CN109437884A - The preparation method of cadmium stannate target - Google Patents
The preparation method of cadmium stannate target Download PDFInfo
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- CN109437884A CN109437884A CN201811220400.8A CN201811220400A CN109437884A CN 109437884 A CN109437884 A CN 109437884A CN 201811220400 A CN201811220400 A CN 201811220400A CN 109437884 A CN109437884 A CN 109437884A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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- 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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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The present invention relates to a kind of preparation methods of cadmium stannate target comprising following steps: S1, raw material mixing；S2, ball milling；S3, isostatic cool pressing；S4, sintering.The preparation method of cadmium stannate target of the present invention prepares cadmium stannate target using the method that isostatic cool pressing and room temperature sintering combine, and is not necessarily to graphite crucible, will not introduce impurity, preparation-obtained cadmium stannate target is relatively denser in 95%, resistivity≤10 Ω cm.
Description
Technical field
The present invention relates to target preparation field more particularly to a kind of preparation methods of cadmium stannate target.
Background technique
Cadmium stannate (Cd2SnO4) it is a kind of ternary oxide, n-type semiconductor makes its tool due to its special electronic structure
There are many excellent optically and electrically characteristic, cadmium stannate has both broad-band gap, low-resistivity, high visible light transmissivity, higher current-carrying
The advantages such as transport factor, resistivity can be down to 10-6The Ω cm order of magnitude, average transmittance reaches 90% in visible-range
More than, it is a kind of transparent conductive material that comprehensive performance is outstanding, it is with the obvious advantage in field of solar energy, a variety of sun can be become
The substitute of energy thin-film material, market prospects are very good.
Sputtering method is to prepare one of major technique of thin-film material, and the raw material of sputter-deposited thin films are targets.Use target
The film consistency of sputtering sedimentation is high, and adhesion is good.Therefore, cadmium stannate film is also generally prepared by sputtering method, and this is first
It first needs that cadmium stannate target is prepared.
Application No. is the Chinese invention patent applications of CN201410559166.7 to propose a kind of cadmium stannate target and its system
Preparation Method is first uniformly mixed using tin oxide and cadmium oxide and sinters Cd into2SnO4After powder, reheating is pressed into target, and this method relates to
And complicated process, and hot pressing centainly need to be with graphite jig be used, graphite has stronger reproducibility, easily reacts with oxide,
Therefore impurity is readily incorporated in preparing powder process, so that the economic value of the target of final molding is had a greatly reduced quality.
Thus, it is necessary to the new preparation method of one kind be designed to solve the above technical problems, the present invention is directed to propose a kind of
The preparation method of cadmium stannate target, does not introduce impurity, can prepare relative density greater than 95%, resistivity≤10 Ω cm tin
Sour cadmium target.
Summary of the invention
It is an object of the invention to propose that one kind does not introduce impurity, prepares relative density and be greater than 95%, resistivity≤10
The preparation method of the cadmium stannate target of Ω cm.
To realize foregoing purpose, the present invention adopts the following technical scheme: a kind of preparation method of cadmium stannate target comprising
Following steps:
S1, raw material mixing: by 5N oxidation cadmium dust and 5N stannic oxide powder, 2 ~ 2.1:1 is mixed to form mixed powder in molar ratio
End, then by the PVA for accounting for mixed-powder mass fraction 1% ~ 3%, account for mixed-powder mass fraction 3% ~ 5% pure water be added mixed powder
End, which is mixed together, is formed uniformly mixture；
S2, ball milling: above-mentioned mixture is put into a ball mill, and ball milling takes out after 4-6 hour, at 70 ~ 100 DEG C dry 1 ~
Obtain drying material within 2 hours；
S3, isostatic cool pressing: drying material is fitted into a stainless steel mould, and stainless steel mould is then put into an isostatic cool pressing furnace
In, it is kept for 1 ~ 3 hour under 300 ~ 400MPa；
S4, sintering: after isostatic cool pressing, blank material is taken out, blank material is put into a sintering furnace, sintering furnace presses the first heating rate
G1 is warming up to 400 ~ 500 DEG C, keeps the temperature the T1 time, then is warming up to 1100 ~ 1250 DEG C with the second heating rate G2, keeps the temperature the T2 time,
After furnace cooling, cadmium stannate target is obtained.
