CN102502653A - System and method for producing high-purity disilane - Google Patents
System and method for producing high-purity disilane Download PDFInfo
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- CN102502653A CN102502653A CN2011104186345A CN201110418634A CN102502653A CN 102502653 A CN102502653 A CN 102502653A CN 2011104186345 A CN2011104186345 A CN 2011104186345A CN 201110418634 A CN201110418634 A CN 201110418634A CN 102502653 A CN102502653 A CN 102502653A
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Abstract
The invention discloses a system and method for producing high-purity disilane. A magnesium silicide and ammonium chloride charging device is connected with a first feeding port of a reaction kettle, a liquid ammonia storage tank is connected with a second feeding port of the reaction kettle, an ammonia backflow port of a condenser is connected with a second feeding port of the reaction kettle, the silane and disilane outlet of the reaction kettle is connected with the gas inlet of the condenser, the gas outlet of the condenser is connected with the inlet of a crude silane purifying device, the outlet of the crude silane purifying device is respectively connected with one end of a first valve and one end of a second valve, the other end of the second valve is connected with the inlet of a disilane liquefying device, the outlet of the disilane liquefying device is respectively connected with one end of a third valve and one end of a fourth valve, the other end of the fourth valve is connected with a disilane purifying device, and the other end of the first valve and the other end of the third valve are connected with the inlet of the silane purifying device. According to the invention, a new production raw material is not needed to be added, the large production equipment is not needed to be increased, and production capacity of high-purity disilane can be formed by increasing disilane liquefying and purifying devices to a silane product line.
Description
Technical field
The present invention relates to a kind of produce high-purity silicoethane system and method thereof.
Background technology
Silicoethane is silicon, hydrogen compound.The same with silane all is one of most important silane gas.Especially the silicoethane situation that obviously is superior to silane has following several kinds:
A, when the glow discharge deposition amorphous silicon membrane, silicoethane sedimentation rate higher at least more than 20 times than silane, and formed film than the thickness of silane many, reach 20 μ m, this silicoethane institute deposit film has higher photoconductive property.
B, when preparing semiconductor silicon with silane, silicoethane decomposition temperature can reduce by 200～300 ℃, the energy consumption of per unit weight semiconductor silicon will descend significantly.
C, in the ion implantation technology process, do the easy build-up of luminance of ion source with silicoethane, electron gun is strong, effect obviously is superior to other gases.
D, silicoethane can be used as the doping agent of III-V group element compound semiconductor material, also can make the phosphorous doped polysilicon material, and with grid and the emtting electrode that is used for integrated device, these advantages all are that silane institute is irreplaceable.
Silicoethane the preparation method:
One, be that initial feed prepares silicoethane with silane
With silane is that initial feed all might make SiH through methods such as photodissociation, photoglow, atomic excitation, electrostatic field, thermolysiss
4Be converted into silicoethane.
Reaction formula:
These methods all are to carry out at (between several torrs～20 torrs) under the very low condition of silane pressure.It is that the silicoethane transformation efficiency is low that silane prepares the subject matter that silicoethane faces through thermolysis, has only about 8%, and is easy to produce pale brown look unbodied (SiH
2) solid matter.More than these methods they all do not have real practical value.
Two, halodisilane reduction method
With lithium aluminum hydride (LiAlH
4) reduction disilicone hexachloride (Si
2Cl
6) the preparation silicoethane.
Reaction formula:
Add the ether that is in the disilicone hexachloride under vacuum and 0 ℃ to the diethyl ether solution of lithium aluminum hydride at leisure and dissolve alkane.The transformation efficiency of this method disilicone hexachloride is 87%, and major part is a silicoethane in the product, and having only a spot of is silicomethane.
Be noted that if not adding solutions of lithium aluminium hydride disilicone hexachloride solution opposite but in the excessive solutions of lithium aluminium hydride of disilicone hexachloride solution adding, then primary product is a silicomethane, having only a spot of is silicoethane.
Present this method only rests in the laboratory, does not also form industrialized production process.
