CN110002407A - A kind of method of carbon-thermal reduction synthesis metal sulfide - Google Patents
A kind of method of carbon-thermal reduction synthesis metal sulfide Download PDFInfo
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- CN110002407A CN110002407A CN201810012050.XA CN201810012050A CN110002407A CN 110002407 A CN110002407 A CN 110002407A CN 201810012050 A CN201810012050 A CN 201810012050A CN 110002407 A CN110002407 A CN 110002407A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/20—Methods for preparing sulfides or polysulfides, in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/70—Sulfides
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/007—Titanium sulfides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses it is a kind of by carbon-thermal reduction react synthesis metal M sulfide method, wherein M be one or more of Ti, Zr, Hf, Cr, Mo, W, V, Nb, Ta, Fe, Co, Ni, Mn, Cu, Zn, Si, Ge, Pb, Sn, Ag, Au, Pt, Pd, Rh, Ir, Ru, Os, Re, Al, B, Ga, In, Tl, Sc, Y, U, group of the lanthanides, actinium series described in M.It is uniformly mixed, mixture is reacted under vacuum environment, to prepare the solid sulfide of metal M by a certain percentage with carbon and sulphur using metal oxide.This method is from metal oxide, and raw materials used cheap and easy to get, simple production process and safe and feasible, reaction speed is fast, provides a kind of new method for the mass production of metal sulfide.
Description
Technical field
The present invention relates to a kind of methods based on carbon-thermal reduction synthesis metal sulfide, belong to technical field of material.
Background technique
Metal sulfide has many special properties and purposes, but in addition to a few metals sulfide is with nature mineral reserve money
Outside source, the sulfide of most metals requires artificial synthesized.The existence form of these metals in nature is mainly oxygen
Compound, since the chemical combination ability of sulphur and metal is often weaker than oxygen, the preparation side of the conventional metals sulfide of metal sulfide
Method often complex process, it is with high costs.Hereafter simply introduced with the synthesis of titanium sulfide.
The synthesis early stage of titanium sulfide used element the direct synthesis or vapour deposition process, such as in patent
U.S.Pat.No.4,007,055, British Pat.No.1,556,503 and Canadian Pat.No.1 in 094,777, is adopted
What is used is high pure metal titanium and elementary sulfur as raw material, is prepared under the inert atmosphere of anhydrous and oxygen-free in 475~600 DEG C of reactions
Titanium sulfide.It is also synthesized using element in patent U.S.Pat.No.4,069,301 and U.S.Pat.No.3,980,761
Method reacts preparation at 630 DEG C~1040 DEG C under inert atmosphere.Mentioning in patent U.S.Pat.No.3,079,229 can be used alkali
Titanium sulfide is prepared with elementsynthesis at 650~1000 DEG C in the fused salt of metal or alkaline-earth halide.But above-mentioned side
Metal titanium material in method is very expensive, be first by TiO2It is reduced into Titanium, but this step is inherently highly difficult.
Another approach is by TiO2Be converted into titanium tetrachloride gases with carbon and chlorine reaction, with hydrogen sulfide gas into
Promoting the circulation of qi mutually synthesizes titanium disulfide at 465~570 DEG C, such as United States Patent (USP) U.S.Pat.No.4, and 259,310, and
U.S.Pat.No.4,137,297.This method and process is complicated, is related to corrosive titanium tetrachloride gases and high risk sexual vulcanization
The operation of hydrogen.In Chinese patent 201410770028.3 using vulcanized sodium in alkali halide fused salt with four chlorinations
Titanium reaction is prepared for large-sized thin slice titanium disulfide.This method avoid the use of hydrogen sulfide gas, but related titanium tetrachloride
Operating difficulties still have.
As it can be seen that perhaps the expensive perhaps experiment condition of raw material sources is harsh or is not easy to advise for the preparation method of titanium sulfide at present
Modelling is realized.Moreover, same difficulty is also prevalent in the preparation of a large amount of metal sulfides such as Zr, Ta, Nb.Therefore, this hair
A kind of bright new method for wishing to develop easy-to-use metal sulfide preparation.
Summary of the invention
The invention proposes a kind of methods of carbon-thermal reduction synthesis metal sulfide, i.e., mix metal oxide and carbon and sulphur
It closes, is reacted in a certain temperature conditions, to prepare the solid sulfide of metal.