As a further improvement of the present invention, the first heating rate G1 is 1 ~ 5 DEG C/min.
As a further improvement of the present invention, the second heating rate G2 is 3 ~ 6 DEG C/min.
As a further improvement of the present invention, the T1 time is 1 ~ 3 hour.
As a further improvement of the present invention, the T2 time is 1 ~ 3 hour.
The preparation method of cadmium stannate target of the present invention is prepared using the method that isostatic cool pressing and room temperature sintering combine
Cadmium stannate target is not necessarily to graphite crucible, will not introduce impurity, and preparation-obtained cadmium stannate target is relatively denser in 95%, electricity
Resistance rate≤10 Ω cm.
Detailed description of the invention
Fig. 1 is the resistivity measurement schematic diagram of the embodiment of the preparation method of cadmium stannate target of the present invention.
Fig. 2 is the resistivity measurement result of the embodiment of the preparation method of cadmium stannate target of the present invention.
Fig. 3 is the impurity content test result of the embodiment of the preparation method of cadmium stannate target of the present invention.
Specific embodiment
Technical solution is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention proposes a kind of preparation method of cadmium stannate target comprising following steps.
S1, raw material mixing: by 5N oxidation cadmium dust and 5N stannic oxide powder, 2 ~ 2.1:1 is mixed to form mixing in molar ratio
Powder, then the PVA(polyvinyl alcohol that mixed-powder mass fraction 1% ~ 3% will be accounted for), account for the pure of mixed-powder mass fraction 3% ~ 5%
Water addition mixed-powder, which is mixed together, is formed uniformly mixture.
S2, ball milling: above-mentioned mixture is put into a ball mill, and ball milling takes out after 4-6 hour, is dried at 70 ~ 100 DEG C
Obtain drying material within dry 1 ~ 2 hour.
S3, isostatic cool pressing: drying material is fitted into a stainless steel mould, and stainless steel mould is then put into an isostatic cool pressing
In furnace, kept for 1 ~ 3 hour under 300 ~ 400MPa.
S4, sintering: after isostatic cool pressing, blank material is taken out, blank material is put into a sintering furnace, sintering furnace presses the first heating
Rate G1 is warming up to 400 ~ 500 DEG C, keeps the temperature the T1 time, then is warming up to 1100 ~ 1250 DEG C with the second heating rate G2, when keeping the temperature T2
Between, after furnace cooling, obtain cadmium stannate target.
In certain embodiments of the present invention, the first heating rate G1 is 1 ~ 5 DEG C/min.
In certain embodiments of the present invention, the second heating rate G2 is 3 ~ 6 DEG C/min.
In certain embodiments of the present invention, the T1 time is 1 ~ 3 hour.
In certain embodiments of the present invention, the T2 time is 1 ~ 3 hour.
Density measurement, resistivity measurement and impurity content test are carried out respectively to obtained cadmium stannate target.
Density measurement: the density of drainage test target is utilized.
Resistivity measurement: and according to the resistivity of method test material shown in FIG. 1: current source is connected to the two of sample
End, the lead of voltmeter are then pressed known distance and are placed, counted according to the distance between the cross-sectional area of sample and voltmeter lead
Calculate resistivity；Wherein: the resistivity of ρ=as unit of centimetre-ohm；V=voltmeter measurement voltage；I=current source
Electric current；The cross-sectional area (w × t) of the sample of A=as unit of centimetres 2.
Impurity content test uses ICP-MS instrument, and (full name is Inductively coupled plasma mass
Spectrometry refers to inductivity coupled plasma mass spectrometry) it is tested.