Three, magnesium silicide and ammonium chloride prepared in reaction silicoethane
Reaction formula:
2Mg
2Si+8NH
4Cl→Si
2H
6+4MgCl
2+H
2+8NH
3
Domestic existing many families utilize the manufacturing enterprise of magnesium silicide and ammonium chloride reacted high purity silane after 2008, and YO is all about 10 tons.Current state is: 1, these producers possibly also not know in the reaction kettle to produce in the process of silane and will inevitably produce silicoethane; Even have silicoethane to produce in the 2 knowing reaction stills but just have no idea to separate silicoethane separately and become a kind of product of putting on market at all.And let this good wasting of resources of silicoethane in vain on the production line of oneself.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of produce high-purity silicoethane system and method thereof.
Produce high-purity silicoethane system comprise magnesium silicide and ammonium chloride feeding device, liquefied ammonia storage tank, reaction kettle, condensing surface, thick silane purifying plant, the dark purifying plant of silane, silicoethane liquefying plant, silicoethane purifying plant, first valve, second valve, the 3rd valve and the 4th valve; Magnesium silicide links to each other with reaction kettle the 1st opening for feed with the ammonium chloride feeding device; The liquefied ammonia storage tank links to each other with reaction kettle the 2nd opening for feed; Condensing surface ammonia refluxing opening links to each other with reaction kettle the 2nd opening for feed; Outlet links to each other with the condensing surface inlet mouth reaction kettle silane with silicoethane, and the condensing surface air outlet links to each other with the import of thick silane purifying plant, and thick silane purifying plant outlet links to each other with an end of first valve and an end of second valve respectively; The other end of second valve links to each other with silicoethane liquefying plant inlet mouth; Silicoethane liquefying plant air outlet links to each other with an end of the 3rd valve and an end of the 4th valve respectively, and the other end of the 4th valve links to each other with silicoethane purifying plant inlet mouth, and the other end of the first valve the other end and the 3rd valve links to each other with the inlet mouth of the dark purifying plant of silane.
Described thick silane purifying plant is that placed in-line two or more diameters are 30cm～40cm, the stainless steel vessel of high 2.5m～3m, and the 4A molecular sieve of 1000 weight parts～1200 weight parts is housed.
Described silicoethane liquefying plant is a stainless steel vessel, and diameter is 12～15cm, and height is 50～80cm.
Described silicoethane purifying plant is placed in-line two or more stainless steel vessels, and diameter is 10～15cm, and height is 1.5～2.0m.And 5A and two kinds of molecular sieves of 13X of 100 weight parts～120 weight parts are housed.The 5A molecular sieve accounts for 90%～92% of inventory, and 13X accounts for 8%～10% of inventory.
Produce high-purity silicoethane method be: the compound of the magnesium silicide of 25～30 weight parts and 75～85 weight part ammonium chlorides is added in the reaction kettle; Add 300～350 weight part liquid ammonias again; And fully stir, temperature of reaction is-20～-25 ℃, reaction pressure is 0.2～0.25Mpa; Obtain three kinds of gaseous substances, i.e. the ammonia of the silicoethane of 9～9.5 weight part silane and 0.1～0.3 weight part and 10-11 weight part; The import that silane, silicoethane and ammonia pass through condensing surface from the air outlet of reaction kettle gets into condensing surface; The temperature of condensing surface is-75 ℃～-80 ℃; Pressure is 0.2～0.25MPa; 99%～99.5% gaseous ammonia liquefy ammonia after the process condensation, liquid ammonia is back to reaction kettle through second opening for feed of reaction kettle; Silane, silicoethane and a small amount of gaseous ammonia get into thick silane purification and put, and a small amount of gaseous ammonia is fully by the 4A molecular sieve adsorption; Silane, silicoethane get into the silicoethane liquefying plant from thick silane purifying plant outlet; Silicoethane becomes liquid state by gaseous state; Silicoethane liquefying-point be-14.5 ℃; The working temperature of cooling agent is-90～-110 ℃ in the silicoethane liquefying plant, and silane is purified from the dark purifying plant of outlet entering silane of silicoethane liquefying plant and is high purity silane; Silicoethane becomes fluent meterial to be stayed in the silicoethane liquefying plant, thereby reaches silane and the abundant isolating purpose of silicoethane; In the time that silicoethane liquefaction bottle is collected the silicoethane of 1 weight part; Close second valve and the 3rd valve; Open first valve, and let the silicoethane liquefying plant separate with cooling agent, the silicoethane liquefying plant heats up gradually;, opens the pressure of silicoethane liquefying plant the 4th valve when reaching 0.1～0.2MPa; B silane gas gets into the silicoethane purifying plant from the silicoethane liquefying plant and purifies, and exports the high-purity silicoethane that obtains 0.1～0.2 weight part from the silicoethane purifying plant, and each items such as high-purity silicoethane foreign matter content oxygen, nitrogen, carbon monoxide, carbonic acid gas, methane, water are carried mark and all are lower than 1 * 10
-5, hydrogenate each item of III-V family element is carried mark and all is lower than 1 * 10
-9
The beneficial effect that the present invention compared with prior art has:
1) silicoethane is just produced a kind of pair of product in the silane process, less investment, energy consumption is low, silicoethane production cost very low.
