CN108179387A - A kind of preparation method of copper indium gallium selenide base system row target - Google Patents
A kind of preparation method of copper indium gallium selenide base system row target Download PDFInfo
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- CN108179387A CN108179387A CN201711455520.1A CN201711455520A CN108179387A CN 108179387 A CN108179387 A CN 108179387A CN 201711455520 A CN201711455520 A CN 201711455520A CN 108179387 A CN108179387 A CN 108179387A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
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- Photovoltaic Devices (AREA)
Abstract
The present invention provides a kind of preparation methods of copper indium gallium selenide base system row target, material powder cold prepressing has first been subjected at a certain pressure, material forming can not only be made, and phenomenon of dusting will not be caused when hot pressing, there is facilitation for the consistency for improving copper indium gallium selenide base system row target.Simultaneously, material powder is that the heating of specific temperature twice and the heat preservation of specific time have been carried out under specific vacuum degree, then heat-insulating pressurizing is carried out under pressure, after heat preservation decompression, specific temperature is cooled to depressurize again, the purity and consistency of copper indium gallium selenide base system row target are not only increased, and effectively increases the compression strength of copper indium gallium selenide base system row target.The experimental results showed that the purity of copper indium gallium selenide base system row target being prepared, in more than 5N, consistency is not less than 98.0%, and impurity content is no more than 3.16ppm.
Description
Technical field
Technical field more particularly to a kind of preparation side of copper indium gallium selenide base system row target the present invention relates to sputtering target material
Method.
Background technology
Copper-indium-galliun-selenium film solar cell has the notable spies such as production cost is low, pollution is small, do not fail, dim light performance is good
Point, photoelectric conversion efficiency are occupied first of various thin film solar cells, close to crystal-silicon solar cell, and cost be crystalline silicon too
/ 3rd of positive electricity pond are referred to as next-generation very promising novel thin film solar cell.
At present, the major technique for preparing CIGS thin-film is sputtering method, and the source material of sputter-deposited thin films is target,
The film consistency deposited with target as sputter is high, and adhesion is good.Copper indium gallium selenide base system row target includes copper and indium target, copper gallium target
With copper and indium gallium target.For target, mainly there are two aspects to influence its quality：1st, the purity of target, the impurities affect of target
The uniformity of film；2nd, high-compactness, high-compactness target have many advantages, such as that conductive, thermal conductivity is good, intensity is high, use this target
Material plated film, sputtering power is small, and rate of film build is high, and film is not easy to crack, and target service life is long.
Therefore, the CIGS thin-film of high quality is obtained, it is necessary to obtain high performance copper indium gallium selenide base system row target.
Invention content
In view of this, the technical problem to be solved in the present invention is to provide a kind of preparation side of copper indium gallium selenide base system row target
Method, the purity and consistency for the copper indium gallium selenide base system row target that this preparation method obtains are higher.
The present invention provides a kind of preparation method of copper indium gallium selenide base system row target, including：
A material powder under 5~10MPa) is subjected to cold prepressing, obtains the powder after cold prepressing；The material powder is
Copper and indium mixed powder, copper gallium mixed powder or copper and indium gallium mixed powder；
B) under conditions of vacuum degree is less than 3Pa, the powder after the cold prepressing is first warming up to 300~400 for the first time
DEG C, 0.2~0.8h is kept the temperature for the first time；It is warming up to 600~700 DEG C for the second time again, after second keeps the temperature 55~65min, starts to protect
Temperature pressurization, then heat preservation decompression；The pressure of the heat-insulating pressurizing is 45~60MPa；
C) after the heat preservation decompression, 100~300 DEG C is cooled the temperature to, is then depressurized, obtains copper indium gallium selenide base system row target
Material.
Preferably, the granularity of the material powder is less than 100 mesh.
Preferably, the temperature of the cold prepressing is 25 DEG C~45 DEG C.
Preferably, step B) in, the vacuum degree is 0.1Pa.
Preferably, the rate of the first time heating is 1~5 DEG C/min.
Preferably, the rate of second of heating is 5~8 DEG C/min.
Preferably, the heat-insulating pressurizing, then heat preservation decompression are specially：
After the heat-insulating pressurizing, the pressure of the heat-insulating pressurizing is laid down, under conditions of heat preservation, carries out nature decompression；
Temperature of the temperature of the heat preservation for second of heat preservation.
Preferably, the time of the heat-insulating pressurizing is 80~120min；The time of the heat preservation decompression is 40~135min.
