of 100g atomic ratio 1:1,100g silicon nitride ball or alumina balls, and 120g dehydrated alcohol mixes, ball milling 2h;
5) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
6) second time thermal treatment: argon atmosphere 1200 DEG C of thermal treatment 2h;
7) third time mixing: powder thermal treatment obtained adds nickel powder and the silica flour that 100g atomic ratio is 1:1,150g silicon nitride ball or alumina balls, and 150g dehydrated alcohol mixes, ball milling 2h;
8) dried and screened: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
9) third time thermal treatment: argon atmosphere 900 DEG C of thermal treatment 5h, obtains the powder needed.
Comparative example 1
A thermal treatment obtains silicide mixed powder
1) by silica flour 136g, iron powder 100g, tungsten powder 100g, 120g silicon nitride ball or alumina balls, 150g dehydrated alcohol mixes, roller ball mill 2h;
2) dry: 40 DEG C of forced air drying 5h, cross 60 mesh sieves;
3) thermal treatment: argon atmosphere 1300 DEG C of thermal treatment 1h, obtains the powder needed;
The SEM shape appearance figure of resultant is shown in Fig. 5, finds from figure, and particle agglomeration forms 25 μm of even larger particles together, and two kinds of silicide dispersions are even not, and parcel is mutually also obviously not as many in Fig. 4 mutually.
From the SEM Comparative result of embodiment 1 and comparative example, the powder that two-step sintering method obtains is thinner, evenly, containing more adjacent or parcel phase.
Claims (10)
1. the raw powder's production technology of metal silicide more than, is characterized in that, the chemical constitution of described many metal silications powder comprises at least two kinds of metal silicides, and described preparation method comprises:
By silica flour Homogeneous phase mixing, the drying of corresponding with it for the first metal ratio, sieve, carry out the first thermal treatment in the first temperature under protection of inert gas and obtain the first metal silication powder;
By the silica flour of corresponding with it for the second metal ratio and described first metal silication powder Homogeneous phase mixing, drying, sieve, under protection of inert gas, carry out in the second temperature heat many metal silications powder that the second process obtains comprising the first metal silicide and the second metal silicide;
Wherein the fusing point of the first metal silicide is greater than the fusing point of the second metal silicide, and the first temperature is higher than the second temperature.
2. preparation method according to claim 1, it is characterized in that, the metallic element in described many metal silications powder is selected from least two kinds in Fe, Cr, Mn, Ti, Sc, Zn, Zr, Cu, W, Mo, Ti, V, Ni, Y, La, Hf, Zr, Nb, Ta, Re, Os, Ir, Pt, Pd, Co, Rh, Ru, Tc.
3. preparation method according to claim 1 and 2, it is characterized in that, described first metal is selected from least one in W, Mo, V, Hf, Ta, described second metal is selected from least one in Fe, Mn, Cu, Ni, Co, Pd, Ti, Pt, Cr, described first temperature is 1300 ~ 1800 DEG C, described second temperature is 800 ~ 1400 DEG C, and the first temperature is higher than the second temperature.
4. preparation method according to claim 3, is characterized in that, described first metal is selected from least one in W, Mo.
5. the preparation method according to claim 3 or 4, is characterized in that, described second metal is selected from least one in Fe, Cr, Mn.
6. preparation method according to any one of claim 1 to 5, is characterized in that, described first metal and/or bimetallic mean particle size are 0.2 ~ 20 μm.
7. preparation method according to any one of claim 1 to 6, is characterized in that, the mean particle size of described silica flour is 0.5 ~ 20 μm.
8. preparation method according to any one of claim 1 to 7, is characterized in that, described preparation method also comprises:
By the silica flour of the 3rd metal ratio corresponding to it and comprise the first metal silicide and the second metal silicide many metal silications powder Homogeneous phase mixing, drying, sieve; carry out in the 3rd temperature heat many metal silications powder that the 3rd process obtains comprising the first metal silicide, the second metal silicide and the 3rd metal silicide under protection of inert gas; the fusing point of described 3rd metal silicide is lower than the fusing point of described second metal silicide, and described 3rd temperature is 600 ~ 1200 DEG C and lower than described second temperature.
9. preparation method according to claim 8, is characterized in that, described first thermal treatment, the second thermal treatment and/or the 3rd heat treated treatment time are respectively 0.5 ~ 5 hour.
10. many metal silications powder of preparing of a preparation method according to any one of claim 1 to 9, it is characterized in that, the median size of described many metal silications powder is 0.1 ~ 30 μm, and wherein at least two kinds of metal silicides combine closely with the form of solid solution or mutual parcel.
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| CN106045525A (en) * | 2016-06-01 | 2016-10-26 | 中国科学院上海硅酸盐研究所 | Silicon nitride sintered body and preparation method thereof |
| CN112110737A (en) * | 2020-09-23 | 2020-12-22 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | High-chromium refractory material and preparation method thereof |
| CN112342422A (en) * | 2020-10-27 | 2021-02-09 | 湖北新蓝天新材料股份有限公司 | Copper-silicon alloy material and preparation method and application thereof |
| CN114410061A (en) * | 2020-10-28 | 2022-04-29 | 中国科学院理化技术研究所 | Thermal interface material with high thermal conductivity and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106045525A (en) * | 2016-06-01 | 2016-10-26 | 中国科学院上海硅酸盐研究所 | Silicon nitride sintered body and preparation method thereof |
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| CN112110737B (en) * | 2020-09-23 | 2022-05-06 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | High-chromium refractory material and preparation method thereof |
| CN112342422A (en) * | 2020-10-27 | 2021-02-09 | 湖北新蓝天新材料股份有限公司 | Copper-silicon alloy material and preparation method and application thereof |
| CN114410061A (en) * | 2020-10-28 | 2022-04-29 | 中国科学院理化技术研究所 | Thermal interface material with high thermal conductivity and preparation process thereof |
| CN114410061B (en) * | 2020-10-28 | 2023-08-01 | 中国科学院理化技术研究所 | Thermal interface material with high thermal conductivity and preparation process thereof |
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