The used technical solution of the present invention is as follows:
A kind of method of carbon-thermal reduction synthesis metal sulfide, by the oxide M O of metal MxIt is mixed with simple substance carbon, elemental sulfur
It closes, isolation air carries out heating reaction, obtains the solid sulfide of metal M；Wherein: the metal M be Ti, Zr, Hf, Cr, Mo,
W、V、Nb、Ta、Fe、Co、Ni、Mn、Cu、Zn、Si、Ge、Pb、Sn、Ag、Au、Pt、Pd、Rh、Ir、Ru、Os、Re、Al、B、Ga、
One or more of In, Tl, Sc, Y, U, group of the lanthanides, actinium series.
Preferably, the above method specifically comprises the following steps:
(1) by MOxWith simple substance carbon, elemental sulfur under dispersing agent help, ball milling mixing is uniform, filtering, drying removal dispersion
Agent obtains MOx/ C/S mix powder；
(2) by MO obtained by step (1)x/ C/S mix powder compression moulding, is placed in vacuum sealing in reactor；
(3) vacuum-packed reactor obtained by step (2) is placed in Muffle furnace and carries out heating reaction, cooling obtains solid-state
Metal sulfide.
Preferably, in mixed raw material, the inventory of simple substance carbon and elemental sulfur is equal to or is greater than MOxDeoxidation simultaneously generates gold
The amount of simple substance carbon and elemental sulfur needed for belonging to sulfide.
Preferably, the inventory of elemental sulfur is relative to simple substance carbon excess, so that excessive simple substance carbon can be changed into gaseous state
CS2。
Preferably, the inventory of simple substance carbon is MOxThe 1 of the amount of deoxidation and simple substance carbon needed for generating metal sulfide is arrived
1.1 again.
Preferably, the inventory of elemental sulfur is MOxThe 1.05 of the amount of deoxidation and elemental sulfur needed for generating metal sulfide
To 1.3 times.
Preferably, the simple substance carbon is active carbon.
Preferably, the elemental sulfur is sublimed sulfur.
Preferably, the metal oxide MOxFor single metal oxide, composite oxides or mixed oxide,
The metal sulfide accordingly obtained is single metal sulfide, composition metal sulfide or mixed metal sulfide.
Preferably, the temperature of the heating reaction is 400-1700 DEG C.
Technical thought of the invention are as follows: in view of for most metal oxides, sulphur can not direct replacement it is therein
Oxygen, the present invention propose to realize metal oxide one in conjunction with metal therein using the oxygen collaboration sulphur in carbon combination metal oxide
Step is changed into metal sulfide.The main chemical reactions that the one-step method is related to can be indicated by following equation:
MOx+ xC+yS=MSy+xCO(>700℃)
Or
MOx+ 0.5xC+yS=MSy+0.5xCO2(<700℃)
After the reaction was completed, solid product is metal sulfide M Sy, and other elements all will in a gaseous form with the metal sulphur
Compound separation.For example, visual response temperature difference C is changed into the CO and CO of different proportion2；By MOxIn O remove completely, C must
Stoichiometry must be equal to and more than, further excessive purpose is to allow excessive C that can be changed into gaseous CS to S2Deng excessive
C is reacted with S generates CS2Equal gases；Excessive sulphur will be with gaseous state S2Form separation, will be only solid in such final reaction product
State metal sulfide.
Compared to traditional method, the method for the present invention has apparent advantage.By taking titanium dioxide as an example, the present invention is not necessarily to will
Titanium dioxide is Titanium, and without being transformed into the intermediate products such as titanium tetrachloride, but single step reaction is changed
For titanium sulfide, thus have process flow short, the advantages such as simple process.Moreover, the method for the present invention is various for preparing
Metal sulfide has universality.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings, but the embodiment in attached drawing is not constituted to any limit of the invention
System.
Fig. 1 is the XRD diffracting spectrum of 2 reaction raw materials of embodiment；
Fig. 2 is the XRD diffracting spectrum of 2 reaction product of embodiment, is shown as titanium sulfide；
Fig. 3 is the scanning electron microscope (SEM) photograph of 2 reaction product of embodiment, is shown as layer structure.
Specific embodiment
Illustrate the present invention below by embodiment, is to further describe and is not intended to limit the present invention.
Embodiment 1
(1) by titanium dioxide (with TiO2Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) is by amount of substance ratio 1:2:2.2
Mixture about 30g is weighed, using ethyl alcohol as dispersing agent, is dried for standby after being mixed by ball-milling method.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 1000 DEG C of reaction 20h, and furnace cooling obtains titanium sulfide.
Embodiment 2
(1) titanium dioxide is (with TiO2Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) is by amount of substance ratio 1:2.1:2.35
Titanium dioxide 13.39g, activated carbon 4.02g, sublimed sulfur 12.59g are weighed, using ethyl alcohol as dispersing agent, is dried after being mixed by ball-milling method
It does spare.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 1200 DEG C of reaction 10h, and furnace cooling obtains titanium sulfide.