Preferably, step C) in, the pressure after the decompression is 5~10MPa.
Preferably, step C) in, it is further included after the decompression and is cooled to less than 35 DEG C.
The present invention provides a kind of preparation method of copper indium gallium selenide base system row target, including：
A material powder under 5~10MPa) is subjected to cold prepressing, obtains the powder after cold prepressing；The material powder is
Copper and indium mixed powder, copper gallium mixed powder or copper and indium gallium mixed powder；
B) under conditions of vacuum degree is less than 3Pa, the powder after the cold prepressing is first warming up to 300~400 for the first time
DEG C, 0.2~0.8h is kept the temperature for the first time；It is warming up to 600~700 DEG C for the second time again, after second keeps the temperature 55~65min, starts to protect
Temperature pressurization, then heat preservation decompression；The pressure of the heat-insulating pressurizing is 45~60MPa；
C) after the heat preservation decompression, 100~300 DEG C is cooled the temperature to, is then depressurized, obtains copper indium gallium selenide base system row target
Material.
Material powder has first been carried out cold prepressing by the present invention at a certain pressure, can not only make material forming, but also
Phenomenon of dusting will not be caused when hot pressing, have facilitation for the consistency for improving copper indium gallium selenide base system row target.Together
When, material powder is that the heating of specific temperature twice and the heat preservation of specific time, Ran Hou have been carried out under specific vacuum degree
Heat-insulating pressurizing is carried out under certain pressure, after heat preservation decompression, specific temperature is cooled to and depressurizes again, not only increase copper indium gallium selenide base
The purity and consistency of serial target, and the compression strength of copper indium gallium selenide base system row target is effectively increased, meanwhile, target
It is combined between crystal grain, even particle size distribution, crystallite dimension is small, and the quality of plated film is higher.The experimental results showed that be prepared
The purity of copper indium gallium selenide base system row target is in more than 5N, and consistency is not less than 98.0%, and impurity content is no more than 3.16ppm, copper
The crystallite dimension of indium gallium seleno series target is less than 40 μm.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's all other embodiments obtained without making creative work, belong to this hair
The range of bright protection.
The present invention provides a kind of preparation method of copper indium gallium selenide base system row target, including：
A material powder under 5~10MPa) is subjected to cold prepressing, obtains the powder after cold prepressing；The material powder is
Copper and indium mixed powder, copper gallium mixed powder or copper and indium gallium mixed powder；
B) under conditions of vacuum degree is less than 3Pa, the powder after the cold prepressing is first warming up to 300~400 for the first time
DEG C, 0.2~0.8h is kept the temperature for the first time；It is warming up to 600~700 DEG C for the second time again, after second keeps the temperature 55~65min, starts to protect
Temperature pressurization, then heat preservation decompression；The pressure of the heat-insulating pressurizing is 45~60MPa；
C) after the heat preservation decompression, 100~300 DEG C is cooled the temperature to, is then depressurized, obtains copper indium gallium selenide base system row target
Material.
The material powder is copper and indium mixed powder, copper gallium mixed powder or copper and indium gallium mixed powder.The present invention is to described
The source of material powder has no special limitation, can be general commercially available.The granularity of the material powder is preferably smaller than 100 mesh.
Material powder is first carried out cold prepressing by the present invention under 5~10MPa, obtains the powder after cold prepressing.It is specifically, excellent
It is selected as：Material powder is packed into mold, cold prepressing is carried out under 5~10MPa, obtains the powder after cold prepressing.The cold prepressing
Pressure be 5~10MPa.In certain embodiments of the present invention, the pressure of the cold prepressing is 7MPa, 8MPa or 10MPa.Institute
The temperature for stating cold prepressing is preferably 25 DEG C~45 DEG C.The mold is preferably graphite jig.The cold prepressing is preferably in Vacuum Heat
It is carried out in pressure stove.Material powder has first been carried out cold prepressing by the present invention at a certain pressure, can not only make material forming, and
And phenomenon of dusting will not be caused when hot pressing, there is facilitation for the consistency for improving copper indium gallium selenide base system row target,
Meanwhile conducive to the combination between target crystalline grains, promote even particle size distribution, reduce crystallite dimension.
