Alumina target material and preparation method thereof

Abstract

The invention discloses a preparation method of an aluminum oxide target material, which comprises the following steps: carrying out ball-milling treatment on aluminum oxide and ball-milling liquid according to a weight ratio of 5: 2, after ball-milling is finished, carrying out compression molding in a mold, and then carrying out sintering improvement to obtain the aluminum oxide target material. According to the aluminum oxide target material, aluminum oxide is subjected to ball-milling liquid treatment, then enters a mold and is sintered and improved to obtain the aluminum oxide target material, the compactness and transparency of a product are harmoniously improved, and the acid corrosion resistance stability effect of the product is remarkable.

Description

Technical Field

[0001] The present invention relates to the technical field of target materials, and in particular to an aluminum oxide target material and a preparation method thereof. Background Art

[0002] As an important coating material, target materials are widely used in integrated circuits, flat panel displays, optical devices and other fields. The preparation methods of target materials include smelting method and powder metallurgy method. Among them, powder metallurgy method can directly make porous, semi-dense or fully dense products. The obtained products have unique chemical composition, mechanical and physical properties. Therefore, powder metallurgy technology has become the main preparation method for preparing target materials.

[0003] The existing alumina target material has poor density and poor transparency. The density and transparency of the product are difficult to coordinate and improve. In addition, the product has poor acid corrosion resistance, which limits the use efficiency of the product. Summary of the invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide an aluminum oxide target material and a preparation method thereof to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solution: The present invention provides a method for preparing an aluminum oxide target, comprising the following steps: Alumina and ball milling liquid are ball milled in a weight ratio of 5:2, and after ball milling, the alumina target is pressed into a mold, and then sintered to obtain an alumina target. The ball milling liquid includes silane coupling agent KH550, modified chitosan agent and sodium alginate liquid; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate liquid is 2:5:7.

[0006] Preferably, the ball milling speed of the ball milling treatment is 1000-1500 r / min, and the ball milling is for 2 hours.

[0007] Preferably, the pressing pressure is 35-40 MPa, and the pressing time is 2 h.

[0008] Preferably, the sintering temperature of the improved sintering is 1150-1200° C., and the sintering time is 1 hour.

[0009] Preferably, the preparation method of the modified chitosan agent is: Immerse 4-7 parts of hydroxyapatite in 5-8 parts of yttrium nitrate solution, then add 1-3 parts of sodium carboxymethyl cellulose and 1-2 parts of stearic acid, mix and ball-mill at a speed of 1500 r / min for 2 hours, filter and dry to obtain a hydroxyapatite agent; Chitosan, water and citric acid are uniformly stirred in a weight ratio of 3:7:1, and then 4-7% of the total amount of chitosan hydroxyapatite is added thereto, and the mixture is stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

[0010] Preferably, the mass fraction of the yttrium nitrate solution is 2-5%.

[0011] Preferably, the preparation method of the sodium alginate solution is: Preheat the nano-silicon dioxide at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 2-5 times the total amount of the nano-silicon dioxide, and then add a sodium alginate solution that is 10-15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0012] Preferably, the mass fraction of the dopamine hydrochloride solution is 2-5%; the mass fraction of the sodium alginate solution is 4-7%.

[0013] The invention also provides an aluminum oxide target material prepared by a method for preparing the aluminum oxide target material.

[0014] Compared with the prior art, the present invention has the following beneficial effects: The aluminum oxide target material of the invention is prepared by treating aluminum oxide with a ball milling liquid, then putting it into a mold, and sintering and improving it to obtain the aluminum oxide target material. The compactness and transparency of the product are improved in a coordinated manner, and the acid corrosion resistance and stability of the product are significantly improved. The ball milling liquid is prepared by blending a silane coupling agent KH550, a modified chitosan agent and a sodium alginate liquid. At the same time, the hydroxyapatite in the modified chitosan agent is treated with a specific process, and is matched with chitosan, water and citric acid raw materials in a blending system, and then coordinated with a sodium alginate liquid prepared by blending nano silicon dioxide, a dopamine hydrochloride solution and sodium alginate. Through the coordinated improvement between the raw materials, the product performance is further improved. DETAILED DESCRIPTION

[0015] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0016] A method for preparing an aluminum oxide target material in this embodiment includes the following steps: Alumina and ball milling liquid are ball milled in a weight ratio of 5:2, and after ball milling, the alumina target is pressed into a mold, and then sintered to obtain an alumina target. The ball milling liquid includes silane coupling agent KH550, modified chitosan agent and sodium alginate liquid; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate liquid is 2:5:7.

[0017] The ball milling speed of the ball milling treatment in this embodiment is 1000-1500 r / min, and the ball milling is 2 h.

[0018] The pressing pressure of this embodiment is 35-40 MPa, and the pressing time is 2 hours.

[0019] The improved sintering temperature of this embodiment is 1150-1200° C., and the sintering time is 1 hour.