The product that titanium dioxide and step (2) obtain is subjected to XRD detection respectively, obtained diffracting spectrum such as Fig. 1 and 2 institute
Show, shows that the product that reaction obtains is titanium sulfide.The product that step (2) obtains is characterized by scanning electron microscope, as shown in figure 3, table
Bright product is layer structure.
Embodiment 3
(1) aluminum oxide is (with Al2O3Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) press the mass ratio of the material 1:3.1:
3.4 weigh aluminum oxide 12.34g, activated carbon 4.5g, and sublimed sulfur 13.16g is mixed using ethyl alcohol as dispersing agent by ball-milling method
After be dried for standby.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 1650 DEG C of reaction 10h, and furnace cooling obtains aluminium sulfide.
Embodiment 4
(1) gallic oxide is (with Ga2O3Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) press amount of substance ratio 1:1.5:
3.4 weigh gallic oxide 17.88g, activated carbon 1.72g, sublimed sulfur 10.41g, mixed by ball-milling method using ethyl alcohol as dispersing agent
It is dried for standby after conjunction.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 450 DEG C of reaction 20h, and furnace cooling obtains vulcanization gallium.
Embodiment 5
(1) germanium dioxide is (with GeO2Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) is by amount of substance ratio 1:1.5:2.4
Germanium dioxide 15.77g, activated carbon 2.71g, sublimed sulfur 11.53g are weighed, using ethyl alcohol as dispersing agent, is dried after being mixed by ball-milling method
It does spare.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 500 DEG C of reaction 20h, and furnace cooling obtains germanium sulfide.
Embodiment 6
(1) tantalum pentoxide is (with Ta2O5Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) press amount of substance ratio 1:5.1:
4.3 weigh tantalum pentoxide 20.69g, activated carbon 2.87g, and sublimed sulfur 6.44g is mixed using ethyl alcohol as dispersing agent by ball-milling method
After be dried for standby.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 1100 DEG C of reaction 8h, and furnace cooling obtains vulcanization tantalum.
Embodiment 7
(1) niobium pentaoxide is (with Nb2O5Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) press amount of substance ratio 1:5.1:
4.3 weigh niobium pentaoxide 17.17g, activated carbon 3.95g, and sublimed sulfur 8.88g is mixed using ethyl alcohol as dispersing agent by ball-milling method
After be dried for standby.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 950 DEG C of reaction 20h, and furnace cooling obtains vulcanization niobium.
Embodiment 8
(1) di-iron trioxide is (with Fe2O3Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) press amount of substance ratio 1:1.7:
2.3 weigh di-iron trioxide 18.9g, activated carbon 2.41g, and sublimed sulfur 8.69g is mixed using ethyl alcohol as dispersing agent by ball-milling method
After be dried for standby.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 500 DEG C of reaction 20h, and furnace cooling obtains iron sulfide.
Embodiment 9
(1) ilmenite is (with FeTiO3Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) is by amount of substance ratio 1:3.1:2.3
Ilmenite 17.35g, activated carbon 4.25g, sublimed sulfur 8.4g are weighed, using ethyl alcohol as dispersing agent, is dried after being mixed by ball-milling method standby
With.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 1200 DEG C of reaction 10h, and furnace cooling obtains the mixture of iron sulfide and titanium sulfide.
Embodiment 10
(1) di-iron trioxide 9.65g, copper oxide 9.65g, activated carbon 2.03g, sublimed sulfur 8.68g are weighed, is point with ethyl alcohol
Powder is dried for standby after being mixed by ball-milling method.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 500 DEG C of reaction 20h, and furnace cooling obtains copper and iron complex sulfide.
Embodiment 11
(1) silica is (with SiO2Meter)/activated carbon (in terms of C /) sublimed sulfur (in terms of S) is by amount of substance ratio 1:2.1:2.4
Mixture about 30g is weighed, using ethyl alcohol as dispersing agent, is dried for standby after being mixed by ball-milling method.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 1450 DEG C of reaction 10h, and furnace cooling obtains silicon sulfide.
Embodiment 12
(1) titanium dioxide 13.4g, activated carbon 4.1g, sublimed sulfur 11g are weighed, it is mixed by ball-milling method using ethyl alcohol as dispersing agent
It is dried for standby after conjunction.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 1300 DEG C of reaction 4h, and furnace cooling obtains titanium sulfide.
Embodiment 13
(1) 15g CoO and 7.7g distillation sulphur powder are weighed and 2.5g activated carbon is placed in ball grinder, is dispersion with ethyl alcohol
Agent is dried for standby after being mixed by ball-milling method.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 900 DEG C of reaction 4h, and furnace cooling obtains vulcanizing sub- cobalt.