After obtaining the powder after cold prepressing, the powder after the cold prepressing is subjected to vacuum heating-press sintering.Specially：True
Reciprocal of duty cycle is less than under conditions of 3Pa, and the powder after the cold prepressing is first warming up to 300~400 DEG C for the first time, is kept the temperature for the first time
0.2~0.8h；It is warming up to 600~700 DEG C for the second time again, after second keeps the temperature 55~65min, starts heat-insulating pressurizing, Ran Houbao
Temperature drop pressure.
The vacuum degree is less than 3Pa, preferably 0.1~3Pa.In certain embodiments of the present invention, the vacuum degree is
0.1Pa。
The temperature of the first time heating is 300~400 DEG C.In certain embodiments of the present invention, the first time liter
The temperature of temperature is 300 DEG C or 350 DEG C.The rate of the first time heating is preferably 1~5 DEG C/min.In certain realities of the present invention
It applies in example, the rate that the first time heats up is 2 DEG C/min, 3 DEG C/min or 5 DEG C/min.The temperature of first time heat preservation with
The temperature of the first time heating is identical.The time of the first time heat preservation is 0.2~0.8h.In certain embodiments of the present invention
In, the time of the first time heat preservation is 0.5h, 0.6h or 0.8h.
The temperature of second of heating is 600~700 DEG C.In certain embodiments of the present invention, described second liter
The temperature of temperature is 600 DEG C, 650 DEG C or 700 DEG C.The rate of second of heating is preferably 5~8 DEG C/min.The present invention's
In some embodiments, second of rate to heat up is 5 DEG C/min, 7 DEG C/min or 8 DEG C/min.Second of heat preservation
Temperature is identical with the temperature of second of heating.The time of second of heat preservation is 55~65min.In the certain of the present invention
In embodiment, the time of second of heat preservation is 60min or 65min.
The heating of the present invention is two sections, and two sections of heatings are the consistency that target is improved to preferably be vented, meanwhile, it is right
The purity and compression strength for improving target have facilitation.The hop count that heats up, which increases, either to be reduced, and can all cause the densification of target
Degree reduces, meanwhile, purity, compression strength and the crystallite dimension and size distribution of target can also be affected.
After second of heat preservation, 55~65min, start heat-insulating pressurizing, then heat preservation decompression.
Specifically, the heat-insulating pressurizing, then heat preservation decompression are preferably：
After the heat-insulating pressurizing, the pressure of the heat-insulating pressurizing is laid down, under conditions of heat preservation, carries out nature decompression；
Temperature of the temperature of the heat preservation for second of heat preservation.
In the present invention, the pressure of the heat-insulating pressurizing is 45~60MPa.In certain embodiments of the present invention, it is described
The pressure of heat-insulating pressurizing is 55MPa, 58MPa or 60MPa.The time of the heat-insulating pressurizing is preferably 80~120min.In this hair
In bright some embodiments, the time of the heat-insulating pressurizing is 80min, 100min or 120min.
The time of the heat preservation decompression is preferably 40~135min.In certain embodiments of the present invention, the heat preservation drop
The time of pressure is 40min, 55min or 135min.
After the heat preservation decompression, 100~300 DEG C are cooled the temperature to, is then depressurized, obtains copper indium gallium selenide base system row target.
In the present invention, it is described cool the temperature to 100~300 DEG C preferably naturally be depressured under conditions of carry out.The present invention is to the temperature
The rate of temperature fall that degree is down to 100~300 DEG C has no special limitation, the preferred natural cooling of the present invention.
The present invention first cools the temperature to 100~300 DEG C, then depressurizes again, and the crystallite dimension of acquisition is smaller, meanwhile, favorably
Combination between crystal grain promotes epigranular distribution, has facilitation for the consistency and compression strength that improve target.
In certain embodiments of the present invention, after the heat preservation decompression, 150 DEG C or 250 DEG C are cooled the temperature to.Pressure after the decompression is excellent
It is selected as 5~10MPa.In certain embodiments of the present invention, the pressure after the decompression is 8MPAa or 10MPa.
After the decompression, cooling is preferably further included.The temperature of the cooling is preferably less than 35 DEG C.
After the cooling, demoulding is preferably further included, obtains thick target.The thick target is obtained into preferably through mechanical processing
The copper indium gallium selenide base system row target of product.