The present invention is using the advantage that isostatic cool pressing and room temperature are sintered: in high volume being synchronized and is produced, to mold
It is required that low and do not react with mold, in the prior art, need to use hot pressing, and hot pressing centainly need to be with using graphite mo(u)ld
Tool, graphite have stronger reproducibility, easily react with oxide, and isostatic cool pressing is formed using steel mold, after molding under normal pressure
Sintering, hot stage are not necessarily to mold, will not introduce impurity pollution target.
Embodiment 1.
By 5N oxidation cadmium dust and 5N stannic oxide powder, 2:1 is mixed to form mixed-powder in molar ratio, then will account for mixing
The PVA of powder quality score 1%, account for mixed-powder mass fraction 3% pure water be added mixed-powder be mixed together be formed uniformly it is mixed
Close material.Mixture is put into a ball milling bucket, ball milling takes out after 4 hours, and drying material is dried 2 hours to obtain at 70 DEG C.It will drying
It is fitted into a stainless steel mould after material sampling, then stainless steel mould is put into an isostatic cool pressing furnace, holding 3 is small under 300MPa
When.After isostatic cool pressing, blank material is taken out, blank material is put into a sintering furnace, sintering furnace heats up by the heating rate of 2 DEG C/min
It to 450 DEG C, is kept for 2 hours, then is warming up to 1200 DEG C with the heating rate of 6 DEG C/min, kept for 2 hours.After furnace cooling, obtain
Cadmium stannate target.
Preparation-obtained test density, resistivity and impurity content are tested respectively, test result is shown in Fig. 2,3.
Embodiment 2.
By 5N oxidation cadmium dust and 5N stannic oxide powder, 2.1:1 is mixed to form mixed-powder in molar ratio, then will account for mixed
The PVA of conjunction powder quality score 3%, the pure water addition mixed-powder for accounting for mixed-powder mass fraction 5%, which are mixed together, to be formed uniformly
Mixture.Mixture is put into a ball milling bucket, ball milling takes out after 6 hours, and drying material is dried 1 hour to obtain at 100 DEG C.It will dry
It is fitted into a stainless steel mould after siccative sampling, then stainless steel mould is put into an isostatic cool pressing furnace, keep 1 under 400MPa
Hour.After isostatic cool pressing, blank material is taken out, blank material is put into a sintering furnace, sintering furnace presses the heating rate liter of 1 DEG C/min
Temperature is kept for 2 hours to 400 DEG C, then is warming up to 1100 DEG C with the heating rate of 5 DEG C/min, is kept for 2 hours.After furnace cooling, obtain
To cadmium stannate target.
Preparation-obtained test density, resistivity and impurity content are tested respectively, test result is shown in Fig. 2,3.
Embodiment 3.
By 5N oxidation cadmium dust and 5N stannic oxide powder, 2.05:1 is mixed to form mixed-powder in molar ratio, then will account for mixed
The PVA of conjunction powder quality score 2%, the pure water addition mixed-powder for accounting for mixed-powder mass fraction 4%, which are mixed together, to be formed uniformly
Mixture.Mixture is put into a ball milling bucket, ball milling takes out after 5 hours, and drying material is dried 1.5 hours to obtain at 90 DEG C.It will
It is fitted into a stainless steel mould after drying material sampling, then stainless steel mould is put into an isostatic cool pressing furnace, protected under 350MPa
It holds 2 hours.After isostatic cool pressing, blank material is taken out, blank material is put into a sintering furnace, sintering furnace is fast by the heating of 5 DEG C/min
Rate is warming up to 500 DEG C, is kept for 2 hours, then is warming up to 1250 DEG C with the heating rate of 6 DEG C/min, is kept for 3 hours.Furnace cooling
Afterwards, cadmium stannate target is obtained.
Preparation-obtained test density, resistivity and impurity content are tested respectively, test result is shown in Fig. 2,3.
The preparation method of cadmium stannate target of the present invention is prepared using the method that isostatic cool pressing and room temperature sintering combine
Cadmium stannate target is not necessarily to graphite crucible, will not introduce impurity, and preparation-obtained cadmium stannate target is relatively denser in 95%, electricity
Resistance rate≤10 Ω cm.