[0020] The preparation method of the modified chitosan agent of this embodiment is: Immerse 4-7 parts of hydroxyapatite in 5-8 parts of yttrium nitrate solution, then add 1-3 parts of sodium carboxymethyl cellulose and 1-2 parts of stearic acid, mix and ball-mill at a speed of 1500 r / min for 2 hours, filter and dry to obtain a hydroxyapatite agent; Chitosan, water and citric acid are uniformly stirred in a weight ratio of 3:7:1, and then 4-7% of the total amount of chitosan hydroxyapatite is added thereto, and the mixture is stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

[0021] The mass fraction of the yttrium nitrate solution in this embodiment is 2-5%.

[0022] The preparation method of the sodium alginate solution of this embodiment is: Preheat the nano-silicon dioxide at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 2-5 times the total amount of the nano-silicon dioxide, and then add a sodium alginate solution that is 10-15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0023] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2-5%; the mass fraction of the sodium alginate solution is 4-7%.

[0024] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0025] Example 1. A method for preparing an aluminum oxide target material in this embodiment includes the following steps: Alumina and ball milling liquid are ball milled in a weight ratio of 5:2, and after ball milling, the alumina target is pressed into a mold, and then sintered to obtain an alumina target. The ball milling liquid includes silane coupling agent KH550, modified chitosan agent and sodium alginate liquid; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate liquid is 2:5:7.

[0026] The ball milling speed of the ball milling treatment in this embodiment is 1000 r / min, and the ball milling is 2 h.

[0027] The pressing pressure of this embodiment is 35 MPa and the pressing time is 2 h.

[0028] The improved sintering temperature of this embodiment is 1150° C. and the sintering time is 1 hour.

[0029] The preparation method of the modified chitosan agent of this embodiment is: Immerse 4 parts of hydroxyapatite in 5 parts of yttrium nitrate solution, then add 1 part of sodium carboxymethyl cellulose and 1 part of stearic acid and mix them for ball milling at a speed of 1500 r / min for 2 hours. After the ball milling is completed, filter and dry to obtain a hydroxyapatite agent; Chitosan, water and citric acid were uniformly stirred in a weight ratio of 3:7:1, and then 4% of the total amount of chitosan hydroxyapatite was added thereto, and the mixture was stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

[0030] The mass fraction of the yttrium nitrate solution in this embodiment is 2%.

[0031] The preparation method of the sodium alginate solution of this embodiment is: Preheat the nano-silicon dioxide at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is twice the total amount of the nano-silicon dioxide, and then add a sodium alginate solution that is 10% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0032] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2%; the mass fraction of the sodium alginate solution is 4%.

[0033] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0034] Example 2. A method for preparing an aluminum oxide target material in this embodiment includes the following steps: Alumina and ball milling liquid are ball milled in a weight ratio of 5:2, and after ball milling, the alumina target is pressed into a mold, and then sintered to obtain an alumina target. The ball milling liquid includes silane coupling agent KH550, modified chitosan agent and sodium alginate liquid; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate liquid is 2:5:7.

[0035] The ball milling speed of the ball milling treatment in this embodiment is 1500 r / min, and the ball milling is 2 h.

[0036] The pressing pressure of this embodiment is 40 MPa and the pressing time is 2 h.

[0037] The improved sintering temperature of this embodiment is 1200° C. and the sintering time is 1 hour.

[0038] The preparation method of the modified chitosan agent of this embodiment is: 7 parts of hydroxyapatite are immersed in 8 parts of yttrium nitrate solution, and then 3 parts of sodium carboxymethyl cellulose and 2 parts of stearic acid are added and mixed and ball-milled at a ball-milling speed of 1500 r / min for 2 hours. After the ball-milling is completed, the mixture is filtered and dried to obtain a hydroxyapatite agent; Chitosan, water and citric acid were uniformly stirred in a weight ratio of 3:7:1, and then 7% of the total amount of chitosan hydroxyapatite was added thereto, and the mixture was stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

[0039] The mass fraction of the yttrium nitrate solution in this embodiment is 5%.

[0040] The preparation method of the sodium alginate solution of this embodiment is: Preheat the nano-silicon dioxide at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 5 times the total amount of the nano-silicon dioxide, and then add a sodium alginate solution that is 15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0041] The mass fraction of the dopamine hydrochloride solution in this embodiment is 5%; the mass fraction of the sodium alginate solution is 7%.

[0042] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0043] Example 3. A method for preparing an aluminum oxide target material in this embodiment includes the following steps: Alumina and ball milling liquid are ball milled in a weight ratio of 5:2, and after ball milling, the alumina target is pressed into a mold, and then sintered to obtain an alumina target. The ball milling liquid includes silane coupling agent KH550, modified chitosan agent and sodium alginate liquid; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate liquid is 2:5:7.

[0044] The ball milling speed of the ball milling treatment in this embodiment is 1250 r / min, and the ball milling is performed for 2 h.