The present invention provides a kind of preparation method of copper indium gallium selenide base system row target, including：
A material powder under 5~10MPa) is subjected to cold prepressing, obtains the powder after cold prepressing；The material powder is
Copper and indium mixed powder, copper gallium mixed powder or copper and indium gallium mixed powder；
B) under conditions of vacuum degree is less than 3Pa, the powder after the cold prepressing is first warming up to 300~400 for the first time
DEG C, 0.2~0.8h is kept the temperature for the first time；It is warming up to 600~700 DEG C for the second time again, after second keeps the temperature 55~65min, starts to protect
Temperature pressurization, then heat preservation decompression；The pressure of the heat-insulating pressurizing is 45~60MPa；
C) after the heat preservation decompression, 100~300 DEG C is cooled the temperature to, is then depressurized, obtains copper indium gallium selenide base system row target
Material.
Material powder has first been carried out cold prepressing by the present invention at a certain pressure, can not only make material forming, but also
Phenomenon of dusting will not be caused when hot pressing, have facilitation for the consistency for improving copper indium gallium selenide base system row target.Together
When, material powder is that the heating of specific temperature twice and the heat preservation of specific time, Ran Hou have been carried out under specific vacuum degree
Heat-insulating pressurizing is carried out under certain pressure, after heat preservation decompression, specific temperature is cooled to and depressurizes again, not only increase copper indium gallium selenide base
The purity and consistency of serial target, and the compression strength of copper indium gallium selenide base system row target is effectively increased, meanwhile, target
It is combined between crystal grain, even particle size distribution, crystallite dimension is small, and the quality of plated film is higher.The experimental results showed that be prepared
The purity of copper indium gallium selenide base system row target is in more than 5N, and consistency is not less than 98.0%, and impurity content is no more than 3.16ppm, copper
The crystallite dimension of indium gallium seleno series target is less than 40 μm.
In order to further illustrate the present invention, with reference to embodiments to a kind of copper indium gallium selenide base system row target provided by the invention
The preparation method of material is described in detail, but cannot be understood as limiting the scope of the present invention.
Raw material used in following embodiment is commercially available.
Embodiment 1
The copper and indium mixed powder that granularity is less than to 100 mesh is fitted into graphite jig, is flattened with tenderizer, is put into vacuum hotpressing
In stove.Opening pressure system is pressurizeed, and cold prepressing, pressure 8Mpa are carried out to powder.Hot pressing furnace is vacuumized, works as vacuum degree
After reaching 0.1pa, heating is opened, 350 DEG C are warming up to 2 DEG C/min.Keep the temperature 0.8h.Continue to heat up, be warming up to 7 DEG C/min
700 DEG C, 65min is kept the temperature, then, starts to pressurize under the conditions of 700 DEG C, moulding pressure 60Mpa keeps 100min.Lay down institute
The pressure of heat-insulating pressurizing is stated, under conditions of heat preservation, carries out nature decompression.Naturally the time being depressured is 135min.Then,
Cool down under conditions of being depressured naturally, after temperature is down to 250 DEG C, start to depressurize, it is naturally cold after pressure is down to 10MPa
But to less than 35 DEG C.Fire door is opened, after demoulding, thick target is obtained, finished product copper and indium target is obtained through over mechanical processing.
Obtained finished product target metallographic microscope is measured into crystallite dimension, obtains, is combined between the crystal grain of target, grain
Degree is evenly distributed, and crystallite dimension is less than 40 microns, and therefore, the quality of institute's plated film is higher.
Embodiment 2
The copper gallium mixed powder that granularity is less than to 100 mesh is fitted into graphite jig, is flattened with tenderizer, is put into vacuum hotpressing
In stove.Opening pressure system is pressurizeed, and cold prepressing, pressure 10Mpa are carried out to powder.Hot pressing furnace is vacuumized, works as vacuum
After degree reaches 0.1pa, heating is opened, 300 DEG C are warming up to 5 DEG C/min.Keep the temperature 0.6h.Continue to heat up, be warming up to 5 DEG C/min
600 DEG C, 60min is kept the temperature, then, starts to pressurize under the conditions of 600 DEG C, moulding pressure 55Mpa keeps 80min.It lays down described
The pressure of heat-insulating pressurizing under conditions of heat preservation, carries out nature decompression.Naturally the time being depressured is 40min.Then, exist
Naturally cool down under conditions of being depressured, after temperature is down to 150 DEG C, start to depressurize, after pressure is down to 8MPa, naturally cool to
Less than 35 DEG C.Fire door is opened, after demoulding, thick target is obtained, finished product copper gallium target is obtained through over mechanical processing.
Obtained finished product target metallographic microscope is measured into crystallite dimension, obtains, is combined between the crystal grain of target, grain
Degree is evenly distributed, and crystallite dimension is less than 40 microns, and therefore, the quality of institute's plated film is higher.