Although for illustrative purposes, the preferred embodiment of the present invention is had been disclosed, but the ordinary skill people of this field
Member will realize without departing from the scope and spirit of the invention as disclosed by the appended claims, various to change
Into, increase and replace be possible.
Claims (5)
1. a kind of preparation method of cadmium stannate target, it is characterised in that: it includes the following steps:
S1, raw material mixing: by 5N oxidation cadmium dust and 5N stannic oxide powder, 2 ~ 2.1:1 is mixed to form mixed powder in molar ratio
End, then by the PVA for accounting for mixed-powder mass fraction 1% ~ 3%, account for mixed-powder mass fraction 3% ~ 5% pure water be added mixed powder
End, which is mixed together, is formed uniformly mixture；
S2, ball milling: above-mentioned mixture is put into a ball mill, and ball milling takes out after 4-6 hour, at 70 ~ 100 DEG C dry 1 ~
Obtain drying material within 2 hours；
S3, isostatic cool pressing: drying material is fitted into a stainless steel mould, and stainless steel mould is then put into an isostatic cool pressing furnace
In, it is kept for 1 ~ 3 hour under 300 ~ 400MPa；
S4, sintering: after isostatic cool pressing, blank material is taken out, blank material is put into a sintering furnace, sintering furnace presses the first heating rate
G1 is warming up to 400 ~ 500 DEG C, keeps the temperature the T1 time, then is warming up to 1100 ~ 1250 DEG C with the second heating rate G2, keeps the temperature the T2 time,
After furnace cooling, cadmium stannate target is obtained.
2. the preparation method of the cadmium stannate target according to claim 1, it is characterised in that: the first heating rate G1
For 1 ~ 5 DEG C/min.
3. the preparation method of the cadmium stannate target according to claim 1, it is characterised in that: the second heating rate G2
For 3 ~ 6 DEG C/min.
4. the preparation method of the cadmium stannate target according to claim 1, it is characterised in that: the T1 time is 1 ~ 3 small
When.
5. the preparation method of the cadmium stannate target according to claim 1, it is characterised in that: the T2 time is 1 ~ 3 small
When.
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| CN201811220400.8A CN109437884A (en) | 2018-10-19 | 2018-10-19 | The preparation method of cadmium stannate target |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113213914A (en) * | 2021-04-19 | 2021-08-06 | 先导薄膜材料（广东）有限公司 | Preparation method of cadmium stannate target |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0500031A1 (en) * | 1991-02-19 | 1992-08-26 | Mitsubishi Materials Corporation | Method of manufacturing a sputtering target |
| CN102191466A (en) * | 2010-03-18 | 2011-09-21 | 中国科学院福建物质结构研究所 | Gallium doped zinc oxide target and preparation method of transparent conductive film thereof |
| CN202087824U (en) * | 2011-04-27 | 2011-12-28 | 锦州市锦利电器有限公司 | Stainless steel mold special for sintering |
| CN105585317A (en) * | 2014-10-20 | 2016-05-18 | 北京有色金属研究总院 | Cadmium stannate target material and preparation method thereof |
-
2018
- 2018-10-19 CN CN201811220400.8A patent/CN109437884A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0500031A1 (en) * | 1991-02-19 | 1992-08-26 | Mitsubishi Materials Corporation | Method of manufacturing a sputtering target |
| CN102191466A (en) * | 2010-03-18 | 2011-09-21 | 中国科学院福建物质结构研究所 | Gallium doped zinc oxide target and preparation method of transparent conductive film thereof |
| CN202087824U (en) * | 2011-04-27 | 2011-12-28 | 锦州市锦利电器有限公司 | Stainless steel mold special for sintering |
| CN105585317A (en) * | 2014-10-20 | 2016-05-18 | 北京有色金属研究总院 | Cadmium stannate target material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113213914A (en) * | 2021-04-19 | 2021-08-06 | 先导薄膜材料（广东）有限公司 | Preparation method of cadmium stannate target |
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Application publication date: 20190308 |