[0045] The pressing pressure of this embodiment is 37.5 MPa and the pressing time is 2 h.

[0046] The improved sintering temperature of this embodiment is 1175° C. and the sintering time is 1 hour.

[0047] The preparation method of the modified chitosan agent of this embodiment is: 5.5 parts of hydroxyapatite are immersed in 6.5 parts of yttrium nitrate solution, and then 2 parts of sodium carboxymethyl cellulose and 1.5 parts of stearic acid are added and mixed and ball-milled at a ball-milling speed of 1500 r / min for 2 hours. After the ball-milling is completed, the mixture is filtered and dried to obtain a hydroxyapatite agent; Chitosan, water and citric acid were uniformly stirred in a weight ratio of 3:7:1, and then hydroxyapatite agent of 5% of the total amount of chitosan was added thereto, and the mixture was stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

[0048] The mass fraction of the yttrium nitrate solution in this embodiment is 3.5%.

[0049] The preparation method of the sodium alginate solution of this embodiment is: Preheat the nano-silicon dioxide at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 3.5 times the total amount of the nano-silicon dioxide, and then add a sodium alginate solution that is 12.5% ​​of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0050] The mass fraction of the dopamine hydrochloride solution in this embodiment is 3.5%; the mass fraction of the sodium alginate solution is 5.5%.

[0051] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0052] Comparative Example 1. The difference from Example 3 is that no modified chitosan agent is added.

[0053] Comparative Example 2. The difference from Example 3 is that no hydroxyapatite agent is added to the modified chitosan agent.

[0054] Comparative Example 3. The difference from Example 3 is that the hydroxyapatite agent is replaced by hydroxyapatite raw material.

[0055] Comparative Example 4. The difference from Example 3 is that the sodium alginate solution is replaced by water.

[0056] Comparative Example 5. The difference from Example 3 is that the method for preparing the sodium alginate solution is different: no preheated nano-silicon dioxide is added.

[0057] The product performance tests of Examples 1-3 and Comparative Examples 1-5 are as follows:

[0058] It can be seen from Comparative Examples 1-5 and Examples 1-3 that the compactness and transparency of the products of the present invention are improved in a coordinated manner, and the acid mist resistance stability of the products is significant; the products do not add modified chitosan agent, and the sodium alginate solution is replaced by water, and the performance of the products has a significant downward trend. At the same time, no hydroxyapatite agent is added to the modified chitosan agent, the hydroxyapatite agent is replaced by hydroxyapatite raw material, and the sodium alginate solution is prepared by different methods, and the product performance has a downward trend. Although other modification methods can improve product performance, the improvement effect is not as significant as the modification method of the present invention.

[0059] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0060] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A method for preparing an aluminum oxide target, characterized in that: The following steps are involved: Alumina and ball milling liquid are ball milled in a weight ratio of 5:2, and after ball milling, the alumina target is pressed into a mold, and then sintered to obtain an alumina target. The ball milling liquid includes silane coupling agent KH550, modified chitosan agent and sodium alginate liquid; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate liquid is 2:5:

7.

2. The method for preparing an aluminum oxide target according to claim 1, characterized in that: The ball milling process is performed at a ball milling speed of 1000-1500 r / min for 2 hours.

3. The method for preparing an aluminum oxide target according to claim 1, characterized in that: The pressing pressure is 35-40 MPa, and the pressing time is 2 h.

4. The method for preparing an aluminum oxide target according to claim 1, characterized in that: The improved sintering temperature is 1150-1200° C. and the sintering time is 1 hour.

5. The method for preparing an aluminum oxide target according to claim 1, characterized in that: The preparation method of the modified chitosan agent is: Immerse 4-7 parts of hydroxyapatite in 5-8 parts of yttrium nitrate solution, then add 1-3 parts of sodium carboxymethyl cellulose and 1-2 parts of stearic acid, mix and ball-mill at a speed of 1500 r / min for 2 hours, filter and dry to obtain a hydroxyapatite agent; Chitosan, water and citric acid are uniformly stirred in a weight ratio of 3:7:1, and then 4-7% of the total amount of chitosan hydroxyapatite is added thereto, and the mixture is stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

6. The method for preparing an aluminum oxide target according to claim 5, characterized in that: The mass fraction of the yttrium nitrate solution is 2-5%.

7. The method for preparing an aluminum oxide target according to claim 1, characterized in that: The preparation method of the sodium alginate solution is: Preheat the nano-silicon dioxide at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 2-5 times the total amount of the nano-silicon dioxide, and then add a sodium alginate solution that is 10-15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

8. The method for preparing an aluminum oxide target according to claim 7, characterized in that: The mass fraction of the dopamine hydrochloride solution is 2-5%; the mass fraction of the sodium alginate solution is 4-7%.

9. An alumina target material prepared by the method for preparing an alumina target material according to any one of claims 1 to 8.

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