2) the high O of silicoethane purity
2, H
2O, N
2, CO
2, CO, CH
4Deng impurity all 1 * 10
-5Below, the hydrogenate of III, V group element can drop to 1 * 10
-9Below.
3) calculate with the industrial scale of producing 50 tons of silane per year, the silicoethane YO can reach 500～600 kilograms.Continuous development along with science and technology; In case silicoethane demand rise rapidly; If to improve silicoethane year production level; As long as change the processing condition of production silane such as the synthesis temperature of magnesium silicide, the temperature of reaction of silane reaction still ... Deng just can improve by a relatively large margin silicoethane throughput.
Description of drawings
Accompanying drawing is to produce high-purity silicoethane system architecture synoptic diagram.
Embodiment
The reaction formula of reaction kettle of the present invention is:
a、
b、2Mg
2Si+8NH
4Cl→4MgCl
2+Si
2H
6+H
2+8NH
3
Shown in accompanying drawing, produce high-purity silicoethane system comprise the dark purifying plant of magnesium silicide and ammonium chloride feeding device 1, liquefied ammonia storage tank 2, reaction kettle 3, condensing surface 4, thick silane purifying plant 5, silane 6, silicoethane liquefying plant 7, silicoethane purifying plant 8, first valve 9, second valve 10, the 3rd valve 11 and the 4th valve 12; Magnesium silicide links to each other with reaction kettle 3 the 1st opening for feed with ammonium chloride feeding device 1; Liquefied ammonia storage tank 2 links to each other with reaction kettle 3 the 2nd opening for feed; Condensing surface, ammonia refluxing opening and link to each other with reaction kettle 3 the 2nd opening for feed; Outlet links to each other with condensing surface 4 inlet mouths reaction kettle 3 silane with silicoethane, and condensing surface 4 air outlets link to each other with thick silane purifying plant 5 imports, and thick silane purifying plant 5 outlets link to each other with an end of first valve 9 and an end of second valve 10 respectively; The other end of second valve 10 links to each other with silicoethane liquefying plant 7 inlet mouths; Silicoethane liquefying plant 7 air outlets link to each other with an end of the 3rd valve 11 and an end of the 4th valve 12 respectively, and the other end of the 4th valve 12 links to each other with silicoethane purifying plant 8 inlet mouths, and the other end of first valve, 9 the other ends and the 3rd valve 11 links to each other with the inlet mouth of the dark purifying plant 6 of silane.
Described thick silane purifying plant 5 is 30cm～40cm for placed in-line two or more diameters, the stainless steel vessel of high 2.5m～3m, and the 4A molecular sieve of 1000 weight parts～1200 weight parts is housed.
Described silicoethane liquefying plant 7 is a stainless steel vessel, and diameter is 12～15cm, and height is 50～80cm.
Described silicoethane purifying plant 8 is placed in-line two or more stainless steel vessels, and diameter is 10～15cm, and height is 1.5～2.0m.And 5A and two kinds of molecular sieves of 13X of 100 weight parts are housed.The 5A molecular sieve accounts for 90%～92% of inventory, and 13X accounts for 8%～10% of inventory.