Embodiment 3
The copper and indium gallium mixed powder that granularity is less than to 100 mesh is fitted into graphite jig, is flattened with tenderizer, is put into Vacuum Heat
It presses in stove.Opening pressure system is pressurizeed, and cold prepressing, pressure 7Mpa are carried out to powder.Hot pressing furnace is vacuumized, works as vacuum
After degree reaches 0.1pa, heating is opened, 350 DEG C are warming up to 3 DEG C/min.Keep the temperature 0.5h.Continue to heat up, be warming up to 8 DEG C/min
650 DEG C, 65min is kept the temperature, then, starts to pressurize under the conditions of 650 DEG C, moulding pressure 58Mpa keeps 120min.Lay down institute
The pressure of heat-insulating pressurizing is stated, under conditions of heat preservation, carries out nature decompression.Naturally the time being depressured is 55min.Then,
Cool down under conditions of being depressured naturally, after temperature is down to 250 DEG C, start to depressurize, after pressure is down to 8MPa, natural cooling
To less than 35 DEG C.Fire door is opened, after demoulding, thick target is obtained, finished product copper and indium gallium target is obtained through over mechanical processing.
Obtained finished product target metallographic microscope is measured into crystallite dimension, obtains, is combined between the crystal grain of target, grain
Degree is evenly distributed, and crystallite dimension is less than 40 microns, and therefore, the quality of institute's plated film is higher.
Embodiment 4
Examples 1 to 3 is obtained respectively using drainage and ICP-OES (inductive coupling plasma emission spectrograph)
Finished product target carries out consistency detection and impurity content detection, and the results are shown in Table 1.
The consistency of the finished product target of 1 Examples 1 to 3 of table and impurity content (ppm)
From table 1, it can be seen that the consistency of copper indium gallium selenide base system row target produced by the present invention is not less than 98.0%,
Impurity content is no more than 3.16ppm, and the purity of copper indium gallium selenide base system row target is in more than 5N.
The explanation of above example is only intended to facilitate the understanding of the method and its core concept of the invention.To these embodiments
A variety of modifications will be apparent for those skilled in the art, the general principles defined herein can be with
Without departing from the spirit or scope of the present invention, it realizes in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to the most wide model consistent with the principles and novel features disclosed herein
It encloses.
Claims (10)
1. a kind of preparation method of copper indium gallium selenide base system row target, including：
A material powder under 5~10MPa) is subjected to cold prepressing, obtains the powder after cold prepressing；The material powder is copper and indium
Mixed powder, copper gallium mixed powder or copper and indium gallium mixed powder；
B) under conditions of vacuum degree is less than 3Pa, the powder after the cold prepressing is first warming up to 300~400 DEG C for the first time, the
0.2~0.8h of primary heat preservation；It is warming up to 600~700 DEG C for the second time again, after second keeps the temperature 55~65min, starts heat preservation and add
Pressure, then heat preservation decompression；The pressure of the heat-insulating pressurizing is 45~60MPa；
C) after the heat preservation decompression, 100~300 DEG C is cooled the temperature to, is then depressurized, obtains copper indium gallium selenide base system row target.
2. preparation method according to claim 1, which is characterized in that the granularity of the material powder is less than 100 mesh.
3. preparation method according to claim 1, which is characterized in that the temperature of the cold prepressing is 25 DEG C~45 DEG C.
4. preparation method according to claim 1, which is characterized in that step B) in, the vacuum degree is 0.1Pa.
5. preparation method according to claim 1, which is characterized in that the rate of first time heating for 1~5 DEG C/
min。
6. preparation method according to claim 1, which is characterized in that the rate of second heating for 5~8 DEG C/
min。
7. preparation method according to claim 1, which is characterized in that the heat-insulating pressurizing, then heat preservation decompression are specially：
After the heat-insulating pressurizing, the pressure of the heat-insulating pressurizing is laid down, under conditions of heat preservation, carries out nature decompression；
Temperature of the temperature of the heat preservation for second of heat preservation.
8. preparation method according to claim 1, which is characterized in that the time of the heat-insulating pressurizing is 80~120min；
The time of the heat preservation decompression is 40~135min.
9. preparation method according to claim 1, which is characterized in that step C) in, pressure after the decompression for 5~
10MPa。
10. preparation method according to claim 1, which is characterized in that step C) in, it further includes and is cooled to after the decompression
Less than 35 DEG C.
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