Embodiment 14
(1) 15g FeO and 7.8g distillation sulphur powder are weighed and 2.6g activated carbon is placed in ball grinder, is dispersion with ethyl alcohol
Agent is dried for standby after being mixed by ball-milling method.
(2) uniformly mixed 1~5g of powder is taken, the mold with diameter for 20cm is pressed into cylindric under 20Mpa pressure
Test piece, then the test piece of compacting is put into alundum tube and vacuumizes sealing.The reactor being sealed is placed in vertical horse
Not in furnace, temperature rises to 950 DEG C of reaction 4h, and furnace cooling obtains ferrous sulfide.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of method of carbon-thermal reduction synthesis metal sulfide, it is characterised in that: by the oxide M O of metal MxWith simple substance carbon,
Elemental sulfur mixing, isolation air carry out heating reaction, obtain the solid sulfide of metal M；Wherein: the metal M be Ti, Zr,
Hf、Cr、Mo、W、V、Nb、Ta、Fe、Co、Ni、Mn、Cu、Zn、Si、Ge、Pb、Sn、Ag、Au、Pt、Pd、Rh、Ir、Ru、Os、Re、
One or more of Al, B, Ga, In, Tl, Sc, Y, U, group of the lanthanides, actinium series.
2. according to the method described in claim 1, it is characterized by: specifically comprising the following steps:
(1) by MOxWith simple substance carbon, elemental sulfur under dispersing agent help, ball milling mixing is uniform, and filtering, drying removal dispersing agent obtain
To MOx/ C/S mix powder；
(2) by MO obtained by step (1)x/ C/S mix powder compression moulding, is placed in vacuum sealing in reactor；
(3) vacuum-packed reactor obtained by step (2) is placed in Muffle furnace and carries out heating reaction, cooling obtains solid metallic
Sulfide.
3. according to the method described in claim 1, it is characterized by: the inventory of simple substance carbon and elemental sulfur is equal in mixed raw material
Equal to or more than MOxThe amount of deoxidation and simple substance carbon and elemental sulfur needed for generating metal sulfide.
4. according to the method described in claim 3, it is characterized by: the inventory of elemental sulfur relative to simple substance carbon excess so that
Excessive simple substance carbon can be changed into gaseous CS2。
5. according to the method described in claim 1, it is characterized by: the inventory of simple substance carbon is MOxDeoxidation simultaneously generates metal vulcanization
1 to 1.1 times of the amount of simple substance carbon needed for object.
6. according to the method described in claim 1, it is characterized by: the inventory of elemental sulfur is MOxDeoxidation simultaneously generates metal vulcanization
1.05 to 1.3 times of the amount of elemental sulfur needed for object.
7. the method according to claim 1, wherein the simple substance carbon is active carbon.
8. the method according to claim 1, wherein the elemental sulfur is sublimed sulfur.
9. the method according to claim 1, wherein the metal oxide MOxFor single metal oxide,
Composite oxides perhaps the corresponding metal sulfide of mixed oxide be single metal sulfide, composition metal sulfide or
Mixed metal sulfide.
10. the method according to claim 1, wherein the temperature of the heating reaction is 400-1700 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563013A (en) * | 2019-08-26 | 2019-12-13 | 浙江工业大学 | Ball-milling synthesis method of aluminum sulfide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911787A (en) * | 2006-08-25 | 2007-02-14 | 南京大学 | Preparation method of nanometer metal sulfide |
| WO2015189053A1 (en) * | 2014-06-13 | 2015-12-17 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for producing alkali metal sulphide nanoparticles, alkali metal sulphide nanoparticles, use of the alkali metal sulphide nanoparticles, and alkali metal sulphur battery |
| CN108675267A (en) * | 2018-06-14 | 2018-10-19 | 西南大学 | An a kind of step prepares the universal method of nano metal sulphide and its compound |
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2018
- 2018-01-05 CN CN201810012050.XA patent/CN110002407B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911787A (en) * | 2006-08-25 | 2007-02-14 | 南京大学 | Preparation method of nanometer metal sulfide |
| WO2015189053A1 (en) * | 2014-06-13 | 2015-12-17 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for producing alkali metal sulphide nanoparticles, alkali metal sulphide nanoparticles, use of the alkali metal sulphide nanoparticles, and alkali metal sulphur battery |
| CN108675267A (en) * | 2018-06-14 | 2018-10-19 | 西南大学 | An a kind of step prepares the universal method of nano metal sulphide and its compound |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563013A (en) * | 2019-08-26 | 2019-12-13 | 浙江工业大学 | Ball-milling synthesis method of aluminum sulfide |
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