Produce high-purity silicoethane method be: the compound of the magnesium silicide of 25～30 weight parts and 75～85 weight part ammonium chlorides is added in the reaction kettle 3; Add 300～350 weight part liquid ammonias again; And fully stir, temperature of reaction is-20～-25 ℃, reaction pressure is 0.2～0.25Mpa; Obtain three kinds of gaseous substances, i.e. the ammonia of the silicoethane of 9～9.5 weight part silane and 0.1～0.3 weight part and 10-11 weight part; The import that silane, silicoethane and ammonia pass through condensing surface 4 from the air outlet of reaction kettle 3 gets into condensing surface; The temperature of condensing surface is-75 ℃～-80 ℃; Pressure is 0.2～0.25MPa; Through 99%～99.5% gaseous ammonia liquefy ammonia after the condensation, second opening for feed through liquid ammonia reaction kettle 3 is back to reaction kettle; Silane, silicoethane and a small amount of gaseous ammonia get into thick silane purification and put 5, and a small amount of gaseous ammonia is fully by the 4A molecular sieve adsorption; Silane, silicoethane are purified from thick silane and are put 5 outlet entering silicoethane liquefying plants 7; Silicoethane becomes liquid state by gaseous state; Silicoethane liquefying-point be-14.5 ℃; The working temperature of cooling agent is-90～-110 ℃ in the silicoethane liquefying plant 7, and silane is purified from the dark purifying plant 6 of outlet entering silane of silicoethane liquefying plant 7 and is high purity silane; Silicoethane becomes fluent meterial to be stayed in the silicoethane liquefying plant 7, thereby reaches silane and the abundant isolating purpose of silicoethane; In the time that silicoethane liquefaction bottle is collected the silicoethane of 1 weight part; Close second valve 10 and the 3rd valve 11; Open first valve 9, and let silicoethane liquefying plant 7 separate with cooling agent, silicoethane liquefying plant 7 heats up gradually;, opens the pressure of silicoethane liquefying plant 7 the 4th valve 12 when reaching 0.1～0.2MPa; B silane gas gets into silicoethane purifying plant 8 from silicoethane liquefying plant 7 and purifies, and exports the high-purity silicoethane that obtains 0.1～0.2 weight part from silicoethane purifying plant 8, and each items such as high-purity silicoethane foreign matter content oxygen, nitrogen, carbon monoxide, carbonic acid gas, methane, water are carried mark and all are lower than 1 * 10
-5, hydrogenate each item of III-V family element is carried mark and all is lower than 1 * 10
-9
Close No. 9 and No. 12 valves, open No. 10 and No. 11 valves.The compound of 25 kilograms of magnesium silicides and 75 kilograms of ammonium chlorides is slowly added the silane reaction still, and in reaction kettle, add 350 kilograms liquefied ammonia gradually, start whisking appliance and fully stir.Temperature of reaction is-20 ℃, and the WP of reaction kettle is 0.2MPa.Gaseous substance silane, silicoethane and ammonia that reaction kettle produces carry out condensing surface from the outlet of reaction kettle.The temperature of condensing surface is-78 ℃.Gaseous ammonia becomes liquid ammonia and returns reaction kettle.Silane, silicoethane get into the silicoethane liquefying plant after the thick silane purifying plant of silane is purified, silicoethane is under-90～-110 ℃ of low temperature, and liquefy is stayed in the liquefaction bottle.Silane is still gaseous state, and gaseous silane gets into the dark purifying plant of silane by the outlet of silicoethane liquefaction bottle.
The total system operation is after 2 hours; Close valve No. 10, No. 11; Open No. 9 valve, silicoethane liquefaction bottle is separated with refrigerator, let silicoethane liquefaction bottle temperature go up gradually; Pressure reaches opens No. 12 valves behind 0.1MPa～0.2MPa, and we collect that to obtain high-purity silicoethane be 0.1 kilogram to silicoethane in its exit behind dark purifying plant.
Close No. 9 and No. 12 valves, open No. 10 and No. 11 valves.The compound of 50 kilograms of magnesium silicides and 150 kilograms of ammonium chlorides is slowly added the silane reaction still, and in reaction kettle, add 700 kilograms liquefied ammonia gradually, start whisking appliance and fully stir.Temperature of reaction is-20 ℃, and the WP of reaction kettle is 0.2MPa.Gaseous substance silane, silicoethane and ammonia that reaction kettle produces carry out condensing surface from the outlet of reaction kettle.The temperature of condensing surface is-78 ℃.Gaseous ammonia becomes liquid ammonia and returns reaction kettle.Silane, silicoethane get into the silicoethane liquefying plant after the thick silane purifying plant of silane is purified, silicoethane is under-90～-110 ℃ of low temperature, and liquefy is stayed in the liquefaction bottle.Silane is still gaseous state, and gaseous silane gets into the dark purifying plant of silane by the outlet of silicoethane liquefaction bottle.
The total system operation is after 4 hours; Close valve No. 10, No. 11; Open No. 9 valve, silicoethane liquefaction bottle is separated with refrigerator, let silicoethane liquefaction bottle temperature go up gradually; Pressure reaches opens No. 12 valves behind 0.1MPa～0.2MPa, and we collect that to obtain high-purity silicoethane be 0.2 kilogram to silicoethane in its exit behind dark purifying plant.
Embodiment 3
Close No. 9 and No. 12 valves, open No. 10 and No. 11 valves.The compound of 250 kilograms of magnesium silicides and 750 kilograms of ammonium chlorides is slowly added the silane reaction still, and in reaction kettle, add 3500 kilograms liquefied ammonia gradually, start whisking appliance and fully stir.Temperature of reaction is-20 ℃, and the WP of reaction kettle is 0.2MPa.Gaseous substance silane, silicoethane and ammonia that reaction kettle produces carry out condensing surface from the outlet of reaction kettle.The temperature of condensing surface is-78 ℃.Gaseous ammonia becomes liquid ammonia and returns reaction kettle.Silane, silicoethane get into the silicoethane liquefying plant after the thick silane purifying plant of silane is purified, silicoethane is under-90～-110 ℃ of low temperature, and liquefy is stayed in the liquefaction bottle.Silane is still gaseous state, and gaseous silane gets into the dark purifying plant of silane by the outlet of silicoethane liquefaction bottle.
The total system operation is after 20 hours; Close valve No. 10, No. 11; Open No. 9 valve, silicoethane liquefaction bottle is separated with refrigerator, let silicoethane liquefaction bottle temperature go up gradually; Pressure reaches opens No. 12 valves behind 0.1MPa～0.2MPa, and we collect that to obtain high-purity silicoethane be 1 kilogram to silicoethane in its exit behind dark purifying plant.
Claims (5)
- One kind produce high-purity silicoethane system, it is characterized in that comprising magnesium silicide and ammonium chloride feeding device (1), liquefied ammonia storage tank (2), reaction kettle (3), condensing surface (4), thick silane purifying plant (5), the dark purifying plant of silane (6), silicoethane liquefying plant (7), silicoethane purifying plant (8), first valve (9), second valve (10), the 3rd valve (11) and the 4th valve (12); Magnesium silicide links to each other with reaction kettle (3) the 1st opening for feed with ammonium chloride feeding device (1); Liquefied ammonia storage tank (2) links to each other with reaction kettle (3) the 2nd opening for feed; Condensing surface (4) ammonia refluxing opening with link to each other with reaction kettle (3) the 2nd opening for feed; Outlet links to each other with condensing surface (4) inlet mouth reaction kettle (3) silane with silicoethane; Condensing surface (4) air outlet links to each other with thick silane purifying plant (5) import; Thick silane purifying plant (5) outlet links to each other with an end of first valve (9) and an end of second valve (10) respectively, and the other end of second valve (10) links to each other with silicoethane liquefying plant (7) inlet mouth, and silicoethane liquefying plant (7) air outlet links to each other with an end of the 3rd valve (11) and an end of the 4th valve (12) respectively; The other end of the 4th valve (12) links to each other with silicoethane purifying plant (8) inlet mouth, and the other end of first valve (9) the other end and the 3rd valve (11) links to each other with the inlet mouth of the dark purifying plant of silane (6).
- 2. according to claim 1 a kind of produce high-purity silicoethane system; It is characterized in that described thick silane purifying plant (5) is 30cm～40cm for placed in-line two or more diameters; The stainless steel vessel of high 2.5m～3m, and the 4A molecular sieve of 1000 weight parts～1200 weight parts is housed.
- 3. according to claim 1 a kind of produce high-purity silicoethane system, it is characterized in that described silicoethane liquefying plant (7) is a stainless steel vessel, diameter is 12～15cm, height is 50～80cm.
- 4. according to claim 1 a kind of produce high-purity silicoethane system; It is characterized in that described silicoethane purifying plant (8) is placed in-line two or more stainless steel vessels; Diameter is 10～15cm, and height is 1.5～2.0 m, and 5A and two kinds of molecular sieves of 13X of 100 weight parts are housed; The 5A molecular sieve accounts for 90%～92% of inventory, and 13X accounts for 8%～10% of inventory.
- The high-purity silicoethane of production that uses system according to claim 1 method; It is characterized in that the magnesium silicide of 25～30 weight parts and the compound of 75～85 weight part ammonium chlorides are added in the reaction kettle (3), add 300～350 weight part liquid ammonias again, and fully stir; Temperature of reaction is-20～-25 ℃; Reaction pressure is 0.2～0.25Mpa, obtains three kinds of gaseous substances, i.e. the ammonia of the silicoethane of 9～9.5 weight part silane and 0.1～0.3 weight part and 10-11 weight part; The import that silane, silicoethane and ammonia pass through condensing surface (4) from the air outlet of reaction kettle (3) gets into condensing surface; The temperature of condensing surface is-75 ℃～-80 ℃; Pressure is 0.2～0.25MPa; 99%～99.5% gaseous ammonia liquefy ammonia after the process condensation, liquid ammonia is back to reaction kettle through second opening for feed of reaction kettle (3); Silane, silicoethane and a small amount of gaseous ammonia get into thick silane purification and put (5), and a small amount of gaseous ammonia is fully by the 4A molecular sieve adsorption; Silane, silicoethane are purified from thick silane and are put (5) outlet entering silicoethane liquefying plant (7); Silicoethane becomes liquid state by gaseous state; Silicoethane liquefying-point be-14.5 ℃; The working temperature of cooling agent is-90～-110 ℃ in the silicoethane liquefying plant (7), and silane is purified from the outlet entering dark purifying plant of silane (6) of silicoethane liquefying plant (7) and is high purity silane; Silicoethane becomes fluent meterial to be stayed in the silicoethane liquefying plant (7), thereby reaches silane and the abundant isolating purpose of silicoethane; In the time that silicoethane liquefaction bottle is collected the silicoethane of 1 weight part; Close second valve (10) and the 3rd valve (11); Open first valve (9), and let silicoethane liquefying plant (7) separate with cooling agent, silicoethane liquefying plant (7) heats up gradually;, opens the pressure of silicoethane liquefying plant (7) the 4th valve (12) when reaching 0.1～0.2MPa; B silane gas gets into silicoethane purifying plant (8) from silicoethane liquefying plant (7) and purifies, and exports the high-purity silicoethane that obtains 0.1～0.2 weight part from silicoethane purifying plant (8), and each items such as high-purity silicoethane foreign matter content oxygen, nitrogen, carbon monoxide, carbonic acid gas, methane, water are carried mark and all are lower than 1 * 10 -5, hydrogenate each item of III-group is carried mark and all is lower than 1 * 10 -9
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Cited By (11)
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|---|---|---|---|---|
| CN102936014A (en) * | 2012-10-22 | 2013-02-20 | 贺孝鸣 | Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia |
| CN103529132A (en) * | 2012-07-02 | 2014-01-22 | 福州市产品质量检验所 | Gas detection pretreatment device and gas detection method |
| US8865850B2 (en) | 2012-06-14 | 2014-10-21 | Dow Corning Corporation | Method of selectively forming a reaction product in the presence of a metal silicide |
| CN105800616A (en) * | 2016-05-09 | 2016-07-27 | 浙江迅鼎半导体材料科技有限公司 | Method for preparing disilane |
| CN106115718A (en) * | 2016-06-25 | 2016-11-16 | 浙江迅鼎半导体材料科技有限公司 | A kind of Disilicoethane process units |
| CN106145119A (en) * | 2016-06-25 | 2016-11-23 | 浙江迅鼎半导体材料科技有限公司 | A kind of disilane reactor |
| CN109626379A (en) * | 2017-10-09 | 2019-04-16 | 烟台万华电子材料有限公司 | Alloying compound reacts the method and apparatus of production silanes product with ammonium chloride in liquefied ammonia |
| CN112694091A (en) * | 2021-02-25 | 2021-04-23 | 刘振宇 | Electronic gas preparation system and method based on chip and intelligent manufacturing |
| CN112723359A (en) * | 2020-12-30 | 2021-04-30 | 烟台万华电子材料有限公司 | Method and system for preparing disilane by reaction of multi-metal silicide and ammonium chloride |
| CN112858555A (en) * | 2021-01-08 | 2021-05-28 | 烟台万华电子材料有限公司 | Analysis method of high-purity disilane |
| CN114715900A (en) * | 2022-05-18 | 2022-07-08 | 北京化工大学 | Continuous production preparation system and production process of electronic-grade disilane |
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